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The Quanta FEG User Operation Manual

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1. Software Control xT microscope Control Software Digital Zaam 10 The Digital Zoom Module The procedure takes place in the computer memory only and helps to navigate across the enlarged view Click the magnifying glass icon to enlarge the view in the active quad Drag and move the green bordered area with the left mouse button inside the digital zoom image to change an observed area in the active quad When the digital zoom ratio is applied the icon appears in the appropriate quad 11 The Enhanced Image Module consists of four tabbed sections offering various digital image enhancements In contrary to Detector module Contrast and Brightness functions these enhancements are applied only to the active quad independently The digital processing can be applied to any live paused or loaded image including an optical one see Chapter 5 FIGURE 4 12 THE ENHANCED IMAGE MODULE Enhanced Image Enhanced Image Enhanced Image LUT Mix 3 Mix 4 Color LUT Mix 3 Mix 4 Color LUT Mix 3 Mix 4 Color Multiple 2 v Pseudo Colors 2 O Contrast 1 2 D Bright 0 00 Source 1 33 Source 2 33 a m Aid 7 Bj il mo Uu Gamma 8 Ine D Ine a gm m 5 Source 3 3396 Select Hi um Bue Wh Iw Enable Save 12 The Alignments Module Alignments contains alignments which enable to optimize the system performance see Chapter 6 nos eo lots The Alignments list box contains list of Alignment proce
2. mi spat det WO mad pressure Active electron quad 15 00 kK 25 ETO 170mm es 4 bbe 3 Pa Cuanta FEG q 15 00 amp 25 ETO 17 0 mm 700x 4 66e 3 Pa Guanta FEG Active optical quad 1 u x 367 urm 24148PM IR y 2 mm Note The Databar information is always related to the displayed image If the image is paused or loaded from a file they could differ from the actual system conditions E Beam Control e Navigation Processing Alignments a BS e X m v P o Vacuum Pump ent Made C High sacuum e Low Vacuum Water ESEM Water Chamber Pressure ely wd xxx Software Control xT microscope Control Software PAGES ALT P AND MODULES The software controls on the right side of the screen are organized into Pages which are divided into Modules holding specific functions The required page can be selected either from the Pages menu by pressing the corresponding icon button or with the use of short cuts see table 4 5 TABLE 4 1 PAGES AND MODULES LIST Pages Modules Tabs Beam Control 1 Vacuum Mode 2 Column 3 Detectors 4 Magnification 5 Beam 6 Tuning 7 Status Navigation 1 Vacuum Mode 2 Column 3 Detectors 8 Stage Map Coordinates Tilt Navigation 7 Status Processing 9 Measurement Annotation 10 Digital Zoom 11 Enhanced Image LUT Mix 3 Mix 4 Color 3 Detectors 7 Status 12 Alignments Instructions Individual
3. System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 Temperature Stage Control Cooling Temperature Humidity Actual Target Ramp ub Bit C min 3410 Foo hs Temperature Profile lt de Heating Temperature Advanced Actual Target Ramp ae C Omin a wo so Temperature Profile Soak time Start Temp Ramp Soak time Temperature Stage Control SOFIWARE CONTROL Temperature Stage Control Module n The cooling heating stage is software controlled using the xT microscope Control software Temperature Page added when any temperature stage is installed Temperature Stage Control module The Cooling Heating button activates the Cooling Heating stage software control When the stage is active inactive the corresponding button is Yellow Grey The Temperature tab The Actual read out box displays the actual temperature measured by the temperature stage hardware the same value is used in the databar The Target edit box sets the target temperature It is active when either stage is enabled and no profile is running The Ramp edit box sets the speed of the temperature change It is active when either stage is enabled and no profile is running Clicking the Go To button starts to proceed to the target temperature It is active when no profile
4. Dialogue 2 0 0 cece eee ee eee 4 27 FEI User Management Software LLs s 4 35 Control possibilities 0 eee nee 4 35 FEI Account Administrators 0 000 llle 4 35 PCCOUNV EOOGING a tro eg aac ch Gai i oh Solar disk iode MG Ile Men 4 37 Entering Commands in Summary 4 38 Using the Mouse uu ud Eu m eir cte que ees etos Sees 4 38 Using the KeybOard isis setae aide et di 4 39 Chapter 5 Operations Specimen Preparation and Handling 5 2 Needed temuco a ewe dte ene ee te ba eee eS 5 2 Natural specimen 1 eee eens 5 2 Coated SpeciIMe i sen do ce wie es hee ed v den alee oa eee 5 2 Mounting the Specimen to the Holder 5 2 Inserting Exchanging a Specimen and or a Detector 5 3 Obtaining an Image 5 2 4 a 5 4 Operation Pre Check curd pen tente bition E erg aate dris atit 5 4 Selecting Vacuum Mode 0 00 eee 5 5 DOL SIZ Os resid cette ines stad aida hee d dit ee la le Se hee 5 6 Obtaining an Image on Screen n nannan aaaea 5 7 Optimising an Image 5 7 Principles of SEM imaging 0 eee eens 5 7 Mirsteinlezule PDC PCT 5 7 Scan Speed and Filtering llle 5 8 Contrast and Bugniness sisas pb dc Re aed Aria 5 9 FOCUSING mM TP CT 5 10 Correcting Astigmatism 0 0 0 5 10 Pressure and Working Distance WD o o oooo o 5 11 Digital Image Enhance
5. During the purging procedure the chamber pressure is not ready for SEM operation the vacuum status is Pumping Therefore pressing the Purge button automatically switches off the accelerating voltage The Purge Settings is not remembered separately for each user If it is of any importance please check these Preferences before starting the ESEM Low Vacuum operation After xT microscope Server restart it is set to Automatic A gt Software Control xT microscope Control Software xTm Preferences Some changes required restart of xT microscope Control application To apply these changes please restart xT microscope Contrar Ul Appearance Image and Graphics Microscope Operation Mame Icon style Toolbar listhox style Toolbar spinner style Image dimension controls Frame active quad Enable zooming on mouse click and drag switch sample tracking on mouse wheel click spot size step Enhanced Contrast slider beside Contrast The General Tab contains variety of user settings of both Ul behaviour and microscope operation which are of less importance and or does not logically belong to other Preferences section FIGURE 4 18 GENERAL PREFERENCES xIm Preferences Databar Units Presets Scanning ESEM General Movie Sensitivity Category Quanta Reduced Left Right Magnificatio Ma Icon style Toolbar listhox style Toolbar spinner style Image dimension co
6. HH Brightness 53 8 ml m B arcs E 0 0 5 Emitter Startup Alignments 5 Emitter Startup This procedure enables electron source switching On Off In cases of emergency shut down or the microscope mains switch off the lon Getter Pumps IGP keep pumping the FEG source area backed up by the Battery Supply Unit BSU However the main IGP power supply is switched off at this time so it is necessary to turn it on when the mains power is recovered The BSU battery provides about nine hours of uninterrupted power when fully charged and having full capacity If the microscope was without the power longer than nine hours it is usually not possible to start the IGP s by this alignment procedure It is necessary to call the service to run the bake out procedure first Alignments 5 Emitter Startup Alignments Instructions This procedure starts or stops the emitter Mo step 1 Check the Gun vacuum page if it is IGP ON click the Next button If it is OFF click the IGP On button to automatically start the ion pump This procedure takes a few minutes If the ion pump start is not successful call service 2 Click the Emitter On Off button to start stop the emission of electrons Note If the Emitter On button is disabled and the IGP s are running restart the xT Microscope Server and try again Alignments Alignments 5 Emitter Startup 5 Emitter Startup Instructions Instr
7. Note Clicking above the 2D box with the right mouse button opens a menu with following particular features The Zero sets the Stigmator value to zero switches off stigmator The Clear Memory clears the record A few last used conditions HV WD are recorded automatically When changing the conditions the value is set either to the last one used if recorded or to an estimated one based on the available record The Reset sets the Beam Shift value to zero and moves the stage to compensate the resulting image shift same as the Stage menu Beam Shift Reset function 6 The Tuning Module enables a fine electron source alignment providing the aperture is mechanically well aligned and a coarse pre alignment via the Gun alignment procedure is done Note The alignment stored by the Gun Alignment procedure see Chapter 6 is not overridden by this module control The Source Tilt 2D Control corrects an image illumination drop by changing an effective angle of the beam coming from the gun area into the electron column In the Crossover mode activated with the button the onscreen image shows the electron source tip instead of the sample surface The Lens Alignment 2D Control minimizes the objective image shift during focusing The 2D control indicates an actual beam position setting relative to the final lens aperture The Lens Align button starts automatic objective current oscillation periodically under and over
8. The Selected Area Zooming In Out is a quick way of zooming in out on an area of interest Click with the left mouse button into the image hold it and drag to make a dotted box over the area of interest the cursor changes to a magnifying glass with a sign Release the button and the selected area increases to fill the whole quad window with respect to the sides ratio Using the left mouse button Shift key consecutively reverses the above described technique the cursor changes to a magnifying glass with a sign The escape button cancels the operation at any time The Magnification module see Chapter 4 The Digital Zoom module see Chapter 4 SCAN SPEED AND FILTERING To make a good image it is necessary to find a balance between scan speed charge sample damage and signal to noise ratio A noisy image can be improved by decreasing the scan speed If charge or sample damage are the limiting factors it is better to use a faster scan speed in combination with an Average or Integrate filter see Chapter 4 E Operations Optimising an Image CONTRAST AND BRIGHTNESS tae The contrast and brightness can be set manually either by adjusting Contrast 38 4 the Detectors module controls see Chapter 4 or using the MUI E B option Brightness 500 TABLE 5 7 CONTRAST 8 BRIGHTNESS SETTING E El p Step Action 1 Select a medium speed scan in an active quad Increase the contrast so that the signal leve
9. be removed that additional user s data is removed without warnings FEI User Management Delete userdata A Are you sure to delete userdata of accountadmin w Set password click to make a password for the user The user FEI User Management Set password must first be highlighted in the tree An FEI Account Administrator can change the password for any user from a lower level account X User name supervisor FEI Supervisor Users New password Confirm password FEI Uzer Management Set user group Set user group click to set the group for the user The user must first be highlighted in the tree When confirmed the user is moved to selected group When moving a user from the FEI Microscope Users group to the FEI Non active Users group his user data will be removed A warning is displayed in this case Uses nera aiupernmie FE Superma Users Sglqi up i ERIT TAS ee ee FEI User Management ccount properties User nera superis FEl Superga Users augent Full name rai d epar Same dor Desenphon Liparmust change perswoed al mod logan Liber cant Change passend Pescword rerenr opns TO Arenunt ik dagike Copy Ctrl Z Remove Legend About FEI User Management Legend Members of this group cannot log on Group can be accessed Group cannot be accessed Member of group which cannot log on Standard user Logged on use
10. greyscale image file The TIF 24 file colour image type The JPG file is a compressed file format employing a lossy compression algorithm resulting in the small file size with a little loss of information depending on the particular image appearance and the compression level factory preset to 80 The 8 24 bit depth is automatically selected when saving the greyscale colour image file he BMP file the 8 24 bit depth is automatically selected when saving the greyscale colour image file Operations Capturing and Handling a Single Image SAVING OPENING PRINTING Sl ee The following universal file handling functions could be used e Save Ctrl S stores the image to the predetermined location Open E ries with the last used filename including an incremental number Save AS Save As opens a dialogue for saving images this provides an opportunity to change the file name its location and the possibility Record Movie to save also Databar and overlaid graphics Both functions can be Import d linked to the Snapshot Photo function see the Preferences Export Scanning tab Print Ctrl P TABLE 5 12 IMAGE CAPTURING PROCEDURE Log Off Factory Step Action Exit Select the area of interest and set the Magnification the Scan condition the image pixel Resolution and the Databar informations that are required in the saved image Use the Snapshot F4 Photo F2 Pause F6 func
11. 600 Both holders have the same threaded shaft which screws into the stage rotation head center The specimen should not be thicker than 2 mm or it is impossible to bring it to the eucentric position FIGURE 7 4 QUANTA FEG 400 600 STANDARD SAMPLE HOLDERS Stages Stages Types and Accessories Eucentric position EUCENTRIC POSITION This should be adjusted after loading any new sample other than wafer or for the greatest accuracy as the sample loading procedure clears all position informations At the eucentric position one can use various system components such as the EDX in a safe and optimal way FIGURE 7 5 EUCENTRIC POSITION PRINCIPLE Beam Eucentric position Point of interest Point of interest Tilt 1 The point of interest is focused below the Eucentric 2 Tilting the stage moves the point of interest out of the point see 2 beam Eucentric position Feature is at 3 and Point of interest eucentric position Pa D di w a Atm Z adjustment 1 The point of interest is focused at the Eucentric point 3 Tilting the stage does not move the point of interest out see 4 of the beam At the eucentric position the stage tilt and the electron beam axes intersect When the stage is tilted or rotated in any direction this point remains focused and almost does not shift TABLE 7 1 FINDING EUCENTRIC POSITION PROCEDURE Step Acti
12. Click the text with the left mouse button or press the enter key to confirm it and the text appears onscreen b Operations Measurement and Annotation Functions Shape Editing Once a Measurement or Annotation symbol has been drawn it can be modified Selected graphic is denoted by the addition of resizing handles to the graphic outline use pointer cursor Size and position the graphic correctly over the area of interest A number of other choices are available in the Property editor for each graphics drawn e Moving graphic place the cursor inside the boundary of the graphic and hold the left mouse button while dragging it use move cursor e Resizing graphic hold the left mouse button and drag the resizing handle until the desired size is reached use horizontal vertical or diagonal resizing cursor Holding CTRL key while dragging forces dimensions to be changed proportionally Precise dimensions could be also entered in the Property editor Selecting all Items in an active quad press Ctrl A Delete selected Item s click the Trash can icon or press the Delete key Operations Measurement and Annotation Functions 6 ALIGNMENTS List of alignments accessible for a supervisor e Final Lens Aperture Strip Alignment e 1 Gun Alignment 2 Stigmator Alignment e 3 Stage Rotation Center e 5 Emitter Startup Only alignments No 2 and 3 are enabled for a User Recommendation Total alignment of t
13. Contrast 3 55 El El Brightness 30 00 E Nm Alignments 1 Gun Alignment Alignments I Gun Alignment Alignments I Gun Alignment m Alignments Gun Alignment Instructions Adjust the Gun Tilt 2D control a for a maximum illumination Adjust the Contrast and Brightness when necessary Turn the Modulator on Adjust the Gun Shift 20 control to place the image rotation center under the screen center cross Turn the Modulator off Bring the feature back under the center cross with the Image Shift 20 control step 3 ofS spot 3 8 6 spots remain setting is copied to Spot 2 5 sun Tilt Gun Shift Auto BENE Crossover Modulator Image Shit Instructions Tick the Finish procedure check box to move to the final step Click the Save button to store the settings step 4 of 5 Finish procedure Save Instructions Click the Finish button to save new settings and to quit step 5 ofS Contrast 37 55 E n m Brightness 30 00 E s Cancel Cancel Alignments 2 Stigmator Alignment 2 Stigmator Alignment Particular Control Elements The Modulator button starts automatic stigmator oscillation to facilitate the process The Clear Memory button resets the stigmator settings Alignments Alignments 2 Stigmator Alignment 2 Stigmator Alignment Previous Next Previous Alignments Instruction
14. ma M 7601160 M 826x1169in OH mm Viewed Length L Scanned Length 1 SAMPLE QUANTA FEG ox 20 0kv 35 512x442 912x442 104004 040x160 4096x5556 Software Control xT microscope Control Software Keyboard Shortcuts The shortcuts list in tables is displayed in the same way as the on line documentation see above and with the same behaviour About xTUI displays a window with a microscope picture containing information about the product version The window automatically disappears after the first mouse click THE TOOL BAR displayed below the Menu bar is made up of functional icons linked to the most frequently used system controls It also contains group of icons for quick switching between UI Pages The tool bar can be a bit different in content or style see the Preferences General tab FIGURE 4 9 THE TOOL BAR WA RO Vee mal as 22 39 OI we 66 ARMAS Rest the cursor above the icon for two seconds without clicking it to see its explanatory tool tip Whenever you select a function the corresponding icon is highlighted to indicate that the function is active except of auto functions which display a progress dialogue Note If any icon represents a menu function refer to the corresponding menu for its description Magnification High Voltage Spot List Boxes Click the list box to open a selection of the
15. Ctrl F11 e activates the automatic procedure to correct the astigmatism see Chapter 5 Set Default Parameters Ctrl D loads default settings for the current Vacuum Mode The function switches UI to quad Image mode and selects the default detector for quad 1 and the CCD camera for quad 4 The microscope and image parameters are selected so that there is a big chance to get an usable image immediately Display Saturation Shift F11 displays signal clipping in the active quad by means of replacing the full black white with dark blue yellow colour The function can be used both for live and paused electron images but cannot be applied to the optical quad image xTm Autofunction Information E The Auto Contrast Brightness procedure is running Massima Help X4 Center Cross Shift F5 Alignment Rectangle Shift F6 CCD 10 mm Marker Crosshair Cursor Redo digital zoom 2x Single Quad Image Mode F5 E oo FJ e g Software Control xT microscope Control Software The saturation display is selected independently for each quad A tick next to the menu item indicates whether the function is active for the active quad Lab Notes opens the Windows Notepad application above quad 4 for the user to make immediate notes and remarks The Lab Notes can be used to open edit and save any text file without the necessity to hide the xT Ul FEI Movie Creator provides a dialogue above quad
16. Vacuum Modes 5 524 mi ius stati ieee ie 3 4 High Vacuum HiVac Mode 0 00 eee 3 4 Low Vacuum LoVac and ESEM Modes 0 00 00 3 4 Quanta FEG System States 0 cece ees 3 7 FONT O ari mu Biot ata ceases Sic ride ta ama sie tpe aa agitate Boe 3 9 Chapter 4 Software Control Other Software and Hardware 00 cee ee ees 4 1 Software Interface Elements 4 2 CONS eme ds rr teh ee hee et ub do d 4 2 A Cr ELUCET 4 2 Pull down Menus lel 4 2 COMMING BIOS isso Lv epa aca oem ee NECI sa fe dee d 4 3 L DBO OG REOR E E ETT ATE ETT LT T TuS TO I T 4 3 PIODOFTV ECHOES 3 d egeo circa A Qu Robo ai S 4 3 EJIDO iat hee hr a ine aid acp ud uud d tetra RO Rr Dope 4 3 Radio Buttons Check BoxeS 0 ccc eee 4 3 AUS Sunat du Scenes t d x bd aid cato ms pd ie Eu RA 4 4 2D GA A ee ce ee am em ee 4 5 MOUSE Roh ata Ok 4 5 BS A a a e a e E 4 5 Aaa ath es o loa a eo ese anes A 4 5 Progress Dal Su iei suce e ad dnce ao ore taion Gane ar ent 4 5 xT microscope Server Software lelle 4 6 xT microscope Control Software L s 4 7 INe TUS BS uidit odi dtu tend tolonddt ia dicta WA uh oua 4 8 The Men Barca atado o 4 8 The TOOL Bas cu educ Se aa et be ub a e ORO b RR 4 19 Mage VVIDIOOWS sis aia id ORC MC de dens d uc o tua a 4 20 Pages Alt P and Modules 0 0 00 cece ene eee 4 21 Preferences
17. high current contacts of a Vacuum Evaporator unit Use a pressure of 1 3x10 Pa 1x10 Torr and heat until white hot to flash decontaminate Do not allow the Vacuum Evaporator to contact the atmosphere until the foil boat is cool When the aperture has cooled down place it on the foil vacate and reheat the foil to red heat on the aperture for 4 20 seconds Take care that the aperture does not melt or become stuck to the foil Again do not allow the Vacuum Evaporator to contact the atmosphere until the foil boat and aperture is cool Caution Do not attempt to clean apertures just by washing in solvent as this can have an adverse affect just by shifting contamination back onto the aperture p Maintenance and Troubleshooting The Standard Insert Polishing scratches the soft material and makes the aperture unusable for high resolution All apertures must be cleaned and must not have scratches at the center hole The top aperture should not have any scratches or defects PLATINUM APERTURES INSTALLING 1 Place the aperture holder with its open slotted end on the aperture positioning tool pin Set the nut height so that the top of the spike is below the holder top to leave enough space to put apertures in FIGURE 8 4 INSTALLING APERTURES TO THE INSERT TWEEZERS A H Fu C CLIP INJECTOR INJECTOR MOTE Insert Platinum apertures with sharp edge facing upwards i e towards the electron source APERTURE HOLD
18. if the air soeed near the column is higher than 5 m min it may cause an image drift due to the temperature fluctuation Compressed air interlock failure If the compressed air is not supplied or its pressure is too low the Application Status window with the respective message pops up see Chapter 4 Check the compressed air pressure at the microscope input either on compressor or at the local air distribution The input pressure must be within the range 5 5 8 0 bar 550 800 kPa Note The compressed air is essential for the system which cannot work without it Emission lost after power failure e Run the 5 Emitter Startup procedure to start the emission see Chapter 6 e Run the 5 Emitter Startup procedure to start the emission see Chapter 6 If this is not possible restart the whole system and try again e If this doesn t help run the Diagnostics Auto Report and Simple TAD utilities see below Specimen holder wizard doesn t e Read the Specimen Holder Wizard procedure for the proceed possible reasons stub holder height manual tilt stage tilt angle readout see Chapter 7 Pressure doesn t reach the target value Check the water bottle to be sealed properly to be filled when using the water in the ESEM with the water and the heating plate is warm see LoVac mode above Touch Alarm is active e Remove the specimen holder away from the chamber e Check the presence of a short co
19. not de ionized until 1 3 full 5 Mount the rubber plug and install the water bottle in the reverse order of that described above 6 Pump the system Switch to LoVac ESEM mode to force automatic purging to flush any air out of the bottle and connecting tubes Note The first time the system is pumped to LoVac ESEM mode after filling the bottle Auto purging may be erratic until the bottle pressure has steadied The removal of all the gas from the liquid must be accomplished before good imaging is possible This is done correctly when no bubbles are produced in the water when increasing the pressure in the chamber The heating plate under the bottle should be warm AB GQ NO LR Maintenance and Troubleshooting Pre Vacuum Pump Maintenance Pre Vacuum Pump Maintenance The Rotary pump supplied with the Inspect F is used to directly pump parts of the vacuum system such as the specimen chamber after a sample exchange and for backing the main pumping system Turbo Mechanical Pump TMP PERIODIC CHECK Because the pump has to process large volumes of air loss of oil level over time is inevitable The oil level check should be planned every 3 months The level indicator window is usually found on the front end of the Rotary pump and shows minimum and maximum level markers Venting the chamber shuts off the rotary pumps Although it is necessary when changing the total oil reserve Service function it is not absol
20. v Movie iv TIF The Movie check box AVI Digital Video timer After the Delay time the image of each resumed quad is stored immediately even in the middle of the frame as a new frame in the video stream The TIF check box After the Delay time images series of each resumed quad are stored at the end of the running scan the system waits in TIF format e Inthe read only area additional information are given about the number of stills frames per time unit seconds minutes If both TIF and Movie check boxes are selected AVI and also TIF files are stored In this case the AVI file is not reconstructed from TIF files which means the directly recorded movie can be different from the movie reconstructed from TIF files Note TIF files are better to save in many cases as they can be built into a faster AVI and the databar display can be customized when building an AVI file see below If both AVI and TIF are recorded the AVI may be jerky due to delays when writing TIF files to a disk TIF delay must always be longer than or equal to the Movie delay File module Names of Movie TIF files are composed as follows File name quad name Numeric seed series number avi tif For example MovieName Quad1 015 00023 avi tif The series number always has five digits form with leading zeros The File Name a generic file name must be entered here otherwise the Movie tab cannot be closed Do not use punc
21. which contains Nitrogen Vessel Vessel Stand e Vessel Plug System Options Quanta Morphologi FP 2201 73 Quanta Morphologi FP 2201 73 Quanta Morphologi is a method for precise determination of size and shape of submicron particles dispersed in a dilution It is a complex method which consists of sample preparation image acquisition and image analysis SAMPLE PREPARATION ITO slides Dilution with dispersed particles is deposited on the conductive side of the ITO Indium Tin Oxide slide and left to dry out Fully dried ITO Slide is laid on the holder tightened by the screw and easily attached to the single stub holder Note The ITO slide holder is constructed for safe rotation of 360 when the free working distance FWD Z axis is 10 mm Otherwise the ITO Slide holder can touch parts of the specimen chamber FIGURE 9 38 ITO SLIDE FIXED TO THE HOLDER Filter membranes Use of filter membranes is another eventuality of sample preparation Dilution containing particles is passed through a filter membrane with pores of diameter of 50 nm or less Particles are caught on the membrane that is further fixed on the 25 mm stub by the conductive carbon tape In this case wet membranes can be fixed on the stub and inserted to the specimen chamber System Options Quanta Morphologi FP 2201 73 FIGURE 9 39 FILTER MEMBRANE IMAGE ACQUISITION All analyzed particles must fill certain number o
22. 9 It is strongly suggested to always leave the chamber in HiVac mode when not being used When the sample chamber is left in the LoVac ESEM mode water vapour is likely to accumulate in it PVP lifetime decreases and the water reservoir or gas cylinder empties prematurely d The Complete shutdown procedure brings the system to the non powered state where the vacuum in the column area is no longer supported by running pumps All valves are closed and the electron column and specimen chamber areas are vented This should only be carried out by a FEI service engineer Normally it is used for a system transportation or for service actions like repair to essential systems electrical and air supplies Switching off the console when Emitter is On is not optimal and sparing way for the emitter User should use the Shutdown System button only in case of emergency need EB o System Operation Quanta FEG System States POWER OFF Take sufficient measures to avoid power failures as much as possible If it occurs while the instrument is completely operational the microscope comes down to a safe state and the following happens The HV is switched off abruptly The specimen chamber vents gently automatically The momentary adjustments of all system parameters accelerating voltage magnification stage positions are lost if they were not saved The Emergency Off is similar to that which would happen after a MAINS powe
23. Any Software Control xT microscope Control Software The stage movement can be aborted by hitting the keyboard Esc key Don t hesitate to do so if you are not sure that the initiated movement is safe FIGURE 4 11 THE STAGE MODULE otage otage Map Coordinates Titt Navigation Map Coordinates Tilt Navigation Actual s Go To jn x EN m Dynamic Focus ce 3 7701 mm m E J 9 9588 mm Im n I Em Tilt Correction Tilt Angle lw Automatic E E EEE Last Position Add specimen Pre tilt 00 20 E 4 gt an Update pl Ej gt E Remove The Navigation tab Click the Get button to capture a live image into the Navigation tab Drawing a green bordered box with the left mouse button inside it depicts an observed area from that point on By dragging and moving the box inside the navigation image an observed position could be changed affecting the active quad By dragging its boundary a box size could be changed or it is also possible to draw a new one 9 he Measurement Annotation Module combines tools for measuring and making annotations in electron images A measurement tool an annotation shape or a text label can be selected from the first three icons on top of the module and then drawn in an electron image quad All objects are sequentially indexed and displayed in the list box below icons The properties of the objects is possible to change in the property editor see Chapter 5
24. Enter your Username and Password 2 When the xT microscope Control software is available the Beam Control page displays on screen 8 Switch on the Emitter see Chapter 6 9 Click the Vacuum module Pump Button Wait for the Pumped status ann 10 Click the Column module Beam On button must be yellow 4 Full 11 Select a quad a detector and beam Operation parameters and resume the quad Note a Once you have your FEI Microscope user or Supervisor n f account set up via FEI User management software by FEI Account Administrator see Chapter 4 you can use your name and password to access both Windows xP system and the xT microscope Control software Take note of the case sensitive passwords necessary at Windows xP and xT microscope Control server Log On points A password is advisable for logging on to protect individual settings and results RUNNING Y O Motion Q Imaging Ul State STARTING 3 Microscope Stop Shutdown System Hide Ul Stop Ul Advanced gt gt gt xTm Log On Lisernarne Password Sene FEI UserManagement Y System Operation Quanta FEG System States E Edit Detectors Open Save Save AS Record Movie Import Export Print scan E Ctl S Ctrl P TABLE 3 3 SHUT DOWN PROCEDURE GENERALLY System State Action 1 Click the Column module Beam On button must be grey 2 Click the Vacuum module Vent button Wait f
25. FA Ctl M Ctrl B Cirl shift Ctl shift Ctm Cole Shift F 12 Chl o SCAN ROTATION SHIFT F12 This function activates the onscreen tool to rotate the scan and align the image Because it is solely a scan coil function it has no effect on the stage movements It is used to orient the image relative to mechanical rotation and detector direction Clicking the Scan menu Scan Rotation places a green circle in the image window The green triangle on its perimeter denotes by its position the sample rotation relative to its original position when mounted on the stage Initially this is in the 12 o clock position Drag it with the left mouse button around the circle to choose a new sample rotation The readouts displayed at the image window bottom provide information about the Actual Rotation original position and the Target Rotation the selected position Clicking the written angles around the circle perimeter 0 90 180 270 or the perimeter anywhere drives the stage to that rotation position and the green triangle updates onscreen Clicking the framed sign increases decreases the rotation angel by an incremental value FIGURE 7 14 SCAN ROTATION Once selected the compucentric rotation control disappears automatically after 10 seconds of no use see the Preferences General tab The smaller circle in the top right of an optical quad remains onscreen when the Scan Rotation a
26. Into cave users and groups save the System Info Create the ZIP file save the minidumps save Dr Watson crash log Start 2 Write down how to reproduce the problem and choose a problem class when prompted by the tool 3 Arrange the screen that you want to capture e g flags in the image when prompted by the tool 4 The tool proceeds with collecting of the system information 5 The tool creates a file on the PC s desktop Send it to a Field Service Engineer Finished 1 The report is created and can be found as a zip file J on the desktop named QuantaDa375 20060720 183948 zip 6 Close the window Maintenance and Troubleshooting Troubleshooting SIMPLE TAD If the xT Microscope Server is running the Simple TAD automatically performs all the tests communication optics supplies etc If it is exited only the communication tests proceed 1 Run the file located in C TAD Simpletad_collector exe Click the Start button Simple TAD data collector Click Start to begin 2 he tool proceeds with the collecting of the system information A file is saved to the location specified by the software Send it to a Field Service Engineer Simple TAD data collector Done Log saved to C Program Files FENlog Simple ADlog_D83 5_060720_184256 stad 3 Exit the window SYSTEM OPTIONS This chapter covers hardware and software that is an option either integrated in or acces
27. L Red coloured parts belong only to Hs 1500 Heating stage Assembly specimen Chamber Interior Heating Stages Assembly is mounted onto the microscope stage using the dovetail stage adapter The HS 1000 and the HS 1500 have the same construction and look similar Each stage is appropriately labelled engraved on the top surface Caution The presence of water hoses and cables inside the chamber causes a risk of heating stage and further the vacuum system damage the hoses could be pulled out of the stage and water could spill into the vacuum port in the chamber bottom Once the heating stage assembly is installed it should be moved only about 10 mm from the home position in X Y axes Rotation and Tilting are locked automatically Tilt can be released by the user in the Stage module Coordinates tab Tilt check box see Chapter 7 Be aware of the limitation u System Options Heating Stage 1000 C FP 2300 02 Heating Stage 1500 FP 2300 06 FIGURE 9 20 HEATING STAGE ASSEMBLY The dovetail mounting adapter enables to attach the Heating stage to the microscope stage The Heating stage base 5 holds all components The Top and Bottom Insulators 2 and 3 are a disk shaped pads made of aluminous foam placed inside the assembly e The Heater sits between the top and bottom insulators lt is a micro furnace in which samples are heated
28. Mo step 150 Heating Stage Settings This is the supervisor alignment procedure Step 1 the Temperature Ramping Limit could be set up to 300 K min default value is 50 K min Caution Ramp speed higher than 100 K min strongly decreases the heater lifetime and leads to regulation instability Step 2 applicable for HS 1500 only highly advanced setting intended for practised HS users Alignments 150 Heating Stage Settings Adjust the Temperature Ramping Limit using the slider Press Reset button for the factory defaults Caution The ramping speed higher than 100 kimin may reduce the lifetime of the Heating Stage significantly Instructions step 1 of 2 Temperature Ramping Limit min KE E Reset Cancel Alignments 150 Heating Stage Settings Instructions cet the temperature Switching Point to define the lower range below the switching point and the higher range above the switching point Adjust the Hysteresis value Set the Bias presets associated with each temperature range Press Reset button for the factory defaults step 2 of 2 switching Paint ava kK En g Hysteresis 5 K EN mm Lower Temperature Range sample Bias 50 r EE p Heat Shield Bias 200 EN m Uu Higher Temperature Range sample Bias 5 4 El Bip Heat Shield Bias Bl s B M El Reset Carcel Alignments IB Temperature Calibration Instructions Th
29. Module 0 0 0 c eee eee Replacing the Aperture rod llle 8 8 Aperture availability llle 8 8 Gaseous Detectors sidecases coe ew dos A ane eee 8 9 Cleaning the GSED LFD 0 0 0 0 eee 8 9 Cleaning the GBOD scars oe ache asada ae be ee een a coe eee 8 9 Stage maintenance esr aed bea ee ea m ees 8 10 Stage MECHANICS casos did x baci ed headed aa eee d whee 8 10 Specimen Holders 0 00 eee ees 8 10 Refilling the Water Bottle 0 0 cee es 8 11 Pre Vacuum Pump Maintenance lesse 8 12 Ho M T CT LHP A 8 12 Troubleshoollng sesion cita 8 13 Diagnostics Auto Report llle 8 15 SMPS TAD ops ais eh S d ARE Aran aaron eh Gace dp ree ze es 8 16 Chapter 9 System Options Manual User Interface FP 2311 05 9 2 Joystick EP 2311 01 x dro um Ex qe E ei ete Roues 9 2 Automatic Aperture System FP 2202 00 9 3 6 Aperture Alignment llle 9 4 Optional Detectors erica 9 5 Gaseous Back scattered Electron Detector FP 2303 00 9 5 Scanning Transmission Electrons Microscopy Detector FP 6903 01 9 6 Electron Backscattered Diffraction Pattern Detector EBSD 9 8 Photo Multiplier Tube Backscattered Electron Detector PMT BSE 9 8 Energy Dispersive X ray EDX Analysis 9 9 The Support Po FP 2353 02 n9 vad e eae cheater ig ee aa A 9 9 mile VACUUM P
30. SIZES AND THEIR USE otandard Option Option Recommended use No FP 6174 55 FP 6174 33 FP 6174 37 related to Standard sizes ER CA O a High current applications er mapping of low Z elements at low voltages mms General imaging or X ray analysis Demi experiments 7 j2oum 80pm 10pm High resolution imaging The left hand turn of the large ring moves the aperture holder outwards towards the larger aperture After the aperture change it is necessary to tune its position by using the inner knob and the one on the right side controlling horizontal plane fine movements see Chapter 6 FIGURE 2 6 FINAL LENS APERTURE STRIP CONTROL KNOB oes eet at tons oo CEE YT WARNING A Aligning the final lens aperture is a mechanical process It is possible to misalign the aperture strip and obscure the beam from reaching the sample Adjustment should only be done by those with the understanding of how to proceed The aperture holes edges cleanness is also very important see Chapter 8 m System Overview Quanta FEG Options Quanta FEG Options A range of hardware and software is available as options for the Quanta FEG system which list is introduced here see Chapter 9 for a detailed description of some of them H The Support PC FP 2353 02 connects your work space to the network and can hold some other software utilities The Manual User Interface MU
31. THE GBSD 1 Perform steps 1 and 2 above to remove the GBSD printed circuit board from the chamber The GBSD is easily cleaned with a toothbrush Soft Scrub CIF cleaner and water as with the GSED To access the PLA and converter plate remove the two screws holding the collector grid to the printed circuit board Scrub the SE grid gently as this can be easily damaged FIGURE 8 7 DISASSEMBLING THE GBSD Maintenance and Troubleshooting Stage maintenance Stage maintenance STAGE MECHANICS Checking the condition of the stage should be a weekly exercise as many different samples may be exchanged in this time period Some samples may be powders or composite materials that inadvertently drop particles on or in the stage If a silicon wafer breaks in the chamber it can shatter into hundreds of pieces In this case the stage should be thoroughly cleaned before attempting movement again Cleaning Stage parts Abrasive and solvents must not be used on the moving stage parts Cleaning by a suction is the ideal method If not available cleaning should be done by using dry nitrogen gas bursts around the stage mechanics to blow out any foreign materials Make sure the final lens and detectors are protected from the turbulence Do not use sharp metal objects to scrape away debris A fine pair of plastic tweezers can be used to pick up difficult particles Spillage on the stage should be wiped up using a lint free cloth followed by su
32. Water Flow Box Control Board 0000 eee eee 9 15 Connecting the Water Flow Box 00 0 cece eee eee 9 16 Adding Water to Cooling Stage Base 0000 cee eee 9 20 Chamber feed through Plate Inside 9 22 Heating Stage System Block Diagram 9 23 Heating Stage Assembly 0 00 cece ee eee 9 24 Outer Cable and Inner Cables 0 ccc eee 9 25 High Temperature GSED 0 0 0 ees 9 25 C viii A 1500 C Heat Shield Assembly Small Chamber 9 26 Adjustment of the 1500 C Heat Shield o o ooooooo 9 27 Installing the Heating Stages llli 9 28 Connections to the Heating Stage 0 0 cc ee 9 28 MUI buttons new functionality llle 9 29 Temperature Profile llle 9 32 Temperature and Conductivity llle 9 32 Inclined Crystal EDX Detector Configuration o 9 33 Position of the High Temperature GSED 00 02 eae 9 34 Positioning for EDX Performance 00 cee eee eee eee 9 34 1500 C Heater Lifetime 0 n E ene 9 35 Nitrogen Vessel and Vacuum Vessel with accessories 9 37 CryoCleaner Flanges 0 ccc eee eee teens 9 38 CryoCleaner Plastic Cap Funnel 0 00 0 eee ees 9 39 Nitrogen Vessel placed in Stand 0 0 ees 9 40 ITO slide fixed to th
33. a red circle the current active position 9 Blue a new location not stored White on a green background indicates a stored position highlighted in the location list Stages Software Stage Functions Radar view The small circle in the stage schema top right corner conveys the stage rotation at any time by the black triangle and perpendicular lines position To rotate the stage click and hold with the left mouse button the triangle on the circle perimeter Move it round and release the mouse button at the desired position the stage rotates accordingly Location area The Location list shows the Current Position and the Last Position the stage position before any movement as default When expanded it shows the positions list with a scroll bar Double clicking anywhere in the circle area with the left mouse button marks a new location 9 and moves the stage to it The position selected becomes the current active position and it is highlighted in the list and also on the map 8 Clicking a position name allows the user to edit it Pressing the Enter key or clicking a different item confirms the new name pressing the Escape key restores the old name The Open button opens a stored Stage Map file stg The Save button saves a Stage Map file to disk When closing the UI the system registry automatically keeps the otage Map file with the specific User name to be loaded after the log in procedure The Cle
34. alignment you can apply steps 5 and 6 separately for fine electrical alignment gun shift of the final lens Pressing and holding the left mouse button in image area activates a quad arrow ended cursor Try to achieve no image shift considering the middle alignment cross This alignment could be used any time o Click the Lens Alignment tool bar icon The scanning sets 1 Gun Alignment Alignments Instructions Mate Use Quad 1 for the procedure This alignment procedure centers the electron beam at various High voltages and opotsizes Mo step Alignments 1 Gun Alignment After finishing the procedure there should be no image shift no out of focus and no brightness change during microscope operation Alignments I Gun Alignment m Instructions Focus the image Adjust the Contrast and Brightness when necessary Bring a recognizable feature under the center cross by the stage movement step 1 ofS Contrast 45 67 E i B Brightness 53 8 ul B Cancel Alignments I Gun Alignment Next Instructions select the High Voltage Focus the image Adjust the Contrast and Brightness when necessary Bring the recognizable feature back under the center crass using the Image Shift 20 control Tick the Copy alignment to next spot check box to copy last set values as a starting point for another spot setting step 2 ofS High voltage 30 ky Image Shit
