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Scanning Electron Microscope Operation

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1. 45 SM oM eub Mu MM I M D S 16 SNOWN INA E e 30 PESE DAA RR ER EET TE TTE 65 Specimen Chan ee COH ise eri RR RUE GRE Do RUM D Mr DR MR Tn arti vod desde res qae re e uus 44 SPECIMEN current VIGIL OM 2c cists E 46 Spectra Ca DUG WIN Wa a 56 Spectra Title entry EDA Xd 60 Spectra A 51 Title Scanning Electron Microscope Operation Page 83 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas spectrum era DN SCIE r a a dto 63 A err 40 sSputteraepo SI EI ON I dE accact oat a dta o eld Ata ooo 13 sputter depositlon SVSEefmiausd edere hv AAA A A A eia V aa ad a EQ E VERS 13 A O 51 A TEE ET EO OT EDS 22 Stage Control WIN Wise esae aod d 24 SETS OI E CHI Ol x ceututasnsas tec in dado 24 A I BE caca statuto cipes et ted pase tract wis sin ag b stu td Me a MED SUM MS IARE 24 SEAS SOU OW m e 24 stage SIS CO oC TEENS 23 Standard COMM strain dandoles taria tec es ciao 46 standard A te M CEU E cnp acd ceti e uem tis ean see ce 19 Standard Map EDAX qom 65 Stancdardiess ME s EDAD 60 STEM Scanning Transmission Electron Microscope esseesseeeseeeen enne en nnn nnns 78 buf A A AAA 31 SUENAN os 30 SubsututioOVetay EDAX tii ad 71 suntace preparation EBSD ias 74 T TEN modes OroODServa OM alada tt iaa 78 Tilting the SAO ii A AA AA A oceans 24 dias
2. stage could charge up to thousands of volts and zap the pico ammeter when the cable is plugged back in You will be given an opportunity to create an SEM password after your specific training on the SEM If you sign up you are expected to keep your appointment with the SEM Remember the current rule is that if you sign up and then you need to cancel you must cancel 24 hours before your scheduled time This means that if you sign up the day before and discover you can t make it you may pay for the time anyway unless you make arrangements with another user to create a scheduled use time in your time slot Standard Configuration When you complete your operation return the machine to standard SEM configuration If you have been trained on one of the several subsystems and you leave the tool set up for that system the common SEM user may not know how to return to the standard operation Specifically if you have used the Nabity E Beam lithography system please set the Nabity Mode back to SEM and also set the SEM electron detector back to SE2 and not the in lens system Remove Sample When you complete your time on the machine remove your sample Also whisk your sample away from the SEM don t leave it lying around on the table etc It will be subject to destruction by the staff cleaning up the table Logbook Fill in the logbook If you leave blanks you could be subject to denied use of the SEM Purpose Com
3. always use the joystick Title Scanning Electron Microscope Operation Page 24 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas while watching the video camera The real value in being able to load stage coordinates comes after the stage is in position under the objective lens and the stage needs to be driven in x and y to a known or mapped sample location Coordination of Stage and SEM Image Movement In spite of the multiplicity of coordinate systems and apparent conflict of motions there is an easy way to coordinate the motions of the SEM Image the Joystick motion and the stage motion in the video camera image On the SEM Keyboard there is a knob entitled Scan Rotation If we set this to 90 degrees then the SEM image the joystick and the stage as viewed in the video camera image will all move in the same direction according to the operator perspective To do this we will need the Hard Front Panel option active This pair of windows will show the exact value of each of the knob settings and will change to which ever knob we turn To set the 90 degrees simply turn the Scan Rotation knob until 90 deg shows in the window Alternatively you can numerically enter the scan rotation angle in a small Rotate Tilt window by opening the Edge Menu and then clicking on the Rotate Tilt item in the list Set the scan rotation to 90 deg and then close the window Return to STEP 8 SEM Keyboard B
4. 10 A TEE 13 SEI IEOGIET 222 2 2 5 929992399 93 29929 29055 399285290925592 9052 90 2 5922 5090 99 290 0 09 062596220925 16 SEM Image Sc Mii 17 Sample Loading sess na nnns 19 Establishing the Electron Beam rierien rrara e Er r a ar 21 MATE O e UE eed 22 Check Sample Current Monitor Status cccoocccconcnnccncnnonacnnonnnnnnnannnnnos 23 Joystick Stage Control vusciits is 23 Digital Stage CoONtTOl occcoccccccccnccccnnccncnnonocononacnnonncnonnnrnononenononenenonens 24 Coordination of Stage and SEM Image Movement 25 SEN IRC VO AN sott Loire lll ies 25 Finding and Positioning the SEM Image ooccccoccncccccnncnncnnonacncnnacnnonannnos 26 Multi Sample Holder Map eicere inei naa 27 Scan Rotation Coordination with Stage Motion 28 otage Motion Warning cessit theta casis a o oce 29 Title Scanning Electron Microscope Operation Page 2 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Image Positioning Shortcut ooccccocccccccccccccnconononcnonanonnnnnnnncnnnannnnanononcnnnas 29 FOCUS and lama lO m OTT m 29 APeRUSAMO Nasa 31 Brghiness and COn ta Susa 32 JA M RTT ebs 32 Image Capture and Storage sarmi aa 33 special Imaging Techllglde Susto 34 Eucentric Stage ConfiguratiON cccoocccccocncococononocnnonannnonnnnnonannnnnnnncnnnnnnss 34 eure A Pe E E E E E 39 El
5. Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Operating Instructions for EDAX Material Identification System Introduction Note that this is the detailed description section for operating the SEM EDAX Imaging system The EDAX system Figure 27 mounted on our Supra 40 Scanning Electron Microscope is an X Ray analysis system capable of producing an energy spectrum from X Rays emanating from a specimen material that is struck by energetic electrons and analyzing the data to determine what elements are producing the X rays This principle is termed Energy Dispersive X ray Spectroscopy EDS It is a type of X ray Fluorescence Spectroscopy The EDAX X ray detector is a Lithium Drifted Silicon detector To avoid Li migration under the influence of bias and temperature the detector is chilled to liquid nitrogen temperatures If the liquid nitrogen evaporates and the detector warms up above a threshold set in the software the detector is turned off to reduce the bias to zero This helps prevent deterioration of sensitivity because of the thermal and bias drift of the Lithium impurities Filling the LN Dewar is a responsibility of the Clean Room staff If you find that the Dewar is empty ask a staff member to fill it It will take at least an hour before the sensor is stable enough to capture reliable data EDAX LN2 TANK S FILLED EVER EVERY FRIDAY B TO LAST THE WES Fab dd Figure 27 EDAX LN2 De
6. High contrast image with saturation Left Normal image Center Lo contrast image Right Scan Speed ocan speed is an important parameter with many ramifications In general for a fast scan speed the image contains more noise snow and for a slower speed the image becomes less noisy and more highly resolved However the fast scans reflect real time movement of the stage better than the slow scans This gives the operator an easier view of stage movement and allows a faster positioning ability Because the SEM imaging technique is inherently slow any speed improvement will become highly appreciated by the operator as experience level increases When the stage is positioned with the desired image in position the scan rate can be slowed to set the focus and reduce noise for image capture The Title Scanning Electron Microscope Operation Page 32 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas software can be trained to automatically impose the fast scan if you move the stage This command is found in Tools User Preferences stage Fast Scanning ON or OFF There are other digital manipulation techniques to reduce noise in the image Under the scan tab there is a box that allows the user to choose various noise reduction methods such as pixel averaging frame averaging and the extent of averaging In the pixel averaging technique the SEM captures a settable number of brightness samples a
7. lfeinggt inte 45 a Ness PIERDE RU I UMS MEM MEME REESE E Ec abusi tu E 45 time estimate EDAX MaDDIUB is 67 UNE SW AIO PIA ro 45 UETAN t ER cet sve c RETE PIRA 46 A DU D UD UIS m 44 LODO 21010 Vu Eu Iu MI E C M Eid Li riu E uiid iU 41 U WSC A O m s 16 V O tt c RDUM UOS 21 o a eee ee 20 W WARNING Digital Stage driving ni gens 54 WNILLO CONE as 47 Working Distance WD EDA dada io ads Lo 53 X Fe TRAV VAY Sls sas te E eL AE MM EE MEM E Nu d ETE 50 Er VA O E 1 0 OO Re eC e no o y 50 SEE A esate esis tween S M m 51 X ray Miva DOWNS ee O AL 61 Z DAIS VELOC aca tars eens ccs o eue cuentas MEE ME MeL 23 Title Scanning Electron Microscope Operation Page 84 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Title Scanning Electron Microscope Operation Page 85 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas
8. way out of focus it got lost So the auto focus function depends on the target to have sharply contrasted features and at lease one feature edge oriented in the x axis and another edge oriented in the y axis to be successful If the image is low contrast the auto focus function can twiddle until it is lost and you will have to manually re focus Practice is required to improve your skill at this focus task LILILITISJ oo Se I uf FR d a al B E qe IMag 481 Focus 17 mm Figure 20 This is the panel of action icons at the top of the SEM image page The third icon from the right is the auto focus button The numbered boxes are standard scan rates Button 1 is used for finding the image and stage movement Button 2 for stage movement Button 3 for focusing Button 4 for image capture and Button 5 for image capture Return to STEP 10 Aperture Align Any time a different aperture has been selected the beam needs to be realigned After you establish focus at a reasonably high magnification gt 20KX click on the Aperture tab in the menu set at the right of the SEM image window Then click on the Focus Wobble command and set the Wobble to about 5 This will automatically change the focus Title Scanning Electron Microscope Operation Page 31 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas 5 in a repeating fashion The image will appear to go in and
9. 12 2009 Extraction ratio 8 89 TERMINAL io SmartSEM Chambers ILE EN i 6 38AM Figure 13 Screen on the right monitor showing the Stage Manager ChamberScope RemCon32 and EM Server support windows open This is a practical assortment of windows for safe operation of the SEM Note the ChamberScope Eye icon at the lower left of the command line NOTE 1 If you change this arrangement of windows during your SEM session please put them back before you log out so the next user will have a standard display NOTE 2 Do not activate the TV mode under the menu Detectors TV To see the chamber scope window click on the eyeball icon in the bottom command tray of the left monitor Attempting to use the eyeball icon and the detector TV at the same time will crash the SEM software iG Userinterface P PG zm SmartSEM ROGER 3 Start fis Em a E E EM Server Sample Loading Now that the sample is prepared and mounted on the SEM sample mount we have to vent the SEM to load it This is done by clicking on the Sample Exchange icon in the upper left of the SEM image screen Figure 12 Title Scanning Electron Microscope Operation Author Roger Robbins The University of Texas at Dallas Page 19 of 85 Date 9 29 2015 This will turn off the SEM high voltage and in a little pop up window ask if you have retracted all extendable probes EBSD STEM Backscatter detector so that the stage w
10. Data Collection o Click on the Collect button to start the new data acquisition off on toggle switch Step 6 Stop the Spectral Data Collection o If you set the 100 scan limit in the upper right command line the spectra will stop collecting when it has averaged 100 copies of the spectra data o Otherwise when the spectral data profile has become smooth you can click on the Collect button and the collection will stop allowing you to start data analysis Step 7 Auto Identify the Spectral Peaks o Click on the Peak ID button to start the automatic spectral peak identification analysis o Confirm the peak identity by clicking on the HPD button located just under the Peak ID button This will draw a thin blue line outlining the spectral peaks according to the theoretical calculation of the proper line shape and location If this blue line snugly fits the shape of the spectral lines then the automatic peak identification was successful If not then you will have to manually identify the peak Step 7a Manual Identification of the Spectral Peaks o Manual peak identification can be done several ways using the expanded Peak ID panel Figure 35 Click on the up and down carat symbol in the right side panel to expand the Peak ID section Title Scanning Electron Microscope Operation Page 58 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas lxl 7 Amp Time Auto na AL Ta
11. Included at the end of each section is a skeletal outline of procedural steps so the newly trained operator can follow the order of operation without having to read the in depth explanations during real time use Survey Description of SEM Describe reason for following survey topics and limitation i e describing purpose of sensors and when they would be used SEM Concept Describe physics of electron beam formation control and material interaction creating return electrons How does the scanning principle create a magnified image EDAX Concept Describe physics concept of EDAX operation and what information it acquires when it would be used etc Secondary Electron Detectors What are secondary electrons where do they come from How does electron detector work Describe principle of operation of both Everhart Thornton and in lens detectors What information do these detectors acquire and how when are they used Title Scanning Electron Microscope Operation Page 6 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Backscatter Electron Detector What is a backscattered electron and where does it come from How are these electrons different from secondary electrons What information do they contain How does the backscatter electron detector work Electron Back Scatter Diffraction Detector What is back scatter diffraction What is it for How is the diffraction pattern detecte
12. T T EP SD TOM E e v 59 LN A e di a Spatial A Sete AN caste ce tee Leo 2 Rescale SADE cet gt d E VW A ett E Mag 5810 Y E 7 AS oy AA 4 AA Er i 4l O ee TS i Pe Logarithmic 3 Band Coloring vA A ps de UA hs en aas 1o Collect Reso 1024x800 5 2 ENT hr IK C bout Reads 250 i idee uy j Ern abro SERI Sar PF Sts Es pro e lid dE x A Collect 7 AS pru 1 VETUS CO A de Clear l q EL Heo a Maps J Line J Live TTL F Quant PR n i p Spe Drift Reso 255x200 Collect rr 200 Maps X Net Inte Frames 1 iv Use Z List gt HY OFF when done wt x Print amp HP Deskjet 9800 S Portrait Field Stage X Stage Y RES Fields 20 CPS 155090 DT9 amp 100 Lsec 0 2 Cnts 1561 keV 5 060 FS 93758 line 199 Disk 0 1GB Time 3 1hrs Pts 0 E 50 s 221PM Figure 43 This screen capture shows the Map Overlay last blue green red box at the right end with the Process menu open showing the Color and Substitution Overlay choices Note the blue outline below the overlay map This indicates that that window has been selected this blue box should appear around each of the normal element images shift click to select before choosing the overlay action Title Scanning Electron Microscope Operation Page 71 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas o NOTE The overlay is created by the software selecting the element with the bri
13. aes Dee eus Shaw suns Sosa Ups Dos ero la GR ORAL VETE OBL Uo DESI misses M SST E PVT TE IN GRLE Ds 75 EDAX qu rr EDT 50 EDAX BCAMVENGTE V araen n DD DL DT DD 54 EDAX DEGAMIPIITION assumes RAR A N NR a aa 52 EDAX REMCON DOFUDUI t9er 2 untada iS 62 EDAX SA AAA AAA A a NS 72 EDAXSO MN Ware Status 55 EDADES DO td esta as 52 EDAX Spectra errors JN3bIty Tat ose odo eve aa PENNE elita Doa uasa Midas fua e ed UR 63 EDAX SUSLOTIT A p epit IM LEID LEM UI ML MM ERE UD E I b UA EE 50 EDAX Xsray detector otv i eiat aia 50 EDS RN Bu a I MMC M E TE EL Mi id Li iM 50 Siu E 22 BATAN VO AO iii ts 21 A Bere N E ou A D I M EI ee Eee EENE 76 Electro a e dua uU NEU UTE 74 PHO CLO De AREE aa 22 electron detecto ueccsiatesquedvene ie eM Rd M uem etu raza 44 Electron Penetratlon ETTBCES eire a elo a ale AR Sd cias 41 Element WOK SED AX pP AAA 68 element concentration graphs EDA Na 69 Elemental QUantification D Messi a 60 A A aa aa a SEI eM DC M EIC aa a a a 54 end of travel sensor illumination EDAX ioi ec ete eo b e PH TENE EIN EE eeE EAE Wn DR DE eb E 54 enere y Scale EDAX SPECT stesse das 57 enerev spectrum dTrom Xs Rays ss ve de tide tin euis A inainoade bamnade beens de Pastori dS faq 50 eucentric helg ib eonsede et deeds e ORIS A od nativa erc TID edv ae HEUS nU Ter Cede 35 PUCER rc e EDEN PEE 34 EVO ICD eoo M M M oa E Mes n Me MEE 22 Title Scanning Electron Mic
