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EDAX FOCUS 2008 Vol. 6 No.3
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1. Pegasus Course October 20 24 W SNS SSS u EDAX FOCUS Page 6 Copyright 2008 All rights reserved EDAX Inc 2008 Dr Joe Nicolosi is Director of Technology responsible for Research and Hardware Engineering at EDAX s corporate office in Mahwah New Jersey Joe also looks after Technical Support and hardware interface requirements of EMM s Joe holds graduate degrees from both Polytechnic Institute of NY in Crystallography and X ray Physics and a B S in Physics from New York Institute of Technology Joe began his career in 1972 with Philips Research Labs developing new techniques and instrumentation for X ray diffraction and spectroscopy and later moved to the operating division of Philips Electronics Instruments to develop commercial instrumentation In 1998 when the EDAX division of Philips moved to Mahwah NJ Joe took on the role of detector development for EDS Systems In his current position Joe works with product management scientists and engineers in formulating and realizing new capabilities in products for materials and micro analysis Joe and his wife Wendy have been married for 25 years and have three adult children Brooke Joe and Emily a senior at University of Vermont Fond memories remain for Cub Scout and Church Youth Group leadership as well as competitive J 24 sailboat racing These days Joe and Wendy enjoy sailing the New England coast from New York to Maine Their favorite stops include Block Island
2. Cuttyhunk Martha s Vineyard and Nantucket Islands When not shoveling snow in the winter Joe and Wendy enjoy skiing in the Berkshires and Vermont EDAX FOCUS Page 7 Andreas Makat is the Sales Manager for the EDAX Wiesbaden Germany office Andreas was born and raised in Berlin Germany He studied Mineralogy at the Free University and continued his education at the Technical University of Berlin In 1987 he received his Mineralogist certification After receiving his certification Andreas relocated to the city of Wiesbaden where he became a sales engineer for Vacuum Generators VG a UK based company For 7 years he was responsible for the sales of XPS and Auger Spectrometers of VG Scientific in Germany Austria Switzerland and Scandinavia In 1994 Andreas joined Rontgenanalytik Messtechnik GmbH where he was responsible for the sales of EDAX spectrometers in Germany Andreas was key to the growth of the EDAX business in Germany As business grew the organization grew with it and in 1998 Andreas received full responsibility for the EDAX business and was promoted to Sales Manager for EDAX products In 2002 EDAX became a business unit within the AMETEK organization Today the EDAX office in Wiesbaden has grown to include sales service and support of the EDAX products in Germany Austria and Switzerland Andreas resides with his wife and daughter Tabea near the city of Braunfels which is close to the city of Wetzlar In
3. his spare time Andreas enjoys gardening volleyball and motor biking and spending time with his family Copyright 2008 All rights reserved EDAX Inc 2008 CUSTOMER NEWS The University of North Texas The University of North Texas Center for Ad vanced Research and Technology CART is located in Denton Texas approximately 30 miles north of Dallas The CART facility enables research projects from all University departments and disciplines including Materials Science and Engineering Mechanical and Energy Engineering Physics Chemistry and Biology The CART center supports UNT students researchers and faculty from the departments listed above as well as outside University government laboratory and industrial scientists The facility currently has five EDAX systems in their collection of analytical tools These include an FEI Tecnai 200 KV STEM with integrated EDAX EDS FEI Nova 200 FIB SEM with an EDAX Pegasus system FEI Quanta 200 Environmental SEM with a Pegasus system Phillips EM 420 TEM with an XM2 EDS system and a Jeol 5800 with an XM2 EDS Imaging system An Apollo 40 SDD and 3D EBSD software were recently added to the Dual Beam to elevate the capabilities of their existing Pegasus system Brian Gorman a senior researcher within CART is very excited to begin experiments with the 3D software and collaborate with EDAX He plans to utilize the 3D capability to investigate grain boundary orientations in