35. available for 100 mm and 150 mm stages e The button 3 speeds up the stage motion 10x in X Y axis 5x in Z axis 2x in R T axis B o 0 System Options Automatic Aperture System FP 2202 00 Automatic Aperture System FP 2202 00 SEE Stage Tools Window Help Aperture 20 um Home Apertures 30 um 30 Lim Degauss FS 40 um Lens Alignment Shift F4 50 pm 1000 Lm Preferences Ctr oO Beam Current DEEDES emi js The Automatic aperture system AAS option enables a motorized final lens strip aperture exchange The menu Beam Aperture selection list see Chapter 2 and 5 offers available apertures The Home Apertures feature moves the AAS to its home position This is recommended when system cannot operate the apertures properly Note An aperture diameter can also be displayed in the databar Moreover the beam current could be chosen instead of the Spot size see the Preferences General tab to be displayed in the tool bar list box and in the Column module Beam Current preset continuous adjuster The Spot size Beam current control Spot size Beam current select a desired value to be used with the system System Options Automatic Aperture System FP 2202 00 6 APERTURE ALIGNMENT This Supervisor procedure provides a high precision aperture setting Alignments 6 Aperture Alignment start Instructions This alignment procedure defines the apert
36. because contamination evaporates back to the chamber 1 Vent the specimen chamber the excess LN starts to boil do not be concerned 2 Unclip the Nitrogen vessel from the Vacuum vessel Lift the Nitrogen vessel out of the Vacuum vessel by the Safety pliers placed under the ring on the neck of the Deware cylinder 3 Place the Lid over the Vacuum vessel to seal it from the atmosphere fix the clips Pump the specimen chamber again however the microscope vacuum remains cleaner than before and sample contamination is still reduced 4 Remove the cap from the Nitrogen vessel and pour out the excess LN2 into a suitable container ep System Options CryoCleaner FP 2301 25 WARNING A When the LN2 is removed from the nitrogen vessel the bottle still remains at a very low temperature 5 Place the Nitrogen vessel onto the Stand ready for baking Baking Nitrogen Vessel 1 Place the Nitrogen vessel Stand select one of two possible ones on a Suitable heat resistant surface 2 Place the Nitrogen vessel onto it and use an Infra red lamp to bake the base of the bottle Baking should take place for approximately 2 hours Alternatively the Nitrogen vessel can be baked in an oven at 90 C for 2 hours Regenerating the dewar by heat allows removal of condensed contamination and subsequent reuse of the vessel Note The oven that is used must have a venting system to extract any harmfull fumes Alternatively it s
37. center in other case the sample could be tilted When an image is shifted during an immersion ratio change the sample is possibly not parallel with the detector To correct this click the Modulator button the BDV starts to change periodically with the 100 V amplitude With the use of the Compucentric stage rotation stage tilt minimize the image shift in the X Y axis until it is acceptable Switch off the modulator Note An image shift when changing the immersion ratio could be caused by imaging near the sample or any other edge 1 mm tilt Ss Hv Landing E tilt mm pt Cathode Lens Mode HY Landing E 350 kv 500 00 ev O Cathode Lens Mode 350 kv 500 00 ev 5 4 Set the landing energy considering the sample material charging compensation material contrast Set the immersion ratio to optimize the signal Set the brightness contrast and WD according to the requirement 5 Tune the Lens Alignment and the Stigmator both factors remembers the HV and immersion ratio last used 6 Repeat steps 4 and 5 to get the best result Y System Options Specimen Holder Kit Option FP 2301 10 Specimen Holder Kit Option FP 2301 10 The Specimen Holder Kit is Universal The interfacing parts allow the fitting of all the common components to the Inspect S Inspect F Quanta and Quanta FEG Major holders in the kit locate with a 2 pin system originating from the stage rotation head through the interface piece to t
38. centre of the screen Then repeat the procedure above to perform further astigmatism correction You can use reduced area advantageously see Chapter 4 If an astigmatism cannot be corrected there may be some other reason usually the final lens aperture is dirty see Chapter 8 the magnification may be too high for the beam spot size see below or the sample is charging apply conductive layer or use the LoVac ESEM mode PRESSURE AND WORKING DISTANCE WD It is assumed the LoVac ESEM mode is set the GSED or GBSD is installed and the sample is visible in the image display area For standard imaging choose the highest specimen point and bring it to the 10 mm WD the yellow line in an optical quad Focus the image and then link Z to FWD Adjust the chamber pressure to achieve the brightest possible image Lower the pressure about 67 Pa 0 5 Torr from this point FIGURE 5 2 BRIGHTNESS VS PRESSURE Brightness Pressure Operations Optimising an Image SED 6 2 mm WD ve gt Enhanced Image LUT Mix 3 Mix 4 Color b al O Contrast 1 2 D Bright 0 00 x Misi 125 Gamma N ONE Enhanced Image LUT Mix 3 Mix 4 Color Multiple 2 v source 1 33 Source 2 3396 at mui E B o wr B Source 3 33958 Select MI um Adjust contrast and brightness to personal taste to obtain a clear optimized image which should allow small changes about 0 5 mm in WD without the need
39. changing or updating User Units Redefine User Units with Shift as above with the Beam Shift Reset User Units so that they are equal to the Stage Units Show how User Units are now defined displays the current definition with the possibility to move the points step by step Particular dialogue buttons e Finish ends the procedure at the point s 1 2 3 just defined Details displays the resulting coordinates with the possibility to browse them Go to button and edit the values Set button Stages Stage Related Functions FIGURE 7 13 USER UNITS DETAILS xTm Define User Units Details Specimen X User X Y set 0 17 mim 0 082 mim 0 000 LILI 0 000 LILI set 0 010 mim 0 086 mm 1 000 UU 0 000 LILI set 0 02 mim 0 901 mim 0 000 LILI 1 000 LILI Current position on specimen A 0 0239 mm 0 010 Apply TABLE 7 6 USER UNITS DEFINING PROCEDURE Step Action Select a sample surface feature and view it at an appropriate magnification to check its relation to other structures Click the Stage menu Define User Units A Start dialogue appears Click the Define New User Units radio button xTm Define User Units Start Make Selection fe Define New User Units Redefine User Units Redefine User Units with Shift Reset User Units so thatthey are equal to Stage Units f Show how User Units are now defined Details Cancel Click the sample user point 0 0 with the left mouse bu
40. cold surfaces of the dewar as this could result in burns Use the Safety Pliers provided when handling the Nitrogen Vessel 1 Pump the specimen chamber the Vacuum vessel is pumped along with it 2 When the specimen chamber vacuum is ready Pumped status partially fill the dewar with the use of funnel the plastic cap upside down and wait until boiling has stopped do not be concerned 3 Then fill the dewar and place the plastic cap on top of the CryoCleaner The volume of liquid Nitrogen needed is approximately 500 ml Note The LN2 stops boiling very quickly so that no vibration is seen from this device If the CryoCleaner needs to be used for longer periods it can be recharged with LN2 Note Before re filling it is recommended to perform Baking procedure see below Eo o System Options CryoCleaner FP 2301 25 FIGURE 9 36 CRYOCLEANER PLASTIC CAP FUNNEL Removing Nitrogen Vessel WARNING Use the Safety pliers provided when handling the Nitrogen vessel Removing the Nitrogen vessel depends on the level of contamination found in the specimen chamber If the level is unusually high then the CryoCleaner could work continuously till improvement is seen otherwise normally after approximately 2 to 3 hours the Nitrogen vessel can be removed Note Although the dewar can be effective to approximately 9 hours it is not recommended to leave it inside the vacuum vessel after all nitrogen evaporates
41. focuses the image in a narrow range to facilitate the process Try to bring the rotation center to the screen center if the magnification is too high the rotation could seem like a linear motion instead of a rotation Note Clicking above the 2D box with the right mouse button opens a menu with following particular features The Clear Memory few last used user settings are recorded When changing the HV the value is set either to the last value used if recorded or to an estimated value based on the available Software Control xT microscope Control Software Status Chamber Pressure 1 458 4 Pa bie Pa Emission Current 152 n Gun Pressure IGP Upper 2 04e 7 Pa j Column 3 32e 3 Pa Chamber 200 Pa Gun Pressure OFE Emission Current 152 UA Coulomb Tube Current 6 0 yA record The Clear Memory command clears this record The Auto Alignment finds optimal conditions automatically Note The Source Tilt Auto Alignment is available only for spot sizes 5 or higher 7 The Status Module can be found at the base of all pages displaying following information some of them as a tool tip he Chamber Pressure shows the specimen chamber pressure The Gun Pressure shows the electron source space pressure The IGP Upper IGP Lower shows the electron source space pressure in detail e he Column shows the column pressure e The Emission Current shows the electron current emitted
42. from the sides allowing uniform temperature gradients It includes the heating element thermocouple ceramic connectors 4 and crucible in which the sample is placed The Cover Plate 1 holds the heating stage components in place e Two ceramic papers Heater cover and Heater cover 2 sit on top T of the top insulator they reduce heat losses from the heater and BOTTOM protect the insulators OF STAGE To remove the crucible from the stage assembly grasp the edge of the crucible with a pair of tweezers and lift it out There is a hole in CRUCIBLE Push stick through hole to remowe the crucible the bottom of the stage which can be used to remove the crucible AAA KOD OR WOODEN should it become stuck in the heater Use a small rod or wooden uus stick to access the crucible through this hole Chamber Feed through Plate oee the description above the Cooling stage Water Chiller Flow Box and Cooling Water Hoses oee the description above the Cooling stage Heating Stage Controller This microprocessor controlled board provides accurate and stable automatic temperature control of the heating stage and interfaces with the xT microscope Control software It has an internal temperature limit for either stage to protect the equipment The temperature measurement accuracy is determined by the thermocouple and the controller These specifications are as follows e HS sensor accuracy 1 C HS 1000 normal operati
43. gt P i I User Auto Contrast Brightness activates the automatic contrast and brightness routine The system Auto Focus F11 attempts to set the Contrast and Brightness of the selected detector in Auto Stigmator Ctri F11 the active quad to suit the current sample and conditions so that the set Default Parameters CT D majority of grey levels is displayed Display Saturation shift F11 User Auto Contrast Brightness Lab Notes examines gray levels of the active quad image and stores their FEI Movie Creator minimum and maximum Next time the ACB function is used it attempts to set the Contrast and Brightness so that the resulting image gray levels lies between this minimum and maximum instead of Preferences cuo full black and white Application Status A tick next to this menu item indicates the user gray level limits active Clearing the tick reverts the ACB to its default setting Auto Focus F11 bd activates the automatic focus routine The system attempts to correct the focus independently of the working distance or Z coordinate set Note When activated ACB Auto Focus Auto Stigmator the dialogue appears to show the progress The function can be interrupted by clicking the Stop Now button which leaves the image the focus WD at the current stage of progress Clicking the Cancel button before the function ends returns the image back to its original status ETEEN the original WD value Auto Stigmator
44. heading in the brackets for instance Save Ctrl S and in the summary table available from the Help menu Pages are numbered by this way Chapter No Page No within the Chapter Instead of Chapter No you can find an abbreviation C which means content pages e Tables and figures excluding explanatory ones are numbered within each chapter in this way FIGURE Chapter No Figure No within the Chapter TABLE Chapter No Table No within the Chapter Areference to the specific element is highlighted in bold and it guides to its particular Ul placement For instance Clear the Stage module Coordinates tab Z coordinate check box SYSTEM OVERVIEW The Quanta FEG Scanning Electron Microscope SEM produces enlarged images of a variety of specimens achieving magnifications of over 100 000x providing high resolution imaging in a digital format This important and widely used analytical tool provides exceptional field of view minimal specimen preparation and the ability to combine the technique with X ray microanalysis How Quanta FEG SEM Works There are four main components of the microscope Electron source The electron beam is emitted within a small spatial volume with a small angular spread and selectable energy Lens system The beam enters the lens system consisting of several electromagnetic lenses and exits to hit the specimen surface Scan unit The scan generator signal fed to the deflect
45. in that direction trying to move to the stored position the warning dialogue appears Stages Software Stage Functions otage Map Coordinates Tilt Navigation Dynamic Focus Tilt Correction Tilt Angle Iw Automatic Er E specimen Pre tilt OO El El E otage Map Coordinates Tilt Navigation aa e 1 fa ub P el rae eae I When the Compucentric Rotation check box is ticked the R coordinates operates as the Compucentric Rotation function Note The R coordinate is permanently locked and its homing is disabled when the heating or cooling stage is plugged in TILT TAB When the appropriate check box is ticked the function becomes active he Dynamic Focus check box ticked the focus automatically changes as the beam scans from the image top to its bottom trying to follow the tilted specimen working distance change The Tilt Correction check box ticked the flat specimen foreshortening compensation is on in one direction at a known tilt angle when the tilt axis is parallel to the stage XY plane Because the image is a two dimensional representation of a three dimensional object certain distortions occur For instance a square grid image appears rectangular when you tilt the specimen This function corrects the aspect ratio and restores the square appearance he Automatic check box switches between automatic and manual tilt angle settings If ticked the Til
46. installed so that the collection ring does not interfere with the angle of the EDX detector This can be g System Options Heating Stage 1000 FP 2300 02 Heating Stage 1500 C FP 2300 06 done by simply rotating the detector so that one of the gaps in the ring faces the EDX detector In the following photo note that the bars on the collection ring are oriented so that the path from the EDX detector to the GSED is clear Also note that the working distance given may be longer than the recommended 10 mm It has been found that different EDX manufacturers may have optimum collection below 10 mm Each system should be tested to find the optimum working distance before using the heating stage FIGURE 9 31 POSITION OF THE HIGH TEMPERATURE GSED E To door EDX detector EDX Performance Elemental analysis can be performed while heating the heat radiated from the heating stage to the EDX detector is very small under the 400 C and generally does not affect the EDX detector The sides of the crucible and the top edges of the stage interferes with the collection of x rays from the sample Therefore all EDX analysis should be performed on the sample opposite to the EDX detector FIGURE 9 32 POSITIONING FOR EDX PERFORMANCE ELIX cw Detector Ceramic insulator Heater Tilting the stage by no more than 5 toward the EDX detector will improve x ray signal collection as well Count rates for EDX ana
47. interference with other controls If the full mouse motion is not sufficient to get the image in focus release the mouse button at one side of the screen move the mouse cursor to the opposite one and press the right mouse button again over an imaging area to continue focusing A If this is the new specimen first time focusing run the Link Z to FWD function see Chapter 4 To avoid scanning too long and contaminating or even damaging the sample move away from a feature of interest with the stage and focus until the image is sharp on an adjacent area Focusing at a higher magnification makes the result more precise For example for an output at the 2000x magnification focus at 4000x 8000x magnification Focusing with the MUI option Use coarse and fine focus knobs to focus the image The image immediately responds to the MUI Note nui it I Use also the following functions to focus the image see Chapiei Reduced area F7 Auto Focus F11 CORRECTING ASTIGMATISM This optical aberration is caused by different focal lengths for rays of various orientation resulting in a directional image blur horizontal and vertical rays are not focused to the same plane on the image edges Note L For normal astigmatism correction use the automatic procedure E Ctrl F11 or follow the procedure below if you want to reach the best results There are special coils serving to correct this imperfection which is us
48. is indicated as Ext in the databar The CCD camera reflects the inner space of the specimen chamber The Mix sets a possibility to interfuse signals from 2 or 3 detectors Detector Settings The selected detector settings mode grid voltage used segments etc can be dynamically changed in this module The Detector list box contains list of currently available detectors the same as enabled items in the Detectors menu The list box always displays the detector currently selected The rest of the module dynamically changes according to the selected detector and its parameters see Chapter 5 Beam Stage Fause Snapshot Photo Videoscope Reduced Area Full Frame Spot Line External Beam Blank Slow Scan Fast Scan Slower Scan Faster Scan Mains Lock Live Tools Window F6 F4 F2 F3 F7 Ctri M Ctrl B Ctrl Shift Ctrl Shift Cte Ctro Average 16 frames Integrate 256 frames Scan Rotation Preferences g Shit F12 Colo F Software Control xT microscope Control Software The Scan Menu Alt C opens the scanning control functions Pause F6 I l pauses the image This function is used automatically with Snapshot and Photo functions Select Pause or press F6 or click the Pause icon once twice double click to stop scanning at the end of the current frame immediately When the quad is going to be paused at the end of the frame t
49. is running and after any change in the Target Ramp edit box The Temperature Profile edit boxes are used to define temperature profiles or cycles Each row pertains to a single heating cycle Temp target temperature which should be reached e Ramp speed of a temperature increase decrease e Soak time specifies time hours minutes seconds for how long the target temperature should be hold after it is reached Edits are active when any temperature stage is enabled and the profile is not running When the profile is running the box mark at the end of the current step line is displayed in Yellow The Start Stop toggle button starts stops the Temperature profile The profile starts with step one The first step with a non filled or a zero Ramp or with a zero Temp value stops execution of the profile The Next Clear toggle button when profile is running the caption is Next and clicking the button bypasses a current cooling cycle in a multiple set immediately When no profile is running the caption is Clear and clicking the button resets all values The button is disabled when the Hold button is active The Hold button switches keeping of the Actual current temperature invariable on off Clicking the button turns it to Yellow It can be used to interrupt a ramping cycle and maintain the controller at the current set point When clicking the Hold button during a ramping cycle the controller holds the current
50. left to the right in the Databar Preview The Label Show Beam Icon Micronbar check boxes set the display of the appropriate items in the Databar The Micronbar scales to the magnification The Units button sets the Units of Measure Pressure Temperature used in the movie Databar display E o Operations Recording Movies Saving Multiple Images Preview tab Once the movie is set up opening the Preview tab automatically displays the first image of the movie sequence FIGURE 5 12 FEI MOVIE CREATOR TAB PREVIEW fi FEI Movie Creator The Start Pause Stop button starts pauses stops the movie play back By dragging the adjuster one can run forward or backward through the movie PLAYING A MOVIE The AVI file movie can be played in the Windows Media Player or any another more advanced movie editing program recognising the avi file type Operations Measurement and Annotation Functions Measurement and Annotation Functions Measurement Annotation Color E Line Width 1 End Type None End Point Both Direction Any EM Bannan Rectangle Measurement Circle Measurement Angle Measurement Line Measurement X Y Coordinates L EN E l 4 Rectangle Circle O Line p Faint The Processing page Measurement Annotation functions give the user many capabilities to measure distances angles diameters and areas as well as locating and labelling items that are of
51. not be used frequently may highlight features by contrast not easily seen otherwise Loading samples Materials or hard samples should be prepared as for the TEM by appropriate thinning technique The STEM holder which is a part of the detector assembly can either be loaded with samples while outside the microscope chamber which is more convenient or when itis mounted and fixed to the stage 1 Remove the holder top by loosening the central screw This exposes the 8 grid positions round holes with tweezers slots 2 Load the TEM grids with samples face up into the grid holes The holder top has raised rings to press down in the grid holes to hold the TEM grids firmly in place The holder top numbers should overlay the same ones on the base plate 3 Replace the holder top carefully and tighten down the central screw To remove sample grids proceed in the reverse order System Options Optional Detectors Obtaining an image 1 Switch on the accelerating voltage at 20 kV set the spot size to 3 2 Using a fast scan focus the top of the STEM holder surface with SE detector 3 Link Z to FWD and bring the focused surface to a5 mm WD 4 Move to the appropriate sample position and focus the TEM grid bars The WD and Z position has now lengthened and re setting of the Z axis value to 5 mm Is necessary This procedure is necessary to prevent inadvertently bringing the detector in contact with the final lens The minimum s
52. not to exceed 50 C min ramp speed otherwise your heater lifetime shortens For advanced users ONLY Additional HS 1500 features The Bias Presets check box allows the user to apply sample and shield bias values according to settings in the alignment procedure 150 see below The Heat Shield and Sample Bias sliders are used for the manual sample and shield bias values setting The power and biases can also be controlled via Manual User Interface MUI modified knobs which is a part of the 1500 C heating stage option The MUI performance could be set in the Preferences General tab where the following line appears MUI knobs assignment Default Heating stage The Default setting always keeps the original functionality The Heating Stage setting assigns MUI knobs another functionality when the Temperature Control module Heating button is clicked When the HS is turned off or removed the habitual functionality is restored see above FIGURE 9 27 MUI BUTTONS NEW FUNCTIONALITY the Stigmator X knob change to the Power knob the Stigmator Y knob change to the Enhanced Contrast knob the Shift X knob changes to the Sample Bias knob the Shift Y knob changes to the Heat Shield Bias knob System Options Heating Stage 1000 C FP 2300 02 Heating Stage 1500 FP 2300 06 Alignments 150 Heating Stage Settings start Instructions This alignment procedure sets parameters for the Heating otage
53. on the top of the holder for 2x 12 5 mm stubs All stubs are screw fixed The Angled Stub Holder fits to the Interface pillar by a captive centre screw Eo o o System Options Specimen Holder Kit Option FP 2301 10 Analytical Holder 3 The Analytical Holder is use in conjunction with an EDX system 2 polished 1inch mounts can be slotted from below into the retaining holes until they become flush to the top of the holder Here they can be locked in place by screws in the holder side wall This gives the specimens a common height with a Faraday cup position drilled into the top of the holder and therefore can be common during x ray analysis There are also 2 positions for 12 5 mm stubs or for standards necessary for the analysis The 2 stubs are each held by a screw in the side wall The Analytical Holder fits to the Interface pillar by two captive screws equally off set from the centre All screws are either Torx or Hex key ended POLISHED MOUNT HOLDERS These comprise of 2 shallow cup holders of different diameters The sizes are 25 mm and 32 mm These are the general size of encapsulated mounts either for Metallurgy or Geology The holders have a split in the side of the cup so as to grip the mount when it is pushed in They have a simple pin the same as the 12 5 mm stubs therefore can be mounted on any of the same fittings as the standard stub FIGURE 9 53 POLISHED MOUNT HOLDERS CLAMP STUBS CLAMP STUBS These are g
54. performed Note The Average is set independently also for the optical window option but using averaging with more than 4 frames is not recommended especially when moving the stage m o Software Control x7 microscope Control Software Integrate allows accumulative noise reduction by true integration over a specified number 1 or more of frames This process continues until the selected number of frames is reached and then pauses the quad automatically During and after image accumulation you cannot change the focus or perform other image influencing actions This can be used as an alternative to slow scanning to obtain high quality images of slightly charging specimens Note Clicking the down arrow next to the icon displays menu items Live Average Integrate Number of Frames enabling to select number of averaged or integrated images depending on the currently active Filter Mode indicated by the icon image for the active quad Clicking the icon itself changes the Live Average Integrate mode in cycle ge Live we Average 4 frames Integrate 1 frame The Number of Frames is set and remembered independently for the Average and Integrate filters Both the Filter mode and Number of Frames is set and remembered per quad so live and filtered images can be observed at the same time Settings are particular for the Reduced Area and for the Full Frame also The Photo function uses the Filter Mode and Number
55. simultaneous use of the EDX It works best at a slow scan conditions The mounting pin below the detector locates into the standard conical single stub mount The detector is connected to an SSD pre amplifier input board Note When the STEM detector is mounted to the chamber stage rotation and tilt are locked automatically for the safety It is possible to unlock these stage movements manually but beware of possible STEM cable damage while rotating or tilting the stage Detector Settings a Segment A Segment B C A B C A B A System Options Optional Detectors FIGURE 9 4 STEM DETECTOR Settings for STEM Detector The detector segmenis A left and B right can be switched independently enabling the bright field BF or dark field DF contrast mode The STEM holder has 8 positions for TEM sample grids The following table refers to the positions numbering and their related capabilities TABLE 9 1 STEM HOLDER POSITIONS Grid Position Observation Mode and Diode switching The object is left right of the segment separator Segment A gives BF DF Segment B gives DF BF 234 BF use Segment B only BF use Segment A only The A B condition default can be used for the first time since the entire detector is working which facilitates to get an image To switch BF DF choose Segment A B in the Detector Settings module Choosing A B gives a negative image that although will
56. take approximately 1 minute Are you sure you wantto continue Operations Specimen Preparation and Handling quality adhesive preferably carbon paint The specimen must be electrically grounded to the sample holder to minimize specimen charging If you are using a vice mechanism or double sided tape make sure the specimen is conductively attached to the holder Note The sample holder is not directly grounded to the chamber ground because it is connected to the BNC feed on the chamber door This allows to measure the sample current Caution Store samples and sample holders in a dry and dust free environment Dust on samples can get drawn into the electron column degrading imaging and requiring an FEI Customer Service INSERTING EXCHANGING A SPECIMEN AND OR A DETECTOR It is assumed that the microscope is in the Full operation state see Chapter 3 TABLE 5 1 INSERTING A SPECIMEN a a Action Otherwise there is a risk of a detector assessment malfunction and as a result the PLA see below is not recognized by the system When vented open the specimen chamber and using lint free gloves or tweezers place a specimen into the specimen holder Secure the specimen stub with an appropriate hex wrench unless a spring clip holder has been used Install any additional detector if it is not already done see below Adjust the Eucentric Position see Chapter 7 Close the specimen chamber door 4 Click t
57. taken at much lower magnification The Sample Navigation can be selected independently for any quad regardless of its current content and status A tick next to the menu item indicates that the function is selected for the active quad As soon as this quad is paused the Sample Navigation indicator appears in the upper right corner of the quad The indicator is green as long as the paused image can be used to navigate the live images otherwise turns read e g when the stage rotation or tilt changes Navigation Montage This procedure takes the image of the sample to be used in the Sample Navigation see Chapter 7 Software Control xT microscope Control Software Specimen Holder Wizard starts a process to capture an image of the multiple specimen holder using the CCD camera The image is then displayed in the Stage module Map and can be used for navigation among a number of samples and or big features The wizard progresses through a number of steps with confirmation dialogues to prevent any specimen detector lens collision due to the stage tilt needed to capture the image Clear Holder Image deletes the Specimen Holder Image from the Stage module Map tab This is used when the specimen holder is to be reloaded with the new specimen stubs and a new image is needed The Tools Menu Alt T opens the Tools menu functions ees Window Help Auto Contrast Brightness FO Auto Contrast Brightness ACB F9
58. temperature indefinitely until the button is clicked again Note Edited values are checked for limits values out of limits are not accepted Zoo System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 The Humidity tab Temperature Stage Control The Humidity tab is displayed only when the CS is connected to the ee feed through plate connector This application controls humidity of wet samples during ESEM microscope operations with the FEI Cooling Stage installed It is Actual Target possible to do so manually by the sample temperature and specimen 90 0 chamber water vapour pressure control User can set a desired sample humidity directly via the Humidity tab Temperature Humidity Note A humidity value can also be displayed in the databar To start the work and control the humidity follow the steps 1 Vent the chamber Install the GSED if it is not 2 Insert a wet sample and add water drops when needed 3 Close the door and pump down the chamber to the ESEM LoVac mode ESTEE 4 Set the Column module Pressure usually 400 Pa Click the Cooling button 6 Set the Temperature tab Target temperature usually 2 5 C and click the Go To button 7 Set Humidity tab Target humidity usually 90 100 and click the Go To button Any pressure change causes a target temperature change and vice versa to keep a desired humidity constant oO Three phase diagram shows a
59. the same time When the stage is homed correctly it ends up in the No E following position X Y position is set to the factory pre set stage rotation centre R 0 T 0 Z preset long working distance depends on the stage type Home Stage Without Rotation executes Home Stage function see above without rotation When the moo xT microscope Control 1 Caution the stage Z axis positive direction is now UP The system cannot recognize height of your specimen To define the minimum Z stage position well please focus on the highest specimen surface Press OK to link or Cancel to quit Do not show this message again cancel g Software Control xT microscope Control Software stage is homed without rotation the stage Rotation reference is greyed out This is useful when a large specimen is inserted and stage rotation could cause a collision with equipment inside the chamber Center Position Ctrl 0 digit moves the stage to coordinates X 0 Y 0 Touch Alarm Enabled activates the Touch Alarm for the stage This function automatically stops the stage movement and displays Touch Alarm warning dialogue whenever the stage or a conductive specimen touches the objective lens or any other equipment conductively connected to the chamber This functionality is used also when the stage engines start to rise the power over the determined level Unlink Z to FWD This feature
60. the left side of the module there is a dwell time preset list with the fixed number of entries Selected Preset values can be changed in iau the Property Editor on the right side of the module Following Snapshot Preset properties are editable depending on the kind of the preset Photo Preset Dwell Time one point beam duration time Resolution no of points Width x Height image resolution Integrate no of integrated frames 1 2 4 8 16 32 64 128 256 Acquisition 8 bits 16 bits sets the captured image bit depth e Action activated at the end of Photo Snapshot function Save saves the taken image using automatic file name and format Save As opens the Save As dialogue to save the taken image None just takes the image and pauses the active quad Following properties are informative and non editable Line Time line scan duration time Frame Time image scan duration time Refresh Rate image refresh frequency Slow Scan tortoise large green sector Fast Scan hare small green sector Snapshot and Photo different cameras preset buttons indicate the matching dwell time value to change it move an icon up or down just by clicking and dragging it only available for Slow Fast scan The Default button restores the default dwell time list and scan functions settings E Software Control xT microscope Control Software The ESEM Tab enables to customize the specimen chamber p
61. the lens insert Second pull the other end of the detector out from the connector FIGURE 9 41 SYMMETRICAL LOW VACUUM DETECTOR SLVD INSTALLED IN THE CHAMBER Sample Navigation Mapping Navigation Montage Mapping Output file properties Path cda Browse Prefix 300nm x4 k ITO10 1 kv Hivac s Image format TIF 15 bit d Single numbering Overwite existing files Region properties Number of images in X Number of images in Y Overlap Status State Idle Progress Time remaining Time required 00 00 52 Stay ontop Switch off beam when finished Start System Options Quanta Morphologi FP 2201 73 MAPPING TOOL It is located in Stage menu Mapping tool or in Windows Start Programs FEl Company Applications Mapping Due to statistical reasons a sufficient number of particles should be calculated Therefore the Mapping tool is applied for the automatic acquisition of user defined number of images Before running the mapping tool all parameters of the image acquisition high voltage spot dwell time etc must be set in the user interface Note For low magnification images use the Navigation Montage together with the Sample Navigation to preview the scanning area and to see the progress of the Mapping procedure Note Using the Mapping tool the images are saved under conditions that are currently preset in the Ul The Mapping tool consists of Output file p
62. to 75 5 to 0 5 to 0 Eucentric Position WD 10 mm 11 6 mm 29 2 mm distance between a sample top surface and the stage base Maximum sample 250 g 2 000 g 5 000g for all tilt angles Eoo Stages Software Stage Functions software Stage Functions The Navigation page Stage module controls the stage movements that locate the position of the specimen by reference to coordinate points It consists of Map Coordinates Tilt Navigation tabs MAP TAB In the map area the stage schema is represented displaying all stored locatable positions which are listed in the Location list box for selecting FIGURE 7 7 MAP AREA ELEMENTS Location ast Position Open 20 3 Save 20 S Clear g TABLE 7 4 MAP AREA ELEMENTS No Function 1 Black mechanical stage center The darker rim the sample holder outline Light grey dashed line physical limit of the stage movement along X and Y axes X Y scroll bar to move the stage schema area in a X Y stage direction at different magnification factors CS Magnification factor of the map area 1x 100x Radar view Black triangle the moveable rotation angle positioner Grey perpendicular lines denote rotation position Grey stored positions as on the map Red ina red circle Blue positions as on the map 7 White x on a red background a stored location with the rotation noted by the black key position 8 Red in
63. types and its application see above HS 1000 MgO crucibles are coated with a conductive platinum paste and a platinum wire runs inside it allowing a sample bias to be applied directly under the sample Crucibles have a finite lifetime the platinum coating wears out after some time Before inserting the crucible into the heater always check the sample bias wire shape to avoid a poor electrical contact The Platinum the heating element is made of reacts with the silicon therefore always avoid free silicon i System Options Heating Stage 1000 FP 2300 02 Heating Stage 1500 C FP 2300 06 HEATING STAGE INSTALLATION 1 Remove a current if any sample holder adapter 2 Install the dovetail included onto the stage rotation base if it is not in place parallel to the door opening direction 3 Slide the stage module onto the dovetail base from the rear forward until it stops 1 The stage has a pin which ensures the sample is centred beneath the beam Note Hoses must be oriented towards the chamber back always 4 Tighten the locking screw on the stage assembly right side 2 FIGURE 9 25 INSTALLING THE HEATING STAGES m Cables and Water Hoses connection 5 Connect the 15 pin connector of the 4 ended Inner Outer cable to the appropriate feed through plate connector Note Check the inner cable corresponds with the stage type 6 Connect the Heater power Thermocouple and S
64. user for adjusting microscope 4 FEI Factory Users factory Factory user for adjusting microscope User factory FEI Factory Users Buffer Software Control FE User Management Software Account Use The File Menu contains the following items Log out Log On click to log on active when user is logged out Refresh FS Log Out click to log off active when user is logged on e Refresh F5 click to refresh the user tree Exit e Exit click to exit the FEI User management program anne Userdata Help Create Ins The Account Menu Remove Del E contains the following items which are accessible only for FEI Set password Account Administrators with the exception of set password set user group fu nction Properties Alt Enter Create Ins click to add a new user or supervisor FEI User Management Add new user Liscenama Password Contr password T T Cusseaune hos Graup FEI Supercivor Livers Full nemz D esenptian j Liger mut chage pastrand al mex logon Uen cannoli change ppaswwnnd DO airaa meer expres Aecaunt it deebled CAE Cancel Remove Del click to remove an existing user The user must be FEI User Management Delete user lt highlighted first A Are you sure to delete user supervisor If an FEI Microscope User has user data the account administrator is warned that user data will be removed also If any additional user is to e
65. 0 eee 3 8 Software Control Pages and Modules LIS 3 225 c vee seed EA ex b EE Vus 4 21 Status Icon Meaning llle 4 24 Mouse Button Functions llle 4 38 Windows System Keys llle 4 39 Function and Specific Key Short cutS 0 0000 cee eee eee 4 39 Operations Inserting a Specimen 1 eee eens 5 3 Quanta FEG Setup Conditions nnno anaa aaaea aa eee 5 4 Selecting Vacuum Mode 2 2 6 cee ee eee 5 5 Spot sizes and recommendation of their use o o oooooooooo 5 6 Optimal Final Lens aperture sizes um and Approximate spot sizes as a function of Beam current and high voltage 5 6 Mading PrOCCQUNG sat barat aora iba i dab dede ds 5 7 Contrast amp Brightness Setting 2l 5 9 C amp B Setting using videoScope a naana aaea 5 9 Focusing Procedure o 5 10 Correcting ASUOETSUSETE s aod den d pisce rng ado m RE 5 11 All Detectors Typ8S o o oooooooooono IIIS 5 14 Image Capturing Procedure llle 5 23 Image Printing Procedure llle 5 23 Set Up and Recording a Movie 0 0 0 ce ee eee 5 26 Alignments Alignment Procedures Overview llle 6 2 Aligning the Final Lens Aperture 2 0000 cece eee ees 6 4 otages Finding Eucentric Position Procedure 000 cece eee 7 4 Sample Positioning Procedure 0c cc ees 7 5 Stage Features and Limits 0 0 0 0 ccc ee
66. 1 The Title bar labels the application 2 The Menu bar contains all operation menus and submenus 3 The Tool bar contains functional icons for the most frequently used microscope controls and for the fast access to the Pages 4 Image windows image windows with adjustable Databar 5 Pages and Modules microscope and image control elements organized into modules making up the pages 6 The Preferences dialogue presetting of operating conditions Software Control xT microscope Control Software THE TITLE BAR displays the application icon and name plus the standard Windows buttons Minimize and Close which are enabled FIGURE 4 3 THE TITLE BAR EJ x The Close button quits the xT microscope Control software accelerating and detectors voltages are switched off for the security reasons THE MENU BAR displays pull down menus across the screen below the Title Bar FIGURE 4 4 THE MENU BAR File Edit Detectors Scan Beam Stage Tools Window Help SS Pages Select pull down menus from the menu bar by pressing e the left mouse button on the Menu title ALT underscored keyboard letters e ALT and then use keyboard arrows Note Some menu functions have their equivalents in the tool bar In such cases the corresponding tool bar icon is shown next to the function title in the following text The File Menu Alt F Edito Detectors Scan B opens File menu administrative functions Open
67. 3 XT ATO Feature 2i a3 b idees n ed diee ut ati eee rua CR wake 7 14 User Units Detalls duis soa dr dele AC te gar ae don ir eai CS tow is das 7 16 Scam FOAM ON EDI 7 20 Maintenance and Troubleshooting Standard Insert Components 000 c eee ee eee 8 4 Universal Detector Tool 0 ccc eens 8 4 Removing and Disassembling the Insert liliis 8 5 Installing Apertures to the Insert 0 0000 cee eee ee 8 6 Aperture Strip Module 0 cc eens 8 7 Removing the GSED Assembly 0 0000 cee eee 8 9 Disassembling the GBSD 0 0c eee 8 9 System Options Wt PM atic eters ics BIE Made tect Gabe alate ib PIECE yao ee PEU 9 2 DOV cue ap PR a aeteas dct dba MELDE 9 2 GBSD Operational Schema 00 dadia eee eee ees 9 5 STEM Detector 0 cc eee eens 9 7 Inspect Standard Layout Scheme 0 000 cece ee eens 9 9 X ray Imaging in HiVac Mode 0 eee eee 9 9 LFD Configuration for the EDX Analysis o oooooo o 9 10 X ray Imaging with the GSED llle 9 10 X Ray GAD Configuration in ESEM Mode ss 9 11 Cooling Stage System Block Diagram LL 9 12 Cooling Stage Assembly 5s x descr a eed 9 13 Cooling Stage Assembly Mounting Adapter with Mounting Screw 9 14 Chamber feed through Plate Inside Outside 9 14 Outer and Inner Cables 1 0 0 cc eens 9 15 The