14. at ground level Figure 30 Backscatter electron emission as a function of substrate angle with the primary beam This shows that as the angle between The potential above the the electron beam and the surface tilts more sample is set by the voltage electrons escape Data from Kanter H of the substrate and as 1957 electrons from the beam enter this field they are deflected This can shift the beam and thus move the SEM image In some cases you might be able to take advantage of a physical characteristic of electron collision with a tilted surface to help balance the incoming electron charge with the electron charge leaving the surface via scattering From the data in Figure 30 you can see that as the sample surface is tilted more parallel to the beam setting a shallow grazing angle that more electrons scatter out of the surface If the substrate drain path current can be balanced with the escaping electron charge rate then the surface could be brought to neutral voltage and the image would become non charging Other things can happen on a more local basis as electrons are captured in local regions These regions will cause the SEM image to blossom into bright random shaped phantom objects in the picture due to clouds of Title Scanning Electron Microscope Operation Page 40 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas excess electrons bleeding off of the surface and entering the electron
15. by a set of 4 quick sequential keyboard strokes as follows Ctrl Alt Tab and then a number 1 2 or 3 Number 1 links to the EDAX computer Number 2 links to the Nabity e beam lithography computer and Number 3 links to the Zyvex nano manipulator computer for probing samples The EDAX software is executed on the Right side multiplexed monitor and the program start icon EDAX Genesis is shown in Figure 31 The EDAX computer is selected on the keyboard by rapidly clicking in sequence the following keys Ctrl Alt and Tab and then the number 1 When the EDAX screen comes up click on the Genesis icon to start the program Title Scanning Electron Microscope Operation Page 55 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas EDA Genesis GET Figure 31 Genesis icon that starts the EDAX program Figure 32 shows the full screen spectra capture window with various software control command sub windows The following paragraphs will outline the steps required to establish and analyze a spectrum Note the three tabs at the top of the program opening screen This is the key to three different aspects of the EDAX program Bc ERAX Spectrum Image MapsiLine ES File Edit View Proc Auto Setup Window Help gt 3 Y S O El 26 IN A Jk T w V Analyzer Det 1 gt Preset 100 0 Live Amp Time Auto Y Iu E c edax32 genesis genspc spc ky Tilt A Tungsten Co
16. detector signal Many other consequences can also happen but they all prevent a true image from being captured Therefore considerable effort is required in some cases to prevent charging Electron Penetration Effects The SEM imaging technique sometimes determines whether you can see the aspects of your substrate that you are interested in For example if you need information from the topography of the sample you should consider the penetration depth of the probe electrons As electrons enter the sample surface they penetrate into the body of the material a distance depending on several parameters chiefly the energy of the electron itself and the material The deeper they penetrate the less surface information is contained in the image and the more material parameter information they convey However the higher energy electrons produce a higher geometric image resolution This occurs because higher energy electron beams are distorted less by the SEM hardware than lower energy beams Therefore you will need to find an appropriate compromise to meet your requirements Backscattered Electron Image By collecting mostly backscattered electrons from elastic collisions with atoms in the substrate you can obtain an image with contrast more from the material type than from the topography See the topic of Backscatter Electron Detector Figure 24 shows a graph of backscattering coefficient as a function of Z Atomic Number As the atomic number
17. goes up the material becomes more efficient at producing inelastically backscattered electrons which can be captured by backscattered electron detector This will produce an image with material contrast where material consisting of heaver atoms show up as brighter regions in the image Title Scanning Electron Microscope Operation Page 41 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Figure 24 Electron backscatter coefficient vs Atomic number Z This characteristic increase in electron emission with Z creates image contrast in Z or mass contrast Secondary Electron Image The standard SEM image is generated by secondary electron emission from the substrate These are low energy electrons less than 50 eV produced both by the primary electron beam and the high energy backscattered electrons However while the primary electron beam can penetrate the substrate by several or many microns the escape depth for the secondary electrons is only on the order of tens or hundreds of angstroms Thus they are generated very close to the surface Figure 25 Title Scanning Electron Microscope Operation Page 42 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas incident electron beam Secondary ES electron S E d Sin Specimen P Secondary electron A sE AC Li out A 7 Backscattered electron 1 pm Figure 25 This schematic depicts generati
18. holder This can be done with the Copper sticky tape looped around the edge to the top surface of your sample If your sample is an insulator then you may need to coat it with a conductive material i e Au Pd or Carbon Title Scanning Electron Microscope Operation Page 12 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Sample Coating Fortunately we have a Hummer VI sputter deposition system located in Bay 5 just for this task It has a Gold Palladium target and a sputter deposition rate of about 38 Angstroms per minute Thus about 1 0 1 5 minutes of sputtering will apply enough metal to conduct the SEM electrons to ground and prevent charging without noticeably altering the topography of your substrate The Hummer VI is shown in Figure 6 Note that if you coat an insulator substrate you will need to connect the newly conducting top side to ground with a copper tape Figure 6 Hummer VI sputter deposition system for coating insulating SEM samples Preliminary Checks before operating the Hummer Before operating the Hummer VI locate the High Voltage Control Knob in the top right hand corner of the instrument panel and make sure it is at zero Secondly make sure the High Voltage Control Switch located just to the right of the HV knob is in the off position The Mode knob should be set to Plate DC and the Pulse switch to the off position See Figure 7 for location of Knobs Hummer Ope
19. holder left and SEM stage right Title Scanning Electron Microscope Operation Page 7 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Figure 2 Examples of STEM images Crystallites left and semiconductor device defect right Nano Manipulator Stage Describe the purpose of the nano manipulator and the structure of the stage What is special about the probes In general how is it used How small of an object can it touch probe or move When do you use it What is involved in installing and setting it up Staff only setup Low Noise Electrical Probe System General brief description of the low noise probe system This is a specialty system Electron Beam Lithography System Describe what the electron beam lithography system is and how it is controlled What are the writing specs i e field size critical dimension limits substrate capability alignment capability What is this specialty system used for Title Scanning Electron Microscope Operation Page 8 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Operating Instructions for SEM Introduction This document is intended to be a user friendly operating manual for the UTD Cleanroom Zeiss Supra 40 high resolution Scanning Electron Microscope The SEM is primarily used by researchers in the cleanroom to examine the structures made in the cleanroom However it is also available to qualified researchers i
20. in case the link to the secure drive is temporarily broken However any data stored on the computer s drive can be erased without notice by staff if necessary to allow the SEM to run I e reduce data on a full drive that is preventing operating system function Image capture is accomplished by freezing the image at the End of Frame and clicking on the Microsoft File menu at the far upper left of Set Freeze on end of Frame by opening the top row Scan Menu and selecting Freeze on End of Frame Title Scanning Electron Microscope Operation Page 33 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas the screen Clicking on the Save Image selection in the File menu list brings up a reduced size window with commands to save the image Figure 22 ix Export TIFF D User Images Roger SEM Specification 1kvss41 tif Filename 1kvss81 tif AJA Al 27 etche NormalContrast Next AJA Al 27 polish Drift101 tiF Format Mas 30 Chars E Digits g vi Drift10delay 1 tif Drift11 tif Drift21 tif Merge Drift 31 tif Seem Sample ID Drift41 tif Drift51 tif Colour M Drft i i El Eon Merge Store resolution 1024 768 wv Drift71 tif Se Drift7ZImageJum User Text od E v Se2 Det 30 micron App 25 kV Au Fe rock target WD 8 Bel ll LA gt Save File 1 tif pup Figure 22 Image capture screen To save an image with support data select your directo
21. out of focus as well as oscillate in its position Your task to align the beam to the aperture is to adjust the x and y Aperture knobs on the keyboard until the image does not move wobble any more it should just go in and out of focus in the same location When you have stabilized the image wobble just click on the Wobble command and it will stop Then repeat the focus and astigmatism correction Brightness and Contrast The gray level and contrast of the image are set by the two knobs on the upper right corner of the keyboard The concept in setting these parameters is to have a brightness level that shows dim objects but a contrast level that avoids white saturation Contrast also determines the edge definition of objects when looking for sharp high contrast edges Electrically the brightness knob sets the zero offset of the gray level and the contrast knob sets the gray level gain By gain mean that increasing the contrast knob increases the brightness of the bright objects faster than it does the darker objects increases the slope angle These knobs are linear in effect but affect each other i e increasing the contrast makes the image brighter but so does the brightness knob r a 100 nm BHT 25 00 kV Signal A SE Date 11 2007 1 100 nm EHT 25 00 kV Signal A SE Date 11 2007 ZEISS 109 nm EHT 25 00 kV WO fmm Photo Ni 1172 T 17 WO 8mm Photo No 1173 Tire 20 38 54 WO 8 mm km Figure 21
22. radius of the rotating plate but the top of the stage is located Title Scanning Electron Microscope Operation Page 34 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas near the axis of tilt so the sample will not move away from the impingement location of the electron beam scan field The schematic drawing in Figure 23 depicts this arrangement Note that the eucentricity does not depend on the Z position of the stage because the center of rotation of the stage moves up and down with the Z axis movement The eucentric height of the sample is measured from the top of the stage sample mounting base to the top of the sample itself 9 24 15 RR SAMPLE AT EucENTR C Height JL EUCENTRIC HEIGHT Figure 23 Geometric depiction of a eucentric stage bolted to the rotating plate on the front door such that the sample is aligned to the rotation axis of the tilt function This alignment prevents the sample from drifting out of the image scan and out of focus as the stage is moved in x or y directions Title Scanning Electron Microscope Operation Page 35 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas To further illustrate this arrangement Figure 24 shows a depiction of a generic SEM stage also mounted on the front door and in the tilted orientation with the sample stage close to the center of rotation so that a sample can be mounted and fixed at the exact center of rotat
23. the beam is scanning E SmartSEM ChamberScope PUCEECOULO oe a REMOTE REN Illumination 47 2 Status Properties Points List Scanning Survey g Delta x 66 185 mm 66 185 mm v 65 291 mm 6529mm Z 38 646 mm 38 646 mm T Fone 0 0 R 267 67 o iR M 000mm Field Movement ay gt MU C Move using Stage Scanning fields Compuc Mode Off Stage Is Idle Undo Stage Goto Clear Options Log File Size 7329 KiloBytes __ Time Message QQ 06 14 18 12 2009 Loading Hard Front Panel 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 06 14 18 12 2009 Loaded Tracker Ball Bar Loading Thumbnail Bar Loading SEM Status Loading NewStatusBar toolbar Loading MiniBar Loading CZToolbarxP CZ ToolbarXP Loaded Loading Annotation toolbar SmartSEM Load Complete Application SmartSEM Remote Control V04 04 23rd August 2006 Registered Application SmartSEM ChamberScope Via CZ EM Parameter Manager Contr Application SmartSEM Remote Control V04 04 23rd August 2006 Revoked R Application SmartSEM Remote Control V04 04 23rd August 2006 Registered 06 22 18 12 2009 Extraction at EHT Off 157 uA O 06 23 18 12 2009 Extraction at 19 2 kV 143 uA O 06 23 18
24. the validity of the identification by clicking on the HPD Halographic Peak Deconvolution button This will add a blue outline around all the identified spectral peaks This blue line is the theoretical line location and shape for the element chosen If it fits snuggly around the spectral line the identity is probably correct if it is shifted or does not fit the shape then more effort is needed to identify the material 7 Select Maps o Click on the Maps button Title Scanning Electron Microscope Operation Page 64 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas o The other option is Line which is utilized later after a map is already obtained 8 Select Map Type o Standard Map Type With no boxes checked under the Maps button the system will capture X ray data at every pixel for the selected dwell time The data for that pixel is recorded and immediately updated into the map o Live Map Type Fast mapping This map type rasters very quickly over the entire map area set by the SEM magnification and presents the data for the complete map 1 frame This is repeated and the maps are updated pixel by pixel until the map is stopped by the user or when the set number of frames is reached o Spc Type Live Spectrum Mapping Live and Spc boxes checked rasters frame after frame over the entire map area storing the entire spectral information while updating the images and the cum
25. the x y motion is slow and vice versa Stage rotation is effected by twisting the RIGHT joystick handle one way or the other Twisting the handle to the right clockwise will cause the stage to rotate about stage center in a clockwise direction If your target is far away from the stage center it will appear to translate off the screen because this rotation center is independent of your sample location Note that x and y movements can be somewhat confusing because there may be as many as four or five independent coordinate systems involved in the movement For example Substrate coordinate system Stage coordinate system Beam coordinate system Joystick coordinate system Chamber Scope coordinate system and a software coordinate compensation interpretation system that tries to make user sense out of all the above complications Digital Stage Control If you open the Stage Manager window and place it in the right screen then you will see two sets of coordinate values for each of the stage coordinate axes The right hand column is a command listing and if you double click in a coordinate box you can type in a coordinate number hit enter and the stage will move to that coordinate value It will move fast not coordinated with the magnification so this method of moving the stage is loaded with danger of collision recommend that an operator never use this method for moving the stage up to operating height from the loading position
26. Figure 45 Surface appearance left and EBSD pattern right after 3 micron diamond paste polish no EBSD pattern Title Scanning Electron Microscope Operation Page 75 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Figure 46 Surface appearance left and EBSD pattern right after 1 micron alpha alumina polish EBSD pattern quality 28 Figure 47 Surface appearance left and EBSD pattern right after 0 3 micron alpha alumina polish EBSD pattern quality 166 Figure 48 Surface appearance left and EBSD pattern right after 10 min polish with colloidal silica EBSD pattern quality 177 Figure 49 Surface appearance left and EBSD pattern right after 30 min polish with colloidal silica EBSD pattern quality 224 Even though the above sequence of polishing appears to have produced a good EBSD image quality there may be some circumstances that require even more preparation before good EBSD images can be obtained This extra polish step can involve elther electro polish or chemical polish Electro polish involves Title Scanning Electron Microscope Operation Page 76 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas immersing the sample in an electrolyte solution and using an electric bias to remove the remnant deformation layers and surface irregularities left after polishing This method grows an anodic film on the surface and then slowly removes it t