4. on the drop down menus from the file bar Try learning a new capability or two just by exploring what the software has to offer f you do find that you need further help or support go to our website at www edax com service service cfm to check out our new on line support capabilities Copyright 2008 All rights reserved EDAX Inc 2008 EDX is a fast and easy way to get information on samples requiring microanalysis on a SEM or Dualbeam One limitation to EDX is peak overlaps where two X ray lines from different elements have peaks at the same energy and can not be reliably distinguished using EDX One example is the tungsten Ma and silicon Ka overlap seen in semiconductor samples which will be examined in this article Other examples include PbSMo and Bali in minerals HfTaSi in nickel based alloys CrMn in steels and InCd in solar panels WDX in comparison has better resolution compared to EDX and is able to resolve most EDX overlaps In this case only WDX can resolve W from Si In Figure 2 data was acquired at 5kV in the raster region Typically peak intensities are measured from a region of interest ROI around the peak centroid but the ROIs for tungsten Ma and silicon Ka are too similar to resolve one from the other Using WDX the peaks for Si and W are fully resolved and can be accurately measured The EDAX Trident and Neptune combined EDX and WDX systems are very useful for analyzing such samples Data was acq
5. polycrystalline solar cells and compositional microstructures of aerospace materials Art amp Layout Christine Meehan toot The University is most impressed with the phase ID capabilities the Pegasus system provides The ability to collect EDS and EBSD data simultaneously is a powerful tool and is very helpful in distinguishing subtle differences in our samples notes Brian He is also pleased to have the high throughput of EDS counts the Apollo 40 will provide This capability shortens 4 D spectral image acquisition times allowing for more users to take advantage of the technology Brian also states that the dual beam is the most heavily used instrument in the facility It is presently use for TEM and Atom Probe specimen prep and 3D serial FF sectioning Brian is p interested in very acquiring a LEXS WDS system to enhance the ability to collect light element data at low KV conditions Brian is very pleased with the EDAX systems and would recommend EDAX for any lab conducting high tech research He is most impressed with the breadth of knowledge that the EDAX EBSD applications and developers possess and enjoys developing techniques with them in conjunction with his research Contributing Writers Andreas Makat Dr Joe Nicolosi Tara Nylese Jack Rosek Dr Bruce Scruggs Craig Theberge ahamed manera E SLNE ATRL S SS A Copyright 2008 EDAX Inc No part of this publication may be reproduce
6. to use analysis software Orbis users can make elemental analyses on small samples such as particles fragments and inclusions or automated multi point and elemental imaging analysis on larger samples with all the benefits and simplicity of an XRF analyzer Benefits include Non destructive measurement Minimal sample preparation e g no sample coating is necessary Improved sensitivity for many elements in comparison to SEM EDS Inclusion and coating thickness analysis with the penetrating power of X rays Analysis of wet samples The Orbis can provide solutions in a wide variety of analytical applications including Criminal Forensics fragments GSR inks pigments trace evidence Industrial Forensics and Quality Control wear metal debris contaminant corrosion analysis materials verification elemental distributions and imaging pharmaceutical tablets and packaging Non Destructive Testing Museum artifacts paper documentation and currencies gemstones authentication Materials metal glass ceramics cement concrete catalysts Electronics RoHS layer thickness and composition solder joints Geology Process Control and more Orbis Configuration Orbis e 300 um or 100 um mono capillary e Dual CCD video 10x and 100x e Standard precision XYZ motorized stage Orbis PC e 30 um poly capillary e Dual CCD video 10x and 75x with 3x digital zoom e High precision XYZ motorized stage Automated
7. Inside This Issue Page 2 EDAX Introduces the New Orbis Micro XRF Spectrometer Page 3 System Automation Making the Genesis System Work for You Page 4 Resolving EDS Overlaps Using WDS Page 6 Training and Events Page 7 Employee Spotlight Page 8 Customer News Vol 6 No 3 EDAX Introduces the New Orbis Micro XRF Spectrometer Building on more than 10 years of Micro XRF experience the Orbis spectrometer yields a system with excellent Micro XRF capability while setting a new standard in analytical flexibility The Orbis incorporates a unique motorized turret integrating video and X ray optics allowing coaxial sample view and X ray analysis Primary beam filters can be used with a variety of X ray optics to allow true XRF analytical capabilities in a micro spot analysis The working distance is increased to allow analysis over a rougher sample topography without sacrificing signal intensity Two additional X ray collimators can be added to the optical turret for a total of three X ray beam sizes to expand the Orbis analytical capabilities beyond traditional Micro XRF analysis Ca P Si elemental map of fossilized bone using a Red Green Blue mixer to create overlay eeeeseaasss a a E Micro XRF scan of the Co concentration depleted zone on the exterior surface of sintered polycrystalline diamond compact All this analytical flexibility is packaged into a table top unit with powerful easy