68. 30 instruments and want to use this kit FIGURE 9 50 OLDER INTERFACE ADAPTER INTERFACE PILLAR This component is used to attach the 3 multi holders individually to the stage It is fixed to the stage by the captive centre screw System Options Specimen Holder Kit Option FP 2301 10 FIGURE 9 51 INTERFACE PILLAR FOR MULTI HOLDERS Analytical holder screw positions Location pins MULTI HOLDERS The Multi Holders fit individually on the Interface pillar using the same pin location system Numbers 1 and 2 have a captive centre screw for fixing to the Interface pillar where as number 3 has two captive screws Offset from the centre POI vo a Up 3 ape i FIGURE 9 52 THE MULTI HOLDERS Sr ai HE MER U wr 16 Position Stub Holder 1 This can be used for 12 5 mm pin stubs the Clamp stubs the Polished mount holders or any pinned small holder The pins are held by spring pressure to prevent vibration or falling out Using the location pin position with homing of the stage each time will allow one to map the holder into the stage location system The 16 Position Stub Holder fits to the Interface pillar by a captive centre screw Angled Stub Holder 2 This holder can be used for a pre tilt condition where either there is no wish to tilt the stage or additional tilt is needed beyond the stage tilt capabilities The set angle is 45 and holds 4 x 12 5 mm stubs at this angle There are also 2 positions
69. 35 Operations Monitor Image and Scanned Sample lusus 5 8 Brightness vs Pressure at us ads ack o n cR a A acd 5 11 BSED GAD Diode UniS sima RR ar Eb a TRECE Ran 5 15 GAD Installation and Holder Position sels 5 16 LP Dana ts COMmigquravulon sa aca iu acd ox e area or ie atem e Seat n 5 17 GSED and Tis colligll atiis 5 ou dea e cher Eo cendo e GS T aus A at 5 18 The GSED Installed in the SEM lesus 5 18 Movie Preferences 0 cc eee ee ees 5 24 FEI Movie Creator TAB File ix ka pi wad are Ae aw exa 5 27 Browse DIAIO GUC ca ssi doe M acide cie ede o RC US C tone Sat ae af a tona 5 27 FEI Movie Creator TAB Databar 0 00 0 cee 5 28 FEI Movie Creator TAB Preview 0 0 0 eee ee ee 5 29 C vii stages Quanta FEG 200 Stage 4 axes motorised 0 000 eee 7 2 Quanta FEG 200 Standard Sample Holders 7 2 Quanta FEG 400 600 Stage Controls ooooooooo 7 3 Quanta FEG 400 600 Standard Sample Holders 7 3 Eucentric Position Principle llle 7 4 Stage Movement Schema eee eens 7 6 Map Area Elements 0 0 cc eee eee eee eee 7 7 The Map Dialogue 4 5 bei hos eb alib ad 7 8 DISCI E UC HOD scare sani ce vis oe seated diria e doa ts es ea as ad 7 11 Get FUOD 2 x ach gba or dt dea a o 7 12 Compucentric Rotation 0 0 cc ee eee 7 1
70. 4 for setting up a collection of sequenced TIF images and lining them up into an AVI movie see Chapter 5 Application status displays a dialogue above quad 4 with continuously updated system messages Pop up on Message Severity None Error Warning All specifies which kind of messages is going to be shown automatically on screen Three icons in the lower right corner enable to switch on off displaying of Error Warning Information messages The Clear button clears all current messages from the window The Hide button hides Application Status window but leaves the messages untouched FIGURE 4 7 APPLICATION STATUS xIm Application Status Time Description Source 10 39 47 The FWD value is not accurate anymore re link xTm to FWD ta FWD 10 00 34 The FEG source is operational Feg Source 10 00 30 The water cooling is off SENICE Fop up on Message Severity Mone Error e Warning All The Window Menu Alt W opens the Window menu functions Center Cross Shift F5 places a cross in the center of all electron image quads This function is automatically used in Alignment procedures to aid the centering of features and can be used to align a sample against a stored image in another quad Software Control xT microscope Control Software Alignment Rectangle Shift F6 places a dashed rectangle in the center of all electron image quads This function is used for some Alignm
71. 58 System Options Heating Stage 1000 FP 2300 02 Heating Stage 1500 FP 2300 06 Consumables TABLE 9 3 HS 1000 1500 CONSUMABLE PARTS HS 1000 Standard crucible 10 pcs 4022 298 00681 Low crucible 10 pcs 4022 298 00691 HS 1500 Standard crucible 10 pcs 4022 298 00711 Low crucible 10 pcs 4022 298 00721 HS 1000 and 1500 Graphite crucible 50 pcs 4022 298 00701 HS 1000 and 1500 Heater cover 20 pcs 4022 298 00731 Heater cover 2 20 pcs 4022 298 00871 HS 1500 Heat shield isolation 4022 298 00741 20 pcs Old version HS 1000 Specimen cup 10 pcs 4022 298 00751 HS 1000 and 1500 Detector Cap 4022 293 22561 HS 1000 and 1500 Hook Wire adapter 4022 293 22521 HS 1000 and 1500 Ceramic paper pad 50 pcs 4022 298 00831 System Options CryoCleaner FP 2301 25 CryoCleaner FP 2301 25 This equipment allows to decrease the contamination level in the system The kit consists of e Vacuum vessel including o rings screws e Vacuum vessel lid Nitrogen vessel Dewar with cap including proper warning labels Nitrogen vessel stand Nitrogen vessel safety Pliers e Manual WARNING This option uses liquid Nitrogen LN2 which may cause serious cold burns PARTS AND ACCESSORIES The CryoCleaner consists of a Nitrogen vessel that is surrounded by an outer container the Vacuum vessel which is connected to one of the specimen chamber ports by a vacuum seal The space b
72. 8 16 bit image offers 256 65 536 levels of grey Live Averaged and Integrated images are scanned as 8 16 bit ones For the Mix quad images a selection between the 8 or 16 bit mode is possible The Colour 24 bit image offers 256 levels of each primary colour red green blue Digital colours coming from the Display Saturation feature from the Image Enhancement module Color tab from the Mix quad with colour mode set changes an image bit depth so there is no way to save it without them When user wants to obtain the image without these colour enhancements it is necessary to turn off the respective UI functions Coloured digital overlaid graphics Measurement and Annotation are possible to save with without an image see the respective checkbox in the Save As dialogue Other types of overlaid graphics over an image are never saved icons controls videoscope etc Digital File Formats The image captured can be saved in various digital formats depending on the resulting colour and bit depth needed Generally there is no reason to save an image with a higher bit and colour depth than available in an original one Over against saving an image with a lower bit and colour depth than available leads to the loss of information The message is displayed in this case onscreen Snag de ree n ie TIFA format redoces me color niermamen er the number ef gay levee Condes aman Do net how tas messes qan The TIF 8 16
73. 8 FEI COMPANY The Quanta FEG User Operation Manual oth Edition 21 04 2008 Copyright 2008 FEI Company All rights reserved Trademark Acknowledgments FrameMaker is a trademark of Adobe Systems Incorporated Microsoft is a registered trademark of Microsoft Corporation Windows XP is a trademark of Microsoft Corporation Production Acknowledgments This manual was produced using FrameMaker M document publishing software Technical Authors Martin Dufek TABLE OF CONTENTS J Chapter 1 Preface User Manuals 3o pb eux ax CEP EE a eae 1 1 The User Safety Manual 0 0 0 0 renra i aa ees 1 1 The User Operation Manual llle 1 1 How to Use this Manual Leer 1 2 Chapter 2 System Overview How Quanta FEG SEM Works eere 2 1 Vacuum SYSIEM ccc iii do Rede eR Re ERU RE oe Ad a 2 2 Image Viewing and Capture 0 0 ee ee 2 3 Positioning of the stage cose esata belie ceed aele eee hs 2 3 System Layout of Quanta FEG 0 0 ee 2 4 Software Interface Elements 0 00 0 cece eee eee 2 4 Hardware Interface Elements 0 000 cece ee eee 2 4 Quanta FEG ODTONS siii ra ic a urn dover o Ra ec 2 7 Chapter 3 System Operation Quanta FEG Vacuum System eller eere 3 2 Vacuum Slatuse s iii ai ai 3 3 ANS A on ora ae UU 3 3 VENTE DURO asias ee aco ta aegis ais detenta lens a nit Agia io 3 3
74. Chapter 6 Not possible to adjust the Check there is only one Gun Tilt position with 1 Gun alignment maximum illumination If there are more of them place the Gun Tilt cross among them see Chapter 6 If illumination is lost during a Gun Shift adjustment Modulator is on re adjust the Gun Tilt position Crossover mode to find the illumination again see Chapter 6 Run the Diagnostics Auto Report and Simple TAD utilities see below Maintenance and Troubleshooting Troubleshooting TABLE 8 2 POSSIBLE PROBLEMS AND CORRECTIVE ACTIONS Poor ETD image e Select the ETD Open the Detectors menu Detector Settings Select the Mode Custom Change the Grid Voltage from maximum to minimum see Chapter 5 e There should be a visible change of the contrast an image is getting darker with lower voltage If not run the Diagnostics Auto Report and Simple TAD utilities see below i Alternating lighter and darker image e Run the Purging procedure see Chapters 3 and 4 bands visible in the ESEM LoVac mode Check the water bottle to be sealed properly see above Discharging and white stripes e Decrease the Detector module Contrast value see in ESEM LoVac mode Chapter 4 Water interlock failure e When cooling water does not flow the Application Status window with the respective message pops up see Chapter 4 Check the cooling water flow Note The system is designed to work without the cooling water However
75. Contrast Operations Detector Types and Usage LARGE FIELD DETECTOR LFD This detector is used with the standard insert The field of view is unrestricted and the magnification range is identical to that of HiVac mode assuming no other pole piece accessory is mounted The signal from the LFD contains more BSE information than the GSED signal The detector is ideal for general imaging it is also the only gaseous SE detector that can be used simultaneously with a BSED Detector FIGURE 5 5 LFD AND ITS CONFIGURATION Installing and Setting the LFD The LFD plugs into the signal connector behind the conical lens In some cases the user is prompted for the PLA size Select No Accessory in the Pole Piece Configuration dialogue or appropriate Cone if installed Note After inserting the LFD Preferences ESEM tab Purge mode changes to Automatic despite any previous selection This ensures that the proper chamber environment is achieved see Chapter 4 THE CCD CAMERA enables to view the inner space of the specimen chamber an optical quad It assists with an overall sample orientation and during a stage movement to prevent its collision with the lens pole IR LEDs are used to light the specimen chamber interior Operations Detector Types and Usage xTm Detector Settings Detector Settings Detector GSED Enhanced Contrast EN A 55 5 Clase GASEOUS SECONDARY ELECTRON DETECTOR GSE
76. D The GSED is integrated into a flexible printed circuit board and plugs into the signal connector behind the conical lens It is used for general wet imaging and for high pressure imaging with auxiliary gases FIGURE 5 6 GSED AND ITS CONFIGURATION Conical Objective Gaseous Secondary Electron Detector as flow Sample gam The overall image consists of a very pure SE signal with very little BSE signal component due to the detector design and chamber geometry This pure SE signal makes this detector best suited for resolution imaging The field of view is less than the LFD at the lowest magnification The lower magnification range is about 240x at 7 mm WD Installing and setting the GSED 1 With your gloved hand grasp the detector by the rigid connector end Hold it with the detector head facing towards you and the yellow Torlon ring facing up 2 Insert the detector gold fingers facing forward into the connector located at the back of the chamber behind the conical lens This is made easier by inserting the right side of the detector in to the visible portion of the connector then rotating the detector into position A keyed connector position prevents the user from inserting the detector upside down 3 Place the yellow Torlon ring of the detector head under the lens insert and press the detector head up onto the insert This requires little force and can be done with one finger The yellow Torlon seal should b
77. D1000 5905 v C Encryption Let server Choose Default w In case your configuration consists of both Microscope PC and Support PC you need to connect to the Support PC Type the Support PC name followed by the colon and the port number 5905 into the Server field Press OK button 3 Some secure key and signature related dialogues may appear Confirm all of them by pressing OK or Yes button VNC Viewer Information x VNC Viewer Information l A secure key wil now be generated This may take a few minutes l Anew secure key has been generated and stored VNC Viewer Warning No signature has been stored for this vNC Server so its identity cannot be verified Dio you wish to accept the signature and continue connecting 4 In the Authentication dialogue fill in your microscope Username and the corresponding Password Press OK button VNC Viewer Authentication 128 bit AES Encryption VA Username Supervisor o ox O c jJ When this step successfully passes you are connected to the Microscope PC and the VNC window with its desktop opens Emo o System Options Remote Imaging FP 2415 00 When connecting remotely be aware of the fact that there might be some person operating the microscope locally i e working directly with the Microscope PC To close the remote connection to the Microscope PC just close the VNC Viewer window MICROSCOPE PC S DESKTOP SHARING several users ca
78. ER 2 Using tweezers step by step carefully insert all the apertures 5 pcs sharp edge uppermost into the seating on the upper end of the holder Gradually screw the nut down 3 Using the tweezers insert the c clip into the tube of the injector provided 4 Depress the plunger slightly until the plane of the c clip within the tube is approximately at a right angle to the axis of the tube Release the plunger 5 Place the injector vertically into the aperture holder so that the tube rests on top of the aperture 6 Depress the plunger to push out the c clip The pressure must be continued while retracting the body of the injector so that the c clip remains in place in the holder seating Use the large end of the aperture removal tool to seat the c clip firmly into the bottom of the injector so it is flat Blow with clean air to remove any fibres etc 7 Remove the injector and check that the aperture is properly clamped by the c clip This can be done either by inverting the holder over a Petri dish and tapping lightly or by observing the position of the c clip with a magnifying glass Note Always check the mounted aperture under a binocular microscope or with a magnifying glass to make sure that no hairs or other contaminants are on the aperture or between the aperture and the c clip Be careful not to lose small parts especially the c clip The following additional instructions on inserting the apertures should also b
79. FEG el XT Microscope server The standard layout of the Quanta FEG 200 400 and 600 systems is based around a dedicated microscope controller The user interface devices are peripherals to the microscope controller either software or hardware FIGURE 2 3 QUANTA FEG STANDARD LAYOUT SCHEME Electrical Microscope Microscope Console Console Controller Customer s Microscope en Hetwork Keyboard Mouse SOFTWARE INTERFACE ELEMENTS The software control contains graphic applications within Windows XP operating environment xT microscope Server starts and stops the basic microscope functions It makes possible to open and close the xT microscope Control software UI user interface or sometimes xTUI in the dialogue boxes which controls system functions including detection and analysis scanning image gathering manipulation and output magnification pressure etc All user account levels created via FEI User Management software ensure for the particular users admission to both the operating system Windows XP and the xT microscope Control software The hierarchy of user account levels consists of the following e FEI Account Administrator e FEI Supervisor Users e FEI Microscope Users e FEI Non active Users see Chapters 3 and 4 for more information on Logging on and Logging off the start up of the system and all the features of the user interface elements HARDWARE INTERFACE ELEMENTS T
80. FP 2301 10 The Electrostatic Beam Blanker FP 6842 25 The Keithley picoamper meter 9432 909 96402 The Picoamper meter Switch Box FP 2308 01 The Mains Matching and Isolation Transformer FP 6343 02 provides a galvanic isolated AC regulated power source with the 115 230 V 50 60 Hz output The CryoCleaner anti contamination device FP 2301 25 The Video Hard Copy Unit 9432 909 92223 5 paper rolls for video hard copy unit 9432 909 92351 The Gaseous Analytical Detector GAD FP 2304 11 is the low voltage BSED with an additional X ray cone with a 500 um Pressure Limiting Aperture which seals to the objective pole piece The Gaseous Back Scatter Electron Detector GBSD FP 2303 00 allows BSE imaging in ESEM mode i e at a high chamber pressure it uses a gas amplification to compensate a System Overview Quanta FEG Options signal loss Other back scattered electron detectors solid state or scintillate type BSE detectors typically work with a pressure up to 100 Pa but tend to get very noisy at this condition The small diameter low voltage Back Scatter Electron Detector BSED FP 2304 05 The STEM Detector FP 6903 01 allows detection of electrons transmitted through the sample Regular voltage range is from 30 kV down to around 5 kV which is of course dependent on the sample thickness The Annular STEM detector FP 6903 06 The Gaseous Secondary Electrons Detector GSED FP 2304 15 with the 1000 um ap
81. Heat Shield If the heat shield touches the high temperature GSED or sits farther than 2 mm from it the arm needs to be adjusted It must be centred in the X Y directions too this may not typically need to be adjusted 1 Loosen the Z adjustment hex screw and move the heat shield up so that the tip of the GSED sits in the heat shield hole 2 Use the X Y adjustment screws to make any necessary centring adjustments FIGURE 9 24 ADJUSTMENT OF THE 1500 C HEAT SHIELD ATA shield shield Y ADJUSTMENT in E Z ADJUSTMENT Chamber Feedthrough Plate A ADJUSTMENT to SSB Controller 3 Move the arm to the 2 mm distance from the GSED and re tighten the Z adjustment screw Note For the 150 mm stage the extender must be installed Heat Shield and Sample Bias SSB board This board provides voltages used for the following features e A heat shield bias voltage 0 300 V draws the electrons from the sample through a small opening in the heat shield Atlow temperatures the sample bias 50 V is negative with respect to ground and pushes the electrons to the detector At higher temperatures this bias is positive to suppress the thermal electrons which are generated by a sample Note The safety A C Interlock causes the bias voltages to switch off whenever the specimen chamber is vented however make sure the supply is turned off before changing any connection Crucibles The crucible
82. I FP 2311 05 provides direct manual control of microscope parameters such as focus magnification contrast brightness beam shift and Stigmator The Joystick FP 2311 01 brings another possibility to control the basic stage movements The Cooling Stage FP 2300 12 enables to image and analyse specimens cooled between 0 and 10 C of very diverse nature at relative humidity conditions up to 10096 typical chamber pressures required are in the range 300 1000 Pa Humidity experiments could characterize the sample morphology and phase distribution The stage is cooled by water The Waterless Cooling Stage FP 2300 21 uses copper belt to detract heat excess The 1000 C Heating Stage FP 2300 02 is used to view heated samples up to 1000 C and record in situ morphological changes The 1500 C Heating Stage FP 2300 06 enables to heat samples up to 1500 C This option includes two 1500 C and one 1000 C heating stages The Cooling Heating Stage control kit FP 2300 42 The Feed through Port Relocator FP 6762 42 52 pin Electrical Feed through FP 6822 10 7 pin Electrical Feed through FP 6823 10 The Compressor 115 V 50 60 Hz with 4 liter Tank 9432 909 96411 The Compressor 230 V 50 60 Hz with 4 liter Tank 9432 909 96391 The Thermo Neslab Water Cooler 50 Hz 9432 909 96721 The Thermo Neslab Water Cooler 60 Hz 9432 909 96731 The Acoustic Enclosure FP 3440 52 for Pre vacuum Pump The Specimen Holder Kit
83. Move button to move in unlocked axes only axes are locked not available or limited by software Stages Software Stage Functions e Clicking the Remove selected position item deletes the selected location s from the map and from the Location list The Coordinates tab Remove button has the same functionality Clicking the Magnification item provides menu allowing the Map area magnification factor 5 to be selected Scroll bars 4 appear if necessary to move over the whole Map area The Center view item brings the selected location to the center of view e When the Auto center on target item is ticked and the Magnification factor is used the active location remains in the center of view The Zero radar view item resets the stage rotation to 0 which is represented by the black triangle 12 o clock position The Stage location overlay item toggles the detector and chamber door position display in relationship to a sample COORDINATES TAB Three modes are possible via the list box The Actual mode default displays actual position coordinates in the edit boxes The Target mode activates when clicking a stored position or when editing a coordinate value The Relative mode is used to move stage by a given value and to repeat it several times if needed Clicking the Go To button drives the stage to a new location This only acts on just edited coordinates with a tick mark Pressing the Enter key a
84. OPERATION TERMINATION 1 2 3 Let the stage cool to the room temperature Shut down the water chiller Disconnect one of the water hoses coming out the water flow box to the chamber Push START FLOW button and push the water out from the lines with the use of the compressed air breath Make sure the system is drained before disconnecting the inner hoses This prevents excess water from dropping into the chamber and slowing the time it takes for the chamber to pump down again Install one water line plug into each water fitting on the inside of the Chamber feed through plate The water fittings on the inside of the feed through plate are designed to create a pressure seal whenever the water lines on stage are not connected If there is any debris in the cooling water it can collect on the fitting o ring seals and cause a leak To prevent this water plugs must be installed over the fittings on the inside of the feed through plate whenever the stage is removed FIGURE 9 18 CHAMBER FEED THROUGH PLATE INSIDE 6 Once the stage has been drained and both water lines have been removed blot out any remaining water from the connectors using a cotton swab or paper towel Another way to remove water from the connectors is to pump down directly to Wet mode this causes the pump down to take longer than usual Note When pumping down to Hivac mode after the stage use always enter Wet mode first otherwise the system ma
85. Open Save Ctri s displays a standard dialogue for opening images previously stored to Save As a media Supported file formats are TIF8 16 24 JPG and BMP but only files saved from xTUI in TIF format contain the active processing Record Movie information which could be utilized later for a databar setting see the nape Preferences Databar tab Export d i The dialogue displays by default the location path last used to open Print Ctrl F or save files from the xTUI Log Off Factory Save Ctrl S Exit saves the image using the format location and base of name set by the last used Save As function in that quad An incremental suffix with a selectable number of digits ensures that every image is saved as a new file e g Name_001 tif Name_002 tif etc Save As opens a dialogue for saving images which provides an opportunity to change the file name and location An image can be saved in TIF8 16 24 JPG or BMP file format Software Control xT microscope Control Software FIGURE 4 5 SAVE AS DIALOGUE Save in e Local Disk C My Recent Documents and Settings Documents C3kkol 3 Blog QNYCE3000 Desktop Program Files ICISYSTEM SAV Tad QWINDOWS My Documents 35 My Computer My Network Places File name Stage50_tilt_003 tif v Save as type tif8 Image files tif v Cancel Save image with Databar Save image with overlaid graphics The dialogue d
86. Pause Sample Navigation etc At any time just one quad is active has focus and all functions related to a single quad applies only to an image in this quad Pause Sample Navigation image processing The Active quad is marked by the highlighted blue Databar and optionally also by the blue frame selectable in Preferences General Depending on the quad content and status some mouse functions are available over its area see table 4 4 Electron image incl External and Mix focus stigmate Beam Shift change magnification coarse fine lens alignment Scan Compucentric Rotation active XY move get or tracking mode zoom in out Optical image option place 10 mm Marker Compucentric Rotation active Z move tracking Tilt Note Due to a hardware limitations some detectors cannot be used simultaneously They can still be selected for different quads at the same time but if one of them is started the other quads with incompatible detectors are automatically paused The optical quad is automatically resumed if it is paused when the venting procedure starts The Databar displays Instrument Image and labelling information This can be a combination of Date Time HV Detector Stage coordinates for instance They can be placed in any order and expand or contract to fit the quad width as long as there is enough room see the Preferences Databar tab FIGURE 4 10 THE DATA BAR EXAMPLES
87. R T LEM 9 9 LED ED XUAN SIS aud dese Sta SEQ O acm CRF a AS de acte cd do dish 9 10 OSED EDX ANAYSSI Se zt x cts Ameen Ai ada 9 10 aAD EDX AlidlySlS 24 atit diete cate aci Epp ceca Snape ata dite antea 9 11 STEMJEDXAHAIVSIS ui si io Sane p e Re Re dna 9 11 Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 9 12 Cooling Stage T ars dub Mee Moers aeo RUD aad 9 12 Cooling Stage Installation o o oooooomoooooooo 9 15 OOIWale CONTO s extat riada eni an eee eee 9 18 Cooling Stages Basic Operations 0 0 00 cee eee eee 9 20 Water Cooled Temperature Stage Operation Termination 9 22 Heating Stage 1000 C FP 2300 02 Heating Stage 1500 C FP 2300 06 lt lt lt lt lt lt lt lt lt ee 9 23 Heating Stages Parts 0 ccc ees 9 23 Heating Stage Installation llle 9 28 Software CONO negas duis mca ce SER V Era ote RT eO Deae pi ers 9 29 Heating Stages Basic Operations llli sn 9 31 HS Maintenance llle 9 35 CryoCleaner FP 2301 25 2 2 eee eee 9 37 Parts and Accessories 0 cc eee 9 37 C iv g CryoCleaner Operation snoa nanana eee eee 9 38 ME INGO intr Seas ho e E AR eg fou 9 41 Spare Vessel FP 2301 26 i beide Re wx Ep ee Ew eae 9 41 Quanta Morphologi FP 2201 73 lle 9 42 Sample preparation o oooocococoooe n 9 42 Im
88. SING COLOR TAB Stop Hide Ul Ele Edit etectors Scan Beam Stage Took Window Heb Pages lezeoix 10 0kv 30 e gin EE mld 1015 gt me 1029994 9 EB M awry 0 ub eq M Enhanced Image LUT Mix 3 Mix 4 Color Pseudo Colors 1 4 22 2008 curr mag pressure 1 21 32 PM 10 s kV_ 0 10 nA 82 801 x 9 dis mm 70Pa RECOMMENDED SETTINGS Several ways of image acquisition can be applied depending on the character of particles General recommendations for settings are described below but user tests must be done to found out the ideal settings for each type of sample ITO slides Low Vacuum Symmetrical Low Vacuum Detector Use all types of conductive and nonconductive particles e pressure of 50 130 Pa e accelerating voltage gt 5 kV spot size gt 2 5 free working distance FWD 7 10 mm e image resolution gt 1024x884 dwell time gt 10 us High Vacuum ET detector conductive and selected non conductive particles with diameters of 100 nm and less BSE detector solid conductive and selected non conductive particles except those with atomic number close to 50 e accelerating voltage gt 5 kV Spotsize 2 5 free working distance FWD 7 10 mm e image resolution gt 1024x884 dwell time gt 10 us a System Options Quanta Morphologi FP 2201 73 Filter membranes Particles on filter membranes can be observed almost directly afte
89. The Flow box and Cooling water hoses FIGURE 9 10 COOLING STAGE SYSTEM BLOCK DIAGRAM xT microscope Control Chamber Feedthrough Plate software CS Interface Cable Controller Cooling Stage Mater Water Sealine Wi H PESE Chiller Flow Box ooling Water Hoses fo specimen Chamber Interior The Cooling Stage Assembly is mounted onto the microscope stage using the mounting adapter Caution The presence of water hoses and cables inside the chamber causes a risk of cooling stage and further the vacuum system damage the hoses could be pulled out of the stage and water could spill into the vacuum port in the chamber bottom Once the cooling stage assembly is installed it should be moved only about 10 mm from the home position in X Y axes Rotation and Tilting are locked automatically Tilt can be released by the user in the Stage module Coordinates tab Tilt check box see Chapter 7 Be aware of the limitation 90 System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 FIGURE 9 11 COOLING STAGE ASSEMBLY sample holder n Delrin cower a iM m specimen holder Inc thermistor Lm Thermoelectric module 7 Cooling stage base gt Mount lacking screw NENNEN cd The mounting adapter enables to attach the Cooling stage to the microscope stage The Cooling stage base holds the thermoelectric module and the specim
90. X ray analysis EBSP Note When changing the spot size adjustment of the Detector module Contrast and or Brightness may be necessary to optimize the image An alternate approach is to use the Auto Contrast Brightness F9 function The Beam Current could be controlled by changing the spot size and by selecting the final lens aperture see Chapter 2 A hint on a proper setting gives the following table TABLE 5 5 OPTIMAL FINAL LENS APERTURE SIZES um AND APPROXIMATE SPOT SIZES AS A FUNCTION OF BEAM CURRENT AND HIGH VOLTAGE Beam Current nA Column E spot samon efv 40 High W oltage ely 20 00 kw Magnification 10511 x Ki B Bl A Detectors Contrast 38 4 a Bl B Brightness 50 0 E E E Operations Optimising an Image OBTAINING AN IMAGE ON SCREEN The following assumes that the electron emission is on TABLE 5 6 IMAGING PROCEDURE Step Action chosen quad Click the Column module Beam On button to ramp up the accelerating voltage An image appears in the active quad Adjust to a suitable magnification optimize the image with Contrast and Brightness focus Stigmator see below 13 Focus the image and Link Z to FWD see Chapter 4 Optimising an Image DV M PRINCIPLES OF SEM IMAGING All scanning beam microscopes produce images with the same fundamental technique The primary beam is scanned across the specimen surface in a regular pattern called a raster N
91. a Name Prefix Pl amp Spartan amp Channel 1 001 m Time Period a 1000 MEME E Gray Movie From NK To o2 Save in ECdtemplda File Mama Pl Spartan 4 Channel 1 001 avi Databar Preview 3292005 wwe M po CUFF det HF 4 ww j JT m DU ns 30k 356p LFD 112 um Guanta The Name Prefix click the button to browse the TIF files with the desired sequence prefix directory It is not necessary to choose the first file in a row FIGURE 5 10 BROWSE DIALOGUE Lookin O New Folder amp movie Channel 1 009 00001 tf amp movie Channel 1 009 00002 tif amp movie Channel 1 009 00003 tf E movie Channel 1 009 00004 tf amp movie Channel 1 009 00005 tif movie Channel 1 009 00006 tif amp movie Channel 1 009 00007 tif File name TIE T Files of type T IFF files from Movie tif Cancel e The Time Period tick the ms radio button to select a custom timing for the movie playback One may experiment 200 ms is good for most movies to speed it up Tick the TIF Time radio button to select a real timing for the movie playback The Gray Movie button suppresses the colours in the resulting movie ee Operations Recording Movies Saving Multiple Images e From To enter the number of the starting ending frame This field is filled automatically with the first last frame available e Save in enter t
92. abelled Tab Clicking the Tab brings it to the foreground displaying the corresponding group of interface elements PROGRESS BARS indicate progress of a long ongoing procedure over time It is often displayed in a dedicated dialogue Software Control xT microscope Server Software xT microscope Server Software Ff Service Tools T Supervisor Tools f User Tools Gh xT microscope Server fan FEIL Company X Microscope server amp xT microscope Server Server state Console devices STOPPED KO motion Imaging Ll State STOPPED x Microscope stop shutdown System Hide UI stop Ul Advanced gt gt gt xT microscope Server Server state Console devices RUNNING Y Motion Q Imaging Ul State RUNNING Y Microscope Stop Shutdown System Hide Ul Stop Ul Advanced gt gt gt Administration C Program Files fei exe Autorun Ul v lt lt lt Service tools Terminal window gt gt gt 0 BhvSessionManager Aa Unknown O BhwPersistency Stopped BhyvimageAlignments cocreated Install directory Active configuration 0 BhvColdStage Q BhvHotStage ObjectModel OMinstrument OMPositioning Omvacuum OMEBeam OMlmaging Q OMDetectors OMOnptions Q OMPatteming Q OMSenice D Active viewServer Created Connected Started initialized v Follow Active Grab Debug a Output The xT m
93. activates a preset scan see the Preferences Scanning tab The tool bar icon corresponds to the Photo function The Scan menu Pause F6 function stops the scanning at the end of the current scan so that an image can be saved To resume the scanning activate the Pause function again FILTERING FUNCTIONS The Average function improves an image by continuously averaging 2 or more frames It is especially useful for fast scans to decrease the image noise level The Integrate function adds up frames into a single averaged image This process continues until the predefined number of frames is reached and then stops and pauses automatically Operations Capturing and Handling a Single Image IMAGE TYPES A computer perceives an image as a two dimensional array of numbers bitmap Each array element is called a pixel and is represented as an integer value Frequently the pixel is represented as an unsigned 8 bit integer in the range 0 255 with O 255 corresponding to black white and shades of gray distributed over the middle values A 16 bit representation produces up to 65 536 different shades of gray it is not possible to distinguish onscreen which may be crucial for obtaining accurate data in analysis The raw scanned image is always a greyscale bitmap The colours are possible to add digitally as a result of particular features The Ul is able to display and save images with a various bit depth The Greyscale
94. afe distance to the sample surface is 1 mm Be aware that the STEM holder surface is now closer to the lens than the sample By moving off the grid bars and fine focusing most imaging corrections image rotation astigmatism can be performed in the SE Mode 5 Choose the Detectors menu STEM detector and select the segment mode depending on the sample position in the holder A transmission sample image should be visible at a low magnification e The BF image change the accelerating voltage to suit the contrast necessary through the sample For example light element materials such as silicon or silicon oxide may work better with 5 10 kV to create contrast whereas dense materials such as metals may require 10 20 kV or higher Finally set the magnification fine focus and correct the astigmatism If the aperture adjustment is needed it may be achieved more easily by momentarily switching to ETD because a faster scan speed can be used The DF image the samples that reside in the 1D and 5D positions can be observed in the dark field mode The separator line of the two diodes crosses vertically the positions of 1D and 5D An area of interest on the left right side of the line can be observed with the right hand left hand diode for DF BF observation DF observation may require higher HV to create a suitable image as the angle subtended to the detection diode can be wide Choosing 2x the value used for BF is a good guide le
95. age acquisition out de a espe CR UP e in a oet 9 43 Recommended settings 0 0 0 ccc ee ee o 9 44 symmetrical Low Vacuum Detector SLVD 9 45 IWIADOING OO eT a E we Boe ae 9 46 image Analy SiS cenre SUE Dux ee hee d 9 47 Measurement Accuracy VerificatiON o o ooooooooo 9 47 Remote Imaging FP 2415 00 ee 9 50 Connection to the Microscope PC 0 ee 9 50 Microscope PC s desktop Sharing llli 9 51 Controlling the microscope remotely o o o oooooooo ooo 9 51 Beam Deceleration FP 6842 22 es 9 52 Detection Principles 0 0 0 0 0c ee eee 9 52 Beam Deceleration Module 0 00 eee eee 9 54 Specimen Holder Kit Option FP 2301 10 9 56 Locallon POSITIONS sae isos deseos at is By Sew UR Gea Bed odds 9 56 Older Interface Adapter 0 0 0c ee ee 9 57 Interface DIIGE ca cite m e d Nica Gh Ake ani apa etna 9 57 MulER oO der 5h casemate o See TIS D 1 disco dd a 9 58 Polished Mount Holders o o ooooooooronoo eens 9 59 Clamp UDS rar epar ded RA Hee SURE 0r SCR RA dol fot aca 9 59 TORS DIVE 25 s ouem Segui cttm eM caesi oU IRI Ge a ath e URS st Ouod Bees 9 59 C vi LIST OF FIGURES q System Overview SEM Schematic Overview 0 0 cc ee eee 2 2 Quanta FEG 200 esae d o HR Redde Wea Sa eked eee awed ER 2 3 Quanta FEG Standard Layout Scheme 00 00 ee
96. aging image and movie gathering manipulation output detection and analysis stage and pressure OTHER SOFTWARE AND HARDWARE Call Customer Service for advice before installing software or hardware that is not required for system operation Other software such as screen savers or hardware network cards may corrupt the xT microscope Server Control software under some circumstances and may invalidate warranty For more detailed information about Windows XP refer to the Microsoft Windows User s Guide shipped with your system Software Control Software Interface Elements Software Interface Elements 32 e e ES Mlicr os cope v Live Average 4 frames Integrate 1 frame A a r Select Filter Mode zm Edit Detectors Open Save Ctri 5 Save As scan E Record Movie Import Export Print Ctrl F Log Off Factory Exit sa Help Shift F5 Shift F6 w Center Cross Alignment Rectangle COD 10 mm Marker Crosshair Cursor Redo digital zoom 2x Single Quacd Image Mode F5 E oo FJ e ICONS are small symbols indicating a specific software application Double click the icon to activate the program There are also functional icons in the tool bar for selecting some software functions quickly Clicking causes it to press in and activate clicking it again or clicking another one depending on a particular case causes it to spring out and deactivate Some functional ic
97. al one Software Control Software Interface Elements Contrast source 1 3396 gBi g mM MN J ADJUSTERS allow to change parameters such as contrast brightness gamma etc in a continuous way by clicking and dragging the middle adjuster or clicking in the grey bar They always have a label in the upper left and right corners for readout information Double click the value in the upper right corner enables to enter a precise value and the unit in particular cases using the keyboard Continuous Adjuster The large adjuster for relative adjustments It has exponential response the further from the center the adjuster button is pulled the larger is the relative change The adjuster button always snaps back to the center of the slider The slider grey bar for larger adjustments The end arrows for finer adjustments single step increments The small adjuster for linear adjustment continuous response The adjuster button position always corresponds to the actual parameter value within an available range Linear Continuous Adjuster This is a linear response adjuster Behaviour is the same as for the Small adjuster see above Preset Continuous Adjuster is used for values that have both a continuous range a list of presets and direct value editing to achieve total control over one function The button on the left side of the adjuster toggles between modes e Drop down list clicking th
98. am Deceleration are BSE ones placed closely under or directly inside the column Their efficiency depends on their active area the smaller the active area inner diameter the better The standard ETD could also be used but its efficiency is low mo System Options Beam Deceleration FP 6842 22 Beam Deceleration Applications The BDM enables detection of the BSE when the landing energy is under the detection limit of the detector The BDM expands the Landing Energy range under the minimum HV limit 200 V for the standard Quanta microscope Besides it enables a smooth landing energy change with the 10 V precision The BDM improves the microscope resolution at low accelerating voltages A conventional microscope resolution is limited by a chromatic aberration at low electron energies The higher is the Immersion Ratio the smaller are the aberrations and a loss of resolution at low landing energies is well compensated The BDM enables to detect electrons heading nearly parallel to a surface which accentuates a surface roughness Application Restrictions In the LoVac mode the chamber environment is rather electrically conductive so it is not possible to raise the BDV it is disabled by a safety interlock and the BDM is not available The sample tilt causes an electrical field deformation which adds not correctable aberrations a chromatic aberration and an image distortion An acceptable sample tilt is about a few degrees fo
99. ample Bias for HS 1500 connectors Also plug the water hoses FIGURE 9 26 CONNECTIONS TO THE HEATING STAGE 7 The greater spherical Chamber Interface 4 ended cable connector fits to the outside of the Chamber feed through plate on the connector labelled Heating stage The lesser spherical connector works with the CS 8 The 25 pin connector fits to the HS Controller and the 9 pin connector to the SSB only for HS 1500 The Water Flow Box installation and Operation See description above the Cooling stage Eo o System Options Heating Stage 1000 FP 2300 02 Heating Stage 1500 FP 2300 06 Temperature Stage Control Heating Cooling Temperature Advanced Actual ale fd Target Power I 200 O Auto Power Bias Presets Power 0 0 Heat Shield Blas sample Bias SOFTWARE CONTROL The Temperature tab See description above the Cooling stage The Advanced tab The Advanced tab is displayed only when the HS is connected to the feed through plate connector The Auto Power check box is cleared the Power slider becomes active and user can apply desired power directly to the heater The functionality is useful when working at temps above 1300 C when regulation can be affected by a sample outgassing or a leakage current Caution The slider button shows 96 of maximum allowed power Apply just as many Watts as needed in order
100. an X ray is received for each energy level The higher a peak in a spectrum the more concentrated the element is in the specimen THE SUPPORT PC FP 2353 02 includes a PC a LCD monitor and a software controlled Switch Box It is required for the EDX functionality and can also hold some other software utilities FIGURE 9 5 INSPECT STANDARD LAYOUT SCHEME Microscope Microscope Support Console Controller Computer Customer s LAN Microscope Hetwork d prp eS ar ar mnes E Keyboard Mouse HIGH VACUUM HiVac operation gives the most accurate X ray results but the sample must be electrically conducting FIGURE 9 6 X RAY IMAGING IN HIVAC MODE Electron Sample g System Options Energy Dispersive X ray EDX Analysis LFD EDX ANALYSIS EDX analysis should be performed at the lowest possible gas pressure so it should be done with the LFD Normally X ray analysis is performed with a relatively high beam current so that there is enough signal for a good LFD image even at very low gas pressure The Hot Stage cone can also be used with the LFD for X ray analysis and has a field of view twice as large as the X ray PLA FIGURE 9 7 LFD CONFIGURATION FOR THE EDX ANALYSIS Electran beam EDX Detector Fay PLA Cap Minimal beam skirt with Sample close to the final PLA 357 TOR ET Sample GSED EDX ANALYSIS The ESEM mode allows observation of electrically insulating samples but care mu
101. apter 5 xTm Detector Settings Detector Settings Note Detector GSD El the GBSD or other gaseous detectors do not need to be removed to pump to HiVac at the end of a day They may be left in the place Mode Secondary Electrons However stages with water lines inside the chamber must be removed E eser SE BEE At the Detector Settings module the following options are possible El Mode list box with choices The Secondary Electrons SE mode the converter plate voltage is reversed and a second positive voltage is applied to the SE collection grid SE from the sample are collected directly and the SE image is similar to the GSED image All SE generated by BSE at the converter plate are drawn back to the converter plate The Backscatter Electrons BSE mode BSE generated by the Mode Secondary Electrons _ primary beam strike the BSE converter plate and generate SE Secondary Electrans which are accelerated repelled by a negative voltage placed on the Enhanced ceu 1 BSE converter plate A zero voltage potential is applied to the SE 1 Mix collection grid When the electrons strike a gas molecule with g System Options Optional Detectors enough energy they ionize it The two electrons are further accelerated causing more collisions The SE signal is amplified in the gas with gains up to a few thousand resulting in BSE image the MIX mode is a combination of a negative potential on the converter