27. File Edit View Beam Detection Image Scanning Stage Vacuum Tools Help LEEENA E i Brightness 44 7 Contrast 36 3 LA SA x Detectors Scanning Vacuum Gun Apertures Stage Aperture Size 11 30 00 um Standard iv Focus Wobble Wobble Fast ror Amplitude 5 5 Beam Blanked Emi Beam Shift 29 L High Current specimen 48 7 p SCM Status Off E SCM On C Spot EHT 19 24 kV Signal A SE2 Date 18 Dec 2009 WD 8mm Photo No 156 Time 6 27 58 Ready LB Mag 139 24 K X MB WD 8mm Fine O NV SERE mug sx ums AN EDO b ol a Figure 12 User interface on the Left monitor after Log On Note the Imaging control icons in the upper row and the 6 tab command panel at the right side of the screen Measuring and documentation icons are along the bottom Also note the dual boxes at the upper left with Brightness 44 7 and contrast 36 3 this is the handy HFP window that shows the value in range of any adjustment knob on the keyboard The strip of information at the bottom of the image frame is called the Data Zone and contains the micron bar EHT WD etc this strip is saved with the image The thin blue right side border of the image viewing field opens into a menu list of additional operation windows Edge Menu One of the handiest tools hidden in the View menu is the Hard Front Panel option If you pull down the View menu an
28. NGING IMA isis 53 Title Scanning Electron Microscope Operation Page 3 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas SEUNG VWorkifg Distant aaa 53 DEMENCIA DEEST 94 Tutor Chamber LED MUMIMANON usituitess iaa 54 Illumination Error Recovery c occcocccnncccncncncncnncnnncnonanonnconncnonanonaronnnnnnanenos 54 Aperture SO Misas 55 EDAX Operational Proecegll 6a n oon ei dius Put Eod Pur aai 55 Select an AMO Maa 57 Step 2 Preset a Collection COUNt occccconcccccnnncconnnocononocnanononanononannnnnos 57 Step 3 Clear the Old Spectra and Peak Labels 57 Step 4 Adjust the Spectrum Scale cccconcccconococococonacononanonnnnnnnnnns 57 Step 5 Start the Spectral Data Collection 58 Step 6 Stop the Spectral Data Collection 58 Step 7 Auto Identify the Spectral Peaks eeessessse 58 Step 7a Manual Identification of the Spectral Peaks 58 Step 8 Type in a Label for the Spectra sssss 60 Step 9 Elemental Quantification of a Mixed Material 60 Step 10 Printing the SpectrUM ooccccoccncccccnccoccnoconononanononannnnnnnncnnnnnnnnos 61 Step 11 Save the Spectra into a File sseeesssesss 61 EDAX X Ray Mapping Operating Procedure c
29. Scanning Electron Microscope Operation Zeiss Supra 40 Roger Robbins 9 10 2010 Update 9 29 2015 Erik Jonsson School of Engineering The University of Texas at Dallas Title Scanning Electron Microscope Operation Page 1 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Scanning Electron Microscope Operation Zeiss Supra 40 Roger Robbins 9 10 2010 Update 9 29 2015 Table of Contents Tal gore Ele Loa eee o ONDE EET 6 Survey Description Of SE Mi IAS 6 SEM GORCODIE s ee decide diu daa 6 EDAX eM E 6 secondary Electron DeteGlOlS druide ceti cet mie s esto id 6 Backscatter EIeclromJDeleclOfsastusia irte ru qu R o UP QUA SPUR Ru D ead ev uv uL Pavo aw v PUE ud 7 Electron Back Scatter Diffraction Detector oooocccooncccconncccconoconcnnaconcnnacononnnos 7 scanning Transmission Electron Microscope System ssss 7 Nano Manipulator lager dido 8 Low Noise Electrical Probe SysteM cccoocnccccccncccccnccononoconononanononannnonncnnnoncnnss 8 Electron Beam Lithography Syste Mian aa 8 Operating Instructions for SEM c ooccnccccnncccccncconcnononnnononononacononarononannnnoncnononens 9 HAF OOUGTION EE a 9 Slain GME CK NS E tees eect ete ete ede eee eee N 9 Operating Procede NER ERE 9 Time Scheduling and Logbook STEP Tassie aa aE 9 Sample PRED AAU Mts iii deidad talado Ue le ies 10 Sample Hole EE e ii o 12 Sample Cro UAdIMO M T TT 12
30. a la taa E 78 Region Of Interest ROI EDAX daa 67 Remconsa2 errorTemediatioOle EDAX ceca ues eio ob tup tu tu S deb mus dcs seva lucem eerie 64 remote SOC UNS CLIVE T u 33 48 Resol TON E DAA ia di 63 resolution parameter EDAX eon a da ii Eds 63 Qn DE 45 Sample clean b opc WP 45 sample Current Monto Ra ina Sedes EO du Cadena Uta incase 22 23 Sample dz emineat mmc em 19 Sample Noder te a a 12 Sample NOS aii RA AA A A 12 SL debates tii nadebabodeit inten batete pe uto wah cdes p osos e cde teas Dae iran teeta ters LM eee tues 17 Sample EO ION E ducis oam aita ot eit atat caia 19 Sample loading EDAX iie d rente Peleo A A t eee o Pe ea cea AS 53 SAN LS MOUM eem eee ro ROO 10 Sample preconaitiOHllipsnt soa txsad i bera sentation aia 11 Sample EMO ASA m 44 Sample pes NOt AllOw eG SEM iia delete dota laicdaiasS 11 SAO N e ry 32 save INM ais 34 o E cog ene Nee ST CTS ET E Mu Mu i M 34 DAVE tres pectta EDS AA 61 SCROLL AME dede 28 Scan ROION Setting Mer iaa 29 o de PT 32 Scanning Transmission Electron Microscope STEM cccssccsseccscecseccenccenceseeceenceeeeceaueesenceseeseuceseeeeenes 78 SEZ SetEIDg TOM ED Aaa 63 secondary electron ems OM 42 secondar eleccion ene AAA 43 SECU OMING A EBSD oi pon 74 SEM SEN edu rs 52 RARE 20 o RA 44 A 2a M E
31. ages EDA Acs 60 mosaic Map ED os 71 Mounting EBSCO A AAA 74 MUNDI sampe NO Rao 27 Multiplexed mohltor sWIEEDITIB A A 55 miultissample holder iii AAA AAA AA Feed ode du du 27 N NI t recent eet ali tae teat asmuirhiea gts icine A hath aulalick hale Mas haehga uses enaeesaamaetue sen anas 33 NGM PrUme timie OUTS a ARA A A EAN 45 Normalloperatine CONdItIOA Sia za 21 O OPLUMUMEDASS Nadando 55 Over av graph E DA acia 70 OVETIAV NOTES EDAX SA A AS 72 P ape IOSD OOK RA A ALA A AAA A AS 10 A lO sai cs E Uu UR ER gate E NM E Mer iade ds faded cme haar 16 46 Peak PED D aaa 58 PEAK IID DOK ED ccc 68 PCA SOUL ONS DA cananea 64 Penetito dept as 41 Pico Amp Meter unplugging PronhibitiON sccsscosscosscosccssccessonscuessscessecsscoessoessosetesstssceuscossecesseseress 46 SII ISTE IARE DOO T mom 33 OMS Mil eBBSD an i oido 75 77 Powders mr SEM tnotsalloWed cion Lid IN DD DUE 11 Pre et DOX EDAD mann dub A ivt VD LO VERE E POIL RR EDT mice Wah alae rca Nor UE IE UU eru Udo pd aine 63 Prime NOUS ana ids 45 PRINTING MaD EDA Ks HE 72 Printing the Spectrum e ED A iS 61 purchasing special SAN PS Nolder Sa 12 Title Scanning Electron Microscope Operation Page 82 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Q Quant Mapping dp cad 65 R ETNE E A E EA E E OE ias 23 hegduse EDAN o oti dd E E E T R T AA E OR 63 Reduced Raste anarai A A AAA 30 rerocUsIMP STE Mait
32. al logbook before starting mandatory Operating Procedure Time Scheduling and Logbook STEP 1 scheduling time on the SEM requires logging in to the FOM calendar at the web location https msefom campus ad utdallas edu fom and selecting time on the calendar to reserve This calendar will then switch on the control monitor at the SEM to allow usage Return to STEP 1 Title Scanning Electron Microscope Operation Page 9 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas There is also a paper logbook at the SEM that users must fill out completely lt is for the purpose of recording the actual SEM use in order to help staff with problem solving as well as administrative details This gives the staff archival information on what the tool is used for how long it is to be used who is using it and for what subsystem In addition the blank Purpose comments area gives you the space to tell the staff about SEM problems or remind you what you did during this SEM session etc Statements on what you were doing also help staff understand how the SEM is being used and enable better support Figure 3 shows a sample log sheet Return to STEP 2 Date Sponser Start Time Circle Use SEM EDAX EBSD STEM Nabity Litho Bakscatter Finish Time Sample Purpose Comments Figure 3 Sample SEM log sheet kept at the SEM Sample Preparation Your sample can be mounted on one of a number of sample mounts The simplest mo
33. ase turn off the gauge when finished Figure 27 Setting sample height for establishing eucentric sample position for our stage First reset the gauge to Zero left then lift the probe and set your sample and support stack under the probe and gently let it down center Adjust the sample height and clamp with the set screw at the 0 566 inch 14 376 mm stack height Title Scanning Electron Microscope Operation Page 38 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas lf you are using standard silicon wafer thickness substrates you can simplify the adjustment procedure by slipping a 0 003 inch 0 0762 mm paper shim Figure 28 under the pin mount and just seat the pin mount on the shim this will result in almost the exact height for the eucentric position Figure 28 Material stack alternative to achieve the Eucentric height Key element is seating the pin mount on a 0 003 inch thick paper shim for standard Si wafer thickness When you begin tilting your sample in the SEM start at low magnification and watch the video screen to see that you don t crash into the conical lens suggest starting at a working distance of about 10 mm and a magnification around 500 X As the angle approaches the view desired then magnify to the appropriate value to see the detail you are interested in During the tilt action the image may drift a small amount depending on the actual sample height proximity to the exact eucent
34. balt disc Take Off Angle Counts Ma Collect uf Clear EviChan 10 0 Method Auto Type Curve o Method ZAF SEC EDAX Q Type Elements Stds None Quant Save E HP Deskjet 9800 Print amp Portrait DT96 38 Lseci00 Cnts 3736 kev 8 410 FS 12819 AmpT 25 6 Det SUTW Res 133 92 Figure 32 EDAX spectra capture window with some of the spectral peaks identified Note the three tabs at the very top of the screen these open three different aspects of the program Title Scanning Electron Microscope Operation Page 56 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Select an Amp Time Select an Amp Time based on the count rate so that the dead time is between 20 and 40 This is the percentage of the time required by the electronics to count and fill the energy level bins in the software so that a spectrum can be generated Usually the Auto selection will work fine The window for setting the Amp Time is in the upper right command line as shown in Figure 330 The smaller the number of X ray counts per second the larger the Amp Time required Analyzer Det 1 Preset 100 0 Live Amp Time Auto nm de Figure 33 Upper command line showing the Amp Time window Step 2 Preset a Collection Count O If desired set a preset collection count by clicking in the Preset Box Figure 33 above and typing a number into the box This preset co
35. cccoocccccccccconcncconcncnoncncnnncnnnnos 61 A eto nstoe senna t scale et thet AT 61 Operational Steps for MappinQ cccccoccnccoccnccncnncnncncnnncnnonacononannnnnncnononons 62 1 Set Preliminary Parameters occcccocccccccnncconnnonocnnonannnonannnnonnnononens 62 2 ebopeclrum Parallels cree ei dere oce dedero eed eres 63 3 oetimage Patrammelels eer er rte ete e eee ei ettet 63 4 Collect Electron IMage occccccccccccnncoconncoconnnonacononannononcncnnnnncnnns 63 de X ollect X ray SPSCUUIN ucciso pce pe sn E sese pct TEE 64 6 Identify the Spectral PeaksS coooccccccnncocononococononannncnannnnncnonnns 64 A A et one cet ORE RE RE IDA AU ee eRe eRe eee 64 8 Select MAD IDO dao ada peda 65 9 Set Mapping Parameters ii ls 66 10 AGONSCHING a MAD eccssessoxcsussaecvooweavoposesanstancusuiearsusedteysuasieencusydeauseans 67 WAP AAIY lee Ed 67 ne Scan ANalySIS iret estis A Renee ee ADAE 67 MaD OV GAY Siempre 71 FUNINO MAPS aan isis ios 72 Gompletion Check lacra ronda 72 Rules or EDAX Opera ss id sea dated des EH b ee PME 72 Additional EDAX Software Details ooocccoocccoccncconnccnnnccncnconnncnncnnonons 73 Special Purpose Subsystems 0 riore rerit eene ode eure eae ee ius 73 Electron Backscatter Detector OperatiON occccocccccocnccccncnoonononncnnanonnnnnnnanoss 73 Electron Back Scatter Diffraction System oooooccccooncccconoccnconaconcnnancncnnnncnnnns 74 Sample Preparation OVEIVIEW cs
36. ction parameters Start the map collection Use the identified material ID to auto define Regions of Interest Turn off the High Voltage when scanning is complete Execute the auto LUT Look Up Table to set image intensity Print Image Multi field Mapping auto move stage to defined spots Figure 38 Mapping command panel at right side of mapping screen Operational Steps for Mapping 1 Set Preliminary Parameters O O Title Scanning Electron Microscope Operation Author Roger Robbins Make sure that the Chamber Scope illumination on the SEM is turned off to prevent problems with the X ray detector Enter the number of Spectral scans you want in the Preset box at the upper right of the EDAX command line you can have None in the box for this operation to produce unlimited scans Set the Amp Time to Auto to insure that the dead time is between 20 and 40 Make sure the RemCon32_EDAX program is talking to the EDAX program by opening the program and verifying that text is being produced If it is not then make sure that port number 2 Page 62 of 85 Date 9 29 2015 The University of Texas at Dallas is set and open You will have to restart the EDAX program to reconnect o Also set the SEM Electron detector to SE2 2 Set Spectrum Parameters o Clear the prior spectrum with the clear button at the right side of the Collect button in the right panel o Clear the spectral line labels by e
37. d and what electrons does it acquire Scanning Transmission Electron Microscope System Explain what a scanning transmission electron microscope is How are electrons detected What electrons are detected Where is the detector How do electrons get through material What does the image look like What information does it display When do you use it Our Scanning Electron Microscope has an optional accessory that enables the system to produce Scanning Transmission Electron Microscope STEM images This configuration sets the sample to be imaged on a special sample mount such that the STEM detector which is mounted on a long rod that extends out of the side of the sample chamber can align to the underside of the sample Electrons from the column penetrate the thinned sample and collide with atoms in the sample and then pass through the sample and are detected by diode detectors at the end of the probe The STEM can produce very high resolution material density images in both bright and dark field modes with high signal to noise ratio and sharp contrast It is used to examine the cross section of semiconductor device elements crystal grain boundaries as well as other material boundaries The EDAX material analysis system can identify properties of highly localized features in thin samples Conical SEM Final Lens STEM Probe home STEM Sample Holder Stage Door Latch SEM Stage hd e a ae Figure 1 Images of STEM sample
38. d click on the Toolbars command a new window will appear having an option for HFP Status with a check box next to it Click in the box and close the windows This will produce a pair of small window boxes with numbers in them There will be a label assigning these numbers to a parameter pair such as Magnification Focus which will correspond to the numeric value of the designated knob positions by percent travel from their origin This conveniently gives you a numeric gauge for the amount of adjustment the knob is providing If you grab the boundary of this window pair you can move it to a convenient location in your user interface screen This way you will Know how much magnification you are requesting for example The functions listed in the window match all the adjustment knobs on the keyboard and automatically appear when any of the knobs are just slightly touched Title Scanning Electron Microscope Operation Page 18 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Also you can activate a scan marker option which places a small line projecting from the left edge of the SEM image showing where the scan is at any moment This option is found under the Tools menu in the top row command list Click on the User Preferences option and then the Scan Marker item in the SEM conditions section This is handy in situations when the beam is stable and it is difficult to tell where
39. e NUN VON a atte d vestis cse Gina de t Ud UI dq UE 39 Tra Rp E 33 48 Mage capa rr a O ds 34 Im se Positiomfs NOR ae al inci iq uud dualidad dab d ade 29 Initiallzatiornrcormimalid e Stage EDAX A d Ivo Ci pav i eet YVES I AA vit oet EP RIA VEUA aede rta teda 54 SUTIN S SUB stats 39 J JOO COMPIETION Checklist iecit TE ad v Or ren rede ma tr tec epo tO vens ven eden 45 JOYSTICK TICO CONO iaa anida Pasar M dade 23 JOVSUICK SLAC CONTO be m 23 K KEV DOAN PP TN 26 KOOD DOSI ONS odds 18 L Ldbelspectra ED a 60 line scamenalysise EDAX cM I MEL MR D iM Md E iM 67 Eine Sean Procedure EDAD AAA 67 ve Map EL OO ETE 65 UN lecitina 52 Title Scanning Electron Microscope Operation Page 81 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas ENDS Walle MINNE ad T UU P O 50 HOV lt EOC Cita ad aida 53 location Tidp SAI DIC it AA AAA AAA 27 A 10 RRA 46 52 ferro rodelueslot ba unceist a ed auene a ood visnew ot au one sav OE 44 M Manual peak identification ED Asiatico dis rco onde eds AAA A AAA AAA EA cede 58 MAVE VEEDAN a ida dnd 71 map resolition EDAX diia 66 Maps EDAX oia 64 materialicontra Suri ells liliana eds 41 Material Quantification ASSUMPTIONS ccccccseccseccsecsccseecseccseccseceseceusceuseeccusceueseetseceseceseceussesssaeenaes 60 Mechanical POSING lt EBS Dierre E E ios 74 FICE OND AU ee T TIE 18 MOr ASC VICO ia 22 Mixture Percent