8. d stored in a retrieval system or transmitted in any form or by any means without prior written permission of EDAX Inc EDAX Inc e 91 McKee Drive Mahwah NJ 07430 e Phone 201 529 4880 e E mail info edax ametek com e www edax com EDAX FOCUS Page 8 Copyright 2008 All rights reserved EDAX Inc 2008
9. e spectra then click SPC gt gt BMP JPEG or PNG are selected in the setup area Take advantage of the Help options directly available on your system The Help Contents area is a standard MS Windows format which allows for easy searching by Keyword by a Table of Contents or by an Index You can even bookmark pages and topics that you might want to go back to for future reference The entire Genesis User Manual is located within the Help menu of the system and can be launched right from Genesis Search for your topic within the Table of Contents or flip through the pages for a good refresher on functions and capabilities that you may have forgotten about Does everyone in your lab want to learn how to use your EDAX system The User Manual is in PDF format and can be copied from your system PC to any other desktop or laptop PCs allowing anyone to access it anywhere anytime without tying up the system Detailed information about the New Features that are included in your latest version of software can be found by going to the Help menu then selecting New Features This document contains descriptions of the features as well as detailed instructions on how to use them Are you unfamiliar with some of those unusual looking icons Simply activate Tooltips in the Help menu when you pass your cursor over an icon a description of that icon will appear Click around the software most functions have logical names
10. ed ASM Pittsburgh PA October 14 17 15th ENFSI EWG Firearms GSR Meeting Dubrovnik Croatia October 16 17 AReMS Appalachian Regional Microscopy Society Boone NC November 2 7 APMC9 9th Asia Pacific Microscopy Conference Jeju Korea November 5 6 NWAFS Meeting Northwest Association of Forensic Scientists Boise ID December 2 4 MRS Materials Research Society Boston MA Please see our website www edax com for a complete list of our tradeshows World Wide Training To help our present and potential customers obtain the most from their equipment and to increase their expertise in EDS microanalysis WDS microanalysis EBSD OIM and Micro XRF we organize a number of Operator Courses at the EDAX facilities in North America Tilburg NL Wiesbaden Germany and Japan North America Tilburg T in English Wiesbaden W in German unless stated otherwise Microanalysis Courses 3 4 Day November 3 6 November 24 26 W Microanalysis Courses Microanalysis Courses October 1 3 Tokyo October 27 31 Mahwah NJ November 5 7 Osaka December 1 5 Mahwah NJ Particle Course November 11 13 Mahwah NJ 2D WDS Course ay November 18 20 Mahwah NJ October 30 31 T For more information on our EBSD OIM Academy Course training classes please visit By October 14 16 Draper UT our website at www edax con service Micro XRF Course user cim October 7 9 Mahwah NJ LEX Course October 7 9 T
11. ered high sensitivity bulk analysis or fast mapping along with Micro XRF analysis e Analytical Software Qualitative and quantitative analysis with or without standards a Automated Multi point analysis Elemental imaging and linear scans a Alloy identification Layer thickness and composition Spectral map data set generated by Micro XRF showing A Video B X ray count map and C Elemental overlay Copyright 2008 All rights reserved EDAX Inc 2008 TIPS amp Tricks System Automation Making the Genesis System Work for You Collecting a series of spectra from one set of samples Use the Save in Sequence function from the File drop down menu in the Spectrum tab and designate a starting Filename Each time you collect a new spectrum click the Save in Sequence icon on the tool bar and that spectrum will automatically be saved as the next number in the sequence Make use of the new Auto Amplifier time function and allow the system processor to optimize itself for the active kV and beam current conditons Select Auto in the toolbar Amp Time drop down list and the software will automatically select the closest amp time that yields about 30 dead time for the active count rate Looking to batch quantify a series of spectra Simply collect and save all of your spectra then click on the Auto drop down menu in the Spectrum tab and select Process ate Spectra Choo