102. ar button clears the existing Stage Map file including the Location list It is possible to load save stg file also with the use of File menu Import Export functions see Chapter 4 Map Menu Clicking the right mouse button while over the Map area provides the dropdown menu FIGURE 7 8 THE MAP DIALOGUE Add current stage position Update to current stage position Remove selected position Magnification 1x 2x Center view 5 4 Auto center on target 10 Zero radarview Stage ti s vl ge location overlay CO LOO Clicking the Add current stage position item adds a new Location list entry using the current active position The new entry is named Position X X 1 2 3 Ifa name already exists because the user loaded a Map list from a Stage Map file the value is heightened until a unique name is obtained The Coordinates tab Add button has the same functionality Clicking the Update to current stage position item stores the edited coordinate values under the currently selected name an overwriting confirmation dialogue appears The Coordinates tab Update button has the same functionality o otage Map Coordinates ritt Navigation Actual Go To Tx 05824 mm a m 3 7701 mm hal rz 9 9 9588 mm a rr Jw TR 00 d Compucentric Rotation Last Position 4 Add js Update Remove tt a e Qu The stage cannot move to the target position Some Press
103. ars Save Ctl S xTm Incorrect video resolution Save AS Record Movie Please select a resolution for the full frame mode that is compatible with video recording Import d Export d Resolution 512 x 422 Print Ctrl P x Log Off Factory Exit Choose either of the offered Resolution values at which the movie starts to record EFE window Help I Select the File menu Record Movie again or click the tool Auto Contrast Brightness E bar red square button to stop the movie recording User Auto Contrast Brightness Auto Focus Fil Auto Stigmator Ctri F11 FEI MOVIE CREATOR Set Default Parameters Ctri D un This is a separate program that creates a movie from a sequence of Eee heen shift F11 TIF images Click the Tools menu FEI Movie Creator to activate Lab Notes the tabbed dialogues porous The following items are common for all tabs Applets The Databar Preview displays the databar created in the Databar Preferences Colo tab Operations Recording Movies Saving Multiple Images The Status displays the progress of movie creation process The Create Movie button opens the File tab and starts the movie creation process from the TIF files to a single AVI file The Stop button stops the creation process The Close button closes the FEI Movie Creator program File Tab FIGURE 5 9 FEI MOVIE CREATOR TAB FILE Ei FEI Movie Creator File Databar Preview ECdtempl
104. ases decreases the magnification Ctrl Wheel Coarse Control moving the wheel Up Down increases decreases the magnification Ctrl An electron image quad with the wheel pressed Wheel Press like a button the TRACK mode for joystick like movement over the sample surface is activated Optical quad activates the stage Z movement stage Tilt With the wheel pressed moving the mouse up or down left or right moves the stage up or down tilts the stage left or right which can be seen live Note The given sequence of key and button pressing is important for some functions Key Key Software Control Entering Commands in Summary USING THE KEYBOARD TABLE 4 4 WINDOWS SYSTEM KEYS Key Key Function Equivalent to OK in a dialogue box 1 Equivalent to the Cancel button 2 Cancels the click and drag function 3 Stops the stage motion at that point Note During some procedures Home Stage for instance use the software Cancel or Stop button Step key to highlight items in a dialogue box 1 Use to select between items in a group when in a list box 2 When image quad is active and on focus the stage moves approximately 4096 8096 of the field of view in any direction by clicking the appropriate keyboard Arrow key Alt or F10 Activates menu of the active application Pressing the underlined character in the menu bar pulls down the corresponding menu Alt Tab Use to switch between runni
105. ast Scan Ctrl Shift sons gt e brings the scanning condition to the preset Q 4 50 ns P Slow left icon Fast right icon scan value see the Preferences Scanning tab When either of the two presets are active or selected the respective icon is highlighted Slower Faster Scan Ctrl sets the scanning condition to the next preset Slower left arrow Faster right arrow value see the Preferences Scanning tab The spinner box shows the current dwell time but does not enable to change or select directly its value the values are changed one step up or down Mains Lock When ticked the scanning line or frame sawtooth signal is synchronized with the mains AC oscillation This greatly diminishes blurring and jittering of the electron image resulting in smooth image edges at higher magnifications and slow scan conditions It has no influence on fast scan images Live Bem un is the default imaging mode leaving the image unfiltered for collecting raw direct images one frame follows another Average gH continuously averages a specified number 2 or more of frames resulting in a better signal to noise ratio This process continues until stopped by changing the scanning condition or by pausing the quad This is used mostly for fast scanning to reduce image noise During averaging the image is updated continuously and actions such as focusing moving the stage etc can still be
106. ating stage is being operated with the BSED which should only be installed for temperatures up to 400 C the working distance should be kept greater than 9 mm Using the HS with EDX Detectors There are a number of variables to be taken into account then selecting operating temperatures for EDX detectors Some of these include window materials window thickness window support structure and the closeness of the window Above 400 C the sample begins to radiate infrared light and this blinds the EDX detector preventing further analysis For this reason do not perform elemental analysis above 400 C It is also advisable to retract the EDX detector fully when temperatures above 400 C are to be attempted Caution Be very careful when determining operating temperatures To avoid damaging a detector always consult the EDX manufacturer for guidelines and operating limits Once cooled swing the heat shield out of the way of the stage the optical image may be helpful to see into the chamber Raise the stage to a working distance of 12 mm the GSED is 8 mm then collect X rays as usual Inclined Crystal EDX Detectors The detector comes in at a take off angle TOA of 35 and the sample is not tilted This illustration is shown with the high temperature GSED installed FIGURE 9 30 INCLINED CRYSTAL EDX DETECTOR CONFIGURATION Electran sample Positioning the High Temperature GSED The high temperature GSED must be
107. ation helpful when calling the service The Autorun UI checkbox when ticked default the Start button automatically starts xT microscope Control after starting the Server Console devices Motion Imaging Software Control xT microscope Control Software xT microscope Control Software xT microscope Control also called User Interface Ul or xTUI is made up of several elements which compose the main window displaying status and control features FIGURE 4 2 THE MAIN WINDOW B xT microscope Control a Stop Hide Ul Stop Ul x Fie Edit Detectors Scan Beam Stage Tools Window Help 2 5 Pages 2303x zookw j0 AA DT 0 ma Al ais gt ae 102x004 e MI any 03 235 2 Es Vacuum Pump Vent Mode High Vacuum C Low Vacuum Water v ESEM Water v Chamber Pressure y 30 00 Pa Column es Spot xTm Preferences a High Voltage Databar Units Presets Scanning ESEM General Movie Sensitivity 20 00 kV Detectors Units of Measure millimeter mm Contrast 0 0 ET El p Pressure Pascal Pa e Brightness 50 0 Temperature Kelvin K a m gt 30 um J normal mode Magnification 2303 x E El n Beam Stigmator Beam Shift Cancel Tuning Source Tilt Lens Alignment Crossover Lens Align Status Chamber Pressure 1 45e 4 Pa Gun Pressure 2 49e 7 Pa Emission Current 152 pA
108. ave and closes the dialogue It has the same effect as closing the dialogue with the cross Alt F4 e The Next button moves the user to the following dialogue after necessary settings have been done e The Previous button moves the user to the previous page when settings need to be changed LIST BOXES contain available choices such as screen resolution magnification settings etc Click the List box to roll down a list of available values then click the desired one The dropdown list automatically closes and displays the new value as the actual one The change of the setting is immediate PROPERTY EDITORS group list of related parameters and their values The editable parameters have a white background the fixed parameters are shaded The user should click in the Value side of the relevant property Name and then select its value from the drop down list or enter it using a keyboard EDIT BOXES let you input text information such as passwords labels or precise numbers using the keyboard Some edit boxes which are not part of a dialogue require to confirm the input by pressing Enter If you press Esc before leaving the edit box its previous value is restored RADIO BUTTONS CHECK BOXES Within a group of related round Radio buttons only one selection can be made active at any time by clicking in the individual box A single one or a group of square Check boxes can be ticked cleared by clicking inside the individu
109. ber change influences both the focused electron beam area and the Beam Current The lower is the Spot number the lower is the Beam Current 3 The Detectors Module contains continuous adjusters to control the active detector Contrast detector voltage and Brightness voltage offset The values are remembered for each detector and a quad The adjusters are disabled if the detector is not available or cannot be controlled e g CCD camera or an External detector The Contrast Brightness Enhance Continuous Adjusters Regardless of the detector actual gain range the Contrast and Brightness range is always 0 100 and the small large step size is 0 1 1 the Brightness step size may differ for some detectors in order to achieve a sufficient sensitivity A direct value can be entered by double clicking the Contrast Brightness value The Enhance adjuster electronic gain is displayed here or in the Detector Settings see the Preferences General tab Note The label Enhance is truncated because of a space The full name should be the Enhanced Contrast 4 The Magnification HFW Module The continuous adjuster offers a variety of ways to control the current image magnification see above The magnification range changes dynamically according to the working distance and can also be controlled with the use of other tools see Chapter 5 The Magnification is possible to display as the Horizontal Field Width HFW alternat
110. by selecting an appropriate mode radio button nothing happens unless there is a different gas type being used for the two modes In this case the appropriate gas type is selected When Low Vacuum ESEM mode is entered from High Vacuum mode Vented status by selecting an appropriate mode radio button the system prompts the user with the Pole Piece Configuration PPC dialogue this happens only for the first time after a particular Vent procedure It is followed by a new mode initializing dialogue and then by the manual EBV open dialogue Pressure The Pressure adjuster is used to set and display the target chamber pressure Pascal Torr or Millibar units are available and can be selected in Preferences Units see Chapter 4 When the system is in Low Vacuum or ESEM mode and the Chamber Pressure value is changed the pressure automatically changes to the new value When the system is in any other state and the chamber pressure value is changed the new value is used as the target pressure when the system starts pumping to a Low Vacuum or ESEM mode again The actual specimen chamber pressure is displayed in the Status module Chamber Pressure field Pressure Limiting Aperture PLA and Cones The maximum allowed specimen chamber pressure in LoVac or ESEM mode is determined by the size of the PLA and a gas type The PPC dialogue prompts to inform the system about the used PLA in case it is not a part of a dedicated gaseous det
111. calculation can be found in the Morphologi user manual In case of issues with Morphologi SW contact Malvern Instruments service centre phone 44 1684 891800 6 30 to 18 00 UK time during weekdays email Helodesk malvern com MEASUREMENT ACCURACY VERIFICATION Use the 300 nm and 1 um polystyrene latex spheres standards to verify the accuracy of the calculation Both standards are located in the ITO slide test sample kit Use Mapping tool and save appropriate number of images to have at least 80 spheres calculated for both the 300 nm and 1 um standard Contrast and brightness of images should be like in the following examples FIGURE 9 42 IMAGES OF 300 nm and 1 um SPHERES Load images to Morphologi and set Image Processing to discriminate spheres from background Check and tune settings in several pictures System Options mage Analysis SEM File Analysis 300test vsemsop Qu OLD Ala HITA FIGURE 9 43 IMAGE PROCESSING OF STANDARD SPHERES IMAGES SEM File Analysis Qu ODAH ALR gt Image fies Image Processing Sample detais Image Processing Background separation Source view 9096 Analysis settings Fiters Classfication Fusco Original image Import Script Image 300nm Q1 operl measurl CB 1 v standard dev Image Processing Parameters 1 Edge Detection 2 Smoothing 3 False Pixel Removal 4 Gap Closing s pni Threshold 82 Set the Analysis Settings and Filters accordin
112. centred since it shows a relative position against the last saved coordinates Then repeat the procedure when necessary Note When adjusting the 1000 um aperture available on every strip for the service reasons just try to find the maximal illumination do not use the Modulator E ooo 0 System Options Optional Detectors Optional Detectors GASEOUS BACK SCATTERED ELECTRON DETECTOR FP 2303 00 The GBSD is used in place of the standard Gaseous SE GSED ubl lt 2n Beam detector and Large Field Detector LFD It was specifically designed v ETD SE to image at pressures above 4 Torr 534 Pa predominantly in the range of 6 to 9 Torr 800 to 1200 Pa This makes the GBSD best GAD 4 suited for use with the Peltier when both secondary and back scattered images are required PMD BSE This detector is integrated into a flexible PC board and plugs into the External signal connector behind the conical lens CCO FIGURE 9 3 GBSD OPERATIONAL SCHEMA Detector Settings AAA AA Ea E ee L SS tos CONYERTER o II aaa a a PCTS eee eee Bess GLA BURIED SIGNAL TRACK CONVERTED SE GAS CASCADE IN THE 5645 The grid on the bottom of the GBSD board is used to collect all SE signals from the gas This grid the surface of the board around the grid and the PLA1 are connected to high voltages up to 600 V during ESEM operation Installing and Settings the GBSD Follow the same procedure as described for GSED see Ch
113. cope operation Lower stage when venting the chamber Change magnification when pumping Switch of CCD automatically Fause E Beam quads when switching aff H Allow Beam Shift in Get mode Blank beam during long stage moves a Lower stage when venting the chamber Yes No Specifies if the stage should automatically go to a low Z values when venting the chamber This is a recommended not default setting because it greatly diminishes the chance of hitting the pole piece when closing the chamber doors after mounting a higher specimen Change magnification when pumping No Set to 25x Set to 100x Set to 200x opecifies if the magnification should be automatically set to a low value when the chamber is being pumped presumably after replacing the specimen Software Control xT microscope Control Software Switch off CCD automatically No 1 minute 10 minutes 30 minutes 1 hour 2 hours 6 hours opecifies if and when the CCD camera and infrared LEDs should be automatically switched off The countdown starts when resuming the optical quad and continues regardless of the operator activity Pause E Beam quads when switching off HV Yes No Specifies if the electron image quads should be automatically paused when switching off the High Voltage Allow Beam Shift in Get mode Yes No Enables disables automatic using of Beam Shift when the user requires very small point to point movements double click in t
114. cted area The cursor changes to a 2 ended arrow either horizontal or vertical A corner can also be used to move two sides Now drag the side out or in to obtain the desired size and release the mouse button When the Reduced area frame is being manipulated it turns yellow until released then it reverts to green Full Frame Ctrl M is the default scanning mode typical for navigation and imaging Spot In this mode the image pauses and the scanning is switched off The current beam position is represented by a green cross in all paused electron images You can move the cross or click anywhere around the screen with the left mouse button to change the position Software Control xT microscope Control Software Line In this mode the green horizontal line is displayed in all paused electron images The beam scans along this line You can move it or click anywhere around the screen with the left mouse button to change its position External switches to activate external control of the scanning system such as beam control from an EDX system The external scanning mode is indicated by the External label displayed in the upper right corner of all imaging quads Beam Blank Ctrl B e deflects the beam off axis high in the column and protects the specimen from unnecessary exposure When the beam is blanked the tool bar icon is highlighted Clicking it releases the blanker and returns the beam to scan the specimen Slow F
115. ction or blowing with clean gaseous nitrogen SPECIMEN HOLDERS Recommended cleaning procedures are given below for parts which operate in vacuum and which are subject to possible contamination Frequency of cleaning is in most cases determined by necessity image quality or astigmatism level Cleaning 1 Clean these parts using a lint free cloth and a mild abrasive domestic cleaner see above 2 Rinse in tap water 3 Clean in an ultrasonic cleaner for 5 minutes using distilled water 4 Clean in an ultrasonic cleaner for 5 minutes using alcohol p a or isopropanol Caution Do not place parts together in the beakers Wash separately as damage can occur to the metal surfaces 5 Rinse in alcohol p a 6 First blow dry with a compressed air canister then dry thoroughly under an infra red lamp 15 min to 1 hr at a temperature of between 80 C and 100 C Do not bake in an oven Maintenance and Troubleshooting Refilling the Water Bottle Refilling the Water Bottle The water bottle in the instrument typically needs to be filled about once a month if the instrument is used on a regular basis at a high pressure The water reservoir is located in the rear of the column console beneath the frame To fill the bottle do the following Vent the system Turn off any gas connected to the gas inlet Disconnect the quick coupler and pull out the water bottle Remove the rubber plug and refill with distilled water
116. curate reading Use carbon paint or carbon tape to hold samples onto the holder Better contact between the sample and the holder yields better heat transfer Pressure and Temperature control It is better to control the condensation by a pressure control as opposed to temperature control Firstly the thermoelectric module heat pumping capability is very small therefore a temperature is hard to control accurately Secondly it is easier to keep the pressure below the condensation point which prevents water condensate from raising the sample temperature cooling water takes longer time to reach the setpoint As a general rule condensation is achieved by the following procedure 1 Set the pressure to 540 Pa 4 0 Torr 2 Bring the sample to 5 C 3 Raise the pressure until water condenses on the sample Keep the pressure below the condensation point 860 Pa 6 5 Torr Keeping the sample wet Water in the sample tends to evaporate during the pump down cycle The simplest way to keep the sample wet is to accurately control sample temperature and pressure conditions Another method is to cool mounted sample to its operating temperature before it is put into the chamber Then add several drops of water to the stage base this displaces air faster during pump down There is an indentation on each corner of the base for this purpose FIGURE 9 17 ADDING WATER TO COOLING STAGE BASE ADD WATER DROPS HERE IM THE 4 INDENTATIONS Once th
117. d or by the 25 mm internal sample holder setting This allows to load large or differently sized specimens by reducing the internal Z FIGURE 7 1 QUANTA FEG 200 STAGE 4 AXES MOTORISED Legend A Negative end stop 1 Tilt lever B 30 stop 2 Tilt monitor C 45 stop 3 X axis D 75 stop 4 Rotation E Tilt scale 5 Z axis F Stage lock 6 Y axis G Stage ground Quanta FEG 200 Standard Sample holder The single stub holder and the multiple holder are provided with the Quanta FEG 200 The single holder has a spring clip fitting and a secure fitting screw The multiple holder is a 7 stub holding disc with a spring clip fitting only FIGURE 7 2 QUANTA FEG 200 STANDARD SAMPLE HOLDERS Both holders have the same threaded shaft which screws into the stage rotation head center and can be securely attached to the stage by means of the conical locking piece B 0 0 1 Stages Stages Types and Accessories QUANTA FEG 400 600 100 150 mm STAGE The stage has the X Y Z Rotation and Tilt movements motorised all with a manual override All movements are read out on the screen under the software control FIGURE 7 3 QUANTA FEG 400 600 STAGE CONTROLS Tilt 1 Od a Rotation e a E SN y Y axis a y X axis e A Stage ground j and Interface connector EL Quanta 400 600 Standard Sample Holders The single stub holder is provided with the Quanta 400
118. d Brightness when necessary Bring a recognizable feature under the center cross by the stage movement ido not use the Beam Shift Instructions step 1 of 3 stage Position X 46 0504 mm Y 49 7214 mm Contrast 5 ml Bl B fp Brightness 53 8 mg B Cancel The stage rotation has a mechanical center and it can be controlled by changing the Stage module Coordinates tab R value This moves the stage around its mechanical center In some circumstances this is not desired because a rotation around the field of view center would be more useful The following correction is the alignment procedure for the Compucentric Rotation function The X Y offset is calculated so that the Compucentric Rotation is correct from that point on 1 The magnification should be from 500x to 2000x and the sample should have a recognizable feature close to the center of the stub which is mounted in the stage center Make sure the tilt is zero 2 The stage automatically rotates the view 180 Alignments Alignments 3 Stage Rotation Center 3 Stage Rotation Center Previous Next Previous Instructions Instructions Wait until the stage movement Wait until the stage movement is finished Bring the is finished recognizable feature back under the center cross by the stage movement do not use the Beam Shift step 2 of 3 step 3 of 3 stage Position A 43 5374 mm Y 48 1198 mm Contrast ey Tl Ki B B
119. d acting as the additional electrostatic lens Its power is described by the Immersion Ratio IR e HV LE parameter determining how many times the Electrostat primary electron energy e HV is lowered when reaching the sample T surface with the Landing Energy LE e HV BDV Beam Deceleration Voltage specimen D ET E CT O N P R N C P L E S The Beam Deceleration influences both primary and signal electrons Final Lens BSED e As the sample is at the negative potential according to the ground and detectors the SE and BSE are accelerated before the detection When reaching the detector initial electron energy when leaving the surface is intensified by the BDV potential SE BSE are detected with approximately e BDV e HV energy The higher is the IR the lower is the difference between SE and BSE energies e Signal electrons are accelerated upwards and deflected towards the column axis The SE have a low initial soeed and they are usually absorbed into the detector central hole equally like the BSE heading upright Conversely the BSE heading nearly parallel to a surface which normally cannot be detected are driven to a detector By changing the Immersion Ratio an output angle distribution of electrons leaving a surface could be obtained FIGURE 9 46 TYPICAL TRAJECTORIES OF SECONDARY RED AND BACK SCATTERED GREEN ELECTRONS M bL detector specimen Detectors most convenient for the Be
120. d Control Elements 0 0 000 eee eee eee Final Lens Aperture Strip Alignment 1 GUN ANGQNMEN vri a IEEE SUE Rede eee Rd eee 2 Stigmator Alignment oococococcco 3 Stage Rotation Centre i uz IRI XL ERES EXE 9 Emilter Startup cuire IE Chapter 7 Stages Stages Types and Accessories LL Quanta FEG 200 50 mm Slade i ca dicare doe Ea aae caes Quanta FEG 400 600 100 150 mm Stage EUcCOBIIe ROSIE OM rra o hr a eee ara Navigallob Jab aue as Sede oot ea ais be las Be Stage Related Functi0NS 0cccococcccc Sage MOVelneliss s og hut eo eri Pb RES Skee ae IS Specimen Alignment 2 0 2 0 0000 cc ee eee scan ROLUN Colt s 8 y 9 d ID og abc eb te icto n Sox De oz Chapter 8 Maintenance and Troubleshooting Cleaning Procedures Overview 0 ooococcocco List or Applied Cleaners iso oe Rer uEPP Id ERES Cleaning Column PartS 0 00 0 cc cee eee eens Materials and Technique 0 00 c eee eee eee The Standard MSE i vu exon sede SD RE Heri a eral Removing and Disassembling 0 00 cece eee Housing Cleaning 0 0 cee eee ee ene Platinum Apertures Cleaning llle Platinum Apertures Installing o o o oooooooooo Aperture Strip Module 3 err maxuma Removing the Aperture rod llle Cleaning the Aperture Module 0 0 00 cee eee Replacing the Aperture
121. d corresponding live images In other case the upper right corner red icon indicates no functionality in the respective quad EE M M M g Stages Stage Related Functions Specimen Holder Wizard This function creates a loaded multiple holder image in the Stage Sample Navigation i module Map area Navigation Montage Common dialogue buttons Specimen Holder Vizard P e Finalize ends the procedure The Procedure 1 Set the stage tilt to 0 Click the Stage menu Specimen Holder Wizard The Prerequisites dialogue appears Follow the instructions and proceed xIm Specimen Holder Wizard Prerequisites Important Please focus and link to FWD Be aware that 4th quad will be used for getting data from IR camera 2 The Holder Type dialogue appears Choose the one in use by selecting the appropriate radio button xTm Specimen Holder Wizard Holder Type E select Type of Holder m select Type of Holder fe Stub Holder bs i Stub Holder 16 Stub Holder optional e 16 Stub Holder optional Previaus Previous Cancel 3 The Stage Position dialogue needs a confirmation to activate the Set button The stage motion could be interrupted by clicking the Stop button at any time The manual tilt stages dialogue asks to set the stage tilt to the required position depending on the stage and holder types xIm Specimen Holder Wizard Stage Position ES xTm Specimen Holder Wi
122. d for the given mode HiVac LoVac ESEM All valve and pump operations are fully automatic FIGURE 3 1 THE QUANTA FEG VACUUM SYSTEM Auxiliary Bypass Valve for Quanta FEG 600 only Auxiliary Gas Valve By Pass Valve BaraTron Gauge Cold Cathode Gauge Column Isolation Valve Environmental Backing Valve Chamber Evacuation Valve Chamber Isolation Valve lon Getter Pump Needle Valve Control Pre Vacuum Pump Servo Isolation Valve Turbo Molecular Pump Turbo Venting Valve Venting Valve Water Bottle Valve System Operation Vacuum Statuses Vacuum Statuses Vacuum Pump went Mode High acuurn e Low Vacuum Water ESEM Water Chamber Pressure ely als Status Chamber Pressure 1 458 4 Pa Gun Pressure bie Pa Emission Current 152 UA A xTm Vacuum message Are you sure you wantto continue Please confirm specimen chamber vent Venting will take approximately 1 minute The vacuum status controls are in the Vacuum module The Pump button starts pumping for the operating pressure and the Vent button starts venting for a sample or detector exchange In the Status module at the bottom of any page the actual vacuum status is represented by the coloured icon which may have three possible colours with the following meaning e Green PUMPED to the desired vacuum mode Orange TRANSITION between two vacuum modes pumping venting pur
123. dures Stigmator Alignment ilable for th t IU S S 3 Stage Rotation Center available for the current user level User Supervisor or Service 5 Emitter Startup The Instructions info box displays the selected alignment procedure instructions e The Steps module shows an actual alignment page with all necessary components Note The user must understand the procedures at the appropriate level before proceeding with any adjustment Improper alignments can make the system difficult to use Software Control xT microscope Control Software PREFERENCES DIALOGUE This dialogue can be opened by selecting Preferences Ctrl O from the pull down menus Scan Stage and Tools The opened menu from which it is chosen dictates the tab opened on entry Once the Preferences dialogue is opened any of the tabs can be chosen The Preferences dialogue consists of tabbed sections Clicking the required tab opens a section that allows changing and presetting conditions for a group of the related functions Only one tab can be opened at any time The items chosen and changed from any of the preferences tab dialogues remain valid for a specific user until changed next time The Units Tab allows the user to change the Units of Measure Pressure and Temperature The choices affect the Stage module input boxes the databar display the status module and so on FIGURE 4 13 UNITS PREFERENCES xIm Preferences Databar U
124. e buttons on the right of the drop down menu steps through the pre set values Up Down in the list but only shows one value in the text area Clicking the down arrow rolls down the whole list of values If the list extends further than is visible a scroll bar appears Clicking a value in the list enters it as a current value in the text area displayed at the top Double clicking a value in the text area enables to edit it Adjuster mechanism The adjuster has a fine control see above opinner allows to change a parameter in an incremental way from a list of pre defined values by clicking on an arrow The arrows direction left right or up down can be changed in Preferences General tab e Coarse T ero mes Back Reset T E Beam atigmator Beam Shit TT xTm Stage information The stage cannot be moved the Home Stage procedure must be completed first Do you wantto run it now v Home Stage with the rotation axis Yes No otage The Auto Focus procedure is running Software Control Software Interface Elements 2D CONTROLS are represented by an X Y box The position of the crosshair corresponds to the actual parameter value with respect to its full range being represented by the perimeter of the box Click and hold down the crosshair with the left mouse button to display a 4 axis arrow cursor in the image area which can be moved in four directions that correspond to the X Y screen val
125. e 7 6 Map Area Elements 0 0 00 cece eee eee eens 7 7 xT Align Feature Procedure llle 7 14 User Units Defining Procedure 2 0 ce es 7 16 Alignment Type Differences llle 7 17 Maintenance and Troubleshooting Household Cleaners n aaan aaan 8 2 Possible Problems and Corrective Actions llli 8 13 C xI system Options STEM Holder Positions 0 0 0 0 0 0 ccc eee 9 7 Cooling Stage Consumable Parts 0 0 cee eee 9 17 HS 1000 1500 Consumable Parts 0 0 0 0 eee eee 9 36 Size classes recommended for particle analysis 9 43 C xii PREFACE User Manuals THE USER SAFETY MANUAL provides important information required during an operation and a maintenance for a product and personal safety Be sure to read this document which is delivered as the PDF file and in the printed form also at least THE USER OPERATION MANUAL for your Scanning Electron Microscope is divided into the following chapters 1 PREFACE provides information about the manual structure 2 SYSTEM OVERVIEW gives the basics about your system capabilities 3 SYSTEM OPERATION gives the basics about the vacuum system and procedures for several system on off modes including Log On Off Standby Mode Overnight Mode Complete Shutdown and Emergency Shutdown 4 SOFTWARE CONTROL describes the interface that controls system operation giving the functio
126. e Control Imaging FP 2415 00 The SIS Scandium Image software 9432 909 92771 The SIS Scandium desktop license 9432 909 92791 The SIS Scandium webRacer 9432 909 92781 allows regular users with ID passwords provided by the supervisor to view and retrieve worldwide database data using any internet browser and any computer system PC Apple Sun The Quanta Morphologi FP 2201 73 is a method for precise determination of size and shape of submicron particles dispersed in a dilution The Basic SEM Course FP 2490 02 The Advanced Course SEM FP 2490 21 The On site Training Support FP 2490 36 The number mentioned next to a name is an ordering code Contact your FEI sales representative for more up to date information on system options EB o 0 SYSTEM OPERATION This chapter describes The Quanta FEG vacuum system Vacuum status and relevant actions Pump Vent Vacuum modes and relevant actions HiVac LoVac ESEM Quanta FEG System States Start up procedure generally Shut down procedure generally Emergency off EMO Power off System Operation Quanta FEG Vacuum System Quanta FEG Vacuum System There are three main vacuum sections e Gun e Column e Specimen Chamber Both Column and Specimen Chamber sections are vented for a sample exchange In operation the Gun and Column sections are always under the high vacuum The Specimen chamber is at the pressure require
127. e e eee 2 4 System Control Panel Power Button 0 0 00 0c 2 5 Hardware Stage 200 400 600 Controls ooooooo o 2 5 Final Lens Aperture Strip Control Knob ooooccoccococooo o 2 6 System Operation The Quanta FEG Vacuum system 2 2 0 eee 3 2 EMEICNCY SWIG i d doen ene AT oad caca e o d eon t DU rp ud dt dea 3 9 ooftware Control xT microscope Server window 00 cc ees 4 6 THE Mali VVIBIO OW aca ug omen o bo e ERG Unas Re PS oe eis 4 7 ST MV ME Bac A eet ee Go a oe le hoe ahh EA 4 8 TREVISO acts o ecm iene du Ae atia Uso d 4 8 Save As Dialogue 1 ee eee ene 4 9 File Import Export Menu xa 39e tide ale a a A rper een eee 4 9 Application Status xe p mon aa ere ER rr Se ert d ee E E 4 17 DOCUMENTATION 444 4024 bd d deo dee ee o ped db deed 4 18 Me TOOL eos pin ero diosa HU ato RR kee inte a eee 4 19 The Data Ba EXaMpleS 2 995 0d da arra Ea vr a ac S D Tec RES 4 20 The Stage Module o o oooococoncooa ee 4 25 The Enhanced Image Module llle 4 26 Units Preferences erid corar itsin DEEE rns 4 27 Databar Preferences 0s ev td id daa PE 4 28 Presets Preferences llle 4 29 Scanning Prelerenices o torcida od reb P Und E ES en 4 30 ESEM Preferences llle 4 31 General Preferences llle 4 32 Sensitivity Preferences ee eee eee 4 34 FEI Account Administrators control overview 4
128. e fully in contact with the lens FIGURE 5 7 THE GSED INSTALLED IN THE SEM Signal Connector Flexible printed circuit board Mounting collar a inside pole piece __ Press fit onto housing o Operations Detector Types and Usage Removing the GSED CAUTION DO NOT change the order of the following procedure Otherwise you can damage the detector 1 Remove the detector head from the lens insert first Do this by catching a fingernail or thumbnail of the gloved hand on the FRONT of the yellow Torlon ring and pull down there is a shoulder machined into the Torlon ring which is specifically designed for this purpose 2 Pull the other end of the detector out from the connector PLA CONES In some cases it is possible to install a cone on the actual gaseous detector to achieve some special characteristic Here are the possibilities available for the user The Standard Insert is installed at all times Gaseous detector and or the PLA cone are pressed onto the insert to form a gas seal Chamber gas flowing through the detector PLA aperture is pumped out through the holes in the sides of the insert A gas restricting aperture is found at the top of the insert Note This aperture also acts as a final or objective aperture The pressure above this aperture is considered to be very low Any pollution that accumulates on this aperture greatly affects the image If astigmatism is not
129. e holder holder attached to the stage 9 42 Filter miembrahle usas ne es Beene Qd ER Ea DP ow hee Seas 9 43 Setup of contrast using videoscope and using Color tab 9 44 Symmetrical Low Vacuum Detector SLVD installed in the chamber 9 45 Images of 300 nm and 1 um spheres eee 9 47 Image Processing of standard spheres images LL 9 48 Analysis Settings and Size Bands 0 0 0 eee 9 48 Filter settings 300 nm and 1 um spheres llus 9 49 Typical trajectories of secondary red and back scattered green electrons lll 9 52 Signal Distortion and Image Aberrations for Tilted and Rough Sample Tin balls at high Immersion Ratio o ooooooooooo 9 53 Specimen Holder Kit Option llle 9 56 QUANTA 400 Location Positions 0 0 cece 9 57 Older Interface Adapter llle 9 57 Interface Pillar for Multi Holders llle 9 58 The MultisHolders coco weed Ded ii AES 9 58 Polished Mount Holders Clamp Stubs o o oooooooooooo 9 59 C ix LIST OF TABLES q System Overview Aperture Sizes and their Use 0 0 2 0 0 0 cc ees 2 6 system Operation Maximal Chamber Pressure Pa Torr under Different Gaseous Environment 00000 c eee eee eee 3 5 Startup Procedure Generally 0 00 0 eee 3 7 Shut down Procedure Generally 0 00
130. e image area in any direction When the limit of the beam shift has been reached either the Stage button IB button menu Auto Beam Shift Zero or the Beam Shift Reset function needs to be applied see Chapter 4 In this case the beam shift is reset and the observed point position is adapted by the stage wheel up T movement wheel down Releasing the mouse button stops the action wheel press Clamp This feature prevents stage vibrations and drifts at high magnifications While the stage is clamped any Z and Tilt movement requirement automatically unclamps from that point on This feature is dedicated to all stages except the 50 mm stage which has no Clamp but has a Tilt lock instead Zo Tool Window Help xT Align Feature Compucentic Rotation Fiz Define User Units Beam Shift Reset Zero Beam Shift Home Stage Shift F3 Home Stage Without Rotation Center Position Ctri o e Touch Alarm Enabled Sample Navigation Navigation Montage Specimen Holder Wizard Preferences Colo Stages Stage Related Functions Compucentric Rotation F12 Clicking the Stage menu Compucentric Rotation places a green circle in the image window The green triangle on its perimeter denotes by its position the sample rotation relative to its original position when mounted on the stage Initially this is in the 12 o clock position Drag it with the left mouse button around the circle to choose a new samp
131. e noted The platinum apertures must be installed so that the polished side faces up or towards the electron beam source E Maintenance and Troubleshooting Aperture Strip Module Installing the c clip into the insert is done using both the aperture tool and the injector plunger tool Use tweezers to insert the c clip into the injector tool then use the injector tool to install the c clip into the aperture insert e o put on the o ring push it onto and over the top of the insert making sure not to roll or deform it in any way Aperture Strip Module The objective apertures are holed on a Molybdenum strip which is mounted on a metal holder The strip has 5 aperture positions and 1 mm alignment hole in the frame The strip comes aligned in a metal module which is connected to the end of the Aperture rod by a screw The module is considered as a consumable and therefore would be normally replaced when heavily contaminated If a Fischione plasma cleaner is available aperture module can be cleaned while connected to the Aperture rod There is a heater in the rod to assist cleaning anti contamination All screws are made of Titanium not to have any magnetic effect FIGURE 8 5 APERTURE STRIP MODULE REMOVING THE APERTURE ROD 1 With the high voltage off vent the specimen chamber 2 If connected remove the heater cable from the outer end of the rod 3 Unscrew the end of the Aperture rod and carefully remove it from
132. e system enters Wet mode and the chamber pressure has reached the setpoint value the chamber automatically Purges It repeats this process 5 times Wait until the pressure returns to the setpoint Condensation and the Detector When imaging with the GSED water droplets on the sample appear darker than the surrounding features When imaging with the BSED however water appears lighter than the surroundings One exception E System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 to this occurs when imaging an oil water emulsion in which case the oil always appears darker than water CAUTION When using shorter working distances water from the sample can splash onto the GSED To avoid this start with a longer working distance until the sample has equilibrated then move to a shorter working distance to optimize the image With the waterless CS the tilt angle is restricted to 20 when using BSED or GAD detectors due to the cooling braids Using bulk samples For more accurate temperature readings bulk samples should be placed as flat as possible on the holder The further away from the holder surface the sample is the less accurate the temperature reading is Another way to ensure accuracy with bulk samples is to maintain the temperature of the sample for about 5 minutes before condensing This equilibrates the sample so that the temperature is the same throughout High magnification imaging A
133. eam loss with sample sample clase to the detector STEM EDX ANALYSIS Set the sample surface to 10 mm WD Select the area of interest in the STEM mode and perform X ray analysis mapping or line scans as appropriate Because the samples are not bulk in nature the beam spread normally associated with SEM samples is greatly reduced and therefore higher spatial resolution can be obtained with the STEM detector This also provides less background in the spectrum and allows better separation of peaks as well as more accurate lower count rate mapping The high voltage chosen for the analysis still depends mainly on the composition of the sample System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 The Cooling stage CS is used to control the sample temperature 20 C around the ambient uppermost from 25 C to 55 C and to observe it with the use of FEI electron microscope In conjunction with a specimen chamber water vapour pressure it can be used to create a water condensation on the sample surface to keep it wet WARNING A Opening the microscope chamber does not switch off the cooling When operating the Cooling stage please be aware that neighbouring surfaces can become cold COOLING STAGE PARTS The Cooling stage assembly e The Chamber feed through plate The Cooling stage controller and cables The Water chiller
134. ected Items in the Available list can be added removed individually gt lt or as a whole gt gt lt lt to from the Selected list The Selected list contains items that are displayed in the Databar The items in the Selected list can be Moved Up Moved Down Top or Bottom according to priority or preference This in turn changes the order of the displayed items in the databar The Label and Micronbar can be chosen by ticking an appropriate check box Their area expands or contracts as other items are added to or removed from the databar The Micronbar scales to the magnification Clicking the Label button brings up a dialogue to edit the label of any quad s The same dialogue can be opened by double clicking the actual label in any quad Clicking the Add Bitmap button opens a dialogue to load a bitmap into the databar Note The limit for entries is displayed in the dialogue as it is updated It is possible to select more items than can be displayed The databar preview should be used to check available space E Software Control xT microscope Control Software The Presets Tab allows the user to change the pre set values in the High Voltage Magnification and Pressure drop down lists A value can be changed by selecting it in the list and entering a new one in the edit box just below the respective title The new value replaces the selected one and is immediately sorted into the list The number of entries i