40. e easily damaged by a wandering thumb Title Scanning Electron Microscope Operation Page 20 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas After the sample is properly mounted onto the SEM stage and inspected gently close the chamber door Just as it closes it will latch closed by the force of a magnet at the back of the stage so that the door will be held closed against the sealing O ring when the vacuum pump starts thus preventing an old problem of sucking room air into the chamber because the o ring is not well sealed Return to STEP 6 Now click OK in the box on the screen asking Press OK to Pump The pump down sequence will take several minutes to achieve sufficient vacuum in the chamber for the system to open the column valve and establish a beam In the meantime you can click on the Vacuum tab in the right hand panel of the screen to view the vacuum level in the chamber and the gun The gun should be below 8x10 Torr and the chamber vacuum line will be grayed out until the vacuum achieves a measurable level The chamber will eventually achieve something in the low 10 Torr range Return to STEP 7 Establishing the Electron Beam As the vacuum level in the chamber drops below 7 5x10 Torr the column valve will open and the gun EHT High Voltage will Run Up By clicking on the Gun tab on the right side of the SEM screen you can see the gun conditions Normal operating condi
41. e plate of the sample clamp to the surface of the sample must be exactly 0 566 inches 14 376 mm This can be measured by the height gauge sitting next to the Hummer IV sputter deposition tool for the SEM Eucentric Height 0 566 inches 14 376 mm to the top of the sample Figure 26 Height measurement location for determining Eucentric setting height of sample on our Zeiss Supra 40 Scanning Electron Miocroscope SEM stage NOTE Sample must be mounted on this flat type of sample base any size of pin mount can be used Title Scanning Electron Microscope Operation Page 37 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas For our Zeiss Supra 40 stage to position a sample at the eucentric height the flat sample mount shown in Figure 26 must be used and the pin mount sample holder set to a height so that the sample on top of it is at 0 566 inches 14 376 mm above the base of the sample mount Copper clamp Setting the height to the eucentric position above the base of the sample mount in Figure 27 can be accomplished by turning on the height gauge by pressing the on off button with no sample under the probe and actuating the zero function by pressing the off on button briefly Then lift up the measuring probe and set your stack of holders and sample under it and gently set the probe tip on the sample Adjust the height of the sample pin mount and clamp it in position with the horizontal set screw Ple
42. ectron Penelra ton ENOC S aman NA 41 Backscattered Electron IMAGES cua doas oro ooo octo ER ERE Shoda 41 Secoridary EIectron Image usse e e Eo eevee 42 sample BelrioVal s oio ibi use bre oen Y d etra d een rd v ded ds 44 SIMO Wit Procedul ees accidet ode PAG ada 44 Commplellom Gheck EISbass ei laa 45 RUles 0 SEN ODGFAllOI scs acie acto pent Peu ve e ee tie o v E E 45 standard Configuration is 46 REMOVE IMPI 46 E A E 46 PUDOSe COMMONS costra 46 Consolidated SEM Operation INStructiONS cccooncccconcnncocnnonncnnonacononanocnnanononos 47 SPE P aaa 47 STEP 2 maraa da 47 nn 47 AI M HO 47 Sz ui T T POO 47 e A LA LM EL Ed 47 SPEI T een HM IAM AM IMEEM ee ee 47 OTEP O NR T m T TUTTI 48 oOTED S usb LC mI LI I e 48 STEP 10 e Y 48 STEP Tes emm o Im e EM EE 48 cz adir PER eee ee ee ee eee 48 STERT Sie ida 49 JH aed oues da E i M E EE 49 STEP T ovdi idum Ne cipit noe ne ceno cast does iesus ene copas 49 SS eli Lee EE 49 Operating Instructions for EDAX Material Identification System 50 NTOQUCUON Pm 50 EDAX Spectral Analysis Setup Procedure coooccccccnccccccnnccnconanencnnnnencnnnncnnnns 52 OCHECUMNG ING ToO METER EET 52 FIN SOUT WOOD AAA 52 Stanno Checklist aio iecc 52 Establishing X ray CaptUle oocccccccccccocnnococnnonocononacnnonncnnnnnnnonnncnonnnnncnoncnnss 53 Samples LOGGING secnm oot to loteria tarios acd ce 53 PI
43. eed operation Return to STEP 9 Focus and Stigmation To sharpen the nominal low magnification focus used to find the sample gradually increase the magnification and select successively slower scans Title Scanning Electron Microscope Operation Page 29 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas d paro gt to decrease the image noise snow If the image feature moves off screen as you increase the magnification move it back onto the screen with the x y joystick or the neat shortcut outlined in the previous paragraph As the magnification increases and fine details come into view select the Reduced Raster button at the top of the screen This will bring up a small size changeable active box on the image that displays a small portion of the SEM image This allows you to switch to slow scan to bring out sharp details but simultaneously increase the frame rate to make it easier to observe the image focus in relation to focus knob changes Click on scan rate icon 4 to obtain the best image to focus at high magnifications You can now further increase the magnification to finely focus the image Focus technique requires astute observation of the degree of fuzziness in the image The focus procedure is to turn the focus knob until the image begins to become sharply focused continue to turn the focus knob past the sharp focus a small amount and then return to the optimum focus point This insur
44. efore we discuss finding the sample we need a short overview of the SEM control keyboard Figure 16 Title Scanning Electron Microscope Operation Page 25 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Figure 16 Picture of the SEM console keyboard This console contains a standard laptop style keyboard layout in the midst of a number of knobs and buttons The knobs perform repetitive and sensitive operations of SEM control such as focus and magnification among many others The buttons activate conditions for the knob adjustments The SEM keyboard has a number of knobs and buttons to give the operator analogue like control of SEM parameters The large knob on the left is magnification and the large knob on the right is focus The two knobs on the upper right are brightness and contrast And the two knobs on the upper left are stigmators These are the most used knobs and their functions require frequent precise analogue adjustments to achieve visible optimization of image quality The buttons activate key functionality to set up conditions for the analogue knob adjustment The lesser used knobs will be described later These give the more experienced operator the ability to operate the SEM much faster Finding and Positioning the SEM Image Sometimes the SEM will start scanning but the screen will be totally dark How would you find an image from this condition The normal way would be to reduce the magni
45. eol D er 77 chromiatic aberration s SPEM Aa 78 Clear the Old Spectra and Peak Labels EDAX csscssscosscosscosccsscosscoessonssesstsssessccusccsscoessosstessnessesses 57 Collect BUHON S EDA Gar T 58 COMES T 63 collect Maps EDANA C X JL HR 67 Collect Maps DUELtOIt e EDAX sscsitev ies hi aptat ves aae INO aah evi deos eon IIS ves acdnsa ardent Oro e RITUES 66 Collect speetr be EDAX Vus vete iei Seul DUE M M DL LEM Idi EEN D tat EM iam Ld cU 64 CONECTION COUNT EDAX de A a 57 COSO NS O acosa cd 29 Title Scanning Electron Microscope Operation Page 79 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas color coded spectrallihies EDAX a aa 59 COUV a IVE NET rer 21 COMICON Check EISE s ED aos 72 cond ctive TAPIA T T ITE 12 Confirm the peak Identity c EDAX ucc aeleives t nadt ta Gade Inpt etna ct he Dodvp act sack Duo Du et dire ea Nu PT econ E etin et Edu 59 CONTE ASU TN RT trm MR 32 COOFCIM ATS location MaD isisisi renei a Tm 27 coordinate MIOLIONS html dida 25 Coordinate SV SU OI ASEOS 24 Counts per second A an ee ea Dan ee i MOE Ptr edu etai arc rene anne ane eee i car dto ud 55 cross section SANIDICS iia 28 D danteror COMISIOMN ad toas 24 danger stage co lO iii 29 e A A dtd 18 53 Dead limelDTIa A A 55 detqultawel times CDA Xian 66 Draw ness nd MUS 69 UME WCU Ge SEDAN me a aatei tmu tui eaa oca 66 E EBSD image qualltysiscveur a ua ges b Div
46. es and adjust around the center to find your exact target Title Scanning Electron Microscope Operation Page 23 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Tilting the stage is effected by tilting the LEFT joystick to the left or right This also means that while you are raising the stage in the z axis and if you also push the joystick right or left the stage will simultaneously tilt Watch out for this dual motion via the ChamberScope to avoid awkward stage conditions The stage will only tilt toward the detectors on the left side of the SEM chamber which is to the right in the ChamberScope view because the video camera is looking at the stage from the back wall of the SEM chamber If you reach the tilt limit the SEM will stop tilting the stage and show an error TILT LIMIT By the way if you run into a stage limit error just push the lever in the other direction to move away from the limit Nevertheless the correct initial direction to push the tilt stick is to your right You can observe the exact tilt angle in the window executed by the Stage tab on the SEM Control panel to the right of the SEM image screen See Figure 13 This Stage Control window is opened under the Stage command menu in the upper left screen command line The RIGHT joystick x y theta works the same as the LEFT joystick the more tilt you give the joystick the faster the stage moves Also if the magnification is high
47. es that you have seen the best focus and know what to look for to optimize the focus As you increase the magnification focus must be re optimized using the above protocol In cases where the sample is of low contrast or focusing is difficult if you turn the focus knob until the image goes distinctly out of focus note the knob position and then turn the focus knob the other way until the focus is distinctly out of focus by about the same amount as the previous position then true focus will be about in the center of the two knob positions Turn the knob back to this center position and adjust the astigmatism knobs below to improve focus Proceed to further increase magnification If the image is again fuzzy repeat the focus adjustment until the focus is clear Stigmation is observed as focus distortion in the image which gives the image a directional fuzziness This occurs because the electron beam cross section is shaped oblong like an ellipse when it is stigmatic The axis of the oval spot can be in any orientation and the result is that edges of the image parallel to the long axis of the elliptic soot are sharply focused and the perpendicular image edges are fuzzy and axially stretched This gives the image a uniform fuzziness orientation Wo Tem ro Ta adi ES mu oe on uM E wo Tm meme meras DN Figure 19 Example of opposite astigmatism orientation on either side of center focus Left and Right images and fuzzy center focu
48. f Then close the window and menu See Figure 12 to locate the thin blue border with the lt sign embedded Joystick Stage Control The stage movement is controlled manually by a dual joystick desk console shown in Figure 15 In general the LEFT joystick controls the Z axis movement and the stage tilt angle and the RIGHT joystick controls the X Y motion and the stage rotation S axis stage Figure 15 Joystick Stage control LEFT stick performs stage Z travel and Tilt Z travel push lever up or down Tilt push the lever right or left RIGHT joystick moves stage in x and y and twisting the right stick causes the stage to rotate To raise the stage into the ChamberScope view push upwards on the LEFT joystick stage speed is controlled by the amount you push the stick upwards The stage will travel up in Z and the ChamberScope will show its rise Release the joystick to stop motion Note that the z axis velocity is also governed by the image magnification If the magnification is high the stage moves very slowly if it is low the stage moves fast When the stage rises to within about a centimeter of the bottom of the conical lens as seen in the ChamberScope stop The x y position can then be adjusted with the RIGHT joystick so that your sample is under the electron lens Note that the stage x y center is about 65 65 mm If your sample is at the center of the stage then just move the stage to these coordinat
49. f the sample holder you can use the corner values as starting points to find your samples Then you can move the stage and view samples in a row by moving the SEM image with the Joystick along one axis Scan Rotation Coordination with Stage Motion One more trick can be invoked to make finding things easier If you set the rotation angle of the electron beam Scan Rotation to 90 degrees then the movement of the SEM image in the left screen will correlate to the apparent motion of the stage in the right hand screen in the Chamber scope window Of course the joystick x y coordinate system will Title Scanning Electron Microscope Operation Page 28 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas translate to x y and y x where the primed coordinates are the Stage Manager coordinates Setting the Scan Rotation is effected by rotating the Scan Rotation knob on the keyboard and noting the scan angle from the knob readout boxes Hard Front Panel at the top of the SEM image window on the left screen The 90 degrees scan rotation causes the electron beam scan to rotate from the horizontal direction to the vertical direction as it scans across the sample but is unchanged in the screen image this consequently causes the SEM image to rotate 90 degrees Stage Motion Warning Note again that moving the stage using the command boxes in the Stage Manager windows is loaded with danger you
50. fication to minimum and turn up the contrast knob on the SEM keyboard This will usually bring up a gray scanning field with some fuzzy bright spots in it If your stage location has been centered at 65 mm in x and 65 mm in y and your target sample is at center and about 1 cm below the tapered end of the objective lens the fuzzy image will show an out of focus image of your sample and perhaps some stage Title Scanning Electron Microscope Operation Page 26 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas parts Slowly turn the Focus knob on the keyboard to the right clockwise to lengthen the working distance distance between the lens and the beam focus point in Z Soon your image will begin to come into focus Now you can position the stage in x y and working distance 2 appropriate for the sample Multi Sample Holder Map The multi sample holder appears to present a troubling conundrum for new students trying to find the location of each of the samples Figure 17 The reason that there is difficulty in this task is that the default coordinate system of the SEM image on the left screen is at 90 degrees from the motion actuated by the joystick and seen in the video camera image of the stage motion in the Chamberscope screen Also the Chamberscope camera is looking at the sample from the back wall invoking a left right reversal and at a shallow angle so that it is hard to tell where the stage is loca
51. ft screen This will bring up the Log On window in the left screen Figure 11 Enter your username and password and click OK This will bring up the Smart SEM software that runs the SEM NOTE Never use someone else s user ID This is against university policy and can bring on serious punishment Title Scanning Electron Microscope Operation Page 16 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas 3 SE OPEICTBIDI zallas Welcome to SmartSEM Figure 11 Left screen Log On Window Note the ZEISS Smart SEM icon in the left column 5th icon that calls up the log on window SEM Image Screen The next few steps of preparing the SEM for sample loading and image acquisition require commands from the software The SEM user interface is spread across two monitors The user interface screen is shown in Figure 12 The icons in the upper command line are used very frequently in operating the SEM and optimizing the image The set of 6 tabs on the right side of the screen contain command and parameter setting buttons for setting the SEM up for imaging The row of icons at the bottom of the screen has commands allowing you to measure or label things on the image The SEM image appears in the large region in the center Return to STEP 4 Title Scanning Electron Microscope Operation Page 17 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas cn SmartSEM ROGER
52. ghtest normalized pixel intensity to represent that pixel in the overlay Printing maps o The collected maps will appear as a collection of individual element maps in small windows with different color dots corresponding to the specific element This little matrix of elements maps can be printed directly on the HP printer Highlight each map you want printed and then click on the print button in the upper left command menu The trick is to hold down the shift key and click on each map you want to get them selected o If the image is too dark and all you get is black ink on the paper you can reverse the background color to white This usually gives a better map because the paper is not completely saturated with black ink Reverse the background color by opening the command line tab Color and choose Reverse o Print the maps by clicking on the Print button at the bottom of the right panel Completion Check List o When you are finished with the EDAX operation simply close the EDAX program by clicking on the X in the upper right corner of the window o If you need to close out the SEM operation also then follow the SEM operation completion procedure found under Completion Check List Rules of EDAX Operation e Only Staff is allowed to fill the LN2 Dewar e lf you need to use the EDAX system for analysis not data collection requiring SEM operation then you can work out an arrangement with the person using