135. ection HS 1500 contains MgO crucibles with Pt wire in its centre and Pt paint on top and bottom The Pt wire leeds heat from the crucible bottom to its top sample thus the wire and its surrounding has slightly higher temperature compare with the rest of the crucible Both Heating stages have the same heater design which is intended to minimize a sample temperature discrepancies The heater is essentially a micro furnace which provides heating from the bottom and from the sides To obtain accurate heat conduction through the sample it should be cemented or otherwise firmly mounted onto the crucible with a good thermal contact Use conductive carbon paint for temperatures below 900 C and a high temperature adhesive for temperatures above 900 C FIGURE 9 29 TEMPERATURE AND CONDUCTIVITY Heat shield Heat loss sample Heater Thermocouple Crucible MgO TY TTYTTYYTYTY Y Y Y 3 TY TX X 0000 16 B X LOIODX 266886 a 1 System Options Heating Stage 1000 FP 2300 02 Heating Stage 1500 C FP 2300 06 Outgassing Samples oome types of samples may contain compounds which evaporates under high temperatures This does not affect the pressure in the chamber However if large quantities of compounds are given off they may condense and get on the aperture inside of the GSED assembly PLA and then astigmatism could result If this happens the detector must be cleaned Using HS with BSED If the 1000 C he
136. ector mounted Software Control xT microscope Control Software Column ESS spot semon efe 40 s High voltage efe maw e Detectors Contrast 38 4 E gt Brightness 50 0 E El E Detectors Contrast 00 Enhance 20 0 Bm m um ME g a Brightness 45 6 EN i E Magnification 10511 x RI ni T Horizontal Field idth 12 7 mim EJ E pi J Beam stigmator Beam Shift TT 2 The Column Module contains controls for setting the electron beam conditions The Beam On Button switches the accelerating voltage on off When activated deactivated the button changes from gray to yellow yellow to grey The High Voltage Preset Continuous Adjuster enables to adjust the overall electron beam acceleration voltage from 200 V to 30 kV in 100 V steps either continuously or using the pre set values see the Preferences Presets tab The current High Voltage value is displayed in the text area of the adjuster tool bar and in the Databar if selected The Spot Preset Continuous Adjuster enables to adjust the electron beam Spot size numbered from 1 to 7 values from 3 9 to 4 0 are disabled in the selectable accuracy steps see the Preferences General tab The current spot size number from the factory preset list is displayed in the text area of the adjuster tool bar default and in the Databar if selected The Spot num
137. ector when pumping or switching to LoVac or ESEM mode Along with a gas type this information sets pressure limits and rates for pressure changes The PPC dialogue enables to select a PLA of any currently mounted System Operation Vacuum Modes detector the other ones are greyed out or a separate cone see Chapter 5 Selecting a detector informs the system that the respective PLA is mounted on the objective pole piece and after OK is clicked the PLA size is known and the system starts pumping to the LoVac or ESEM mode From that point on this information is automatically used until the system is vented again In this case the vacuum system sets the PLA to unknown because the PLA can only be changed when the system is in Vented status Clicking the Cancel button leaves the system in its current status mode HiVac or Vent Using Gas ESEM and Low Vacuum modes allow the user to image samples in a gaseous atmosphere which can be selected in the drop down list box the Water vapour from a built in water reservoir located in the back part of the microscope console Note On occasion the water reservoir needs to be filled see Chapter 8 e the gaseous environment supplied by the user via the Auxiliary gas inlet placed on the back of the console Caution Maximum overpressure for Auxiliary gas and Nitrogen inlets is 10 kPa 0 1 atm The Nitrogen inlet is used only for venting the chamber with air or the nitrogen preferably W
138. educe the contrast to zero and adjust the brightness level to the lower dashed line black Increase the contrast so that the signal level just clips the upper dashed line white ui If necessary adjust the brightness level once more so that Enhanced Image LUT Mix 3 Mix 4 Color the average signal level is roughly in the middle O Contrast 1 2 D Bright 0 00 Hm m um m n ES 08 Enhanced Image module can be used to adjust the LUT including El gt Gamma control This can be useful for low signal conditions or odd imaging requirements Results affect the videoscope display The high and low peaks should just clip the dashed lines Operations Optimising an Image Note o 0 Use also the following functions to optimize the Contrast Br 1 see Chapter 4 Auto Contrast Brightness F9 User Auto Contrast Brightness Display Saturation Shift F11 FOCUSING Find a feature of interest with distinct edges on a specimen Use a combination of contrast brightness and magnification adjustments to maximize the image quality TABLE 5 9 FOCUSING PROCEDURE Step Action When the mouse cursor is over an imaging area hold the right mouse button pressed the mouse cursor changes to a double ended arrow Move the mouse from side to side until the image in an active quad is sharp then release the mouse button The focus function cursor is active over the whole screen without any
139. edures are given below for parts which operate in vacuum and which are subject to possible contamination LIST OF APPLIED CLEANERS De ionized or distilled water H2O Ethanol CoH5OH e Ethanol p a Pro Analysis 99 8 pure CoH5OH sopropanol Neutral pH cleaning fluid soap solution e CIF or SOFT SCRUB fine abrasive household cleaner or 0 05 uim aluminous powder TABLE 8 1 HOUSEHOLD CLEANERS Australia Finland France II Italy Japan Netherlands Switzerland USA Soft Scrub WARNING The cleaning solvents ethanol and isopropanol are highly flammable Do not use open flames and do not smoke while cleaning Ventilate the room properly CLEANING COLUMN PARTS All column parts are polished before the instrument is delivered For this reason only occasional light polishing is required to remove contamination that may build up on components in the column and specimen chamber as part of normal operation Any part that is exposed to the electron beam should be highly polished and free of contamination and or scratches that can charge and thus degrade the image Parts that can be removed by the general Supervisor User and polished include the following e GSED LFD components Maintenance and Troubleshooting Cleaning Procedures Overview Caution Gold plated parts should not be polished with abrasive MATERIALS AND TECHNIQUE To polish components place a lint free cloth on a fla
140. en holder with the use of a thermal grease Water hoses and the inner cable are connected permanently to the base The thermoelectric module is a small wafer composed of PN semiconductor layers When current passes through these elements one side of the wafer heats and the opposite one cools Reversing the polarity switches cold and hot sides This is referred to as the Peltier effect Thethermistor is placed near the sample inside of the Specimen holder a plate into which the Sample holder is inserted thus giving accurate temperature readings be SOURCE The Delrin cover keeps the entire assembly together e The cooling stage comes with different Sample holders which are used for various sample types see consumables below The Flat holder should be used for flat samples sheets powders etc It can also be used for bulk samples up to 4 mm The Dual cup holder is reversible It has a shallow cup on one side for powders tiny particles or beads A larger cup on the other side should be used for thick liquids and bulk samples between 4 mm and 8 mm he Deep cup holder should be used for all other liquids and bulk samples larger than 8 mm The Wet STEM holder could fit the sample grid for a STEM observation Note All of the sample holders have a groove cut beneath the cup bottom This allows a condensation to escape from beneath the holder so that the liquid do not force the sample holder out f
141. enabling to define them again xT Align Feature Feature Position Pl 0282 mm YS 2764 mm Align Feature fe Horizontal Eg ue Vertical Click in the active Quad to specify the second point F2 Cancel Drag any point to change its position if needed Click the Finish button to orientate the feature either Horizontal or Vertical as selected previously Click the Cancel button anytime to cancel the function xT Align Feature Feature Position Pl X 7 15703 mm YF 0 427 mm Align Feature w Horizontal p 17571 mm ES uo cage ME Aus Move points by dragging them Cancel Finish User Units Clicking the Stage menu User Units activates user defined units as the basis of the stage coordination system A tick mark appears next to the label and UU in the Stage module Coordinates tab next to the X and Y value box The stage coordinate system reverts to the last defined user unit configuration Define User Units This procedure assigns user defined points to stage points The stage coordination system can be anchored to either 1 2 or 3 points depending on the sample management or application For example if you choose a 0 0 position you can drive the stage relative to that origin using user defined units 0 1 1 0 points which may equal to some repeated sample structures etc The Define User Units Start dialogue choices are e Define New User Units see below e Redefine User Units for
142. end of the insert Be sure the parts have a safe clean place to drop onto Maintenance and Troubleshooting The Standard Insert FIGURE 8 3 REMOVING AND DISASSEMBLING THE INSERT Aperture Positioning Tool Inside polepiece Housing Universal detector Final Aperture C clip 3 Inspect the o ring at the bottom of the insert If the o ring looks deformed or damaged replace it This is a critical seal between EC1 and EC2 which is under very low pressure The surface of the o ring must be flush against the insert 4 Inspect the threads on the insert for dirt scratches on the threads etc Clean the insert threads and if damaged replace the insert HOUSING CLEANING Once the entire assembly has been removed and taken apart 1 Clean the standard insert housing with a toothbrush and Soft Scrub CIF or aluminous powder 2 Rinse with de ionized or distilled water 3 Rinse in alcohol or isopropanol and dry with clean compressed air Under normal use the insert should be inspected only when being inserted It should only be removed for cleaning when indicated by poor astigmatism PLATINUM APERTURES CLEANING e Method 1 Heat the aperture held in special tweezers with platinum points in a clean gas flame until red hot for 4 20 seconds Take care that the aperture does not melt or become stuck to the tweezers e Method 2 Connect a V shaped molybdenum foil boat about 2 cm long across the low voltage
143. enerally used for holding thin objects such as a piece of IC wafer Also can be used when adhesive is prohibited They have Hex key screws that clamp with Nylon bushes onto the object Grounding of the specimen may need to be made by another method other than just touch contact TORX DRIVERS Within the kit are two Torx drivers to complete the fitting of the interfacing parts All screws for interfacing connections are Torx All screws for clamping sample stubs are the Hex key type the appropriate Hex key tool is a standard facility ee System Options Specimen Holder kit Option FP 2301 10
144. ent procedures automatically CCD 10 mm Marker places a short horizontal line with 10 mm label in all optical quads to 2 itm help user with a sample positioning to a correct working distance and y with the first focusing Only Supervisor is allowed to change the marker position by double clicking a new position with the left mouse button and by confirming this action in the popped up dialogue Crosshair Cursor shows the cursor as a rectangular cross through the entire quad Undo Redo digital zoom tx When using the digital zoom see below it is possible to undo redo the last magnification reduction step Single Quad Image Mode F5 toggles the image display area between two possibilities e Single Image Mode displays one quad over the whole image area useful for observing details Quad Image Mode is useful for comparing images of the same sample area taken with different detectors or scan properties 1 2 3 4 selects the Active quad indicated by a tick next to the respective number In the quad Image mode quad 1 2 3 4 is displayed top left top right bottom left bottom right When in the Single Image mode the selected quad is displayed The Help Menu Alt H opens the Help menu and system informations functions elp puesumentstism F1 Documentation F1 Keyboard shortcuts The Help window shows complete User Manual in PDF format using an embedded Acrobat Reader with its useful navigatio
145. er for example ALT F for the File menu and then select from the choices with the left mouse button or with the up down left right for submenus arrow keys some often used commands can quickly be activated with the use of shortcut keys a combination of simultaneously pressed keys at any time This possibility is given by a particular button combination on the right side of the pull down menu adjacent to the appropriate command BE o Fump Went cancel m 512x442 512x442 1024x884 040x160 409665556 Color m Line Width 1 End Type None End Point Both Direction Any X 2 8037 mim T 2 6851 mim fe Automatic Custom Dynamic Focus Iw Tilt Correction g Software Control Software Interface Elements COMMAND BUTTONS carry out or cancel functions They press in when clicked and some change colour to show the corresponding function activity Command buttons have labels that describe the actions performed by clicking them The most common ones which are typically used in dialogues are e The OK button applies all changes made in the dialogue and closes it e The Finish button saves new settings ends the procedure and closes the dialogue e The Save button saves new settings at that point without closing the dialogue e The Apply button saves and applies new settings at that point without closing the dialogue The Cancel button discards all changes made from the last s
146. eraction with the specimen surface It is permanently mounted in the chamber above and to one side of Detector ETD z the sample It works in two Modes e Secondary Electrons SE Mode Custom e Backscattered Electrons BSE Detector Settings Grid Voltage E The ETD Settings The Detector Settings Mode list box enables to choose a SE BSE Default Grid Voltage mode the Grid Voltage is set to 250 V 150 V or a Custom mode for which the Grid Voltage could be set by the adjuster in a range from 240 to 260 V When the voltage is negative use a range of 25 to 150 V SE are repelled from the ETD detector and only BSE are detected The Default Grid Voltage button sets the voltage to 0 V BACKSCATTERED ELECTRONS BSED AND GASEOUS ANALYTICAL GAD optional DETECTORS These are two segment low voltage diodes The BSED is designated for a HiVac large field of view The GAD optional has a 500 um PLA cone for the Low Vacuum especially the X ray analysis The cone extends down from the unit to 8 5 mm which reduces the gas path length for electrons to an efficient 1 5 mm at the standard 10 mm analytical WD FIGURE 5 3 BSED GAD DIODE UNITS Either diode has an active area of approximately 125 mm per segment and is positioned directly above the sample to obtain maximum detector efficiency Therefore it causes some limitation in the tilt range Both detectors are connected to an SSD pre a
147. eri will be ignored The particles are stil stored and can be viewed using the partide view using the partide view Save Image Processing to the vsemsop file and run the measurement After measurement check calculated number of particles It should be 80 Then check the CE Diameter D 4 3 um Limit is within range 0 285 0 315 for 300 nm standard spheres and 0 95 1 05 for 1 um spheres Test sample kit containing ITO slides with certified standards of 300 nm and 1 um polystyrene latex spheres can be ordered as spare part System Options Remote Imaging FP 2415 00 Remote Imaging FP 2415 00 The Remote Imaging enables to connect to the Microscope PC via network using the VNC application and to control the microscope operation remotely For information how to install this functionality see nstallation Instructions available on the installation CD For more details on the remote connection and its possibilities see VNC documentation available on the installation CD CONNECTION TO THE MICROSCOPE PC Follow the steps below to connect to the Microscope PC Vm 1 Double click the VNC Viewer icon on the remote PC desktop to V cC launch the VNC Viewer application WNC Viewer 2 In the Connection Details dialogue type the computer name of 4 the Microscope PC you want to connect to followed by colon and the port number 5905 into the Server field VNC Viewer Connection Details VA Server Microscope
148. erture offers a large field of view The Centaurus Detector FP 6901 30 FP 6901 50 with back scatter tip is a retractable scintillate type BSE detector Atomic number discrimination allows a resolution better than 0 1 Z when Z 30 The Cathodoluminiscence Tip FP 6902 30 for the Centaurus Detector enables to convert it to a cathodoluminiscence detector The Beam Deceleration FP 6842 22 improves the microscope resolution at low accelerating voltages and enables to detect electrons heading nearly parallel to a surface which accentuates a surface roughness The WetSTEM detector FP 2303 04 enables in connection with the Cooling Stage to observe wet samples in a STEM mode The Photo Multiplier Tube PMT Interface FP 2310 00 The WDX Completion Kit FP 2307 02 relocates the GSED detector connector bracket and GSED pre amplifier bias feed through to another position in the SEM specimen chamber to avoid geometrical conflicts with the wavelength spectrometer The Automatic Aperture System FP 2202 00 offers the comfort of a motorized final lens strip aperture exchange The alignment procedure provides a high precision of the setting The Strip Aperture FP 6174 33 30 30 40 50 100 1000 um The Strip Aperture FP 6174 37 10 15 20 30 30 1000 um The Strip Aperture FP 6174 55 20 30 30 40 50 1000 um The set of three apertures FP 6129 00 400 um 3 mm diameter The set of two apertures FP 6104 50 1250 uim 3 mm diameter The Remot
149. es on off the grey level distribution corresponding to the active quad image display The left right side corresponds to black white original image pixels The height of the red line is proportional to the number of pixels with the corresponding gray value e The Save button saves the current setting as the custom preset he Default button restores the default values The Mix 3 Mix 4 Tab The Mix feature operates in quad 3 quad 4 and are enabled only if the Detector menu Mix is selected for a quad 3 4 It uses the processed images Average Integrate Digital Contrast Digital Brightness Digital Zoom not the raw detector signals Any combination of live and paused images can be mixed together providing all mixed images have the same pixel resolution However there are some logical limitations and behaviours e The Average and Integrate filters are disabled e Pause Resume influences the mixed image only not its sources Operations Optimising an Image The Mix quad is always paused immediately regardless of the current scanning status e The CCD image is not mixed Note In the Mix 3 tab the Source 3 controls and the Select 1 2 3 button are disabled The Presets list box enables to select the mixing ratios and colours using pre defined or custom presets e The Source 1 2 3 linear continuous adjuster tunes the mixing ratio of quad 1 2 3 images The adjuster values shape correspondingly the r
150. esulting image Changing any Source value influences the other ones automatically to reach the 10096 sum Clicking the Color control areas below each Source adjuster enables to select a colour replacing the source image black left white right one The image gray scale is linearly transformed to a new colour spectrum before it is mixed with other image s Note Colour images see below the Color tab are converted to greyscale ones before mixing The Invert check boxes inverts the corresponding source image spectrum It has the same effect as exchanging the left and right colours selection e The Select 1 2 142 43 button selects between quads 1 2 or quads 1 2 3 mixing modes e The Save button saves the current setting as the custom preset The Color Tab Enhanced Image enables to colorize a gray scale image An image already coloured LUT Mix 3 Mix 4 Color with the use of the Mix 3 Mix 4 tab cannot be coloured again the Pseudo Colors2 vr Color tab is disabled The Presets list box enables to select the colour profile using pre defined or custom presets The Colouring Control area displays the active quad image histogram and enables to create a colour profile Clicking with the right mouse button into the histogram area adds the vertical borderline with a divided triangle on top clicking with the right mouse button onto an existing one removes it Clicking with the left mouse button and dragging a borderl
151. etween is then pumped by the microscope vacuum system FIGURE 9 34 NITROGEN VESSEL AND VACUUM VESSEL WITH ACCESSORIES MR When the specimen chamber together with the CryoCleaner is pumped liquid Nitrogen is introduced to the Nitrogen vessel Its outside cold surface absorbs contaminating products from the specimen chamber The vacuum in the specimen chamber improves over a short period and contamination is now reduced Flanges The Vacuum vessel has special flange enabling to mount it to different column ports with the use of interlink with a desired shape depending on the port to be used and the vicinity a System Options CryoCleaner FP 2301 25 FIGURE 9 35 CRYOCLEANER FLANGES The interlink flanges can be mounted on by means of the 3 screw hole fittings on the perimeter of the vacuum flange Care must be taken that the O ring held in the end of the flange is secure free of dirt and is not crimped when mounting CRYOCLEANER OPERATION Once mounted the Nitrogen vessel can be placed in the Vacuum vessel Secure the two components by fixing the clips to the top of the Nitrogen vessel and locking the clips down Take care that the O ring seal on the Vacuum vessel is secure when joining the two components together Charging WARNING The handling of LN2 should be performed wearing face and hand protection in the form of a face visior and a pair of thermal protective gloves Users must not touch the
152. f it by tweezers between the heater and the crucible sample crucible Heater The Standard MgO crucible is used for thin samples and powders The Low MgO crucible is provided for tall or bulky samples it sits lower into the heater for more uniform sample heating The MgO crucibles can be used for all atmospheres The Graphite crucible are to be used only in an inert or reducing atmosphere below 900 C 1500 C Heating Stage variance 1500 C heating stage assembly has a limited lifetime and has not accurate temperature readings below 800 C Because of these reasons two 1500 C heating stage assemblies and one 1000 C heating stage assembly are supplied within the FP 2300 06 option The inner cable for each stage type is different and marked by a label HS 1000 HS 1500 Heat Shield Assembly is attached to an individual feed through plate The shield comprises multiple layers of aluminous paper supported by netting stainless steel disks is attached to the end of the Swing Arm for a large chamber it is necessary to use the extender The Swing Arm is used to move the shield away by a knob on the outside of the feed through plate FIGURE 9 23 1500 C HEAT SHIELD ASSEMBLY Small Chamber Caution When the Heat shield is installed the stage tilt is limited even if the arm is pushed away Eo o System Options Heating Stage 1000 C FP 2300 02 Heating Stage 1500 FP 2300 06 Adjusting the
153. f pixels in the image for accurate size calculation Therefore table of particle size classes that fulfill the pixel number requirements was defined Use of the size classes for the image acquisition is recommended TABLE 9 4 SIZE CLASSES RECOMMENDED FOR PARTICLE ANALYSIS HFW Min particle Max particle 300000 200000 150000 100000 75000 50000 6 009 06 30000 20000 10000 3000 1000 500 600 935 60 Images for the particle analysis must provide maximum contrast between particles and the ITO slide Contrast and brightness of any applicable detector should be adjusted in this way Videoscope F3 can be used for the best setting see peaks of light spheres on dark substrate in the following Fig 300000 200000 150000 100000 75000 50000 30000 20000 10000 3000 1000 500 Another tool that can be used for the verification of contrast brightness setting is the Processing page Enhanced image module Color tab The coloring control area displays the active quad image histogram and enables to create a color profile Peaks for both the substrate and particles are visible in the histogram when the contrast between particles and substrate is set properly Therefore substrate and particles can be easily distinguished and colorized g System Options Quanta Morphologi FP 2201 73 FIGURE 9 40 SETUP OF CONTRAST Bees VIDEOSCOPE AND U
154. f the specimen contains any volatile components such as water or oil and therefore will not withstand coating then the ESEM mode can be utilised with the correct environment gas and pressure to allow observation of the specimen in its natural state COATED SPECIMEN If the specimen is nonconductive plastic fibre polymer or other substance with an electrical resistance greater than 10 ohms the specimen can be coated with a thin conductive layer This conductive layer reduces beam instability due to sample charging and improves image quality For successful imaging rough surfaced specimens must be evenly coated from every direction Biological cloth and powder specimens may require carbon or other conductive painting on portions of the specimen that are hard to coat Coating reduces beam penetration and makes the image sharper It may mask elements of interest for X ray analysis thus the use of carbon for geological and biological specimens For more information on specific preparation techniques see Scanning Electron Microscopy and X Ray Microanalysis 2nd ed by Joseph Goldstein et al Plenum Press New York 1992 MOUNTING THE SPECIMEN TO THE HOLDER Wafers and PGA devices have individual sample mounting procedures If you are using a wafer piece or other sample attach the specimen to the specimen holder using any suitable SEM vacuum BE xTm Vacuum message A Please confirm specimen chamber vent Venting will
155. forms each cycle in succession starting with the first setpoint and going through each one until finished This feature is useful for performing dynamic experiments with specific temperatures and heating times In the temperature profile example see below there are four setpoints defined each with its own ramp and soak time The ramp Rn and soak Sn periods are pointed out System Options Heating Stage 1000 C FP 2300 02 Heating Stage 1500 C FP 2300 06 FIGURE 9 28 TEMPERATURE PROFILE Temperature Profile Soak time LI Lr f nal LLI LL LI Start When the last cycle is finished the controller holds at 600 C the last setpoint indefinitely until further action is taken Temperature Conductivity The sample crucible temperature matches the thermocouple reading The actual sample temperature however varies depending on the sample thermal conductivity and its thickness The temperature at the conductive sample surface is closer to that at the crucible as heat is more likely to spread throughout The temperature at the non conductive sample top surface is lower than that at the bottom This difference increases with a sample thickness With large samples the exposed surface area provides a great deal of heat loss through radiation therefore the exposed surface is cooler than the bottom which is in contact with the crucible Also higher chamber pressures causes more heat loss through conv
156. from the source The Coulomb Tube Current shows the electron current flowing above the final lens aperture The system conditions are displayed by means of the icons TABLE 4 2 STATUS ICON MEANING otatus Column and Chamber Vented Complete Shutdown see Chapter 3 A O Column and chamber Pumping or Venting Column and Chamber Vacuum ready for the microscope operation A Column Vacuum and Chamber Pumping or Venting Column Vacuum and Chamber Vented ready for a sample and or detector exchange Stage axes Lock any one Unlock all Displays when Dynamic Focus is On LG Displays when Scan Rotation is not zero Displays when External scanning mode is On 8 The Stage Module consists of the tabbed sections see Chapter 7 The Map tab displays the stage positions location in a visual map form and as a list for selection The Coordinates tab displays numerical values of a particular position Stage movements along selected axes could be locked The Tilt tab contains correction features for the tilted image The Navigation tab helps to navigate across the sample surface Note Eo Pri E Att iiil gt Last Position 20 20 Location Open cave Clear Ili gt 4 otage Map Coordinates Tilt Mavigatian ye ns T m A p a H Zr 1 Ne i nl bs ze Color E Line Width 1 End Type None End Point Both Direction
157. from an application point of view The following subjects are covered e Specimen Preparation and Handling e Obtaining an Image e Optimising an Image Detector types and usage e Capturing and Handling a Single Image e Recording Movies Saving Multiple Images Measurement and Annotation Functions Caution These procedures assume you are familiar with the xT microscope server and xT microscope Control software see Chapter 4 which are necessary to start and operate the microscope Operations Specimen Preparation and Handling specimen Preparation and Handling The specimen material for High Vacuum mode must be able to withstand a low pressure environment without outgassing and the bombardment by electrons It must be clean and conductive Oil and dust may contaminate the chamber environment which could hinder or even prevent evacuation to the level needed for standard SEM operation Note Always wear lint powder free clean room gloves when reaching into the specimen chamber to minimise oils dust or other contaminants left inside the chamber NEEDED ITEMS e Class 100 clean room gloves e Specimen stubs and conductive adhesive material Tools tweezers 1 5 mm hex wrench Prepared or natural specimen NATURAL SPECIMEN If no coating is desired the Low Vacuum mode can be used to stabilise the specimen for observation This mode is useful if there is a suspicion that a coating might alter the specimen I
158. fter editing of any coordinate value works as the Go To button short cut Double clicking a stored location moves the stage to the desired position immediately During the stage motion the Go To button changes to the Stop button which stops the stage immediately Coordinates X Y Z R T Edit boxes for X Y Z R and T coordinates are filled with the selected or actual position values The value changed is automatically ticked Caution e Danger of hitting the pole piece The Link Z to FWD procedure did not pass see Chapter 4 The red arrow next the Z axis alerts the positive Z axis stage moving direction is up It means raising a value in the Z axis edit box causes moving the stage up towards the pole piece e After running the Link Z to FWD procedure the symbol and the stage moving direction changes The black arrow next the Z axis indicates the positive Z axis stage moving direction is down The units of measure follow the Preferences Units setting unless the Stage menu User Units function is active in which case UU is displayed for X and Y The software locks prevent inadvertent stage movement of selected axes during particular applications The edit boxes for locked axes are disabled and the stage does not move in these directions When any or all axes are locked the Status module displays a closed lock instead of an open one By default all axes are unlocked When any axis is locked and the stage movement is required
159. functions in an opposite way as the following one The Z coordinate value represents then the distance from the Z home position stage base The dialogue warns you about the stage Z axis positive move direction Link Z to FWD Shift F9 A X A sets the Z coordinate value to the actual Free Working Distance FWD value This allows accurate movement between the sample top surface and the end of the objective lens The related tool bar icon changes according to the Z coordinate status Greyed icon the function is disabled the high voltage is switched off so there could be no electron image or all quads are paused Redquestion mark the function is enabled Z is not linked to FWD Use the function as soon as possible after properly focusing the image e Red circle the function is enabled Z is roughly linked to FWD but it needs correction It happens e g after changing the specimen focusing and linking Z to FWD at a long WD and then moving the stage to a short WD Focus image carefully at a WD around 10 mm and use this function again Green double ended arrow the function is enabled Z is properly linked to FWD Now it should be safe to change the working distance by setting a Z coordinate in the Stage module Sample Navigation toggles on off function that enables to navigate live electron images scan field towards desired places on a specimen using either paused or loaded image of that specimen usually
160. g screw on the stage body side using a metric 0 5 mm hex wrench then place the stage on and over the mounting screw 5 Tighten the mount locking screw The water hose connectors go towards the rear of the chamber Cables and Water Hoses connection 6 The loose end of the inner cable 9 pin D type connector should be installed on the corresponding connector on the feed through plate Also plug the water hoses 7 One end of the outer cable goes to the outside of the Chamber feed through plate on the connector labelled Cooling stage and the other end to the rear of the CS controller The Water Flow Box installation and operation 8 Check that the water dam is fitted into the HiVac port in the chamber bottom 9 Put the Water Flow Box between the chiller and the feed through plate The larger hose should connect from the chiller Outlet to the Flow Box input marked From Chiller The water flow path should make a loop between the chiller through the water flow box and stage then back Note It is important to keep the water chiller away from the microscope console to prevent vibrations FIGURE 9 16 CONNECTING THE WATER FLOW BOX Lee E z Signal Control cable from Stage hose fram chiller hase NH to Stage hose to Chillerhose 10 Plug the water flow box power cable but leave the power switched off The other end of this cable goes to the 24 V power supply inside the microscope conso
161. g to the following pictures FIGURE 9 44 ANALYSIS SETTINGS AND SIZE BANDS 8 size bands Image les Analysis setting Sample details e Image Processing Analysis ID Analysis settings Filters 3 00 Classification v Enable hole filing Size bands Lower size um Upper size um Bands 0 001 3 2000 1000 gt Spacing Size bands um 0 00100 0 00101 0 00103 0 00104 0 00106 0 00108 0 00109 0 00111 0 00112 0 00114 0 00116 0 00117 0 00119 0 00121 0 00123 0 00124 0 00126 0 00128 0 00130 0 00132 0 00134 0 00136 0 00138 mamma System Options mage Analysis FIGURE 9 45 FILTER SETTINGS 300 nm and 1 um SPHERES SEM File Analysis 300test vsemsop SEM File Analysis 1000test_new vsemsop Qe O15 Ald 4 Bo x Qe OF Sl wisi ox Image files Image files Filters Sample details Sample details Image Processing Image Processing Fikers Analysis settings Analysis settings Classification Classification Parameter CE Diameter ym CE Diameter ym Aspect Ratio Crcularity select Parameter perator CE Diameter ym lt CE Diameter um gt Aspect Ratio Crcularity lt select i y Use fikering to remove contaminants from the analysis i Use fikering to remove contaminants from the analysis Particles matching the fiker criteria will be ignored The particles are stil stored and can be viewed Particles matching the filter crit
162. gged accounting log is permanent file to which the previous data are sent when a new session is started This file is only readable by the FEI Supervisor User or higher level These files can only be deleted at factory or service level each one is a text CSV file so it can be loaded into Microsoft Excel for processing RH Software Control Entering Commands in Summary Entering Commands in Summary USING THE MOUSE TABLE 4 3 MOUSE BUTTON FUNCTIONS nn Button Function Control Areas makes selection in control areas single arrow cursor On Screen click and drag a selected area to zoom in magnification to fill the image area with the selection selectable in Preferences Double Click An electron image quad moves the selected point to the middle of the quad Optical me 10 mm marker placement zoom out outthe i image to fit the selected area Shift Left 1 Activates Beam Shift hand cursor 2 Pauses Resumes all quads when clicking the tool bar pause icon To focus with the mouse press and move the mouse to the left or right double ended arrow cursor left T right button O button y wheel up T wheel down wheel press Shift Right To stigmate the image press and move the mouse four ended arrow cursor to the left right X stigmator or up down Y stigmator Ctrl Right Activates Lens Alignment 4 arrow cursor Shift Wheel Fine Control moving the wheel Up Down incre
163. ging Grey VENTED for sample or detector exchange PUMP BUTTON When the Pump button is clicked and the status is Vented or when changing vacuum mode the target pressure that the system pumps to depends on the selected vacuum mode The Pump button is highlighted in and not accessible For the High Vacuum the system achieves the lowest pressure possible For the Low Vacuum or ESEM it achieves the pressure specified in the Vacuum module Chamber Pressure adjuster The purge function can be defined in the Preferences ESEM dialogue When the Pump button is clicked and the status is Transition venting the venting procedure stops and the system immediately starts to pump to the currently selected vacuum mode VENT BUTTON When the Vent button is clicked and the status is Vacuum the confirmation dialogue appears After confirmation the system switches off the detectors voltages high voltage supplies vacuum pumps and uses the appropriate valves to vent the system with the use of an air or a gas the dry Nitrogen typically brought to the Nitrogen Inlet The Nitrogen is recommended to obtain lower pressure for high resolution imaging in HiVac mode The Vent button is highlighted in and not accessible After a specified venting time the venting valve closes and the vacuum status should indicate Vented The button is enabled again When the Vent button is clicked and the status is Transition pumping the dialogue appears After c
164. han the default metric measurements The X and Y coordinates now operate in User Units which are indicated in the Stage module Coordinates tab by the UU symbol Preferences Colo Clamp toggles on off a mechanical stage clamp in order to prevent stage vibrations during high resolution imaging This menu item is greyed out on systems without a securing Clamp 50 mm stage Beam Shift Reset zeroes the beam shift A feature observed with a non zero Beam Shift is automatically moved back to the image center using the stage Zero Beam Shift zeroes the beam shift without moving the stage A feature observed before selecting this function is moved from its position by the measure of the applied beam shift Auto Beam Shift Zero automatically resets the beam shift each time it reaches the maximal value during the Get function the point to point stage movement and corrects the image position with a stage movement Home Stage Shift F3 starts procedure which moves all motorized axes to their hardware xm Stage information limits and ensures that the physical stage position agrees with the erue tee REUS ETE coordinates readout During the home stage procedure the xTm must be completed first Stage Information dialogue displays its progress The stage axes are Do you wantto run it now moved to their end switches in the following order Iv items susgaiwi ETAO E 1 Z to the lowest position 2 T tilt 3 X Y and R rotation at
165. he copying and removal of user data You can start the software from the system Start menu This brings up the Log On dialogue box containing Username and Password text fields for entering the User Management software CONTROL POSSIBILITIES Context menu You can reach some context options by clicking the right mouse button see below Drag and Drop actions Instead of using menu options you can sometimes simply drag and drop items from one icon to another set user group FEI ACCOUNT ADMINISTRATORS As the highest account level FEI Account Administrators have rights that allow them to create and delete users and change their properties over the following user groups in order of significance e FEI Account Administrator e FEI Supervisor Users e FEI Microscope Users e FEI Non active Users Each of these accounts has its own opportunity to operate the xT microscope Server and Control software The first FEI Account Administrator is created during the system installation FIGURE 4 20 FEI ACCOUNT ADMINISTRATORS CONTROL OVERVIEW factory FEI User Management BE ex File Account Liserdata Help LLAFEI Non active Users 4 FEI Microscope Users user Quanta Microscope user 445 FEI Supervisor Users supervisor Microscope Administrator A FEI Account Administrators AccountAdmin Account administrator for user accounts management Afi FEI Service Users support Customer Support
166. he image at high magnifications Blank beam during long stage moves Yes No If Yes is selected the electron beam is automatically blanked during long software controlled stage movements This may protect extremely sensitive samples from exposure to the beam in undesired areas The Sensitivity Tab The preset sliders control the sensitivity of the Manual User Interface MUI option FIGURE 4 19 SENSITIVITY PREFERENCES xIm Preferences Databar Units Presets Scanning ESEM General Mowie Sensitivity KALI Contrast O Coarse Focus E E uM m El ness El m ul gH E HEB E Default M All MUI controls are represented except the Magnification The Default button sets the original settings The Movie Tab provides two groups of controls Timer to set up the movie frame rate and File to set up the path name and format of the resulting movie see Chapter 5 E ooo Software Control FE User Management Software FEI User Management Software Service Tools gt Supervisor Tools CUR te FE User Management eh xT microscope Server us FEI Lisertlana q ement The FEI User management software allows to FEI Account Admistrators FEI Supervisors and FEI Microscope Users to organise user accounts that can possibly be used to run the xT microscope Control software It allows the creation and removal of user accounts the setting of user passwords and group membership as well as t
167. he Pause icon is pressed in and has an orange background When the quad is paused the icon remains pressed in but its background reverts to normal and a green box surrounding two vertical green bars appears in the corresponding quad Select Pause or press F6 or click the Pause icon once to release the pause function the icon button pops out and to return the scanning to the previous state Clicking the Pause icon while holding the Shift key pauses resumes all quads with an electron image at once Snapshot F4 Photo F2 activates a preset scan see the Preferences Scanning tab The tool bar icon corresponds to the Photo function Wa x Videoscope F3 This function shows the video signal intensity along the currently scanned horizontal line for correcting the contrast and brightness Reduced area F7 This mode is useful when focusing and stigmating as the scan speed is faster in the smaller area When Reduced area is chosen the small green area frame appears at the last known place on the screen its area and position are adjustable by mouse It is also possible to adjust scan parameters independently on the full frame setting e Moving Place the mouse cursor over the selected area The arrow changes to a 4 ended arrow Click and hold the left mouse button drag the selected area to the desired position and release the mouse button Changing the size Place the mouse cursor over the edge of the sele
168. he Vacuum module Vent button The confirmation dialogue appears After a High Voltage switch off the vacuum system switches off the pumps and opens the appropriate valves to vent the system After a specified venting time the venting valve will close Note If the venting valve closes before the chamber is at the atmospheric pressure the door is not possible to open click the Vent button once more to open it again If you vent the system in order to change a detector wait until the Status module vacuum icon chamber part is grey Operations Obtaining an Image Obtaining an Image OPERATION PRE CHECK To ensure correct operation in any Vacuum mode check the following list before continuing After obtaining a preliminary image you can then experiment with your settings It is also possible to use Set Default Parameters Ctrl D function found at the Tools menu TABLE 5 2 QUANTA FEG SETUP CONDITIONS Adjustment E BeamsSet ng _ E Beam Setting Vacuum mode HiVac conduc vesamples mode HiVac conductive samples LoVac nonconductive mixed or contaminating samples ESEM wet samples use H5O gas medium High Voltage Select voltage relative to specimen type low voltage for surface imaging beam sensitive samples and slightly charging samples high voltage for conductors high resolution compound info BSE X ray For example biological sample High Voltage 1 10 kV metal sample High Vo
169. he holder All interfacing parts have a 3 point contact to minimize vibration The Specimen Holder Kit comprises of Older type 50 mm stage adapter Interface pillar for all multi fittings e 16 Position stub holder spring held e Angled stub holder 4 at 45 2 at 0 e Analytical holder 2x 1 inch samples e 25 mm and 32 mm diameter Polished mount holders e 2x Clamp stubs e Eucentric stub holder Quanta 400 Quanta FEG 400 Eucentric stub holder Quanta 600 Quanta FEG 600 e 1x No 10 Torx driver e 1x No 6 Torx driver FIGURE 9 48 SPECIMEN HOLDER KIT OPTION LOCATION POSITIONS The interface parts and all fitting holders have a 2 pin 2 hole location system This is present so that holders can be positioned in the same orientation each time they are fitted All stages have 2 holes one is round and the other is a slot This will allow the stage location system to work with a holder for precise specimen position This works directly from the Home condition of the stage The stage needs to be homed before fitting of the Holder interface components Eoo System Options Specimen Holder Kit Option FP 2301 10 FIGURE 9 49 QUANTA 400 LOCATION POSITIONS OLDER INTERFACE ADAPTER This adapter is used on pre Quanta 50 mm stages that had no 2 pin locating holes The old centre rotation head needs to be removed from the stage and this component should replace it It is available for those who have pre Quanta 50 mm stage XL
170. he path where the AVI file should be saved Click the button to browse it File Name enter the resulting AVI file name This field is filled automatically with the first image file name Databar Tab Settings made in this dialogue does not affect the databar or units settings used in the xTUI FIGURE 5 11 FEI MOVIE CREATOR TAB DATABAR Ei FEI Movie Creator File L atabar Preview Available items Filter Frame Time Magnification Pressure ocan Rotation Displayed items Dwell Time High voltage spot Size Beam Current Detector Type Horiz Field idth iw Label Iw Micronbar Databar Preview 22756 PM 100 nz SOR 2 5 9 6 4 LED 112 um Label Status LLL TTT E LL LLL E LLL Create Movie Close e The Available Displayed items lists all items that can be entered in the databar are already present in the databar e gt gt gt lt lt lt buttons adds one all item s from the Available list to the Displayed list removes one all item s from the Displayed list back to the Available list Since there is a finite amount of the databar space the area expands or contracts as other items are added to or removed from the Databar The item exceeding the allowable space is ignored Move Up Move Down Top Bottom buttons move a position up a position down to the top to the bottom in the Displayed list a position to the left a position to the right to the
171. he system is computer controlled and as such has a microscope controller which must be turned on to operate the microscope by means of the software The control software facilities and data are displayed graphically on the LCD monitor and are superimposed around and on the image To control software utilities one can use a keyboard mouse joystick option or the Manual User Interface option System Overview System Layout of Quanta FEG system Control Panel The console system power is activated by pressing the front panel green power button located on the microscope console This switches the sub systems on and allows the interface and communication with the microscope controller Most of the functions are activated via the software control FIGURE 2 4 SYSTEM CONTROL PANEL POWER BUTTON QUANTA 200F Stage Controls The stage is software manually controlled and can be oriented with reference to five axes X Y Z Rotation and Tilt Some stage types have only manually controlled Tilt see Chapter 7 FIGURE 2 5 HARDWARE STAGE 200 400 600 CONTROLS System Overview System Layout of Quanta FEG Final Lens Aperture Strip The strip is made from a Mo coated Si Either manual numbered click stop mechanism positions or Automatic Aperture System AAS motorized software control option see Chapter 9 enables to choose the aperture most applicable to your imaging needs see Chapter 5 TABLE 2 1 APERTURE
172. he system should be made whenever necessary or on a fixed interval schedule The correcting of only one procedure may influence others therefore care should be taken to monitor the influence of actions taken Alignments Quanta FEG System Alignments Quanta FEG System Alignments Alignments At the Alignments page select an alignment procedure available from the list box Always follow the instructions given in the Instructions 1 Gun Alignment module You can find some additional explanation in this chapter Stigmator Alignment 3 Stage Rotation Center 5 Emitter Startup COM MON RULES Alignments should be performed in the quad 1 In other case it is not possible to ensure the correct functionality of the Contrast Brightness and Auto functions used at the Alignments pages Before you align the Electron column be sure that the final lens aperture is clean and properly centred During adjustment procedures it is allowed to change the magnification the scanning speed to use reduced area and to optimize an image contrast brightness It is also possible to correct an astigmatism and to focus an image for a particular alignment it is forbidden During adjustment procedures it is not allowed to change a Vacuum Mode a Spot size and a High Voltage Do not use the Beam Shift at any time during the adjustment procedures as this is set to the zero value at each alignment section All specimen movements can be made using the
173. hen using a particular pressure limiting aperture there are pressure limits for different gases TABLE 3 1 MAXIMAL CHAMBER PRESSURE PA TORR UNDER DIFFERENT GASEOUS ENVIRONMENT Working Gas Working Gas 500 um Aperture 1000 um Aperture 500 um m 1000 um aa Carbon Dioxide CO Nitrogen Dioxide NO 70 He 30 H 1 500 Note Combustible gases acetylene for instance must always be used with respect to safety issues The argon use should be minimized to a short time because the IGP s are not optimized for pumping of it at all System Operation Vacuum Modes Vacuum Pump went Made High Vacuum e Low Vacuum Water ESEM Water Chamber Pressure ely ee als Purging During this procedure the specimen chamber is automatically pumped down to a lower pressure to remove the old gas then it is flooded with the new one selected in the Vacuum Mode module to a higher pressure This takes place several times until the old gas is removed and the chamber is mostly filled with the new gas This is applied when the system is e pumping to the LoVac ESEM mode from the vented status e inthe LoVac ESEM mode and the gas type is changed e in the LoVac ESEM mode and the Purge button is pressed The purging can be set up started and terminated in the Preferences ESEM dialogue see Chapter 4 Note This procedure can take several minutes according to Preferences setting Wait
174. hes at the Start Up Restart the PC If this doesn t help restart the whole system If this doesn t help run the Diagnostics Auto Report and Simple TAD utilities see below No signal illumination Check the Status module Emission Current to be within the range 50 400 yA see Chapter 4 Check the Beam Blank not to be on see Chapter 4 oelect the largest Final Lens Aperture No 1 diameter 1 mm see Chapter 2 Click the Tuning module Crossover button and check the position of the crossover image which should be under the green cross see Chapter 4 oet the Enhanced Image Digital Brightness Gamma Digital Contrast values to the default oet the highest Detector module Contrast value see Chapter 4 Select the Scan menu Full frame see Chapter 4 Use a different detector see Chapter 5 Astigmatism exceeds the UI control Use a different final lens aperture see Chapter 2 limits bad image not possible to focus Run the Final Lens Aperture Strip Alignment at 30 kV spot 3 see Chapter 6 following by the Tuning module Lens Alignment see Chapter 4 Hemove the Standard Insert set the HiVac mode and check the image quality If this helps clean or replace the Standard Insert apertures see above Image shift when focusing Run the Final Lens Aperture Strip Alignment see Chapter 6 following by the Tuning module Lens Alignment see Chapter 4 If this does not help run the 1 Gun Alignment procedure see
175. hould be baked in a fume cupboard using an infra red lamp FIGURE 9 37 NITROGEN VESSEL PLACED IN STAND Replacing Nitrogen Vessel 1 Vent the specimen chamber Allow the Nitrogen vessel to cool down before handling 2 Unlock two clips holding the Vacuum vessel Lid Remove the Lid from the Vacuum vessel 3 The Nitrogen vessel can be placed in the Vacuum vessel taking care that the O ring seal on the Vacuum vessel is secure when joining the two components together Secure the two components by fixing the clips to the top of the Nitrogen vessel and locking the clips down 4 Pump the specimen chamber The Vacuum vessel is pumped along with the specimen chamber E System Options CryoCleaner FP 2301 25 MAINTENANCE The only maintenance necessary is to the following Keep the O rings clean of dust and fibre particles by inspecting the Vacuum vessel main O ring on a regular basis If the Vacuum vessel is removed frequently from the specimen chamber inspect the specimen chamber O ring seal each time e Keep the sealing surfaces of the Nitrogen vessel and the Vacuum vessel Lid clean and free of dust and fibre particles e Do not use any kind of vacuum grease on the O rings Wipe outsides of the stainless steel parts to remove finger stains with a lint free cloth dampened with pH neutral soap solution SPARE VESSEL FP 2301 26 It is possible to obtain secondary nitrogen vessel kit
176. icroscope Server application starts and stops the software service controlling basic microscope functions and also the user interface UI software xT microscope Control Run the xT microscope Server from the Windows Start menu or double click the icon the application window appears The title bar right mouse button clicking opens a dialogue that offers the option to minimize the server to the Ul top bar FIGURE 4 1 xT MICROSCOPE SERVER WINDOW amp xT microscope Server Server state RUNNING Y Ll State RUNNING Y Microscope atop shutdown System Hide LI stop Lil Advanced gt gt gt Show Ul Stop Ul x The Server State Ul State modules display the RUNNING or STOPPED state of the xT microscope Server xT microscope Control software services During a transition between these states STARTING or STOPPING is displayed Some Microscope module buttons change its label and behaviour depending on the actual state The Start Stop button starts stops xT microscope Server services If the xT microscope Control is running Stop button closes it first The Start UI Stop UI button opens closes xT microscope Control software The Show UI Hide UI button calls hides the Ul main window The Shutdown System button closes the xT microscope Control software stops the xT microscope Server services and shuts down the console The Advanced button displays the Administration module containing inform
177. ideo is recording The movie has the following embedded features e Resolution 512 x 442 or 1024 x 884 e Databar image optionally included in the video Average or Integration changeable during recording e Scan speed changeable during recording e Reduced area pauses recording of all quads e Remaining time indicator e Single frame TIF images recordable during video sequence Compressed AVI avi formats e Start Stop and Pause onscreen indicators Preferences set up dialogue Note For the quad s with the Enhanced Image module Color tab Enable check box ticked the Movie recording is paused the coloured TIF files are stored anyway if selected see below MOVIE TAB PREFERENCES DIALOGUE The Preferences Ctrl O Movie tab provides two modules one to set up conditions for timing labelled Timer the other to set up save conditions for the resultant movie labelled File FIGURE 5 8 MOVIE PREFERENCES xIm Preferences Iw Movie iw TIF Delay 0 2 y 5 E y 5 5 still s1 s TIF 25 movie stills File File Marne Save in C Browse Numeric Seed Idea File Size ESO MB File Type AVI video compress ALE Mavi w Record Databar s Operations Recording Movies Saving Multiple Images Timer module The parameters in this section can be changed when the digital video is inactive but are disabled during recording The digital video is recorded asynchronously with the scanning
178. ine changes its position along the histogram Clicking with the left mouse button onto the left right part of the triangle selects the left right border colour The image gray scale between two borderlines is linearly transformed to a new colour spectrum he Hand button enables to select and colour a particular image gray level Clicking it opens the colour selection dialogue select a colour and press the OK button The mouse cursor changes to the hand image Click the feature image you want to highlight New borderline is added into the histogram with a rectangle on top The selected grey level is marked with the chosen colour You can move this borderline and change its colour the same way as a borderline with a triangle on top By dragging the rectangle left right side the highlighted grey level range could be changed he Enable check box switches on off actual colour settings for the active quad image e The Save button saves the current setting as the custom preset di iw Enable Save p Operations Detector Types and Usage Detector Types and Usage caes SCA Beam VEDI The Detectors menu shows all detectors a selected one has a tick mark next to its label Availability of detectors full colour label GAD A depends on the actual vacuum mode The system remembers the last detector used for a particular vacuum mode and its Contrast amp PMD BSE Brightness settings External Note CCD If any detect
179. ion systems moves the beam in a raster pattern over the specimen area The electrical voltage changes as it rasters which provides serial information of the specimen surface This signal modulated by the detection system signal produces the onscreen image Detection unit Electrons striking the specimen react with its surface producing three basic types of signal back scatter electrons secondary electrons and X rays The detection system picks up these signals converts them into an amplified electrical signal which is sent to the control PC and displayed on the monitor System Overview How Quanta FEG SEM Works FIGURE 2 1 SEM SCHEMATIC OVERVIEW FILAMENT PINS ELECTRON GUN EMITTER CONDENSER LENS SYSTEM Seem SCAN UNIT SYSTEM SCAN GENERATOR FINAL LENS DETECTION UNIT SPECIMEN VACUUM SYSTEM The entire electron path from gun to specimen must be under vacuum so that the electrons do not collide with air molecules The Quanta FEG has 3 operating vacuum modes to deal with different sample types e High Vacuum HiVac e Low Vacuum LoVac ESEM Various levels of vacuum are necessary so a Turbo Molecular Pump TMP backed by a rotary pre vacuum pump PVP obtains the necessary specimen chamber pressure In the gaseous modes LoVac ESEM the column is under lower pressure than the specimen chamber where the pressure ranges from 10 to 2600 Pa 0 1 to 20 Torr with auxiliary gas up to 4000 Pa 30 Tor
180. is alignment procedure sets the temperature correction factor for the Heating Stage Mo step Alignments IB Temperature Calibration Instructions Reach the melting point of Ag HS 1000 or Au HS 15001 Put the reported temperature into the Measured field Optionally define a custom calibration paint theoretical and measured values Note Possible correction is limited to 50 K max step 1 of 1 Ag Au melting point Measured 193 K 1337 k Theoretical User defined calibration point Theoretical Measured 273 K 273 K Cancel g System Options Heating Stage 1000 C FP 2300 02 Heating Stage 1500 C FP 2300 06 151 Temperature Calibration This is the supervisor alignment procedure The HS 1000 assembly is calibrated by melting the silver sample 962 C the HS 1500 assembly is calibrated by melting the gold sample 1064 C The calibration samples are a part of accessory The HS assemblies are factory calibrated with the standard ceramic crucible at 400 Pa chamber pressure under a water environment and with the ramp rate 10 K min At these conditions the temperature shift should be less than 50 K In other case contact your local FEI service representative Note Different pressure environment and fast ramp speeds lead to a less accurate sample temperature readout and to incompatible results Checking Calibration The HS assembly calibration typically does not change
181. isabled To enable it again you can try one or more of these actions decreasing the Tilt Angle increasing the magnification or the working distance decreasing accelerating voltage or switching the Tilt Correction on this helps especially at high tilt angles NAVIGATION TAB see Chapter 4 Stages Stage Related Functions otage Related Functions left button wheelup f wheel down wheel press a STAGE MOVEMENTS Track This function allows continuous directional stage movements at a variable speed Press and hold the mouse wheel above an active electron image window the yellow dot appears onscreen at the mouse cursor point Move the mouse to the direction intended for an observation an yellow arrow appears onscreen denoting the direction opposite to the stage motion The motion speed raises with the distance between the arrow and the dot the direction can be changed by moving the mouse When you come to the place of interest release the mouse wheel the action stops In the second possible mode the mouse wheel does not need to be held just click it to start the Track motion and click it again to stop it see the Preferences General tab FIGURE 7 9 TRACK FUNCTION Test label In the optical quad pressing the mouse wheel activates the stage Z movement which can be seen live e With the Mouse Wheel pressed moving the mouse up down moves the stage up down Z coordi
182. isplays by default the location and the name last used to save open a file in the current quad You can choose different location name base or suffix select different image format Save as type and also choose whether to Save the image with without Databar and with without overlaid graphics by ticking clearing an appropriate check box The settings is remembered per quad and used for the subsequent Save actions Record Movie o Ng allows the user to make digital video files AVI for dynamic experiments The tick next to this menu item and the change of the corresponding tool bar icon indicates the movie recording see Chapter 5 Import Export opens a sub menu with selection of importable exportable items Selecting an item opens standard Open Save As dialogue for choosing location and file name Following items can be both imported i e loaded and used and exported e Stage Positions stored with the use of the Stage module stg files Current operation Parameters microscope settings par files FIGURE 4 6 FILE IMPORT EXPORT MENU mi Edit Detectors Scan Beam Stage Tools wv mi Edit Detectors Scan Beam Stage Tools wv Open li a A Open a cave Ctri 5 A Save Ctl s a nave As nave AS Record Movie Import Stage Positions Import Record Movie Export Parameters Stage Positions Parameters Print Ctrl P Print Ctrl P Log Off factory Log Off factory Exit E
183. ively see the Preferences General tab 5 The Beam Module The Stigmator 2D Control enables to correct image astigmatism The crosshair indicates the actual stigmator setting Clicking and holding the left mouse button anywhere inside the 2D control changes the cursor to four ended arrow and moves it to the we Coarse we Coarse Fine Fine ero ero Back Back Clear Memory Reset Tuning source Tilt Lens Alignment Crossover Lens Align e Coarse Fine Zeno Clear Memory Auto Alignment ______________g Software Control xT microscope Control Software screen position corresponding to the actual Stigmator value minimum in the middle of the screen and maximum at the edges Clicking Shift right mouse button over an electron image can be also used for astigmatism correction Unlike the Stigmator 2D control this function is magnification sensitive and therefore it suits for fine corrections at high magnifications The Beam Shift 2D Control indicates and controls the beam shift with respect to the objective lens axis It is useful for fine image shifts without stage movement The control behaviour is similar to the Stigmator control Clicking Shift left mouse button over an electron image also triggers the Beam Shift function The mouse cursor changes to a hand one that holds the image and drags it over the screen Because of a limited Beam Shift range this works well only for high magnifications
184. l shows an image Reduce the contrast to zero and adjust the brightness to a level so that the last gray level can be seen by eye before the screen goes black 4 If necessary adjust the brightness level to improve the image These adjusters always have a label editable value displaying the current Contrast or Brightness level in in the upper left right corner Using Videoscope F3 This mode could facilitate contrast and brightness optimization to obtain full greyscale level range of an image Three yellow horizontal lines placed over the image window indicate white top line grey middle line and black bottom line levels The oscillogram signal amplitude central position reflects a contrast brightness of the just scanned line If the oscillogram is cut by the bottom top line the signal level is clipped in black white This should be avoided because the image details are lost in the clipped areas Tuning the oscillogram exactly between the top and bottom lines for a feature of interest with the use of the reduced area results in the full detailed image The signal clipping may be used to obtain harder contrast conditions when more black and white is needed The signal amplitude lowering decreases the contrast i e the image looks softer TABLE 5 8 C amp BSETTING USING VIDEOSCOPE Step Action 4 Select a slow scan in an active quad 2 Activate the Videoscope F3 tool bar icon Scan menu R
185. le This should have been connected by a service 11 Turn on the water chiller Water does not flow at this point since the valves in the Flow Box are closed when it is off 12 Turn on power to the Flow Box An alarm sounds indicating that there is no flow through the box 13 Push and hold the Start Flow button Keep holding this button down until all the air is out of the water lines this can be seen as water flows through them Once the lines are flowing clear release the button 14 Make sure that the Flow OK light on the Flow Box is on This indicates that water flow is working i e that there are no leaks in the system The light remains illuminated until there is a leak or if the Stop Flow button is pressed which could be done at any time to close the valves and shut off the water flow for whatever M System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 reason which is indicated by an alarm sounds The Start Flow button must be pressed and held again to re establish flow through the system CAUTION Never pump the specimen chamber without checking for water leaks first Consumables TABLE 9 2 COOLING STAGE CONSUMABLE PARTS Sample holder Flat 4022 290 08612 Sample holder Deep 4022 290 08592 Sample holder Dual 4022 290 08602 possible to use both sides Sample holder for Wet STEM assembled Sample holder for Wet STEM parts base 4022 290 32101 lid 4022 290 32111
186. le rotation The readouts displayed at the image window bottom provide information about the Actual Rotation original position and the Target Rotation the selected position Releasing the mouse button updates the stage position to bring the original field of view rotated to the Target Rotation position onscreen With the sample at the eucentric position this can be performed at any sample point irrespective of the mechanical stage center Clicking the written angles around the circle perimeter 0 90 180 270 or the perimeter anywhere drives the stage to that rotation position and the green triangle updates onscreen Clicking the framed sign increases decreases the rotation angel by an incremental value FIGURE 7 11 COMPUCENTRIC ROTATION Once selected the compucentric rotation control disappears automatically after 10 seconds of no use see the Preferences General tab Stages Stage Related Functions Tool Window Help xT Align Feature Compucentric Rotation Fiz Define User Units Beam Shift Reset Zero Beam Shift Home Stage Shift F3 Home Stage Without Rotation Center Position Ctri o e Touch Alarm Enabled Sample Navigation Navigation Montage Specimen Holder Wizard Preferences Colo SPECIMEN ALIGNMENT xT Align Feature This utility is designed specifically for long features extending off the screen at the magnification required for an observation It ap
187. ltage 10 30 kV HiVac and LoVac 3 or 4 ESEM 4 HiVac the lowest LoVac 60 Pa 0 5 Torr ESEM 600 Pa 3 7 Torr HiVac fast dwell time about 0 1 0 3 us LoVac and ESEM slow dwell time about 1 3 us Working oet the highest specimen point to approximately Distance 10 mm yellow mark in an optical quad and press Ctrl F to set WD to 10 mm Magnification Set to lowest from 50x to 200x Standard HiVac ETD SE Detector LoVac LFD ESEM GSED HiVac Average 4 frames for fast scans LoVac and ESEM Live Contrast With contrast at minimum value adjust brightness and Brightness to just show a change in intensity to the screen Increase the contrast to produce a reasonable image on screen Increases in brightness and decreases in contrast produce softer images and vice versa Operations Obtaining an Image SELECTING VACUUM MODE Vacuum When a specimen and appropriate detector s are inserted correctly close the specimen chamber door and follow the instructions Pump went Vine TABLE 5 3 SELECTING VACUUM MODE High acuurn Si E ti e ction Low Vacuum Water Lad A 6 In Vacuum Mode module select the High Vacuum Low C ESEM Water Vacuum ESEM radio button Chamber Pressure efi ls For Low Vacuum ESEM modes use water or select the desired gas environment from the dropdown list box and the target pressure that the system pumps to in the Chamber Pressure adjuster In the Vacuum M
188. lysis may be slightly lower than normal using this heating stage Window Contamination Upon heating certain samples may evolve gases or burn off various residual components such as binders or fillers If the EDX detector is located close to the sample these evaporated components may condense onto the EDX window To prevent this keep the EDX detector retracted away from the stage until it is needed Emo System Options Heating Stage 1000 C FP 2300 02 Heating Stage 1500 C FP 2300 06 Water Cooled Temperature Stage Operation Termination oee description above the Cooling stage HS MAINTENANCE Cleaning The Heating stage could be polluted after a long term use or when using highly outgassing samples To prevent another samples contamination remove and clean the stainless steel cover plate The ceramic paper heater cover should be replaced together Use Heater cover 2 harder paper always on the top The Heat shield isolation should be replaced as well for HS 1500 only Heater breakdown The HS 1500 assembly lifetime is limited and depends strongly on the working temperatures FIGURE 9 33 1500 C HEATER LIFETIME 1500 C Heater Lifetime O g typi ONNI 1100 1200 1300 1400 1500 Temperature C In case of heater failure check its resistivity which should be within the 1 5 Ohm range When the heater breaks down the 1500 C Heating Stage assembly can be ordered under the code 4022 268 009
189. ment Image Mixing Image Colouring 5 12 Detector Types and Usage 2 02 eee ees 5 14 Everhart Thornley Detector ETD 0 00 0 eee 5 15 Backscattered Electrons BSED and Gaseous Analytical GAD optional Detectors 5 15 Large Field Detector LFD llle 5 17 The OODCalela auda dares ac eR CE VP E A dia ie oben i 5 17 Gaseous Secondary Electron Detector GSED 5 18 PEA CONOS 324 eau duas dui a eee eat Sabes ssi aid pardas 5 19 Discharges between the Gaseous Detectors and the Sample 5 20 Obtaining image Procedure for Gaseous Detectors 5 20 Capturing and Handling a Single Image 5 21 Snapshot Photo Pause Button o oooooocooonoo 5 21 Fenno THEICHOTIS 5m eto di o i abo atn ie ao aiat ae Ph et a 5 21 IMAGE YPES iare AE Uto cata Adan d a le I Bebe 0 22 saving Opening Printing llle 5 23 J Recording Movies Saving Multiple Images Movie TAB Preferences Dialogue 0 0 00 cee eee MOVIS PIOCEEHBIE Sura sor ait aria tries ee neo eod sped PE MOVIE Crealo aaa de dC e etd o de e Sd ee te Playing a IO VIG 4 35 Vw pao aco ace NOR Sarda el A ecu RO sta Measurement and Annotation Functions Chapter 6 Alignments Quanta FEG System Alignments Leere COMMON RUES 3 3 Se 15 aede le eth bared e dd cose ee ee MoM da etes Buttons an
190. mplifier input board They can be used down to a high voltage about 1 kV and works best at a slow scan conditions The BSED can be used for HiVac operation and for low magnification imaging in LoVac The GAD can be used both for HiVac and LoVac operation but because it limits the minimum achievable WD it is disadvantageous for high resolution imaging in HiVac Both can be used in parallel with the LFD which allows simultaneous use of SE BSE and X ray detectors in a gaseous environment They should be used at the lower part of a pressure range obtainable for a particular detector E Operations Detector Types and Usage xTm Detector Settings m Detector Settings Detector GAD Made C Z Contrast Topography a Segment A C Segment B Clase Rx Installing the Diode Hold the detector by its sides and push up the back of the diode onto the Standard Insert until it stops The diode should by oriented so that its out coming cables side should be faced and parallel to the chamber door Detector home position While the BSED GAD detector is not used it could be placed into a holder which is mounted on the upper edge of the pole piece saving it from a mechanical damage and pollutions Caution The diode is sensitive to a mechanical damage so the active area shiny diode should never be touched The BSED GAD is mounted close to the optional X ray detector collimator which
191. must not be touched when changing detectors It is advisable to retract the EDX collimator when mounting removing the detector on from the objective pole piece FIGURE 5 4 GAD INSTALLATION AND HOLDER POSITION Detector Settings Select the BSED GAD from the Detector Settings module Detector list box Choose the required Mode by ticking the radio button The Z Contrast A B is the normal BSE image with suppressed topographical contrast and maximum atomic number contrast The Topography A B is the pseudo topographical image with suppressed atomic number contrast and maximum topographical contrast The Segment A B Left Right uses shadows to create strong topographical and atomic number contrast Obtaining Image in BSE Mode 1 Install one of the diodes and select the corresponding Detector 2 Close the chamber door and pump down the chamber When the BSED GAD diode is installed No Accessory GAD cone must be selected in the Pole Piece Configuration dialogue when this appears 3 When the Vacuum is ready switch on the accelerating voltage and slowly increase the contrast and brightness to obtain an image Note Whenever the BSED or GAD is selected the optical quad is paused because the CCD camera infra red LEDs are switched off not to emit the photons supersaturating the detector diode MEL LFD Plug in detector xTm Detector Settings Detector Settings Detector LFD Enhanced
192. n search and About TUI selection tools FIGURE 4 8 DOCUMENTATION amp Acrobat Reader online_doc pdf tT File Edit Document Tools View Window Help C EB amp 8 4 IE I4 42 MQ E S os oe BOWE ido amp Bookmark EJ 22214 Operations Opntimising an image Alternatively Magnification could be expressed as the Horizontal Field Eb L Width HFW specifying dimension of the scanned area see i Preferences General tab The Quanta FEG supports two viewing sizes Quad Image and Single Image modes Magnification is always adjusted in the databar for the current display thus an image at 500x in Quad Image mode is 1000x in the Single Image mode as its size has doubled Thumbnails Bookmarks FIGURE 5 1 MONITOR IMAGE AND SCANNED SAMPLE j MONITOR j Y f SEM j j l 3 Correcting Astigmatism b ee Pressure and Working Diste 1 Digital Image Enhancement __ Magnification Detector Types and Usage m 3 Capturing and Handling a Singh i Changing Magnification E L Recording Movies Saving Multi 10 1 The Toolbar list box is used to select from a predefined values i The Keyboard control the numeric pad plus key the minus key increases decreases the magnification 2x and ati Eh j S rounds the value The star key rounds the magnification value 11 Ali gnments v 1 000 e g 10 063x becomes 10 000x When using the HFW no
193. n connect to the Microscope PC at the same time and thus share its desktop on the remote PC s This can be used e g for the educational purposes The typical scenario is that a dedicated user supervisor controls the microscope locally or remotely and the other connected users can only view the Microscope PC s screen over the network 1 In FEI User Management application create a non active user account for the view only purpose 2 Open the VNC Viewer application on the remote PC of the person who is intended to control the microscope and connect remotely to the Microscope PC as user supervisor 3 Other users will then open the VNC Viewer application on their remote PC s and connect remotely as view only users Note The desktop sharing must be enabled in the VNC Server application on the Microscope PC For instructions how to do so see VNC Server documentation available on the installation CD CONTROLLING THE MICROSCOPE REMOTELY After connecting remotely to the Microscope PC you can do all the tasks as if you work directly with that computer It is possible to control the microscope operation run the supportive applications backup or restore user data view the log files etc In general expect slower response on your commands and actions This limitation comes from the amount of data that have to be transmitted and from the network bandwidth You can decrease the amount of data being sent over network by using a single res
194. n of each tool menu item and control page 5 OPERATIONS gives procedures for how to use the system 6 ALIGNMENTS explains how to align the column and stage to achieve optimal performance 7 STAGES gives a full description of the stage functionality and its software control 8 MAINTENANCE gives step by step cleaning and maintenance procedures 9 SYSTEM OPTIONS explains relevant options that are integrated into or accessory to the system Preface How to Use this Manual How to Use this Manual This manual is available in two forms the electronic PDF file and the printed form option It is recommended to read this manual before operating any of the microscope function Most importantly you should locate the topics necessary to operate the microscope in the proper way to safely achieve the best results In the electronic PDF file you can take advantage of the searching and navigation possibilities offered by this file format In the printout the following conventions are observed to be of help You can search for the information in the main table of contents at the beginning of the User s manual where tables and figures excluding explanatory ones are also listed e Major headings have been hung in the left column to help you scan for the basics within a chapter That column provides space for some explanatory figures and for your own notes as well e Some software functions use short cuts which are given beside the
195. n the list remains fixed FIGURE 4 15 PRESETS PREFERENCES xIm Preferences Datahar Units Presets Scanning ESEM General Movie Sensitivity High voltage Magnification Fressure we The High Voltage list can be changed to span any values from 200 V to 30 kV The values must be entered in kilovolts 0 2 means 200 V The Magnification list can be changed to hold frequently used magnifications Values that are in the pre set list but cannot be applied to the current SEM conditions are not shown in the tool bar Magnification list box Magnification range is from 20x to 1 000 000x Note Alternatively the Magnification could be displayed as the Horizontal Field Width see the Preferences General tab The Pressure list can be changed to hold specific values frequently used in the Low Vacuum and ESEM modes in the range from 10 to 200 Pa from 0 075 to 1 5 Torr Software Control xT microscope Control Software The Scanning Tab allows the user to change the dwell times scanning speeds table and to set up the Slow scan Fast scan Snapshot Photo function FIGURE 4 16 SCANNING PREFERENCES xIm Preferences He 50 0 ns 100 0 ns e 300 0 ns 1 0 ps 3 0 Us 10 0 Us 2 30 0 us Dwell Time Resolution 512442 Line Time 5 4 ms Frame Time eds Refresh Rate 4118 47 mHz 100 0 ps Integrate ix 300 0 ps Acquisition B bits 500 0 ps Action Save As 1 0 ms Default Photo Preset H On
196. nate Holding Ctrl key together with the Mouse Wheel pressed moving the mouse left right tilts the stage left right The direction is indicated by a yellow arrow either pointing up down from the horizontal line or left right from the vertical line Keyboard Stage Shift The stage can be moved about 80 of the field of view in perpendicular direction by clicking the appropriate keyboard Arrow key with the Shift button pressed simultaneously about 40 Stages Stage Related Functions Get This function brings an image point of interest to the screen center Double click an image point with the left mouse button The object is mechanically centred onscreen by moving the stage which is suitable for lower magnifications When working at higher magnifications beam shift could be also employed see the Preferences General tab In this case the object is electronically centred onscreen by moving the electron beam When the beam shift comes to a limit in any direction its value resets and the necessary stage movement adapts the observed point position FIGURE 7 10 GET FUNCTION 30 Jan 01 Det File Filter HF Hv Mag 15 14 43 xxx xxx xxx 1 02 mm 0 00 Y 101x Test label Beam Shift When you want to employ the beam shift only which is suitable for higher magnifications click an image point with the left mouse button while holding the Shift button pressed The Hand cursor allows to move th
197. ng applications This starts from the last used one continue to press the TAB key while holding down the ALT key and applications are shown one by one Releasing the ALT key at any time makes application just listed active Alt F4 Exits active application or Windows operating system Del ete Deletes selected text or items Ctrl A Select all items Ctrl C Copy to clipboard Ctrl Insert Ctrl V Paste from clipboard Shift Insert Ctrl X Cut to clipboard Ctrl Delete TABLE 4 5 FUNCTION AND SPECIFIC KEY SHORT CUTS Function Displays On Line Documentation Shift F3 Toggles Videoscope On Off Starts Home Stage procedure Fa Starts Stops Snapshot Shift F4 Starts Lens Alignment procedure Software Control Entering Commands in Summary TABLE 4 5 FUNCTION AND SPECIFIC KEY SHORT CUTS Key Key Function Fe Pass Resumes Toggles Alignment rectangle display F7 Toggles Reduced Area Full Frame Mode Degauss e A Pegas ES Sans Auto Contrast and Brightness procedure 0007 Fe Stars Auto Focus precede 0000 Starts Auto Stigmator procedure E2 reses Compucentic Rotaiontesl sets Full Frame scanning conditions Selection of the particular page the number corresponds to keyboard the tool bar page icon sequence Ctrl Scales up down the image 2x Digital Zoom Moves the digital zoom area E 5 OPERATIONS This chapter describes how to use the Microscope system
198. ng range limit temperature up to 1000 C 1100 C HS 1500 normal operating range limit temperature up to 1500 C 1530 C Additionally accuracy of temperatures readout depends on sample conductivity thickness shape and general thermoelectric properties that vary by sample and mounting method System Options Heating Stage 1000 FP 2300 02 Heating Stage 1500 C FP 2300 06 Cables The Outer Cable is 4 ended cable connecting the outside of the chamber feed through plate with the HS controller and SSB board The greater lesser spherical connector connects to the connector labelled Heating stage Cooling stage this is used in case your system enables both stages to use only one cable The 25 pin 9 pin connector connects to the HS Controller SSB The Inner Cable is 3 or 4 ended cable connecting the inside of the Chamber feed through plate with the heating stage assembly The 15 pin connector goes to the appropriate inner feed through plate connector the other ones connect connectors ascribed to the Heater to the Sample Bias and to the Thermocouple CANON 9 pins High Temperature GSED The High Temperature GSED must be installed if the heating stage is going to be operated above 500 C up to 1500 C as the standard GSED could be damaged at these conditions It is a PLA cap with cone which is pressed onto the standard insert This cap comes with a printed board adapter which plugs in
199. ngle is different from 0 MAINTENANCE AND TROUBLESHOOTING This section describes necessary microscope maintenance procedures that can be carried out by the FEI Supervisor User FEI Microscope User The user maintenance is at a minimum due to gun and column design providing the long uptime Therefore a complicated maintenance is normally a part of a service contract to be performed by a qualified service engineer Chapter At the User level items such as the following can be maintained Cleaning Procedures Overview The Standard Insert Gaseous Detectors Stage Maintenance Refilling the Water Bottle Rotary Pump Maintenance Caution Parts that operate in vacuum should be handled carefully using clean powder free gloves Parts not in use should be stored in suitable containers or packed in aluminium foil the EDX window if present is very fragile and must be protected from large pressure oscillations It is recommended to remove the detector before major cleaning activities Note Gas back fill No should be maintained while the specimen chamber is at ambient pressure However to avoid gas waste it is recommended that the chamber should be left vented no longer than necessary Maintenance and Troubleshooting Cleaning Procedures Overview Cleaning Procedures Overview Frequency of cleaning is in most cases determined by necessity due to poor image quality or gross astigmatism level Recommended cleaning proc
200. nits Presets Scanning ESEM General Movie Sensitivity Units of Measure millimeter mm Pressure Pascal Fa Temperature Kelvin K Selection possibilities are Units of Measure Millimeter mm Micrometer um Pressure Pascal Pa Torr Torr millibar mbar Temperature Kelvin K Celsius C Fahrenheit F Software Control xT microscope Control Software Edit label Sample lv Quadi Quad2 Quad3 Quad4 The Databar Tab specifies content of the databar displayed at the base of all quads The Databar configuration and available items differ for SEM imaging and optical quads Actual content of the Databar Preferences dialogue corresponds to the currently active quad For all electron imaging quads the Databar configuration is identical except of the Label which can be set independently for each quad FIGURE 4 14 DATABAR PREFERENCES xIm Preferences Diatabar nits Presets Scanning ESEM General Movie Sensitivity Awvallahle Selected Detector Made Frame Time High voltage Working Distance spot Size Detector Type Pressure Magnification Top Move Lp ocan Rotation otage Y Temperature Tilt Vacuum Made Zoom Factor iw Label Label iv Micronbar Add Bitmap Datebar Preview frame HV WD E det g54 ms 5 00 E 10 8 mm 5 0 EID Label There are two lists in the dialogue one labelled Available and the other Sel
201. nnection between the specimen holder and the stage Other problems e Run the Diagnostics Auto Report and Simple TAD utilities see below There are two powerful tools for any system troubleshooting e g flags in the image software problems etc accessible to a Supervisor 0 Maintenance and Troubleshooting Troubleshooting The Diagnostics Auto Report saves a zip file with all the logs system information user s description and screen shots The Simple TAD Simple Test And Diagnostics performs many tests communication with microscope modules supply voltages and electronics boards test for instance and saves a file with the results Generated files are intended to be sent to a local Field Service Engineer Note If Simple TAD procedure is run prior to Diagnostics Auto Report the Simple TAD output file is collected by Diagnostics Auto Report and zipped together with the logs Then it s enough to send only the Diagnostics Auto Report output file DIAGNOSTICS AUTO REPORT To run this procedure the xT Microscope Server can be stopped or running 1 Run the system Start Programs FEI Company User Tools Diagnostics Auto Report Click the Start button Diagnostics Auto Report Collect and prepare data Capture the screen display save files save the TAD Session files save list of installed software save the Registry into cave list of tiles save the Event Log files save file versions save the Processes