53. he material to fit the standard parameter value assumptions used by the calculation o Material Quantification Assumptions o Sample working Distance 8 mm o Stage tilt 0 deg o Material must be mixed homogeneously to the depth of electron penetration Layered material leads to potential erroneous results up to double digit percentages Homogeneous material analysis can be accurate to lt 5 Title Scanning Electron Microscope Operation Page 60 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas E Quantification Results EDAX ZAF Quantification Standardle Element Normalize SEC Table Default Wt X At X K Ratio 29 82 57 51 0 1546 1 1226 0 4616 8 03 11 62 0 0127 1 0987 0 1441 1 36 0 0094 1 0499 0 6253 0 38 0 33 0 0029 1 0164 0 7402 60 34 29 18 0 5532 0 9114 1 0060 100 00 100 00 Element Net Inte Backgrd Inte Error Page Setup Print Results Print Spc and Results Figure 37 Quantification results window showing the percentages of elements in the EDAX sample o Details of high accuracy mixture analysis are beyond the scope of this manual Step 10 Printing the Spectrum o The spectrum and the overlay window showing the quantification results can be printed on a printer sitting on top of the cabinet housing the SEM computers Click on the appropriate print button located in the overlay window showing the quantification table This can also be printed to a file especial
54. ical movements of the stage in real time This is important to help prevent collisions and improve the speed at which you can find your sample If you are watching the SEM image and moving the stage you can increase the image scan rate so the stage motion will be realistic NOTE Never try to open the chamberscope in the SEM screen and also click on the Eyeball icon in the bottom toolbar The SEM software will crash By the way the stage is electrically isolated and if there is a stage collision with anything inside the chamber the SEM will very softly Beep but only if the Sample Current Monitor is OFF Because an immediate emergency has occurred the stage motors will turn off at collision to prevent serious damage If this happens and you know exactly why you can manually back the stage away from the collision if you are uncertain please call the SEM staff person for immediate assistance NOTE The Sample Current Monitor SCM should always be OFF unless the user is actively measuring the sample current Title Scanning Electron Microscope Operation Page 22 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Check Sample Current Monitor Status In order to insure that the Sample Current Monitor is off activate the SCM window by clicking on the thin blue border of the SEM image screen to expand a menu having the SCM selection double click on the SCM listing and note whether it is on or of
55. icroscope consists of a set of diode electron detectors at the end of a long rod that can be positioned under a thinned sample mounted on a special multi sample holder Electrons from the standard scanning electron beam column collide with material in the sample but pass through the thinned sample and spread out in a scanning conical pattern This scanning conical beam Is intercepted by 5 planar electron detectors diodes 4 independent detectors on the top level and a single detector on a lower level that receives electrons through a central hole in the upper detectors at the intersection of their 4 internal corners This arrangement allows 6 different modes of observation 1 Dark Field DF 2 Bright Field BF 3 DF DF 4 BF DF 5 Summed Oriented Dark Field ODF1 ODF2 and 6 ODF1 ODF2 This arrangement avoids the chromatic aberration from non homogeneous electron energies that pure TEM microscopes produce from the refocusing of transmitted electrons In addition because of the lower beam voltage compared to the TEM the STEM system produces higher transmission rates and better signal to noise ratios which in turn create better contrast images with comparable resolution Furthermore because of the thin sample and small diameter of the focused beam the electron collision volume in the sample is very small which enhances the lateral resolution of EDAX material identification This STEM can be used to analyze material morphology in diverse
56. ill not collide with them and damage the very expensive probes Before clicking in the popup window physically go look to see if the probes have been retracted even if you know they have These probes are generally worth as much as a mid size Mercedes Benz Make sure of their status The stage usually vents in about 1 minute When it arrives at atmospheric pressure gently pull the SEM chamber door open The stage table has a stainless steel disk at the center of a Copper table that has a bevel on its rim that fits the reverse bevel on the underside of the sample holder Carefully slide the sample holder over this disk until it docks against the cross bar on top of the SEM stage table Note that the sample holder copper docking disk underneath has a flat side on it this is the side that meets the docking bar on the stage table Take great care in sliding this on or off because there are delicate mechanisms right next to the SEM table and on the stage See the SEM stage in Figure 14 Return to STEP 5 Sample holder bottom Beveled slot flat end Docking bar SS Docking Disk Delicate electrical contact slider D Figure 14 SEM stage showing sample mounting table with small round docking disc and banking bar Hand holding sample holder shows underside of holder with the reverse beveled slot and flat end that dock against the bar on the SEM stage table Also note the delicate fixtures around the SEM stage table that can b
57. in size and cannot be saved Enjoy it while you can or capture it with the Print Screen button on the keyboard and save it in the Paint program o When you are done with the analysis you can return to active data acquisition or just close the EDAX window and go home Note that this analysis does not require actual SEM operation Title Scanning Electron Microscope Operation Page 70 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Map Overlays e A map overlay consists of a mosaic map of up to 6 individual element maps superimposed in a single map This indicates the x ray intensity and location of all the identified elements in a single map o To create this overlay first choose the field of 36 little windows find this selection in the main row of icons at the top of the window and select the icon with lots of windows in it o Highlight each of the maps to be included by holding down the shift key and clicking on each individual map you want included in the overlay o Then pull down the Process menu from the top menu bar and select Color and then Substitution Overlay from the drop down menu There must be one open window in which the overlay can be viewed See Figure 43 Bc EDAX Spectrum Image Maps Line File Edit View Collect Display MultiField Setup Window Help a Analyzer Det 1 Preset None Amp Time 51 2uS gt 3 zn m d b
58. ining good Electron Back Scatter Diffraction images that can be accurately analyzed The EBSD signal is obtained by electron beam interaction with the crystal lattice within 10 to 50 nanometers of the surface This means that if the surface is composed of contamination to this depth then the EBSD signal will be of poor quality or even non existent Therefore surface preparation must result in surface exposure of the undisturbed crystal lattice This section will survey several different preparation techniques Mechanical Polishing Mechanical polishing is usually required to remove surface contamination oxides and distorted crystal material However the methods used to accomplish this are many and vary according to the sample material There are a number of steps to creating a suitably prepared sample for SEM examination 1 Sectioning This term describes the simple step of making an SEM sample from a parent substrate i e cutting out a small piece from a wafer etc 2 Mounting This is a preparation step for treating the surface to make it suitable for EBSD imaging Basically how you hold the sample to treat the surface grinding polishing etc to create the exposed crystal lattice at the surface This could consist of embedding the sample in resin or fixing it to a mount that will enable surface treatment 3 Grinding Grinding removes the macroscopic surface contamination oxides etc and exposes the base material in sequential
59. inking to the secure drive on the campus network Once the link is established then you can down load your images and data but you cannot write to the secure disc from your desk computer This arrangement is our effort to reduce the possibilities of tools catching viruses from memory sticks or general computers accessing data from the SEM and other tools In the case of the cleanroom SEM you also have the privilege of storing images on the SEM computer drive in an assigned folder This represents a backup storage medium in case the link to the secure drive is temporarily broken However any data stored on the computer s drive can be erased without notice by staff if necessary to allow the SEM to run I e reduce data on a full drive that is preventing operating system function Image capture Title Scanning Electron Microscope Operation Page 48 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas STEP 13 Exchange Sample Vent open door change or remove sample close door pump down chamber Never leave sample chamber at atmospheric pressure for very long Jump to Sample Removal STEP 14 Log Off SEM software to stop your session cost timer STEP 15 Log out of paper Logbook and the FOM system do not forget STEP 16 Clean up the SEM and the sample prep table Note that Staff can toss your samples if they are left on the table Title Scanning Electron Microscope Operation Page 49 of 85
60. ion Center of Stage Tilt Eucentric center for sample imaging Tilt Rotation Sample Mount Base Inside view of stage on front door of vacuum chamber Figure 24 Depiction of a tilted SEM stage with the sample mounting platform close to the center of the stage tilt axis Samples would be set at the eucentric height so that the surface of the sample was exactly at the axis of tilt Title Scanning Electron Microscope Operation Page 36 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas To show the difference between eucentricity and non eucentricity Figure 25 shows two sample positions one at the tilt axis eucentric and one above it non eucentric Note that as the stage tilts the non eucentric sample position follows an arc away from the e beam scan field and down away from the focus plane while the sample on the rotation axis just stays in one place but tilts for a side perspective of the object being imaged beam Axis IMAGE TARGET MOVE MENT STAGE TiLT AT i NON ELCENTRIC Ht Miura ae gt TARGET Moves Away d from scaw Field gt desta a ii FONA DISTANCE FROM sucentric H A trie Ht u 0 it a CENTER of Tilt For STAGE STAGE OFFSET IN X Axis Figure 25 Comparison of sample movement in non eucentric position left and the stationary eucentric position right In our Zeiss Supra 40 the eucentric height measured from the bas
61. ke Off Angle Collect uf Clear EviChan 10 0 Collect box expansion symbol Peak Fe ID ClearAll HPD af EPIC al Tas Add Delete Peak ID box contraction symbol Possible AAA Manual Element ID controls Alpha Lines Only C Elem Shell Trans Marker xm lv Abs Ese J Sum Advanced Figure 35 Expanded Peak ID box showing manual peak identify controls and box expansion contraction symbols 4 o To manually identify a peak place the cross cursor over the peak and click the left mouse button This draws the black vertical marker line to the peak Quickly after this the Possible box fills with element symbols representing the most probable element at the black marker location The top element in the list is the most probable match Double clicking on this element or clicking on the Add button will cause it to jump into the Element box and a label will appear on the spectrum In addition for your convenience a set of vertical colored lines representing the most prominent x ray emission lines will also appear on the spectrum The lines are color coded and the green color represents the K series Cyan represents the L series and Yellow represents the M series The height of these lines represents the theoretical relative peak height of each line You can erase these lines by right clicking on the spectrum window o Confirm the peak identity by clicking on the HPD button
62. located just under the Peak ID button This will draw a thin blue line outlining the spectral peaks according to the theoretical calculation of the proper line shape and location If this snugly fits the shape of the line then the automatic peak identification was successful If not then you may have to guess again Title Scanning Electron Microscope Operation Page 59 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Step 8 Type in a Label for the Spectra in the upper left corner of the spectral data window Figure 363 highlight the old label and type in a descriptive title for the new data after the A character You are limited to 216 characters in this title OER Spectrum Image Ma File Edit View Proc Auto Setup Window He zwi s ko 1 c edax32 genesis genspc spc Tungsten Cobalt disc T Figure 36 Spectra Title entry after the A character at the upper left corner of the spectra window Step 9 Elemental Quantification of a Mixed Material o Click the Quantify button found at the lower right region of the command menu at the right side of the Spectral window This will produce an overlay window showing a table of normalized material mixture percentages This is a standardless theoretical calculation based on a set of assumptions and is normalized to 100 o Note that this theoretical calculation can be in considerable error because of situational failures of t
63. ly to a memory stick Step 11 Save the Spectra into a File o The spectra can be saved by clicking on the Save button located at the bottom of the right side panel You can input a file name and location for the storage EDAX X Ray Mapping Operating Procedure Overview X ray mapping is a technique of acquiring spectral data for each pixel in an SEM image and then coloring a map to indicate what material is located where The X Ray mapping procedure is located under the third tab at the top of the EDAX Genesis window On the right side of the mapping screen is a command panel containing control buttons located from top to bottom in the order in which they should be used Figure 38 displays this panel with operational notation Title Scanning Electron Microscope Operation Page 61 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas 1 Xi 1e Amp Time 51 2 uS E ma wv mo Mag 5810 _ Reso 1024x800 Reads 250 Live PF TIL Quant BR LE BR Spe r agi Reso 255x200 Collect Dwell ms 200 nte Maps X iv Use Z List HY OFF when done Auto LUT HP Deskjet 9800 S Field Stage X Stage Y Po Multi oom Ap ral Fields 20 Set imaging parameters Right click menu in this region to expand Collect an electron image Collect a spectrum Identify the spectral peaks Confirm the peak ID select a map or line scan Select the map type Select map colle
64. lysis See the section on SEM imaging Setting Working Distance To set the working distance double click on the Working Distance WD label in the Data Zone at the bottom of the SEM image screen A small window containing the current working distance will pop up and allow you to type in 8 for the new WD This will more than likely throw off the focus you have already established so manually joystick move the sample stage up or down to bring the focus back When you achieve reasonable focus with the stage movement you can perform fine adjustment with the focus knob Title Scanning Electron Microscope Operation Page 53 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Beam Energy If you know what elements to expect in your sample look up the EDAX voltage on the wall chart for the K L and M shell electrons for the sample atoms and determine the highest energy of all elements in the sample Then set the electron beam voltage EHT at twice the highest electron binding energy limited of course by the 30 kV max beam voltage Turn off Chamber LED Illumination Before executing the EDAX software you must turn off the LEDSs that illuminate the interior of the stage vacuum chamber The light from these LEDs causes the X ray detector to count large numbers of phantom X rays and confuses the energy calibration You can turn off the LEDs by Sliding the illumination slider at the top of the Chamber Scope