202. ntrols Frame active quad Enable zooming on mouse click and drag Yes Switch sample tracking on mouse wheel click Yes spot size step 0 1 Restat Average Filter when magnification changes Yes Restat Average Filter when scan rotation changes es Restat Average Filter when beam shit changes es conci Each item of the General Preferences is represented by single line displayed in the property editor Clicking on the corresponding Value displays a drop down list with the settings available for that item Note Some changes become visible after the next UI start Categories To make navigation among the number of preferences easier they are divided into three groups Selecting appropriate group from the Category drop down list will display in the below property editor only the items belonging to this group Selecting Category All will display all items at once Ul appearance e Icon style Nova Quanta Selects appearance of the tool bar icons Toolbar listbox style Reduced Standard Specifies appearance of the High Voltage Magnification and Spot drop downs lists Toolbar spinner style Up Down Left Right Specifies appearance of the Dwell Time spinner Image dimensions control Magnification HFW Selects a way of the magnification representation and control Frame active quad Yes No Switches on off additional highlighting of the active quad Enable zooming on mouse click and drag Yes No Enables disables
203. o IR continuous adjuster sets a ratio between a primary electron energy and the particular landing energy It changes the HV and the BDV together The higher is the immersion ratio the more powerful is the Beam Deceleration Note A Landing energy value can also be displayed in the databar It is also stored within the TIF file header In case the BD is not on Landing E corresponds to the HV System Options Beam Deceleration FP 6842 22 Beam Deceleration Mode Imaging Procedure 1 Put the sample into the chamber and pump to the HiVac In the BDM a sample becomes the electrode Its position size tilt and surface roughness influence an imaging quality At optimal conditions the sample should be symmetrical planar have a size comparable with the detector size and placed perpendicular to the column axis In other conditions a distortion an astigmatism and a blurring caused by the chromatic aberration appear This is even worse when the immersion ratio is higher 2 Select the suitable HV and find an area of interest Set the Eucentric Position see Chapter 7 and tune an image with the Lens Alignment and the Stigmator see Chapter 4 In various quads get the SE ETD and BSE BSED PMD images to observe different imaging simultaneously 3 Click the Mode On button Gradually raise the immersion ratio The SE BSE image is getting dark light At low magnifications an ETD image should become dark symmetrically around the
204. o frames is interrupted but the video streams keep synchronization for the next resuming When the red dot representing Start is pressed it turns to a red square representing Stop Pressing the red square then stops the recording of the video in all quads and closes all video files The red dot with the timer displayed in the top right hand corner indicates that recording Is active in this quad The Pause symbol indicates that the record is running but the data from this quad are not stored the quad is paused The timer indicates the time estimation in the hh mm ss format remaining to the end of the video This is calculated from the average disk space consumption and the disk free space TABLE 5 14 SET UP AND RECORDING A MOVIE Step Action Open the Preferences Movie tab In the Timer module tick the Movie or TIF check box and select the desired Delay time the period between stored frames In the File module fill in the File Name and give the Save in directory path Fill in the Numeric Seed value and the Video File Size Select the File Type and choose whether to record the databar with the Record Databar check box Pause those quads which you don t want to record Set up the imaging parameters in the live quad s Select the File menu Record Movie a tick mark or click Ed 0 no the tool bar red dot button When the scan resolution is Open higher than 1024 x 884 the following dialogue appe
205. ode module click on the Pump button While pumping choose the highest specimen point and bring it to the 10 mm WD yellow line in an optical quad Under normal operation the system knows the PLA size for the detector installed This allows the system to set automatic pressure range limits for the aperture installed thus avoiding vacuum errors when setting chamber pressure In some cases the user is prompted for the PLA size by the Pole Piece Configuration dialogue Wait for the vacuum status Pumped represented in the Status module at the base of the page by the green icon WARNING The system can be damaged by using the Low Vacuum ESEM mode without an appropriate PLA Do not select a PLA Cone which is not actually mounted onto the objective pole piece xTm Pole Piece Configur Low Vacuum and ESEM Modes Which one of these modes is used depends on either the detector installed or some special conditions working with the cooling stage implies ESEM mode for instance te Mo Accessory Low kY Cane Purging The microscope provides automatic sequencing for purging the specimen chamber according to the settings of Purge Mode in the Preferences ESEM tab There may be certain applications e g working with a sensitive sample where the operator needs to change the purging parameters e Select No Purge when purging the specimen chamber is not desired The chamber goes to the set pressure directly and the gas mixtu
206. of Frames pre set see the Preferences Scanning tab Number of Frames As the scanning could take a significantly long time period one can restart it from the beginning with the use of Ctrl R keys Restart ocan Scan Rotation Shift F12 activates the on screen tool to rotate the scan field It has no effect on the stage movements and is solely a scan coil function used to orient the image relative to a specimen feature and or detector direction A non zero scan rotation is indicated by an icon in the Status module and its value can be also displayed in optical quads see Chapter 7 The Beam Menu Alt B opens the Beam menu functions sm Stage Tools Window Degauss FS Degauss F8 triggers the procedure which puts all currently used electron lenses to a normalized state by removing their hysteresis effects For a few seconds while the procedure is running all live images disappear or turn fuzzy and then return back Lens Alignment Shitt F4 Preferences chl O Use this function with almost focused image to obtain the most accurate Magnification Horizontal Field Width HFW and Working Distance WD readouts Lens Alignment Shift F4 This feature activates deactivates the final lens alignment mode for the fine alignment The scanning changes to the fastest scan value lens modulator turns on and the alignment cross appears in the center of all imaging quads Pressing and holding the left m
207. oling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 FIGURE 9 14 OUTER AND INNER CABLES Attached to Stage Water Chiller Flow Box and Cooling Water Hoses Note In case the waterless Cooling stage is installed the following devices are not available An external water chiller is provided to efficiently remove excess heat from the temperature stage FIGURE 9 15 THE WATER FLOW BOX CONTROL BOARD The water flow box is installed between the water chiller and the chamber feed through plate It monitors a water flow via a sensor on each line and closes both solenoid valves if a failure is detected to protect the system against a water leak into the chamber Cooling water hoses are delivered the shortest set of hoses is connected to the stage on one end the other end goes to the inside of the feed through plate One set of hoses goes from the outside of the chamber feed through plate to the water flow box Next one connects the water chiller with the water flow box COOLING STAGE INSTALLATION The chamber feed through plate should be in place and remain installed 1 Vent the specimen chamber and open the door 2 Remove any sample holder from the stage rotation head g System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 3 Place the mounting adapter on the stage rotation head and fix it through the centre using the mounting screw finger tight 4 Slacken off the mount lockin
208. on 2 Display the Window menu Center Cross Shift F5 Focus an image Link Z to FWD and go to 10 mm WD Set stage tilt to 0 Using the Z control coarsely focus the image oet the magnification to 1000x find a recognizable feature and center it under the yellow cross by moving the stage T Watching the feature change the stage tilt to 15 Using the Z control bring the feature back under the cross Stages Stages Types and Accessories TABLE 7 1 FINDING EUCENTRIC POSITION PROCEDURE Step Action Change the stage tilt again to 30 and bring the same feature back under the cross using the Z control Change the tilt to 0 The feature should not shift significantly If the shift is gt 5 um repeat steps 6 to 9 Sample Top Surface Positioning The distance between the observed sample and the stage rotation head surfaces must be properly set to bring the stage to the eucentric position This procedure also prevents the specimen to touch the lens pole when moving the stage in the Z axis direction TABLE 7 2 SAMPLE POSITIONING PROCEDURE 100 150 mm Load a sample onto the specimen holder Adjust the external Z Adjust the Z coordinate to bring the coordinate as high as specimen top surface possible approximately 10 mm below the lens Bring the specimen top surface point to the 2 mm adjuster position by turning the specimen holder internal screw Lock the position with the locking cone Adjust the exte
209. onfirmation the pumping procedure stops and the venting procedure starts When the Vent button is clicked and the status is Vented the dialogue appears After confirmation the venting valves re open for the specified venting time and then the valves close System Operation Vacuum Modes Vacuum Modes Vacuum Pump went Mode High Vacuum Low vacuum Water Water Chamber Pressure ely als MESE xTm Pole Piece Configur a Mo Accessory Low kY Cone Hay Cone pu Hot MEN Lone 1000 um x e The vacuum mode radio buttons in the Vacuum module Mode area are used to select the instrument target operating mode when a Pump sequence is initiated The vacuum system recognizes High Vacuum Low Vacuum and ESEM modes HIGH VACUUM HiVac MODE The high vacuum condition is common throughout the column and specimen chamber The typical pressure value is within the order from 10 to 10 Pa LOW VACUUM LoVac AND ESEM MODES In these modes the column section is under the lower pressure than the specimen chamber where the pressure ranges from 10 to 130 Pa LoVac or from 10 to 4000 Pa ESEM These modes uses water vapour from a built in water reservoir or a gas from an auxiliary gas inlet The system automatically detects the gaseous detector installed and offers a relevant vacuum mode in the Vacuum Mode module When Low Vacuum ESEM mode is entered from ESEM Low Vacuum mode
210. ons have additional down arrow next to the right side Clicking the arrow displays a pull down menu with choices while clicking the icon performs a particular function cyclic changeover of choices setting the default parameters etc There are also some informational icons in the status field for instance that indicate some particular system status TOOL TIPS are activated when the cursor is left over an item on the user interface for more than two seconds A short explanation of the item appears until the cursor is moved away from the item PULL DOWN MENUS The microscope uses menu oriented software you perform functions by choosing items from the Menu bar The Menu bar selections contain pull down menus that display grouped listings of available commands or settings Some menu items are shown in grey and cannot be selected because of the system immediate condition Pull down menu selections followed by the ellipsis indicate that a dialogue box will display the same behaviour occurs when the selection is acommand Selections with a right arrow indicate that an additional submenu of choices will display If a selection is a parameter value the new value is updated immediately and a check mark appears in the pull down menu Using the Mouse Click on the menu item in the Menu bar then drag the cursor down to the desired selection and release the left mouse button Using the Keyboard Press ALT plus the underlined lett
211. or the Vented status Remove your sample if needed and remove the Cooling stage if installed 3 Click the Vacuum module Pump button to pump to the High Vacuum If you want to shutdown the microscope bypass steps 3 8 3 Overnight 4 Select the File menu Log Off to log off the present user and to provide the Log On dialogue for entering another one 5 Switch off the monitor 2 Standby 6 Click the Stop button to stop the xT microscope Server software T Exit XT microscope Server use the right mouse button and Windows xP 8 Switch Off the PC and the monitor 9 Switch off the Emitter see Chapter 6 2 10 Click the Shutdown button to shutdown the console and to stop the xT microscope Server 11 Exit xT microscope Server software use the right mouse button and Windows xP 12 Switch Off the PC and the monitor 0 compete 13 Disconnect the power cord and any other Shutdown optional input output if used Note LLLLZlIIILIIITTTTTT 2 Waiting for a new user leaves the status of the xT microscope Control software non operational and only the xT microscope Server software is active Therefore changing the user does not require Logging off Logging on at Windows xP level but just restarting the UI level 0 The power plug should not be disconnected The system can be left in this state if electrical power is supplied to the instrument because the pumps are running and pumping the column
212. or which is not compatible with the current mode is selected the imaging quad cannot be resumed Detector settings TABLE 5 11 ALL DETECTORS TYPES Maximum Pressure Detector Name Vacuum Mode Detected Signal Pa Note ERE Gaseous Secondary Electron GSED LoVac ESEM 1000 um aperture 750 S 500 M e aperture 2600 CCD camera 0 camera Loc NN light infra red light cc detector detector dependent gt dependent dependent Gaseous Backscattered GBSD LoVac ESEM SE BSE O 500 optimal 2600 Electron Gaseous Analytical GAD HiVac LoVac BSE 2700 ESEM Scanning Transmitted STEM HiVac LoVac TE any Electron Microscopy ESEM Photo Multiplier Tube PMT HiVac LoVac photons BSE 200 Backscattered Electron BSE Energy Dispersive X ray HiVac LoVac X ray photons ESEM Wavelength Dispersive X ray Dispersive X Wavelength Dispersive X ray WDX WDX X ray photons 3x10 x 10 Electron Backscattered EBSD HiVac LoVac BSE diffraction Diffraction Pattern ESEM pattern boldface text preferable vacuum mode SE secondary electrons BSE back scattered electrons TE transmitted electron S standard O optional Note Feed through connectors for some detectors are engraved to the cover next to them Operations Detector Types and Usage EVERHART THORNLEY DETECTOR ETD xTm Detector Settings EJ It is a scintillator photo multiplier type detector monitoring electrons generated by the primary beam int
213. orientation units on dies or RAM arrays the existing location to correct for any distortion correcting for any distortion Change in Scale ocales the axes together X can be scaled differently from Y Change in None Rotates both axes with a X and Y orientation can be Orientation fixed 90 angle between axes different Sample Navigation Navigation Montage This software feature enables to navigate along the sample surface when the field of view is smaller than desired limited by an aperture Target HFW for instance For this purpose it is possible to use up to 3 images which could be changed dynamically capture save or load anytime oet the Target HFW Horizontal Field Width range which influences informations fields the tiles number Map Size the HFW of each tile Single Image HFW and the Estimated Time for the procedure EA Navigation Montage Map Size single Image HF yy 3 4mm Estimated Time 2 13 min The Stage menu Sample Navigation mode is then automatically He P n set For the active quad the upper right corner green icon indicates the functionality A green rectangle showing the actually selected field of view in the active quad appears with the size corresponding to the magnification In quad s using Sample Navigation Selected Area Zooming and Get features could be used Notes The basic condition for a correct functionality is an equal stage rotation value for both captured an
214. ormally this raster consists of a series of lines in the horizontal X axis shifted slightly from one another in the vertical Y axis The lines are made up of many dwell points and the time of each dwell point can be shortened or prolonged dwell time The number of points per line can be increased or decreased as well as the number of effective lines resolution The result is a picture point pixel array Low or high resolution images can be obtained by changing these factors The larger the pixel array the higher the resolution of the image The image is created pixel by pixel in the computer memory and displayed on a monitor screen The signal emitted by the specimen surface as it is illuminated with the primary beam is collected by the detector amplified and used to adjust the intensity of the corresponding image pixel Because of this direct correspondence the image displayed on the monitor is directly related to the specimen surface properties The raster consists of many typically one million individual locations pixels that the beam visits As the beam is scanned the signal emitted by the sample at each beam position is measured and stored in the appropriate digital memory location At any time after the beam scan the computer can access the data and process it to change its properties or use it to generate a display MAGNIFICATION Magnification is calculated as the displayed image dimension L divided by the sample
215. ouse button activates a 4 arrow ended cursor The mouse motion starts the final lens alignment see Chapter 6 de iz g Software Control xT microscope Control Software The Stage Menu Alt S opens the stage and sample navigation functions see Chapter 7 Tool Window Help xT Align Feature xT Align Feature Compucentric Rotation Fle opens a procedure that helps to navigate along a feature that extends pensa serte off the screen at the desired magnification Compucentric Rotation F12 places a green circle in the active quad By rotating the circle a different viewing orientation of the sample area can be achieved by a physical stage rotation and adjustment of X and Y axes Stage rotation keeps the observed feature in the center of the field of view If this does not occur the alignment should be performed to locate the stage Home Stage shit F3 center and calibrate the stage see Chapter 6 Home Stage Without Rotation Center Position Ct 4 Touch Alarm Enabled Beam Shift Reset Zero Beam Shift Define User Units activates a procedure guiding the user to determine User Units for X and Y stage axes These are used for relative stage movements associated with the regular features mapping in particular integrated circuit applications Sample Navigation User Units Navigation Montage i i sic organises the stage software to recognise the defined user units Specimen Holder Wizard rather t
216. over the heater lifetime However if greater precision is required in the actual temperature read out follow the procedure 1 Put a small piece of calibration sample onto the standard ceramic crucible 2 Move the stage about 10 mm from the centre position to protect the sample to be blown away during pumping Pump down the chamber Obtain the sample image onscreen Start the 151 Temperature Calibration alignment 5 Reach the temperature 100 K below the expected melting point 50 K min ramp rate can be used 6 Slower the ramp rate to 10 K min and set the target temperature about 10 K above the expected melting point 7 Observe the sample and stop ramping just when the sample melts Enter obtained temperature to the Ag Au melting point Measured edit box AC By finishing the procedure the temperature readout is corrected to match the theoretical value A readout at a room temperature is not influenced and linear interpolation is applied between these points Other samples with a verified Theoretical melting temperature note the vacuum and chamber environment conditions could influence it can be used in the User defined calibration point edit boxes This introduces another point to the calibration profile HEATING STAGES BASIC OPERATIONS Setting up a Temperature Profile The temperature profile is a series of heating cycles consisting of a setpoint temperature ramping rate and soaking time The controller per
217. perations Detector Types and Usage DISCHARGES BETWEEN THE GASEOUS DETECTORS AND THE SAMPLE Excessive voltage may cause a breakdown between the detector and the sample chamber pole piece etc This could damage the sample at ground but does not damage the detector This condition is indicated by white flashes or streaks across the image and on some systems a large discharge could make the system unstable or cause the chamber to vent and switch off the HV There are several factors that could cause detector voltage breakdown Detectors e Contrast is set too high Contrast 39 4 e Sample is too close to the detector ig Gas pressure is low depending on the detector and the environment e Air in the chamber water vapour purge cycle not complete El B gt e Sample is not grounded to the stage or the stage is not fully grounded BNC plug not connected Brightness 50 0 OBTAINING IMAGE PROCEDURE FOR GASEOUS DETECTORS E 1 After the pumping and purge process click the Beam On button 2 The Contrast detector voltage adjuster in the Detector module is xTm Detector Settings Detector Settings automatically adjusted to 50 of maximum value Adjust it if Detector GSED vw necessary to increase a signal or to stop possible discharges The Enhanced Contrast adjuster electronic gain is set to the value last used 3 Atthe lowest possible magnification adjust the Enhanced Contrast Enhanced Contrast 55 5 and B
218. plate and a positive potential on the SE grid generating a mixed SE BSE image Enhanced Contrast adjuster the GBSD like other back scattered electron detectors works best with high beam currents and voltages Since back scattered electron yield is low for light atomic number elements using high voltages and high beam currents may not be a suitable option for these samples To solve this an additional contrast expansion circuit is provided Obtaining an images with the GBSD 1 Install the GBSD if necessary install the standard insert 2 Pump down and flush the chamber 3 In the Detector menu select GBSD Secondary Electrons Mode 4 From the Mode list box select Secondary Electrons The voltage changes automatically for SE imaging 5 Move the sample to a WD of 9 5 to 10 5 mm Backscatter Electrons Mode 1 From the Mode list box select Backscatter Electrons The voltage changes automatically for BSE imaging 2 Move the sample to a WD of 8 5 to 9 5 mm The closer the sample is to the detector the stronger the BSE signal is Mix Mode 1 Select the Detector menu Mix mode Slowly increase the contrast until an images appears on the screen SCANNING TRANSMISSION ELECTRONS MICROSCOPY DETECTOR FP 6903 01 The STEM is a two segment solid state diode mounted underneath the STEM holder It can be used at any available working distance preferably close to the lens for high resolution or at the eucentric position for
219. plies the mapping process bringing the long feature either to the horizontal or vertical axis to make the navigation easier This can be performed at any point within the stage field limits and takes into account the stage rotation offset FIGURE 7 12 XT ALIGN FEATURE Note xT Align Feature works best at the eucentric position see above Longer distances result in a greater accuracy Caution Watch the obstacles significantly extending from the sample plane as these may interfere with equipment under the lens TABLE 7 5 XT ALIGN FEATURE PROCEDURE Step Action 4 Select a long feature of interest on the sample Click the Stage menu xT Align Feature Choose either Horizontal or Vertical which relates to the desired sample orientation Click the first point along the feature with the left mouse button the P1 coordinates update xT Align Feature Feature Position Align Feature ES e Horizontal pore Vertical Click in the active Quad to specify the first point P1 Cancel otage Map Coordinates ritt Navigation Actual Go Ta x fose2s4s X uu um Mj g 9 9568 mm Liv LIF 0 Compucentric Rotation HE EEE i Last Position Add Update Remove Ma Stages Stage Related Functions TABLE 7 5 XT ALIGN FEATURE PROCEDURE Click the second point along the feature the P2 coordinates update Clicking the right mouse button anywhere in the imaging area deletes points
220. possible to correct it is usually a sign that this aperture needs to be cleaned or replaced The X ray PLA cone option 500 um aperture is used for EDX analysis see Chapter 9 at a longer working distance profile extends down to 8 5 mm Samples are imaged at 10 mm working distance which is the stage eucentric position and the collection point of the EDX detector It is used in conjunction with the LFD The longer profile of this cone minimizes the low voltage beam dispersion and skirting of the primary beam in the gaseous environment of the chamber allowing more electrons to interact with the specimen when focused and increasing the signal to noise ratio To fit the X ray PLA cone remove any existing detector or PLA cone from the standard insert then press the X ray PLA cone into place The Low kV PLA cone 500 um aperture is installed onto the standard insert in case the LFD is used for low vacuum and low voltage imaging i e below 5 kV to reduce beam loss in the gas It is used when imaging at shorter working distances lt 9 mm and restricts the lower magnification limit The Hot Stage cone option 1000 um aperture is used with the heating stage in combination with the hook wire or LFD It can be used without the hot stage when beam protection is desired with a larger field of view Note When the Pole Piece Configuration dialogue appears select the appropriate cone according to the figure and the name O
221. pre set and currently allowed values choose one and it is applied immediately see the Preferences Presets tab The Magnification is possible to display as the Horizontal Field Width HFW alternatively see the Preferences General tab The Spot is defined as the actual electron beam diameter on the specimen surface and it is expressed by a relative number see Chapter 5 Screen Pixel Resolution List Box contains list of the image sizes screen pixel resolutions available for capturing an electron image Selecting a new resolution results in the immediate change of the scanning raster and since the current dwell time remains unchanged the actual scanning frequency both Line and Frame time changes Software Control xT microscope Control Software IMAGE WINDOWS The xT microscope Control software displays images via 4 independent image windows called quads All quads can contain live image from any detector including External and CCD paused images or images loaded from a file Additionally quad 3 can display a mix of images from quads 1 and 2 and quad 4 can display a mix of images from quad 1 2 and 3 The four quads can be displayed either all at the same time in Quad Image Mode or one zoomed quad at a time in Single Image Mode Each quad consists of its image adjustable Databar containing the image parameters selectable overlay user defined colouring annotations measurement and some status symbols
222. pressure vertical axis against actual temperature horizontal axis If the Go To button either at Temperature or at Humidity tab is active which is represented by its yellow colour moving red line appears in the graph to depict actual pressure temperature values If the system is at the stable condition changing target humidity causes a pressure change Calibration For precise humidity control a calibration of each sample must be performed By obtaining condensation on a sample surface and correction of the theoretical 10096 relative humidity value to the actual conditions a temperature difference between thermistor readout and real sample surface temperature can be minimized assuming pressure readout is precise Calibration procedure 1 Set the sample pressure and temperature appropriate to 9096 humidity 2 Obtain a GSED image of your sample surface 3 Slowly increase pressure humidity until water drops start to grow on the surface Calbrate 4 Press right mouse button above the humidity graph area to call the Restore popup menu 5 Click the Calibrate item The Restore item sets calibration values to pure theoretical ones re System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 COOLING STAGES BASIC OPERATIONS Condensation Point When determining the Cooling stage condensation point use the flat sample holder This positions the sample closer to the thermistor thus giving a more ac
223. r Either mode can use water vapours from a built in water reservoir or an auxiliary gas which is supplied by the user and connected to a gas inlet provided for this purpose Observation of outgassing or highly charging materials can be made using one of these modes without the need to metal coat the sample which would be necessary for conventional HiVac mode opecimen exchanges take place through a chamber door which exposes the specimen stage when opened Exchange time takes a few minutes Software and interlocks protect the system against the damage and users against the injury B System Overview How Quanta FEG SEM Works IMAGE VIEWING AND CAPTURE Because the amplified detector signal is displayed synchronously with the beam scanning there is a correspondence between the brightness of an image point on the monitor screen and the signal detected at corresponding point on the specimen Magnification is the ratio of the size of the viewing monitor screen to the size of the area scanned on the specimen Increased magnification is achieved by reducing the size of the area scanned on the specimen POSITIONING OF THE STAGE A choice of computer controlled high accuracy multi axis stages offers precision specimen manipulation and automation for overall Spatial orientation on highly repetitive or extremely irregular samples FIGURE 2 2 QUANTA FEG 200 System Overview System Layout of Quanta FEG system Layout of Quanta
224. r User cannot be accessed Cyan background user has no userdata III A cS aaah About FEI User Management FEI User Management Version 1 0 Copyright FEI Company C 2002 Running on Local machine Red cross user account is disabled or lacked Software Control FE User Management Software Properties Alt Enter click to see and change the properties for that user The user must first be highlighted in the tree he Userdata menu contains the following items Copy Ctrl C click to copy user data from a user of the same or a lower level group Paste Ctrl V click to paste user data into your own account or into the accounts of a lower group level It is not possible to copy user data inside the FEI Supervisors User group e Remove click to delete user data from a selected account of equal or lower group level The Help Menu contains the following items e Legend clicking provides an explanation of icons used in the tree About displays the FEI User Management software version and copyright ACCOUNT LOGGING This accounting utility monitors user log on off actions session time filament lifetime and the UI status It works with two log files located in c Program Files FEl data accounting accounting tmp is a temporary running file during use of the equipment at each user session updated every 15 seconds so that any power down or operating system crash situation can be time lo
225. r sample preparation but in the Low Vacuum mode only Use all types of conductive and nonconductive particles e pressure of 60 100 Pa e accelerating voltage gt 10 kV e spot size gt 3 free working distance FWD 7 10 mm e image resolution gt 1024 x 884 dwell time gt 10 us Note Depending on the particle character electron beam induced jumping of particles can be observed using long dwell times Image integration can be applied to prevent this phenomenon but the calculated result will suffer by an error of app 5 96 Another way to prevent this phenomenon is to coat the filter with thin conductive layer before filtration SYMMETRICAL LOW VACUUM DETECTOR SLVD This detector is used instead the LFD to prevent shadowing effect of the observed particles Installation procedure 1 With your glowed hand grasp the detector by the rigid connector end Hold it with the detector head facing towards you and the four detecting electrodes facing down 2 Insert the detector gold fingers facing forward into the connector located at the back of the chamber behind the conical lens A keyed connector position prevents the user from inserting the detector upside down 3 Hold the detector head by its green sides not electrodes and push back the head onto the Standard Insert until it stops 4 Removing of the detector must be done in the opposite way than installing First remove the detector head from
226. r WENOL to clean parts as these can leave outgassing material Be aware that threaded surfaces should not be polished as these do not have contact to the beam and are a source of outgassing if polish is trapped Wash threads with alcohol or isopropanol if absolutely necessary After cleaning inspect all parts for residue and stains using a light microscope Down time can be reduced by purchasing spare Wehnelt and detector assemblies and having them cleaned and stored in a safe place where they can be ready to be installed into the microscope Maintenance and Troubleshooting The Standard Insert The Standard Insert The following tools and procedures are used to install and remove the standard insert from the lens pole and to assemble Pressure Limiting Apertures and the Insert body REMOVING AND DISASSEMBLING The following instructions describe how to remove and disassemble the standard insert assembly FIGURE 8 1 STANDARD INSERT COMPONENTS Housing O ring 1 Insert the universal detector tool found in the accessory toolbox pins into the matching slots in the insert assembly Once the pins are engaged twist counter clockwise to unscrew the insert from the pole piece FIGURE 8 2 UNIVERSAL DETECTOR TOOL 2 Use the Aperture Positioning Tool to remove the C clip and final apertures from the insert To do this insert the pin of the tool into the wide end of the insert and push the parts out of the narrow
227. r a higher immersion ratio preferably less FIGURE 9 47 SIGNAL DISTORTION AND IMAGE ABERRATIONS FOR TILTED AND ROUGH SAMPLE TIN BALLS AT HIGH IMMERSION RATIO 3 05k 5000eV Cathode Lens Mode Landing E tilt es 0 0 IT System Options Beam Deceleration FP 6842 22 Beam Deceleration Modulator Maximal Immersion Beam Deceleration Voltage 3000 V Landing Energy 2 00 keV E El El Immersion Ratio 2 50 E B HU Hv Landing E S 50k 500 00 e BEAM DECELERATION MODULE The Beam Deceleration module is accessible from the Beam Deceleration Control page It has following features The BD Mode button switches the BDM on off This is available only in the HiVac mode and with the Beam On When switching the beam off the BDM switches off too automatically The Modulator button starts to modulate the BDV in the range 100 V thereby it periodically changes the immersion ratio This is useful for an optimal sample tilt adjustment Checking the Maximum Immersion check box keeps the IR at the maximum for a particular setting BDV is at the maximum The Beam Deceleration Voltage BDV reflects the voltage applied to a sample Minimal value is 50 V The Landing Energy LE preset continuous adjuster sets the energy of the electrons reaching a sample surface This is achieved by changing the BDV when reaching its marginal values by changing the HV The Immersion Rati
228. r off Here are several possibilities how to quickly switch off the electrical power completely in case of emergency 1 2 Strike the large yellow and red EMERGENCY EMO button option If there is no one present proceed to Switch off the breaker switch labelled MAINS S0 through the hole at the cabinet back side which is placed at the very right side in the row If this is not easily accessible Turn off the mains wall switch if present and or disconnect the mains plug from the mains socket FIGURE 3 2 EMERGENCY S WITCH p J y r Ta DE SES a ee eae ats 1 MV va AN et Aa LI e ce D Se SET PORE ar Pig re oe i gt l 3 gt S on w E TT PA ES SF gt a P ad 7e a ie a 17 T J x E N o s E o v E q 4 apes ah N an Im a 0255 6 CAE Y JU UT ts gt a TS MA E SEN Oy Eure System Operation Quanta FEG System States SOFTWARE CONTROL This chapter gives an overview of the xT microscope Control referred to as Ul or sometimes xTUI in dialogue boxes xT microscope Server and FEI User Management software and describes the functionality of each part of the user interface It takes you from the first main window and menu bar through each item on the pull down menus Graphics illustrating most of the choices help you to locate the specific features The software interface controls most system functions including im
229. re in the chamber slowly changes to the selected gas type e Select Automatic to use pre defined values for Minimum eer Maximum Pressure and Number of cycles The Purge Settings displays the current default values e Select Custom to change the Minimum Maximum Pressure and eus the Number of cycles manually using the Custom Edit boxes Caution The maximum allowed pressure is 200 Pa 1 5 Torr for all currently available PLA Cones Hay Cone A Hot es Lone 1000 um p Operations Obtaining an Image Column Shas spot semon efe 0 s High voltage cole 20 00 kw 200x v zookv ao v SPOT SIZE The electron beam diameter usually represented as the Spot size is considered to be close to ideal when its edges just touch the neighbouring spot If it is too large overlaps occur and the image appears out of focus If it is too small electronic noise appears in the image There are factory preset Spot numbers selectable from the Column module Spot number list box and from the tool bar list box The last user spot size value used is also kept in the Spot number list Deciding which spot size is suitable for a particular magnification can be determined when you achieve good focus and astigmatism correction TABLE 5 4 SPOT SIZES AND RECOMMENDATION OF THEIR USE Spot size Best Use 52 Very high resolution mag gt 50 000x Standard imaging SE BSED LFD GSED 56 BSED CL
230. rightness if necessary until the bright circle of the used cone a El can be seen in the centre of the image p 4 Increase magnification and adjust Contrast Enhanced Contrast and Brightness more precisely Detectors Contrast O 0 Enhance 20 0 o m us m u m Brightness 45 6 Ex E la Operations Capturing and Handling a Single Image Capturing and Handling a Single Image ia 3 After obtaining a good image quality the image could be paused and saved It is possible to save an image using the File menu or using the ocandium database software option image saving function Setup the file name label and harddrive destination for the image to be saved using the next available label number prior to the capture session Set the databar informations important for the archiving see the Preferences Databar tab The conditions for good image quality are e Slow scan speed longer dwell time of the beam e Select a pixel resolution from the dropdown list box to suit the detail in the image i e no tearing pixelated edges Increase the magnification at least 2x above the desired value focus and stigmate using the reduced area then return the magnification back e Use the Videoscope to correct the Contrast and Brightness accurately otherwise use the Auto Contrast Brightness procedure SNAPSHOT PHOTO PAUSE BUTTON The Scan menu Snapshot F4 Photo F2 function
231. rnal Z coordinate so that the specimen top surface coincides with the adjuster Eucentric position Close the chamber and pump it down owitch on the beam focus the specimen top surface and run the Link Z to FWD function see Chapter 4 The WD is now recognised by the system as the Stage module Coordinates tab Z value The Z coordinate can now be changed via the manual or software Z control around the eucentric position and further but not less than 1 mm from the lens for safety reasons Stages Stages Types and Accessories STAGE MOVEMENT LIMITS The motorised movements of the stage can be operated under software control for more advanced location mapping This includes Shift Get Track and the Stage module functionality A live image can be repositioned either by the stage movement manual or software or by the Beam Shift The tilting mechanism can be locked for more Stability at high magnifications using the software Clamp feature Note When moving the stage or tilting the specimen the magnification may need to be reduced not to lose the feature of interest off the screen Caution The positive Z value direction depends on the Link Z to FWD status see below FIGURE 7 6 STAGE MOVEMENT SCHEMA stage door TABLE 7 3 STAGE FEATURES AND LIMITS 100 mm 150 mm Note 25 25mm 0 60 mm internal external 25 to 25 mm 50 to 50 mm 75 to 75 mm NENNEN 25 to 25 mm 50 to 50 mm 75to475mm 15
232. rom the specimen holder INSULATO P COMDUCTOR HEAT ABSORBED COLD JUNCTION Ss VN CC Pe laa ee Ed AAA AAA HEAT REJECTED HOT JUNCTION System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 FIGURE 9 12 COOLING STAGE ASSEMBLY MOUNTING ADAPTER WITH MOUNTING SCREW The Chamber feed through Plate provides feed through connectors for the cables and water hoses FIGURE 9 13 CHAMBER FEED THROUGH PLATE INSIDE OUTSIDE Heating Stage connector Water hoses flanges blue colour Cooling Stage connector Cooling Stage Controller This microprocessor controlled board provides accurate and stable automatic temperature control of the cooling stage and interfaces with the xT microscope Control software The temperature measurement accuracy is determined by the thermistor and the controller These specifications are as follows e thermistor accuracy 0 1 C e normal limit temperature range 20 C from an ambient temperature from 25 to 55 C Additionally accuracy of a temperatures readout depends on sample conductivity thickness shape and general thermoelectric properties that vary by sample and mounting method Cables The Outer Cable connects the outer feed through plate side with the controller board The Inner Cable connects the inner feed through plate side with the cooling stage to which the cable is permanently attached moo System Options Co
233. roperties box Path to the directory where the image dataset will be stored Prefix of the file name the file name consist of the prefix plus the sequence number in the matrix and the Image format is defined here Further a choice of Single numbering of stored image files and or Overwrite existing files are available in this box Region properties Number of images in X Y will be saved in a matrix with X rows and Y columns that is specified here Overlap between images can be further preset Note Use negative overlap to ensure a space between acquired images Status Progress in the image acquisition i e total time required for saving defined image dataset and time remaining to the end to the Mapping procedure is shown here Switched off beam when finished check box enables to switch off the electron beam after the image dataset saving is finished Note Due to safety reasons the Mapping tool is preset to Stay on top Caution User Interface is active during the Mapping procedure Any change in the UI high voltage spot magnification free working distance etc will cause change in saving images and devaluation of the image dataset Image Analysis System Options mage Analysis The Morphologi software is used for the image processing of saved images and calculation of morphological data of particles The Morphologi SW is installed on the Support PC Detailed description of the image processing and particle