65. materials like polymers ceramics nano particles crystalline grain boundaries and cross sections of semiconductor devices Please return the SEM to the SE2 electron detector when finished This insures that new users can use the EDAX system to identify materials Nano Manipulator Stage Operation Low Noise Nano Prober System Nabity Electron Beam Lithography System NPGS Title Scanning Electron Microscope Operation Page 78 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Scanning Electron Microscope Operation Zeiss Supra 40 Roger Robbins 9 29 2015 Index A SUS Mente NODOS ba 18 OS 57 ANNO NOM AA MN 34 aporte ac oo pios 31 astigmatismim or Fe Cto usse basati o aso omues Prada daas tela esu A ON taxon AS 31 AUTOFOCUS Mere pee ee enn ROP Reem a a Ad del duse siet 31 Auto GONEITY EDAX inside AAA 58 B Dacksround color reversats ED Adidas 72 Dackscattered elec AAA AAA 41 Deam Curent EDAX en nr nae SP a ST esM MR ELI Pet t M a a aaa EE 55 plue ouine APD EDAX Gore 64 Bightness knob en EE EM ME E EOM mE M n M di Li 32 Bula ines EDAX P c 69 C Chamber LERMA ON iaa pad 54 Chamber COD aaa 22 54 A O E T 19 24 Chamberscope Illumination s EDAX AAA A A AAA 62 charee Dalancine In Sample risas charges Re gat Y UM do dl I eee er E E CNN NN SA 12 NATI sois 39 Chal SING VOI nana 40 Garziaei oz Eire nili Aa
66. ments The Purpose Comments section in the logbook is intended for recording what you did and note any problems encountered This is helpful to staff in diagnosing problems and noting what type of work is done in the SEM for logistic support data Please fill this in Title Scanning Electron Microscope Operation Page 46 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Consolidated SEM Operation Instructions This is an abbreviated list of operating instructions that guide you through the what to do next confusion that may ensue after initial training for a new user or an encounter with the SEM after a long absence from SEM operation It is essentially a step by step listing of the operating sequence tasks with reference links to the full explanation in the instruction sections in case the abbreviated listing does not trigger full understanding In this list of operating steps there will be a blue Jump to word that you can click on and the document will jump back to the full explanation section When you finish reading the explanation click the blue Return to Step n link and the document will return you to the Consolidated Instruction step that you started from STEP 1 Schedule SEM time on FOM scheduler Jump to Time Scheduling STEP 2 Fill out paper Logbook at the SEM Jump to logbook STEP 3 Prepare Sample Cu Tape Hummer Au dep Size sample etc can be done before scheduling SEM a
67. n other departments at UTD and occasionally to other universities as well as to companies with access to the UTD cleanroom Access to this SEM starts with obtaining access to the cleanroom This process starts by following the instructions listed on the home page of the cleanroom web site htto www utdallas edu research cleanroom LabAccess htm After completing all the requirements for cleanroom access you must attend a three hour training class given by the cleanroom SEM owner The next step is to create an account on the Facility On line Management FOM scheduler This step will require a charge account number that the scheduler will use to collect fees for using the SEM in order to pay for the service contract Supporting the tool The FOM calendar is located at the web site https msefom campus ad utdallas edu fom Starting Check List After having scheduled time on the SEM in the FOM scheduler and you arrive at the tool at the starting time of your schedule you will need to sit at an on line computer somewhere in the cleanroom and open the FOM system to tell the calendar that you are present and ready to start When the FOM system is notified of your presence it will turn on the monitors on the SEM system so you can log in to the SEM software However before you start please check to see that all the extra sensors are withdrawn from the chamber and are safe for stage movement and door opening Also sign in to the manu
68. nd Mount Sample on Pin Mount Jump to Sample STEP 4 Log in to SEM software Jump to Login STEP 5 Vent SEM sample chamber Jump to Loading STEP 6 Open door and mount sample on stage Jump to Loading STEP 7 Close door and pump down chamber Jump to Loading Title Scanning Electron Microscope Operation Page 47 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas STEP 8 Position stage under objective lens with joystick watching stage in the Video window Use joystick to raise stage to focus point to avoid collision with lens Jump to Stage Control STEP 9 When system is ready Scanning operational at EHT drive stage to target location at low magnification Jump to SEM Image STEP 10 Focus and correct astigmatism Jump to Focus STEP 11 Optimize image brightness contrast scan speed Jump to Brightness STEP 12 Capture image to Z MSE72017 campus ad utdallas edu datashare1 If the network link is broken you can save to the local hard drive on the SEM computer D Note that data left on the D drive can be erased by staff without notice if necessary Jump to Current policy requires you to store your images on the remote secure drive Z MSE72017 campus ad utdallas edu datashare1 This drive is located in a secret place in the NSERL building and allows read and write privileges for certain tools such as our SEM Downloading your images to your desk computer requires l
69. ndicator on the back of the EDAX preamplifier box just under the big liquid Nitrogen Dewar If it is red the sensor is warm and needs LN2 added to the Dewar If it is green all is well If it is not lit then the power is not on activate the EDAX software and re check Title Scanning Electron Microscope Operation Page 52 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas 2 How do you tell if the LN2 tank is empty There are several tell tale observations that suggest that the tank is empty and the sensor is warm 1 Lift the lid at the top of the EDAX LN2 tank if it is freezing cold and steaming then it is likely there is still LN2 in the tank 2 If the EDAX Genesis program sees no x rays then it is likely that the X Ray detector is shut off because it is above the operating temperature limit 3 If the Status LED on the upper end of the EDAX signal amplifier at the base of the LN2 tank is illuminated in Red the amplifier is turned off because the temperature is out of spec Establishing X ray Capture Sample Loading Sample loading is similar to the SEM loading procedure The only difference from the SEM procedure is that the Working Distance WD for the EDAX should be set to 8 mm in order to optimize the capture of the X rays emitted from the sample Finding Image Follow the standard SEM imaging procedure to find a standard resolution image and focus on the region of interest for EDAX ana
70. need to make sure that the stage will not hit anything along the way to the new coordinates you type into the command windows Also make sure that the Specimen Current Monitor is OFF at all times during stage movement This gives a small amount of insurance against catastrophic damage if the stage does hit anything in that the collision sensor will turn off the motors upon contact but not if the current monitor is ON Image Positioning Shortcut There is another really handy feature of this SEM software that remarkably speeds up the positioning of the sample for a photo This is needed principally because as you increase the magnification the portions of the image outside of the center region of the image on the screen expand and move off screen So after you have obtained the SEM image of your sample by using this handy trick you can drive a specific spot on the image to the center of the screen where a magnification change will not move it again This is accomplished by simultaneously holding down the Ctrl key and the Tab key on the keyboard This action causes a big green crosshair to appear on the screen Move the crosshair with the mouse to the location in the image that you want centered in the screen and click the left mouse button The SEM then either moves the stage or the beam depending on the magnification so that the image at the crosshair moves to the center of the screen This is a magnificent tool to sp
71. o reveal the bulk crystal lattice at the surface Variables that affect this process include the specimen material the electrolyte solution composition operating voltage specimen size temperature age of the electrolyte the circulation rate of the fluid and the time of contact 9 Polishing Chemical etching is another alternative to electro polishing that is less complex and often results in equal EBSD results This method involves dipping the sample in an appropriate etching solution that merely removes deformed crystal layers because of their higher surface energy compared to the regular crystal lattice The etchant must not cause surface steps that might interfere with the EBSD signal In addition the etchant must be selected according to the type of sample involved this is a very particular choice and determines the degree of success achieved If the etching solution leaves a surface film behind then the results will be poor 2 5 KV 60 uA 60 Tilt 30 kV SEM No Etch Etch 120 min Etch 240 min Etch 480 min Figure 50 Examples of chemical etch time on EBSD image quality Title Scanning Electron Microscope Operation Page 77 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas SEM Operating Procedure for Obtaining EBSD Images Scanning Transmission Electron Microscope Detector System Introduction The Scanning Transmission Electron Microscope STEM detector on our scanning electron m
72. oltage is increased past the halfway point o NOTE A plasma is struck when you see a blue glow inside the top of the plasma chamber Figure 9 Figure 9 Plasma glow inside the chamber Begin timing the process as soon as a plasma is struck inside the chamber Normal Gold deposition takes about 1 2 minutes NOTE Monitor the Plasma Discharge Current meter during the run You may have to continue to adjust the voltage to maintain you set current Concluding the Process When the deposition time is up turn off the High Voltage Also turn the High Voltage knob to zero Turn off the Power o This will start the chamber to venting vent requires several seconds When the Plasma Chamber is at atmosphere gently lift the chamber lid Figure 10 Carefully remove the cylindrical glass chamber Using a pair of tweezers remove your sample Title Scanning Electron Microscope Operation Page 15 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Figure 10 Removing the cylindrical chamber for sample retrieval Return to STEP 3 SEM Login You will have a user ID and password assigned to you after initial training Thus when you arrive at the SEM the screen will display a standard Microsoft Windows XP scene waiting for you to execute the SmartSEM software Click on the SmartSEM icon either on the left side of the left screen or the similar but tiny icon in the lower left taskbar of the le
73. on Page 63 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Todo this you have to close the RemCon32 program and open the Nabity RemCon32 program open the SEM Start icon to find menu choice Switch to the Nabity computer by clicking in sequence the buttons 1 Ctrl 2 Alt 3 Tab and then choose the number 2 Then open the Nabity software by clicking on the green Nabity icon in the right hand Multiplexed computer screen Open a Project and find the SEM button on the left side of the Nabity window and click on it This should return control of the SEM column to the SEM which allows the EDAX software to borrow control Switch the multiplexed computer back to the EDAX computer using the Ctrl Alt Tab sequence and the number 1 Before you open the EDAX software close the Nabity RemCon and open the EDAX RemCon software again 5 Collect X ray Spectrum o Press the Collect Spectrum button to obtain the X ray spectral data o Again if none is entered in the preset box then press the Collect button to stop collecting the spectral data otherwise just let the scanning continue until the preset number is reached 6 Identify the Spectral Peaks o Press the Peak ID button to have the software automatically identify the spectral peaks If peaks are left without an identity you may have to manually identify them according to step 8a in the previous section o Confirm
74. on of secondary electrons near the surface from the primary beam and backscattered electrons To the first order the energy distribution of the secondary electrons is independent of the energy of the primary beam Because of this characteristic a universal curve can be generated for all metals Figure 26 The curve rises from a zero emission coefficient for zero secondary electron energy to a peak between 1 3 and 2 5 eV for most metals and then falls to a low value for secondary energies greater than 10 eV For insulators the peak falls at a lower secondary electron energy because there is a lower potential barrier at the surface of insulators than there is with metals and this allows a larger number of slower secondary electrons to escape The SEM video system produces a brighter pixel where the secondary electron current striking the electron detector is greater Relative probability arbitrary units Electron energy ev Figure 26 This graph shows the envelope of probabilities of secondary electron escape from the surface of metals as a function of the secondary electron energy The data shows a probability of escape peak between 1 3 and 2 5 eV This peak denotes the general energy level of the secondary electrons Title Scanning Electron Microscope Operation Page 43 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas This data sets a value for the energy of the secondary electrons collected by the
75. or Roger Robbins Date 9 29 2015 The University of Texas at Dallas Aperture Selection The beam current in the Zeiss Supra 40 SEM is set by choosing different sized apertures The EDAX signal is more dependent on beam current than it is on image resolution A slightly fuzzy image is usually OK But the optimum EDAX signal is such that the EDAX X ray counting rate CPS is sufficient to allow the computer s Dead Time DT to run between 20 and 40 of the capture time This DT number is found at the bottom of the spectra screen next to the left most number in the data line The X ray counting rate counts per second CPS is the actual left most number in the data line ICPS 8027 Figure 30 Data bar at the bottom of the spectra screen showing the parameters for EDAX operation EDAX Operational Procedure Before you try to open the EDAX software first open the RemCon32 EDAX software that communicates between the SEM computer and the EDAX computer This program is found in the Start button menu at the lower left corner of the left side SEM display It will start in the minimized location in the bottom line of the left display SEM display Expand it and it will pop up in the lower left corner of the right SEM display The EDAX computer is connected to the multiplexed display on the right side of the dual SEM display screens This monitor keyboard and mouse is used to control three computers and is directed to each computer
76. perating instructions to perform elementary material analysis at a basic level lt follows the step by step procedure for obtaining the data and generating a simple analysis Students must obtain Staff training on this tool before attempting operation The directions in this section assume that you have been trained and have some experience running the SEM itself Title Scanning Electron Microscope Operation Page 51 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas W La CoKa Figure 29 Example of EDAX spectra X ray counts vs X ray energy The pattern of energy levels is analyzed to determine what element emitted the X rays EDAX Spectral Analysis Setup Procedure Detailed operating procedure from the perspective of a new operator Scheduling the tool This tool falls under the SEM scheduler at the following web site https msefom campus ad utdallas edu tom loginUT Dallas To get started on this scheduler you must create an account following the link on the web page This will involve inputting an account number cost center number that supports your research work Fill out Logbook The paper logbook sitting on the SEM table must be filled out completely Starting Check List Before using the system determine what condition configuration the SEM EDAX is in it should be in a standard state List critical items that must be checked before operating SEM EDAX 1 Check the LED status i
77. r v zl uo 4 6 Maps Line y M l Ju F Orit Points 166 Collect Owedlims Line X frossa ra 4 Use Z List HV OFF when done tT A Ilis ent 3 Portrat Field Stage X Stage Y tet EPStives8 DT 100 Lsec 1945 cris las kev1000 FS11299 Time 55min 72 start ero Fue ES Microsoft cs O wb Figure 41 Screen display after the Line button is pushed and the Draw Line icon is clicked and the Build Line icon is also clicked to bring up the little Build Line window box o Click on the Draw Line icon to expand the SEM image to full screen size Draw a line by left clicking and dragging the line across features you want to analyze o After the line is created click on the Build Line icon This will bring up a little window with choices to make Select the ROI to display element concentration graphs Click on the box by the Average pixel label and enter the averaging matrix size i e 5x5 This will help reduce noise in the graph line by using a running average technique Click Ok and create a name and location to store the resulting name csv file that you can access with MicroSoft EXCEL later o The actual line scan graph will appear in a new window with the number of graph lines determined by the remaining elements in the Element box that you set up previously See the three band graph in the right window in Figure 42 Title Scanning Electron Microscope Operation Page 69 of 85 Author Roge
78. r Robbins Date 9 29 2015 The University of Texas at Dallas Bc ERAX Spectrum Image Maps Line x File Edit view Collect Process MultiField Setup Window Help P e Bs T a um E HJ Ed E FAW SU ES Y HE g Analyzer Det1 y ES None Amp Time 51 2 us 3 2E 00 Mas r Reso 1024x800 E Collect amp fou 250 e Collect B Line Scan RO Counts C IMG USR New Folder AuC_1 Ox ROI Counts C IMG USR New Folder AuC_1 File Edit View Scale ngOvly Image usas tr Pak um a A PA YO P A ALVA WA Maps Line x TLI Quant A Drift Image Display J k LE h L Points l U l f NJ Y Jj N R i VV LUNA vo P uz tine X A iv UseZ List gt H OFF when done t xj Print amp z Deskjet 9800 S rtrait Field Stage x pem Y Fields 20 ICPS 118095 DT 100 Lsec 194 5 Cnts 156 keV 1 000 FS 11299 Time 0 55min id start o 3 Genesis Imaging Map M EDAX Spectral Pro E3 Microsoft Excel BH Line Scan ROI Coun Ed Microsoft Excel gt Figure 42 Line Scan e windows HORNON the pure apum window Right and the veras graph Left Rio La gt o You can create an overlay graph which puts the graph lines on the SEM image so that you can visually see where the x ray intensities for the various elements lie on the image This gives you the visual location of each element you look at Unfortunately this image appears in a new window that is fixed
79. ration details taken from Thomas Brian The Hummer VI www utdallas edu Research Centers Cleanroom Documents eHummer pdf 10 29 2003 Title Scanning Electron Microscope Operation Page 13 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Plasma Chamber Vacuum Gauge High Voltage Control Knob High Voltage Control Switch Mode Knob Pulse Switch Power Switch Plasma Discharge Current Meter 9 Timer Knob 10 Auto Manual Switch OET cd CUM Figure 7 The Hummer VI Control Reference photo Hummer Procedure Placing your sample in the chamber Gently open the lid of the plasma chamber Place your sample inside on the sample platen Figure 8 Gently close the lid Note if you allow the lid to slam down the sputter target will fall off and potentially break your sample It is magnetically held to the top of the chamber ho AA Figure 8 Opening the Plasma Chamber to insert a sample Title Scanning Electron Microscope Operation Page 14 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas urn on the Power switch Wait for the vacuum level to fall to around 150 millitorr Flip the High Voltage control switch on Turn the High Voltage Control Knob until the Plasma Discharge Current meter reads 20 mA o NOTE As you increase the voltage current will not increase until a plasma is struck inside the chamber This may not occur until the v
80. ready to leave remove your sample and pump down the sample chamber When the pump down starts you can log off to end your session and sign out of the logbook The EM Server program will take care of the SEM hardware after you log out The logoff will stop the use timer and log you off so that the tool is ready for the next user At logoff the high voltage for the gun is automatically shut down This will preserve the life of the field emitter tip that produces the electron beam It is expensive many thousands of dollars Title Scanning Electron Microscope Operation Page 44 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Completion Check List Before leaving SEM set the machine to its standard idle configuration mandatory Job Completion Checklist EHT off Return software to standard SEM configuration Remove Sample Re establish vacuum Complete Log Book entries Make sure that the SEM table is clean and free of samples 1 2 3 a 5 Log out of SEM software 6 8 Return tools to their home Rules of SEM Operation The official rules pertaining to time cost and operation follow Time Allocation Because this tool is a high use system we have linked the SEM to the new Facility On line Management FOM scheduler software located at the web page noted below Also listed below are some schedule and cost rules these rules were established to help ensure tha
81. ric height Once you achieve focus at the angle you want you should be able to move the stage in either the x or y axis and scan whatever you need to and still stay in focus Charging Many times during your career at the SEM occasions will arise when you would like to image an insulator material Unfortunately SEM physics objects to that If you were to try to image an insulator the image would appear to contort into strange conditions of brightness shape and aurora like movement This would be due to electrons congregating in ever larger numbers on the surface or body of the insulating substrate thus building up a space charge which severely affects the electron beam This phenomenon can cause many strange and dynamic effects in the picture too numerous to describe here Title Scanning Electron Microscope Operation Page 39 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Figure 23 Examples of objects charging in SEM To avoid charging we normally sputter coat substrates with a very thin film of Gold and Palladium mix so that the coated surface will be able to discharge excess electrons to ground and thus not 10 50 ev cause the imaging beam difficulty Charging in a sample is highly complicated and depends on many things but the balance of electrons hitting the target and those escaping the target is the key to controlling the consequences ldeally the sample potential should remain
82. roscope Operation Page 80 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas F lastscan stage speed pl Mrs a dada 33 o ao ssentiedetucses n m sao sarcauiriascts Mean Use RO scnaeanisemuateesantatewcsouats tamed EC coe tale LU estu DERE ed aged 26 e aon cuta non concede o arae ta ene tote A arena due LE 25 FOCUS TM es 30 FOCUS ana AO o o adnan ts 29 FOCUS Wobble Apertute Alea E R 31 A balun date poss vr er t diae laci m da Ten eae else bras ERES 33 A APP spain meant Ratan E A EA E T actor 30 treezing the lMase Ci tit dass 33 G E aM 55 ghost IMA ais 33 mu Mur E 32 Gundi valora E ara muitis tute or adf ae 74 H Halographic Peak Deconvolution HPD elsssseesseeseeeen eene errasse sen nennen 64 FEU Cle Fel ONT Panel oue acdiadetusu te ama leas ds cate atansmces unte d hd topo ruat o e et ooteda fu e od idt dto 25 Hard Frorit Panel Option vus oia ra ph esu epe ei Een AAA d edt aveo dk ditta Fede ois ea duda 18 AP D Spectra ine QUIN slds murtasce bit panes utes hte tec db iaa 58 Hu Mer Proceed re ia acia 14 HUME RI ites 13 l rolg eum E a E ink Serra A a E EES 31 identi y ar EDAX spectral PESA AAA AAA 59 illumination errors EDAX stage Tal o uc s mH IP SIS 54 iumination sllder EDAX StdBO Sciebat E I PU Re eau tete bI ee trahis uia bau etat uta uas ui edute 54 NALS dnm nsulator adem eve RE LIN EE CUAN H E a RI
83. ry by clicking on Change Directory and selecting your directory It will nominally default to the last drive selected but you will need to select your sub directory on the z datashare1 remote secure drive Type in the name of the image file you want to store Click a check mark into the box titled Annotation to save any screen text annotation with the image Fill in any special text explanation you want to save with the file into the User Text box This text will save into the image file so that you can see it in a directory listing but will not imprint on the image Special Imaging Techniques Eucentric Stage Configuration A Eucentric stage is designed to keep the sample image target in the field of view as the stage is tilted for an angled perspective Unfortunately the stage we have in our SEM is not a eucentric stage However it is possible to position the sample at the eucentric height and thus achieve some of the stability effects of a real eucentric stage The basic principle of Eucentricity is that the sample must be set exactly at the center of tilt of the stage so even if the stage tilts the sample will remain in reasonable focus and stationary in the scan field no matter whether the stage is moved in x or y directions This is made possible by the stage design Our stage is bolted to the bottom of a rotating plate that is mounted to the front door that we open to load samples Thus the bottom of the stage rotates at the
84. s option sets the number of times the field is scanned and data added and averaged to reduce noise o Note that a time estimate is shown in the bottom status bar Figure and will update as the parameters are adjusted For live and live spectrum maps no time estimate is given because the maps can be stopped at any time by the operator This can be used to help arrive at a practical set of parameter values CPS 11 DT 100 Lsec 1310 7 Cnts 2781 kev 1 000 FS 93758 Disk 0 1GB Time 3 2min Genesis Imaging Map Figure 47 Note the estimated time to complete a map is shown in the bottom line 10 Collecting a Map o Click on the Collect Maps button to start the map data collection This will bring up a small window asking you what you want to call the map and where you want to put it Conjure up a name and stash it in a place you can find later o Note that the time estimate in the bottom line will update in real time to help you know when it will be done o If you need to stop the map before the end of time just click on the Collect Maps button again The program will have saved the previous data and will produce a map even though you stopped it Map Analysis Line Scan Analysis e The Line Scan analysis allows the user to draw a line across an SEM image of a recorded spectrum map file type mapname spd and graph the spectral line intensity for each of the ROIs as a function of location on the line Thi
85. s due to residual astigmatism at focus Astigmatism correction is the next step to clear the fuzziness at focus Title Scanning Electron Microscope Operation Page 30 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas To correct astigmatism rotate one of the stigmator knobs until the fuzziness increases noticeably and then rotate it the other way until the fuzziness again increases The proper stigmation correction position is in the middle of these two extreme knob positions See Figure 19 Repeat this approach with the other stigmator knob and then refocus with the big focus knob This should bring the image to a sharp focus and you are done So now that we have covered the manual focus procedure the SmartSEM software in some cases can make this an effortless button push procedure On the row of icons at the top of the screen Figure 20 is a special Auto Focus Stigmate function that is activated by the middle mouse button Roller wheel By clicking on this icon with the roller wheel on the mouse the system will snap into an auto focus mode where the scan is reduced to a small rectangle in the center of the image and a window with a progress bar pops up showing you the focus status Allow this to complete and observe the results in your image The little focus and status box will disappear when the function is complete If the image has sharp details the auto function was successful If the image appears
86. s effectively displays the location of each element along the defined line e Line Scan procedure o Select a saved spectrum map data file type name spd in the File Open menu in the map tab screen Title Scanning Electron Microscope Operation Page 67 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas o Expand the Peak ID box by clicking on the up down carat symbol at the right of the Peak ID button o Delete the unwanted elements from the Element box by highlighting them and clicking the adjacent Delete button Figure 40 This action selects the elements you want to display in the line scan element intensity graph by throwing out the ones you don t want Peak Fe ID HPD mM X Element zf Ze CK Add Possible AIK Aun Delete Del All Z List Fe EPIC FS Alpha Lines Only C Elem C Shell Trans Markers 11 Abs Esc Sum Advanced Figure 40 Expanded Peak ID window showing the Element box and the Delete button o Close the expanded Peak ID window and click on the Line button This will exchange the icons below the button to the relevant line scan icons Title Scanning Electron Microscope Operation Page 68 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas ASERAX Spectrum Image Mapsitine x 23089 TA DBBEBG WS Wi Amm 3 pesao ame mis zm kv 100 Meg swo ia Reso 1024800 y Collect e css 250 coma uf Clea
87. scccsscescsesccessnesssencnesseercsenesessuesseenacesencsieene 74 Mechanical Poll shilPGxivaciu hum ipa intendo um EE 74 SEM Operating Procedure for Obtaining EBSD Images 78 Scanning Transmission Electron Microscope Detector System 78 A AA 78 Title Scanning Electron Microscope Operation Page 4 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Nano Manipulator Stage Operation ccooccncccccncccncnccononononnnonanononannnnnncnnnnnons 78 Low Noise Nano Prober SySIGITI cuisine 78 Nabity Electron Beam Lithography System NPGS cooccccoccccccnccncnccncnnnnnnnos 78 scanning Electron Microscope Operation cccceeccecseeeeneeeeeseeeesseeeesaeneesaaes 79 ZAS SOU 0 E Down Aba 79 farei qe ccr 79 Title Scanning Electron Microscope Operation Page 5 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Scanning Electron Microscope Operation Zeiss Supra 40 Roger Robbins 9 10 2010 Update 9 29 2015 Introduction General introduction to the scope and purpose of this document This is a step by step operation manual written for the Zeiss Supra 40 Scanning Electron Microscope at the University of Texas at Dallas Cleanroom including the numerous optional subsystems mounted on this tool In general the material presented here informs the reader about how the tool works in the order that an operator would proceed in using the tool
88. secondary electron detector in the SEM Thus the Everhard Thornley electron detector with its collection grid has to accelerate the secondary electrons to several hundred eV to cause a phosphor photon to be generated and then converted to an electron current that is multiplied many times by the photo multiplier and video pre amp It is this current that produces the standard SEM image on the computer screen Return to STEP 12 Sample Removal Sample removal is accomplished by clicking on the Specimen Change icon at the top left of the SEM image screen This action will automatically turn off the high voltage and close the column valve before venting the chamber Before you click on this icon please make sure that the stage tilt is O degrees then manually drive the stage down in z to a height of 10 mm then move the stage in x and y to the center at 65 65 mm For the x y move you can type into the go to box in the stage manager menu the 65 65 locations for an auto drive move This will move the stage to a safe position in a safe manner so that there will not be any collisions during the move or the door opening action When you remove your sample and click on the ensuing Press OK to Pump button on the popup window the SEM will re establish vacuum and bring up the High Voltage EHT If you are finished follow the EHT Shutdown Procedure in the next section Return to STEP 13 Shutdown Procedure lf you are done and
89. steps that produce a smooth flat surface ready for further treatment Typically grinding starts with something like 240 grit Silicon Carbide SiC sandpaper and goes through succeeding steps of ever finer grit to 800 or 1200 grit sandpaper Microscopically the surface will look like fine scratches and will need further work to expose the underlying crystal lattice Title Scanning Electron Microscope Operation Page 74 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas 4 Polishing Polishing is used to remove the scratch deformation caused by the grinding step It usually consists of using a colloidal polishing grit on a flat table and swirling the sample around on the table ina rotating figure 8 pattern with coarse grit and then stepping to a finer grit until the desired polish quality is achieved There are many types of grit available but the literature suggests that a commercially available solution of colloidal silica works best for the final stage of EBSD samples This stuff consists of negatively charged particles of SiOz with a pH value between 8 and 11 chemically basic The resulting surface will usually look rather shiny at this point The following images show a link between the degree of surface preparation and the resulting EBSD image quality of a standard Nickel substrate Figure 44 Surface appearance left and EBSD pattern right after 1200 grit SiC paper No EBSD pattern visible
90. t based on the magnification size of the sample features and a nominal time of collection O O For fine featured samples a low resolution 64x50 may not be appropriate because the pixel may be larger than the feature At high magnifications a higher resolution can result in the pixel size being smaller than the diameter of the beam The higher the resolution numbers the longer the collection time o The dwell time is the amount of time that the beam will collect data at each pixel The dwell number for both standard and quant maps is in milliseconds For live maps the dwell is in microseconds O Title Scanning Electron Microscope Operation Author Roger Robbins The default dwell time for live maps is twice the processing time The time can be lengthened but not shortened For Quant maps a minimum dwell of 50 milliseconds is required Since the background subtraction and peak de convolution calculations are performed at each pixel the dwell must be long enough to allow the calculation For Live Spectrum maps the minimum dwell time is 50 microseconds A minimum dwell of 200 microseconds is recommended for the 128x100 resolution but 100 microseconds for 256x200 or higher resolution Page 66 of 85 Date 9 29 2015 The University of Texas at Dallas o The ROI parameter Region Of Interest refers to the number of spectral line elements chosen for mapping This will be the number of maps created o The Frame