234. s Instructions Instructions Nate Use Quad 1 for the Adjust the Contrast and Adjust the Contrast and procedure Brightness when necessary Brightness when necessary This alignment procedure Adjust the Stigmator X Adjust the Stigmator Y minimizes the X Y Stigmator alignment 2D control far a alignment 2D control far a image shift minimum image shift It is minimum image shift It is possible ta increase the possible ta increase the magnification for a better magnification for a better precision The Amplitude for precision The Amplitude for the Modulator could be set the Modulator could be set No step Step 2 of 3 Step 3 of 3 Alignments 2 Stigmator Alignment stigmator X alignment stigmator alignment E Auto Instructions Focus the image Adjust the Contrast and Brightness when necessary Clear Mernory Clear Memory Amplitude 0 0060 Amplitude 0 0060 Ej m g E m g Contrast b2 5 Contrast Be Ei E a E i 3 step 1 of 3 A Brightness ENS Brightness ENS EN p E K E 3 Cancel Cancel Contrast b2 5 E H Ini M Brightness ENS A g Alignments 3 Stage Rotation Centre 3 Stage Rotation Centre Alignments Instructions This alignment procedure sets the stage rotation centre for the compucentric rotation Mo step Alignments 3 Stage Rotation Center Next cet the Working Distance to 10 mm Focus the image Adjust the Contrast an
235. scanned dimension l If the observed sample point size is made smaller while the monitor size remains constant the magnification increases At low magnification you get a large field of view At high magnification you point only a tiny sample area Operations Optimising an Image JO lao SO rx 1 OO a QUOC 10 gogx 30 OOO 100 oaos 300 OI Alternatively Magnification could be expressed as the Horizontal Field Width HFW specifying dimension of the scanned area see the Preferences General tab The Quanta FEG supports two viewing sizes Quad Image and Single Image modes Magnification is always adjusted in the databar for the current display thus an image at 500x in Quad Image mode is 1000x in the Single Image mode as its size has doubled FIGURE 5 1 MONITOR IMAGE AND SCANNED SAMPLE L Wewed length f Scanned length Magnification Monitar Changing Magnification The Tool bar list box is used to select from a predefined values e The Keyboard control the numeric pad plus key the minus key increases decreases the magnification 2x and rounds the value when using the HFW no rounding takes place The star key rounds the magnification HFW value e g 10 063x becomes 10 000x The Mouse wheel control Coarse fine control can be operated by holding the Ctrl Shift keyboard key and moving the mouse wheel up down to increase decrease the magnification
236. significant interest on the sample area TOOLS Selected measurement or annotation tool is displayed as the tool icon Clicking the icon activates deactivates the tool the active one is highlighted Clicking the arrow next the icon symbol opens the list of available tools to choose The appropriate icon is shown from that time on and the item can be drawn on screen The drawn items are listed in the list box The Measurements enable to gain dimension information about a specimen feature by overlaying it with a measurement graphic By changing the magnification these graphic elements resize accordingly The Annotations enable to graphically label items of interest The Text enables to add further information The Trash can button deletes selected item s The Property Editor enables to change a property of a selected Measurement Annotation Text graphic by a selection from the dropdown list or by a direct editing of a text or a value Shape Creating 1 Choose the suitable Measurement Annotation graphic tool 2 Draw the graphic over the area of interest This can be done by dragging the cursor from the top left corner to the right lower corner of the shape holding SHIFT key while dragging the shape starts to grow from the point where you have clicked as from the centre 3 Choose the Text symbol and then just click where you require a text in the image Type the text into the Property editor text field
237. sory to the Quanta System Series The items covered here are e Manual User Interface e Joystick e Automatic Aperture System e Optional Detectors e X ray Analysis for Different Vacuum Modes e Temperature Stages e CryoCleaner Quanta Morphologi e Remote Imaging Beam Deceleration e Specimen Holder Kit option For further information on any of these items please contact your local FEI representative System Options Manual User Interface FP 2311 05 Manual User Interface FP 2311 05 The Manual User Interface MUI provides knobs to perform functions that can also be performed with the software It is connected to the USB connector located on the microscope controller FIGURE 9 1 MUI The MUI offers additional flexibility for controlling magnification beam shift focus astigmatism contrast and brightness Joystick FP 2311 01 The Joystick provides knobs to perform functions that can also be performed with the software It is connected to the USB connector located on the microscope controller FIGURE 9 2 JOYSTICK The Up Down lever motion moves the stage in Y axis The Left Right lever motion moves the stage in X axis The Left Right lever rotation rotates the stage left right The button 1 is not used e he button 2 is used together with the lever motion Up Down moves the stage up down regardless the Link Z to FWD status Left Right tilts the stage left right only
238. st be taken when using this mode to collect X ray results FIGURE 9 8 X RAY IMAGING WITH THE GSED EDX Detector Beam skirt due to gas dispersion Sample Some of the electrons are deflected due to interaction with the chamber gas The deflected electrons form a skirt around the main beam The skirt electrons will hit the sample at points that are remote from the area of interest and generate X rays from these points The number of skirt electrons increases with chamber pressure and the distance that the beam travels through the gas The effect of these skirt electrons can be minimized by reducing gas pressure or by shortening the distance between the sample and the final PLA The X ray detector is designed for the sample to be at 10 mm WD which is too long for optimum imaging with a high pressure detector such as the GSED For this reason the ESEM is supplied with a special X ray PLA which is used in conjunction with the LFD to give the best results Mo System Options Energy Dispersive X ray EDX Analysis GAD EDX ANALYSIS Maximum detector response is around the 8 5 mm WD providing an atomic number contrast when the resolving power is better than O 1 in the Atomic number range around 20 FIGURE 9 9 X RAY GAD CONFIGURATION IN ESEM MODE Electron beam EDA Detector Position cutout towards X ray detector 350 Ton st 3 GAD E 4 X ray cane CHEM Minimal b
239. stage either mechanical or motor driven where appropriate TABLE 6 1 ALIGNMENT PROCEDURES OVERVIEW Procedure Function Final Lens Aperture Strip Mechanical alignment eliminates image shift when focusing Alignment 1 Gun Alignment Centres the electron beam at various high voltages and spot sizes 3 Stage Rotation Center Sets the stage rotation centre for the compucentric rotation 2 Stigmator Alignment Eliminates image shift during normal stigmator correction 5 Emitter Startup Enables electron gun Emitter switching On Off Alignments Quanta FEG System Alignments BUTTONS AND CONTROL ELEMENTS The following particular buttons and control elements have the same behaviours for all alignment procedures when available The Start button starts the procedure and proceeds with following dialogues The End button moves the user to the last step by clicking the Next button to be able to finish the alignment procedure The Contrast Brightness adjusters enable to optimize the image quality during alignment The Auto button executes the appropriate alignment action automatically for a particular voltage spot direction whatever suitable with the use of the Image Recognition software If this utility does not recognize image features well the procedure is aborted and Warning message appears onscreen In this case change the imaging conditions better focus slower scanning or lower magnification and
240. steps 7 Status Note The number before the module name represents an order in which the modules are introduced in the following text 1 The Vacuum Mode module is used to control the pressure and the gas type in the specimen chamber The Pump button starts the pumpdown procedure for the specimen chamber and the column The system allows the accelerating voltage to be switched on only when the column is sufficiently evacuated The Vent button starts venting for a sample or detector exchange after the user confirmation see Chapter 3 and 5 The Mode radio buttons bring the system to the High Vacuum mode which is the conventional operating mode associated with all scanning electron microscopes used for observing conductive specimens that can withstand low pressure conditions and do not outgas In this mode the system pumps continuously to achieve the lowest possible pressure the Low Vacuum for observing non coated and non conductive or partially conductive specimens e the ESEM Mode for observing natural status of samples In these modes the chamber pressure is controlled using the Chamber Pressure preset continuous adjuster while the column is at a much lower pressure The gas environment can be selected from the list box The system automatically switches to one of the modes when the chamber is Vented and a dedicated detector is installed If no dedicated detector is installed user is asked to determine a det
241. t Angle is equal to the stage tilt plus the Specimen Pre tilt linear adjuster value a Tilt Angle correction in case the specimen is not parallel to the stage XY plane The Manual linear adjuster enables to manually set the Tilt Angle from 90 to 90 It is useful when the Dynamic Focus with Automatic Tilt Angle does not give satisfactory results or cannot be used at all because the specimen is tilted in direction different from the stage Tilt When switching from Automatic to Manual mode the actual Tilt Angle is not changed When switching to Automatic mode the Tilt Angle is set to the actual stage tilt If the Dynamic Focus is on and the Tilt Angle is non zero an indicator is displayed in the optical quad see the Preferences General tab Notes Both Dynamic Focus and Tilt Correction work properly only if the specimen scanned area is tilted around the X axis in the same direction as the stage Tilt Therefore they cannot be used with Automatic Tilt Angle in combination with a non zero Scan Rotation If the specimen is tilted in a different direction you have to align the tilt axis horizontally using the Scan Rotation and then optimize the image focus by tuning the Manual Tilt Angle Both functions are also disabled cleared in the Crossover mode Due to the limited range of the dynamic focusing the overall conditions should be in certain limits If the dynamic focus would be out of the range the checkbox becomes d
242. t magnifications above 20 000x water moving through the CS Causes small vibrations To prevent this shut the water off temporarily using the valve on the water hose line attached to the chiller The Stage continues to cool the sample for about 15 minutes without water cooling After this time the sample temperature rises CAUTION If the cooling stage is used without a heat sink connection severe damage may result to the thermoelectric module Do not operate the CS for longer than 15 minutes without cooling water else damage occurs to the device Cooling below Ice Point In most cases the power of the thermoelectric module is not sufficient to freeze large quantities of bulk water Small water drops can be frozen on the stage using the following procedure 1 One can set the external water chiller to 5 C Allow the chiller time to cool the water Keep the pressure in the chamber below 800 Pa 6 Torr to keep water from condensing on the cooling lines 2 Set the temperature of the cooling stage to 5 C As the temperature drops decrease the pressure gradually to 400 Pa 3 Torr at the same time as the temperature reaches 5 C If the pressure is dropped too quickly the bulk water in the sample evaporates conversely if the pressure is reduced too slowly water condenses onto the sample and raise the temperature System Options Cooling Stage FP 2300 12 Waterless Cooling Stage FP 2300 21 WATER COOLED TEMPERATURE STAGE
243. t stage back to 0 to finalize wizard setup Resize the box to capture only the specimen holder top surface refer ta diagram stage Position T 45 2 Fane eer ace oe NEUE Previaus Note When the manual tilt stage is tilted the Ul readout of the tilt angle may be different from the stage scale and the procedure cannot continue It is necessary to set the tilt angle to get the readout within the range 2 from the required value Using the Holder Image When the Specimen Holder Image procedure is completed the bitmap image of the holder loaded taken from the CCD camera is transformed to the Stage module Map tab Clicking any sample image drives the stage to place that sample in the field of view The holder image starts without any Location list positions These can be added to map the positions of all samples The holder image can be enlarged 5x at most see above The Clear Holder Image item removes the holder image from the Map Location positions stored in the holder image mode retain in the Map Location pen cave Clear Last Position 20 20 Stages Stage Related Functions Fause Snapshot Photo Videoscope Reduced Area e Full Frame Spot Line External Beam Blank Slow Scan v Fast Scan Slower Scan Faster Scan Mains Lock v Live Average 16 frames Integrate 256 frames Scan Rotation Preferences Beam Stage Tools Window Hi F6 F4 F2 F3
244. t surface a glass block is ideal and apply a small amount of Soft Scrub or CIF and distilled water to the cloth Place the part to be cleaned on the polish and rub with a circular motion until all contamination has been removed For inner surfaces use a cotton swab or wooden dowel as an applicator A toothpick can be used for small holes Lint free nylon not cotton or latex surgical gloves should be worn while handling parts to avoid contaminating just cleaned surfaces Tweezers should be used to hold small parts After the part has been polished remove the Soft Scrub CIF cleaner by washing in hot water Inspect the part under a stereo microscope at 20x magnification to ensure that there is no remaining contamination or polish residue Wash the part in de ionized or distilled water in a beaker with an ultrasonic cleaner for several minutes Transfer the part to a clean beaker with alcohol or isopropanol and clean ultrasonically again for several minutes Note Do not use an ultrasonic bath to clean the GSED or LFD detector When the components are dry a compressed air duster can speed drying reassemble and return to the column If a part is stained heat it with hot water and immediately rinse with alcohol and dry using compressed air Cleaning Tips Parts exposed to the electron beam require periodic polishing This will ensure maximum performance of the instrument for many years Do not use metal polishes such as POL o
245. ter causes the image to blink and get noisier on the other hand the averaging slows down the image response to the changed parameter Display beam icon in databar Yes No Adds an active beam icon to the first data bar position Blinking pause icon during image integration Yes No If Yes is selected the blinking Pause symbol is displayed in quads which are being stopped Otherwise the Pause symbol appears only after the image acquisition has actually stopped Display Recording Movie message No 1 second 2 seconds 5 seconds 30 seconds At the beginning of the movie recording this message could be displayed in the recorded quads for a selected time period Hide Rotation controls when not used No 10 seconds 30 seconds 60 seconds opecifies if and when the on image Scan Compucentric Rotation control should be automatically switched off Display Scan Rotation in CCD quads Yes No Specifies if the Scan Rotation indicator and value should be permanently displayed in the optical quad s note that only non zero Scan Rotation is displayed Display Tilt Corrections in CCD quads Yes No opecifies if the Dynamic Focus and Tilt Correction indicator and values should be displayed in the optical quad s only non zero values are indicated Reset Enhanced Image parameters on file open Yes No When opening an image applied enhancement corrections remembered for the quad are reset irreversibly Name Micros
246. the function linked to the left mouse button mo Restart Average Filter when magnification changes e Restart Average Filter when scan rotation changes Restart Average Filter when beam shift changes Restart Average Filter when stage moves e Display beam icon in databar Blinking pause icon during image integration Display Recording Movie message Hide Rotation controls when not used Display Scan Rotation in CCO quads Display Tilt Corrections in CCD quads Reset Enhanced Image parameters on file open Software Control xT microscope Control Software Switch sample tracking on mouse wheel click Yes No Switches the tracking movement control linked to the mouse wheel between click and move and click and drag modes Spot Size Step 0 1 0 01 0 001 This enables to set the accuracy of the spot size setting Enhanced Contrast slider besides Contrast Yes No enables to show the Enhanced contrast control next to the Contrast in the Detector module In this case the corresponding control in the Detector Settings module disappears Image and graphics Restart Average Filter when magnification changes Yes No Restart Average Filter when scan rotation changes Yes No Restart Average Filter when beam shift changes Yes No Restart Average Filter when stage moves Yes No The above three items enable to choose whether the image averaging should be restarted when the indicated parameter changes Restarting the Average Fil
247. the microscope Note Preparation to clean or replace apertures should be immediately available as the specimen chamber has to stay at atmospheric pressure for the duration of maintenance A Maintenance and Troubleshooting Aperture Strip Module CLEANING THE APERTURE MODULE This is only possible if a Fischione Plasma cleaner is available 1 Take the complete rod with module attached and place in the TEM Opening on the plasma cleaner The screw at the end of the Aperture rod screws into the TEM opening and seals against the rod o ring 2 Give the rod 5 minutes at 4 5 volts plasma generation This should remove all hydrocarbon base contamination If the contamination is stubborn longer times will be necessary this should not damage the aperture as the plasma only removes organic bases REPLACING THE APERTURE MODULE The new Aperture Module comes in a container has been cleaned and is ready to be fitted to the rod 1 Unscrew the Titanium screw holding the old module onto the rod Keep the screw in the hole of the rod and let the module fall away 2 Open the new module pack and let the new module sit with the connection end uppermost to the edge of the container base 3 Pick up the new module with the Titanium screw end and fasten making sure of a good fit REPLACING THE APERTURE ROD 1 Check that there are no fibres on the rod o ring Do not grease the o ring 2 Replace the Aperture rod back in
248. tion The scan makes one screen quad pass or several passes when the number of integrated frames is larger and pauses The image can now be saved by File menu Save Ctrl S Save As function e Open opens a single image file into the active quad The dialogue displays by default the location used in the last Save As utilization Print Ctrl P opens the printer setup dialogue so that the choice of printer and settings can be established to print the active image Pressing OK in the printer setup dialogue activates the printer to print the job TABLE 5 18 IMAGE PRINTING PROCEDURE oet the Magnification the Scan condition the image pixel Resolution and the required databar informations Capture the image or open an existing image from a memory Click on Print Ctrl P in the File menu a print dialogue appears Complete the print setup and click the OK button The image now goes to the printer Note Some printers may not work with high resolution images because they do not have sufficient memory ee Operations Recording Movies Saving Multiple Images Recording Movies Saving Multiple Images This function captures dynamic experiments performed with the microscope and creates the digital video files AVI Up to 4 imaging quads not the optical one can be recorded simultaneously with a synchronized start It is possible to switch between single and quad image window while the v
249. to alter the chamber pressure High resolution imaging is achieved by moving the sample closer to the pole piece the objective lens performs the better the smaller is the WD Adjust the chamber pressure see above the pressure should be a little higher Note oome experimentation may be necessary as the relationship between WD and chamber pressure is largely sample dependent Caution Always take care when moving the stage up because of possible lens pole contact DIGITAL IMAGE ENHANCEMENT IMAGE MIXING IMAGE COLOURING The Enhanced Image module offers various digital image enhancements Note When saving the image with the digital enhancements applied be sure to choose the correct file format see below The LUT Look Up Table Tab enables to monitor and modify a grey level distribution histogram The Presets list box enables to select the Digital Contrast Digital Brightness and Gamma values using pre defined or custom presets The D Contrast continuous adjuster sets a contrast in the range from 10 to 10 negative values lead to an inverse imaging The D Bright continuous adjuster sets a brightness in the range from 2 0 to 2 0 e The Gamma continuous adjuster corrects image brightness non linearly in the range from 10 to 10 The Graph window graphically displays blue line an applied modification Original modified values are on the horizontal vertical axis The Histogram button switch
250. to the Aperture Adjuster assembly on the column and turn the end screw mechanism until the holder is hand tight 3 Pump the microscope specimen chamber 4 Reconnect the heater cable to the outer end of the rod if necessary 5 Select the 30 um aperture so that alignment can be performed APERTURE AVAILABILITY These apertures are the present used and come in two size types FP 6174 33 Mo Strip Aperture 30 30 40 50 100 micron This type can be used for general applications including EDX e FP 6174 53 Mo Strip Aperture 30 30 50 30 30 micron This type can be used for high resolution applications such as low voltage Note These apertures are on purpose made for the 7 position Aperture Adjuster assembly although they will fit the earlier 4 position design not all apertures can be accessed Gaseous Detectors Maintenance and Troubleshooting Gaseous Detectors CLEANING THE GSED LFD FIGURE 8 6 REMOVING THE GSED ASSEMBLY Vent the chamber Pull the end of the GSED detector head down to remove it from the standard insert The insert will remain inside of the pole piece Pull the GSED pin contact board out of the signal connector mounted to the chamber ceiling The PLA is part of the GSED detector and can be cleaned by inserting a toothpick or something similar into the hole The signal ring is permanently attached to the underside of the detector and can be cleaned in a similar way CLEANING
251. to the signal connector inside the chamber On the other end of this board is a wire which clips onto the cap The detector is located just above the heat shield Any working distance can be used FIGURE 9 22 HIGH TEMPERATURE GSED Note The operating characteristics of the GSED and the high temperature GSED are slightly different Installing the High Temperature GSED a 1 Vent the specimen chamber and open the stage door 2 Snap the wire hook on the printed circuit board onto the cap Y System Options Heating Stage 1000 FP 2300 02 Heating Stage 1500 FP 2300 06 3 Plug the printed circuit board adapter into the connector on the chamber ceiling 4 Press the cap onto the final lens aperture standard insert 1000 C Heating Stage variances Heat Shield is a small part sitting on the HS assembly top The heat shield is most effective above 600 C where the sample is more prone to a radiant heat loss In this environment the heat shield creates an oven effect helping to keep the temperature consistent throughout the sample Crucibles Crucibles have a finite lifetime and are meant to be disposable when it becomes too contaminated and can no longer be cleaned Ceramic crucibles also shrink after some time of use This could cause vibrations if the crucible does not fit tightly in the heater A Ceramic paper pad provided with the HS option is used to fix the crucible Place the paper or a part o
252. try again The Crossover button activates the Crossover mode where the onscreen image shows the electron source tip instead of the sample Alignments Final Lens Aperture Strip Alignment Final Lens Aperture Strip Alignment This mechanical alignment eliminates an image shift when focusing The position of the final aperture should remain constant and should not be changed further during the alignment procedure When the aperture is well aligned the image does not rotate at low magnification or move at high magnification during focusing TABLE 6 2 ALIGNING THE FINAL LENS APERTURE Step Action Set the accelerating voltage 20 kV Spot size 3 WD 10 mm magnification 1000x Click the Stage menu Beam Shift Reset see Chapter 4 Click the Stage menu Zero Beam Shift see Chapter 4 Click above the Tuning module Lens Alignment 2D control with the right mouse button and select Zero see Chapter 4 Find a recognizable feature on the sample surface center it onscreen and optimize an image as best as possible to the fastest value the objective lens modulation starts and the alignment cross appears in all imaging quads center Adjust the aperture position so that the image rotation center is under the alignment cross Increase the magnification to 20 000x if necessary to 40 000x and realign When corrected click the Lens Alignment tool bar icon to switch it off Note After the mechanical
253. tton its coordinates appear in the Details module xTm Define User Units Alignment Point One User Units Definition Move to user point 0 0 to define then click on feature Details User paint in specimen coordinates a 0 174 mm v 0 082 Details Cancel Previous Finish Repeat the step 3 for the sample user point 1 0 xTm Define User Units Alignment Point Two User Units Definition Move to user point 1 0 to define then click on feature Details User paint in specimen coordinates x 0 010 mm Y 0 066 Details Cancel Previous Finish Stages Stage Related Functions TABLE 7 6 USER UNITS DEFINING PROCEDURE Repeat the step 3 for the sample user point 0 1 xTm Define User Units Alignment Point Three User Units Definition Move to user point 0 1 to define then click on feature Details User paint in specimen coordinates x 0 029 mm 0 010 Details Cancel Previous Finish Check the Details if needed or Finish the procedure xTm Define User Units Finish Current User Units defined on three points Warning The angle between the X and Y axis of the User Units is 28 degrees Details Cancel l Finish Using 1 2 or 3 Point Alignments TABLE 7 7 ALIGNMENT TYPE DIFFERENCES 1 Point Alignment 2 Point Alignment 3 Point Alignment Aligning to new point Aligning the stage axes with Transforming to nonstandard directly offset from the specimen X Y
254. tuation dashes or other non alpha numeric characters otherwise the movie maker is not able to build an AVI e The Save in a path to an existing directory must be entered here otherwise the Movie tab cannot be closed Use the Browse button to find the location The Numeric Seed enter any number from 1 to 999 which is converted to the three digit form with leading zeros The numeric seed is automatically incremented after the recording has stopped or the video file size limit has been reached The Video File Size the maximum AVI video file size lower than 2000 in MB must be entered here otherwise the Movie tab cannot be closed After reaching this size the video file is closed and a new one is automatically created without interruption of the recording process A dialogue warning appears if the hard drive lacks sufficient free space The File Type the list box with supported video compression format types Try to change the format if the resulting movie files are too big or if the system is overloaded during the movie recording he Record Databar check box allows the databar to be included in the video tif files Ma Operations Recording Movies Saving Multiple Images MOVIE PROCEDURE The red dot button starts the recording of all live electron image quads at the same moment no video images are stored for paused quads When a quad is paused during the video recording the storing of the vide
255. ually better visible at higher magnifications 3000x or more You need to correct astigmatism when you change the imaging conditions E Sample 4 2 10 mm WE Operations Optimising an Image TABLE 5 10 CORRECTING ASTIGMATISM Step Action to Focus the image as well as possible Bring the image just slightly out of focus The image appears to become sharper in one direction whereas in perpendicular direction image blur increases blurring or stretching of the image Bring the image just slightly out of focus in the other direction to observe the opposite directional blur Focus to the midpoint between the two directions where the blur is visible 1 Use the Beam module Stigmator 2D control 2 The Mouse press shift and hold the right mouse button pressed while in the active quad This results in a 4 arrowed cross appearing on the screen with the cursor position at its centre Still holding the right mouse button down move the cursor around the screen to achieve maximum sharpness When you are satisfied release the mouse button 3 The MUI optional adjust image sharpness with the stigmator X and Y knobs until the best image is achieved The computer beeps when the stigmator limits are reached 6 Repeat steps 1 5 as necessary If astigmatism is severe and the cross is close to the edge of the screen when nearing correction release the right mouse button and reposition the cross in the
256. uctions Press the IGP On button to start the pumps Wart until the acuurn status Press the Emitter On button to start or the Emitter Off button to stop the emitter is OK Wait until the ramping is finished step 1 of 2 step 2 of 2 Gun vacuum page Emitter startup page Emitter Off IGP Upper 1 96e 007 Pa IGP Lower 9 00e 006 Es Remaining time O min DO s supressar 500 W Extractor 4240 Filament 2 290 4 Emission 176 0 uA Emitter Life Time 125 hours OF min 15 s Cancel Cancel 7 STAGES This section describes the stages and their control possibilities The software control is similar for each stage and it is an integrated part of the xT microscope Control software The scopes covered in this Chapter are the following e Stages types and accessories Quanta FEG 200 50 mm 4 axes motorised Quanta FEG 400 100 mm 5 axes motorised Quanta FEG 600 150 mm 5 axes motorised e Software Stage Functions e Stage Related Functions Note The clamping mechanism 100 mm and 150 mm stages is controlled via electrical valve and software control Stages Stages Types and Accessories stages Types and Accessories QUANTA FEG 200 50 mm STAGE The stage has the X Y Z and Rotation movements motorised all with a manual override and the manual Tilt movement All movements are read out on the screen under software control The Z coordinate can be controlled by the external 25 mm Z control an
257. ues Clicking the X Y axis in the same way displays a 2 axis arrow cursor which can be moved in the corresponding direction To fix the values release the mouse button and the position of the crosshair is updated Clicking inside the 2D box with the right mouse button opens a dialogue showing the choices e Coarse Fine switches the 2D control sensitivity e Zero brings the 2D control to the center of the box e Back brings the 2D control one step back only one step is remembered The menu may contain also other functions that are actually available for the particular parameter Select the corresponding menu item to activate the function MODULES visually combine various software elements which are related into a labelled group Complex software elements like Ul pages or dialogues are typically composed of modules DIALOGUES appear when the system needs more information from you before it can carry out a command or want to give you some important actual information Some dialogues do not let you access other functions until you close them other ones let you perform other tasks while they remain onscreen and active for example the Preferences dialogue can remain opened while performing other tasks TABS In modules or dialogues containing more interface elements than would fit into the limited area the Tabs are used These related elements are split into the groups sections and each one is supplemented with the l
258. umed quad only low resolution and slow scan In case the xT microscope Control user interface stops responding or the Server Busy dialogue appears the Microscope PC is probably overloaded and may have problems with the current conditions being operated remotely If such a problem occurs wait till the Microscope PC recovers or restart it yourself when necessary Here are some recommendations for the remote control operation e Bevery careful when navigating the stage Always keep in mind that what you see in the CCD camera image is not the exact position of the stage because of delay in imaging data transmission e You can improve the performance response time by setting the more convenient scanning conditions quad instead of full screen single quad running instead of more quads resumed lower resolution slower scan i e higher dwell time Benefit from the automatic functions that are not affected by the delayed response problem Auto Contrast Brightness Auto Focus Auto Stigmator In case you prefer to focus or use the Stigmator manually it is better to do so in the reduced area g System Options Beam Deceleration FP 6842 22 Beam Deceleration FP 6842 22 The Beam Deceleration mode BDM method is based on a negative voltage up to 4 kV applied to a sample Beam Deceleration Voltage BDV The electrical field between the sample and the nearest surface above a column bottom or a detector is forme
259. until Vacuum status indicates Vacuum because detectors do not start operation till desired pressure is reached System Operation Quanta FEG System States Quanta FEG System States There are several system states Complete Shutdown service and emergency reasons Shutdown when not using the system for more than 10 days Standby when not using the system for more than 1 day Overnight when not using the system overnight Full Operation when working TABLE 3 2 STARTUP PROCEDURE GENERALLY b0N O System State Action 0 Complete 1 Connect the power cord to the microscope Shutdown console a compressed air and a nitrogen inlet optional for venting and cooling Interlocks prevent the vacuum system from operating if any of these are not present with the exception of nitrogen inlet 2 Push the power button on the microscope front control panel 2 Standby 3 Switch on the PC The operating system 2 Windows xP loads and displays the appropriate i icons on the monitor desktop PO 4 Double click the xT microscope Server icon to server start the software all seeming LEDs should be 3 XT microscope Server green Server state Console devices 5 Click the Start icon to start the server Wait until all dialogues are fully functional 3 Overnight 6 Click the Start UI button to start the xT microscope Control software The main window appears behind the XTUI Log On dialogue 7
260. ure strip type and adjusts the positions of the Individual apertures Mo step Alignments 6 Aperture Alignment Instructions elect the aperture strip you A actually use In case the microscope seems to be heavily misaligned aperture position qun tilt shift press Reset Gun E Tables button and Remove User Data button set carefully aperture positions in this procedure and continue with procedure 1 Gun Alignment step 1 of 2 Aperture strip 10 15 20 30 30 um t 20 30 30 40 50 um 30 30 40 50 400 um Gun alignment Reset Gun Tables Aperture alignment Remove User Data Cancel Alignments 6 Aperture Alignment Previous Finish set the aperture Position using the 0 control ta get an illumination Switch on the Modulator and adapt its Amplitude Adjust the position to place the image rotation center under the center crass Repeat these steps for each Aperture Index Press Save button to store the new positions or Reset to discard unsaved values step 2 of 2 Instructions Aperture Index 2 B m Bl Aperture Diameter 3 um Pasitian Modulator Amplitude 25 E ERES Reset Save Contrast 64 80 g E p A Brightness 40 97 EJ El 5 Cancel When you find an illumination and adjust the aperture position near the 2D box border click the Save button This stores the X Y position and the alignment cross is
261. urging which is automatically initiated when the system pumps the vented chamber directly to the ESEM Low Vacuum mode FIGURE 4 17 ESEM PREFERENCES xIm Preferences Databar Units Presets Scanning ESEM General Movie Sensitivity Purge Mode Ho Purge Purge settings Automatic Minimum Pressure BO Pa Maximum Pressure 130 0 Number of Cycles 5 wes Purge Mode module radio buttons NoPurge The purging is switched off and the chamber pressure goes directly to the set ESEM Low Vacuum mode value The gas mixture in the chamber slowly changes to the new gas type e Automatic All purging parameters are set automatically according to the mounted Low Vacuum detector Cone Custom The Custom parameters Minimum Pressure Maximum Pressure Number of cycles defined in the Purge Settings module edit boxes are used The default values are the same as in Automatic mode The Purge button enables to start the purging using the current Purge Mode and Settings manually when the system is already pumped to ESEM Low Vacuum otherwise the button is disabled When the purging is running the Purge button becomes highlighted Clicking on the highlighted button stops the current purging procedure and returns the system to operation in ESEM Low Vacuum Notes The new Purge Mode or Settings is applied immediately after pressing the OK or Apply button even if the purging cycle is already running
262. utely necessary when only topping up the oil level CAUTION Do not allow the pre vacuum pump to emit gases into the work place as this can be a health hazard The Rotary pump may become very hot while in use be careful not to touch the main frame of the pump Venting the chamber will shut off the rotary pump Topping Up The filling position is a plastic hand screw stopper on the top of the same end as the level indicator oWitch off the pump if necessary by venting the chamber Unscrew the stopper Clean around the stopper hole with a lint free cloth Fill with the recommended oil to the upper level Clean up any spillage on the pump Replace the stopper Switch on the pump by pumping the chamber N 0 N CAUTION Never fill the pump through the exhaust hole by removing the exhaust pipe as this results in the oil being removed from the pump by pressure build up Excessive back pressure in the exhaust pipe eventually over heats the pump so it is important to allow good passage for the exhaust gases preferably via an installed factory exhaust system Maintenance and Troubleshooting Troubleshooting Troubleshooting TABLE 8 2 POSSIBLE PROBLEMS AND CORRECTIVE ACTIONS Problem Possible solution Not possible to switch the microscope Check the mains switch and the mains unit circuit or the PC on breakers placed at the microscope back Check the mains and the mains circuit breaker Server cras
263. vel Detector home position While the detector is not used it could be placed into a holder which is mounted inside the specimen chamber saving it from a mechanical damage and pollutions ELECTRON BACKSCATTERED DIFFRACTION PATTERN DETECTOR EBSD See separate manual PHOTO MULTIPLIER TUBE BACKSCATTERED ELECTRON DETECTOR PMT BSE See separate manual E o 0 System Options Energy Dispersive X ray EDX Analysis Energy Dispersive X ray EDX Analysis The EDX sometimes referred to also as EDS analysis is a technique used for identifying the elemental composition of the specimen or an area of interest thereof It works as an integrated feature of a scanning electron microscope SEM and cannot operate on its own without the latter The specimen is bombarded with an electron beam inside the A T microscope column These electrons collide with the specimen atoms rogus LH El i re A SU L Series own electrons knocking some of them off in the process Positions vacated by ejected inner shell electrons are occupied by a higher energy electron from an outer shell while giving up some of its energy DN by emitting an X ray The amount of energy released depends on M Series Lm which shell it is transferring from to The atom of every element Ni ae E releases X rays with unique amounts of energy identifying it The output of an EDX analysis is an EDX spectrum which is just a plot of how frequently
264. xit A g Software Control xT microscope Control Software zem Detectors Scan Delete Del Mares Scan Beam Y ETD SE GAD A PMID BSE External CCD Detector Settings Print Ctrl P opens the print dialogue enabling a choice of printer and settings Suitable to print an image Log Off User logs off a present User and provides the Log On dialogue for the next microscope user When the User logs off the system goes to a safe state the accelerating and detector voltages are switched off automatically Exit closes the xT microscope Control software the current user is automatically logged off first and leaves the user in the operating system environment xT microscope Server is still running and controls the microscope in operation The Edit Menu Alt E opens some helpful functions Delete Del deletes all selected items measurements annotations Select All Ctrl A selects all items within the imaging window measurements annotations The Detectors Menu Alt D opens the selection and setting of all installed Detectors Detector list contains various detectors for the High Vac Low Vac and ESEM operation Detectors not mounted or not serviceable under the current microscope conditions are disabled greyed out The selected detector for the active quad shows a tick next to its label e An External video signal can be selected The signal detector and mode
265. y not pump down to Hivac mode on the first attempt Caution To avoid water leaks in the chamber the stage must be removed and water plugs installed before going into HiVac mode Once the water lines are disconnected and the water plugs installed the temperature stage can be removed from the chamber in the reverse order of as described in the Installation procedure System Options Heating Stage 1000 C FP 2300 02 Heating Stage 1500 FP 2300 06 Heating Stage 1000 C FP 2300 02 Heating Stage 1500 C FP 2300 06 The Heating stage HS is used to control the sample temperature up to 1000 C resp 1500 C and to observe sample with the use of FEI electron microscope WARNING A Opening the microscope chamber does not switch off the heating When operating the Heating stage please be aware that neighbouring surfaces can become hot HEATING STAGES PARTS The Heating stage assembly The Chamber feed through plate The Water chiller The Flow box and water hoses The Heating stage controller and cables The High temperature GSED e The HS 1500 Heat shield assembly e he HS 1500 Heat shield and Sample bias SSB FIGURE 9 19 HEATING STAGE SYSTEM BLOCK DIAGRAM Heat Shield Assembly Control Cable xT microscope Contral Software ee oe eee eee E A E Chamber Feedthrough Plate sl HS Interface Cable Controller l I Water Water Chiller o Flow Box Cooling Water Hoses
266. zard Stage Position E Important Make sure that there are no obstructions because the Important Make sure that there are no obstructions because the stage will move to 60 of tilt stage will move to 60 of tilt When OK tick checkbox v When OK tick checkbox v stage Position Press the Set button to move the stage to stage Position Tilt stage manually to 60 A 12 000 mm 437 mm Cut Y 12 000 mm 10 004 mm o 12 000 mm H T 3 659 mm acquire the specimen holder image 44 4 eae 0 0 0 0 Previous Cancel Previous Cancel 4 Click the Set button and wait until the Next button becomes active after the stage movement In case the Stage cannot reach a desired position the stage information dialogue appears Clicking the OK button returns the stage to the previous position and moves back to the step 3 Zo Stages Stage Related Functions Quit the procedure vent the specimen chamber and adjust the specimen top surface to fit an operation need Then repeat the procedure Specimen Holder Wizard The stage cannot reach the required z position 28 0 mm The specimen holder is too high or too short The stage will return to its previous position 5 The Outline Box dialogue asks to fit the green box around the area to be captured Refer to the example image The manual tilt stages Finalize Setup dialogue asks to set the stage Tilt to 0 xTm Specimen Holder Wizard Outline Box E Til

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