91. t each spot the electron beam moves to in a frame then averages them all together and displays the spot as the average This technique reduces the image noise by reducing the spot noise at each spot and results in a real time moving image if the stage is moving The frame averaging sweeps an entire frame stores it and then averages it with the next frame for a selectable number of frames This creates a dynamic image that produces ghost images for a moving stage that slowly coalesce into the final image when the stage stops moving not so useful for motion situations Return to STEP 11 Image Capture and Storage Current policy requires you to store your images on the remote secure drive Z MSE7201 7 campus ad utdallas edu datashare1 This drive is located in a secret place in the NSERL building and allows read and write privileges for certain tools such as our SEM Downloading your images to your desk computer requires linking to the secure drive on the campus network Once the link is established then you can down load your images and data but you cannot write to the secure disc from your desk computer This arrangement is our effort to reduce the possibilities of tools catching viruses from memory sticks or general computers accessing data from the SEM and other tools In the case of the cleanroom SEM you also have the privilege of storing images on the SEM computer drive in an assigned folder This represents a backup storage medium
92. t the tool is used fully and to alleviate schedule overlaps and conflicts o Network location of FOM scheduler https msefom campus ad utdallas edu fom o There is an SEM calendar and time allotment page that you can log in to and capture time on the machine o Users are permitted to sign up for 10 prime time hours per week Prime time hours are Monday Friday 8 00 AM to 6 00 PM o Signup times are set at half hour time blocks min time allowed o Users are charged for the full time they reserve the tool for unless they cancel at least 24 hours before the start of their session You may swap time with another user if necessary o Non prime time hours Weekends and weekdays from 6 00 PM to 8 00 AM have no restriction on the length of signup time o You must log out of the FOM calendar at the end of your session If you forget you will incur additional charges Fill out the paper logbook at the start of your session Do not store or leave samples at the machine Samples can be thrown away by staff without notification Do not use SEM computer to check e mail or browse the internet or play games Title Scanning Electron Microscope Operation Page 45 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas e Specimen current Monitor SCM should be OFF at all times except for the short time it takes to measure specimen current e Never unplug the Pico Amp Meter cable from the front door while the electron beam is on
93. ted in the front back direction Figure 17 Photo of the rectangular multi pin sample holder To compensate for this confusion and perhaps speed up the effort locating a sample have created a coordinate location map that sets coordinate locations for all four corners and each of the 12 pin mounts This data is only valid if the stage rotation is set to 15 degrees and the sample is mounted on the holding button with the banking bar on the left side of the table as one loads the rectangular multi pin sample holder onto the SEM stage The Pin number is the stamped number on the holder as seen in Figure 17and Figure 18 Title Scanning Electron Microscope Operation Page 27 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas SEM Stage Coordinate Location of Multiple Pin Samples Y Red numerals identify Sample location marks Read Table for Sample 6 Stage Location 64 44 millimeters Upper Left corner Location 43 23 millimeters Table values are only valid for stage rotation set to 15 degrees Corner number related to samples double sticky taped to sidewalls of the holder for90 deg cross section imaging Figure 18 Map of pin locations with stage coordinates Also including corner locations for finding edge profile samples taped to the sidewalls of the holder The significance of the Corner Coordinates is that if you are looking at multiple cross section samples taped to the side o
94. the SEM to work in tandem with him her while not disturbing the SEM operation Note E Beam Lithography uses the EDAX computer screen so tandem operation with lithographers does not work e lf you learn an advanced process which uses different program parameters or windows configuration please return the system to normal conditions before you leave Title Scanning Electron Microscope Operation Page 72 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Additional EDAX Software Details This section can describe the software knobs and buttons in a collected section Special Purpose Subsystems Explain that these systems are beyond the scope of this manual and are special purpose systems and users must undergo extensive specialty training by experts in the subsystem after they become familiar with the standard SEM operation Electron Backscatter Detector Operation Briefly describe how the system is used This is a survey level description with generalities rather than detailed knob operation Title Scanning Electron Microscope Operation Page 73 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Electron Back Scatter Diffraction System Briefly describe how the system is used This is a survey level description with generalities rather than detailed knob operation Sample Preparation Overview Proper sample surface preparation is paramount in obta
95. them in sensitive vacuum systems in Bay 5 If you material can be completely out gassed so that it will not introduce vapors into the SEM then you can pre condition your sample to make it compatible Figure 5 Vacuum desiccator for outgassing SEM samples Characterization Bay 5 Title Scanning Electron Microscope Operation Page 11 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Sample Holders There are a huge number of sample holder designs for SEM samples We have a few Figure 5 However for special sample configurations you should consider purchasing special sample holders that fit your needs and most importantly our SEM Please consult with the Clean Room Staff SEM owner before ordering Figure 5 Sample holders in stock These range from standard small pin mounts to edge profile holders to multiple pin to 4 and 6 wafer holders There is also a transmission electron microscope sample holder second from left on bottom row Sample Grounding The sample needs to be electrically connected to the sample holder to prevent the electron beam from charging the sample and distorting the image This is usually done through conductive tape We have double and single sided Copper sticky tape If you have a conductive sample this simple attachment will work fine If you have an insulator substrate with a conductive film on the top the top film must be electrically connected to the Aluminum sample
96. tions are shown in Table 1 below Table 1 Normal Gun Conditions Parameter Value EHT 19 79 kV Title Scanning Electron Microscope Operation Page 21 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas If the electron beam has been on and at high voltage the system will automatically bring it back on after proper vacuum levels have been reached If the high voltage does not come back on you can switch it back on from the Gun tab window by clicking on the drop down menu under Beam State and click EHT On Stage Control Now that a beam is established the substrate needs to be positioned under the column so the beam can see it This requires moving the stage from its default loading position to the inspection location which may depend on the sample and its size and shape Before moving the stage bring up the Chamber Scope window by clicking on the Eye icon at the lower left task bar of the right side LCD monitor This will bring up a window into the SEM chamber viewed from the rear looking toward the front door The image is an optical image illuminated by 6 LEDs Note that the image shows the stage in a mirror image presentation since the video camera is mounted on the back wall of the chamber looking toward you if the video image moves to the left the stage is moving to the right from the standpoint of a user looking at the stage from the front In any case this allows you to see the mechan
97. ulated spectrum one frame at a time This is the best way to collect data at high speed After capturing the data you can access a complete spectrum at each image pixel You can also build compositional maps of any type including Quant Maps o Quant Mapping This type collects data in the same way as standard mapping However at every pixel a complete background subtraction and peak deconvolution is performed The data could be composed of several types including Net intensities k ratio and ZAF In a Quant map with ZAF weight percent as the data type only one atomic energy level from each element can be used in the map For example if Iron K and L lines are in the peak ID list only iron K will be mapped Title Scanning Electron Microscope Operation Page 65 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas 9 Set Mapping Parameters o Roll the cursor to the right of the Collect Maps button and click the right mouse button A new little window will appear with several options as in Figure 39 Collect Maps 64x50 126x100 w 256x200 512400 1024x600 0481600 YU Maps J iv Live p LE pe iv Spc Drift Maps Resolution Square Images Frames Data Type Spectrum Mapping k Line J TIL Y Quant 4 Feso 256x200 Orwell us 200 Figure 39 Expansion of the parameter listing at the Collect Maps button o The map resolution should be se
98. unt is the pin mount made of Aluminum and shown in Figure 4 Eau e i Figure 4 Simple SEM sample mount showing a metal sample attached with sticky conducting tape The Copper tape affixed to the top of the sample insures a conductive path to ground for the top film esp if the substrate is an insulator Also shown to the right is the removable Aluminum SEM sample Pin Mount The large round table is the Title Scanning Electron Microscope Operation Page 10 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas mounting platform that slides onto the SEM stage The Allen wrench fixes the little sample mount stem to the mounting platform do not over tighten Sample Types Not Allowed in SEM Because the SEM optics column is sensitive to charging form particles or adhesion of insulating films on the walls of the column and specimen chamber there are some sample types that we do not allow in the SEM e Powders of any type cannot be put into the SEM sample chamber o One possible work around from this rule is to adhere powder to adhesive material double sided Cu Tape and blow off the loose powder with a N blow off gun so no particles will be released inside the SEM chamber when the vacuum pump or vent starts e Materials containing volatiles that would outgas into the chamber walls cannot be put into the sample chamber o We do have a simple vacuum chamber Figure 5 for out gassing materials before placing
99. unt will capture the set number of scans and then automatically stop The reason for multiple energy scans is to average out any spectral noise that would cause small spikes in the baseline Usually 100 scans is sufficient to establish a fairly noise free spectrum Step 3 Clear the Old Spectra and Peak Labels O O Click the Clear in the Collect box menu area to erase any old spectra that might appear on the screen Click the Clear All button in the Peak ID menu area to remove the old peak labels Step 4 Adjust the Spectrum Scale o Set the mouse cursor in the left side of the spectrum graph region click and hold the left mouse button down and then drag the mouse horizontally to the right to expand the energy scale at the bottom of the graph until the max voltage is just beyond the most energetic spectral line expected Alternately click on the spectrum window and then move the cursor up to the upper left area and click on one of the expand contract v shaped arrows to accomplish a similar scale adjustment for the expected upper limit of the spectral data Figure 34 Title Scanning Electron Microscope Operation Page 57 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Bc ERAX Spectrum Image MapsiLine File Edit View Proc Auto Setup Window Help 2 E eB Sh K O o vy el AlT wu Figure 341 Location of scale expansion contraction arrow icons Step 5 Start the Spectral
100. war and pre amplifier mounted on the Gemini electron microscope column Title Scanning Electron Microscope Operation Page 50 of 85 Author Roger Robbins Date 9 29 2015 The University of Texas at Dallas Basically the X ray emission is stimulated by electrons from the SEM electron beam striking atoms in the sample material and knocking out inner shell electrons and creating electron holes where the ejected electron used to be Then another electron from an upper shell of the same atom falls into this hole and liberates a photon having energy equal to the difference between the falling electron s home level and the lower level it falls into The energy of this liberated photon is in the range of X ray photons Figure 28 kicked out electron W external i stimulation i radiation energy Figure 28 Sketch of atomic energy levels and x ray photon generation from SEM electron bombardment excitation By counting and sorting each X ray into software bins according to the energy level of each X ray a graph can be fashioned that shows X ray counts vs energy Figure 29 This results in a spectrum characteristic of the quantum energy differences in the electron energy structure of the atoms in the sample material This spectrum can then be analyzed by the software and the elements contained in the material can be identified With more analysis the ratio of elements can also be identified This document is intended to convey o
101. window all the way to the left The screen will go totally dark If after that the window still shows a small spot of light it indicates that the stage End of Travel Sensor is illegally active The only way to cure this is to re initialize the stage which consequently requires re establishing the SEM image at your target Illumination Error Recovery Recovering from the Stage End of Travel Sensor illumination error requires re initializing the stage To do this record the current stage location manually drop the stage back to a safe distance from the objective lens Z 10 mm and then open the Stage menu from the top row of command menus Find the Initialization command at the top of the list and click on it This will cause the stage to automatically drive to the zero end of each axis and reset the stage zero location When it finishes this operation it will have turned off the end of travel sensor illumination This fixes the interference with the X Ray detector and the EDAX system can work now However you have to move the stage to the previous location which you dutifully recorded before starting this operation and find the spot on your sample that you want to record a mass spectrum from WARNING Please do not drive the stage in Z by inputting numbers into the digital move boxes move it manually while watching the video camera so that you wont hit anything Title Scanning Electron Microscope Operation Page 54 of 85 Auth
102. xpanding the Peak ID window and Del All from the element ID box o Scale the spectrum graph axes See Step 5 in the previous section 3 Set Image Parameters o The resolution parameter is accessed by right clicking on the numbers to the right side of the Collect button The resolution number is like a digital camera resolution number higher numbers give clearer pictures however they take longer to acquire The Reads number sets the number of frames to average together to reduce image noise The Resolution and Reads numbers are a little tricky to guess because the combination of these numbers sets the time to acquire the image and could run into hours if they are too big Suggested nominal starting numbers are 256x200 for the Resolution and between 16 and 32 for the Reads 4 Collect Electron Image o Press the Collect e button to start collecting the SEM image over the area of interest for the spectral data collection o If the Preset box has a number in it then the image collection will auto stop when the preset number of scans has been reached o Otherwise you will have to click on the Collect e button again to stop the scanning o NOTE Ifthe spectral lines appear to be high on very light elements and scrambled elsewhere the Nabity software may have to be opened and set to SEM mode to give control back to the SEM and its EDAX software Title Scanning Electron Microscope Operati

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