12. primary beam filter system is standard on all Orbis instrument configurations Features The Orbis Micro XRF system offers a set of features which provide excellent analytical versatility e Co axial X ray optic and sample view for accurate sample positioning and X ray analysis e 8 position primary beam filter system Industry leading 6 filters selectable by software open position plus beam shutter Filters can be used with micro spot X ray optics for flexible Micro XRF analysis a Improved sensitivity Removal of spectral artifacts e Large signal collection area detectors Best resolution 80 mm2 Si Li detector available standard on Orbis and Orbis PC Large area SDD option High processed countrate with excellent resolution LN free e Low and high magnification CCD video sample viewing EDAX FOCUS Page 2 EDAX Introduces the New Orbis Micro XRF Spectrometer conta from rg e Large vacuum sample chamber with longer working distance Accommodates samples up to 270 mm W x 270 mm D x 100 mm H a Analyze over rougher sample topography while maintaining constant distance to the detector with no sacrifice of signal intensity e 1mm and 2 mm collimators available with X ray optic option Industry first motorized turret design integrates video X ray optic 1 mm and 2 mm collimators for optimal analytical flexibility three X ray beam sizes selectable by software Allows filt
13. same Using WDx tungsten Ma and silicon can be resolved at 5kV and W maps will clearly show where tungsten is located in the sample When collecting map data WDX can be used for overlapped lines such as tungsten Ma while most other lines can be mapped successfully using EDX In Figure 4 only tungsten Ma was mapped by WDx all other elements were mapped using EDX WDx in addition to resolving overlaps has a better peak to background ratio and aio f Al K O K K therefore better detection limits compared to Figure 4 Overlay of WDS data along with EDS data o O K and Si EDX For quantitative applications WDX can be used for trace elements and lines that are overlapped while EDX can be used for the major elements This improves the accuracy of trace analysis without requiring long acquisition times for full sample characterization bi om irah hide i mebi eE EDAX would like to thank Doug Hamilton of Xilinx San Jose for providing the samples and allowing EDAX to share their data irae ia Ha Hie a By ee i Hi Lee Fha Therbe I aie Tree i ii ae far dm Bin BE dii ai WAE i Figure 5 An example of a simulation of beam spread on a 1000 tungsten film on a silicon substrate i be bi DE dih it G bi iir Doi EDAX FOCUS Page 5 Copyright 2008 All rights reserved EDAX Inc 2008 World Wide Events October 6 9 MS amp T The Materials Science amp Technology Expo Formerly call
14. se your spectra add them to a the list and give an output filename Next click Process to start the routine When completed you can open the generated report in Excel and see the spreadsheet of all of your quantitative data for all spectra Example output Fons YENE me e Wt Samples Lsec NK OK SiK SiO2 spc 100 0 96 49 17 49 88 Sioxyn spc 100 27 13 19 44 53 42 Take advantage of the Multipoint routine within the Mapping tab You can designate your areas of interest for spectrum collection as a spot reduced raster or a free hand draw Next enter a collection time and an output filename and let the system work while you take a break When the collection is complete just click open to review the data that you spent no time collecting Have you tried using the Multifield collection capability yet On systems with Stage Control go to the Multifield area and easily designate multiple stage collection fields Fields can be individual locations multiple fields along a line or a matrix of fields covering both the x and y direction Just find each location of interest and click on Add for each field you want to analyze This is particularly useful for large mapping areas and particle analysis EDAX FOCUS Page 3 Want to turn all of your spectrum files into image files all at once Use Spectral Utilities to batch convert spc files to omp jpg or png Just select a folder containing the spectra highlight th
15. uired using an EDAX Apollo 40 high solid angle SDD and an EDAX TEXS Parallel Beam PBS WDX Spectrometer PBS systems are compact compared to curved crystal systems and will fit on almost any SEM or Dualbeam The system is designed to act like an EDX system making it easier for new WDX users to operate Eai r o m oe A Bi PEER Gie EJS Figure 1 Top window is WDS showing a fully resolved silicon peak and two resolved tungsten peaks as compared to the lower EDS spectrum in which the lines are not fully resolved EDAX FOCUS Page 4 Resolving EDS Overlaps Using WDS Copyright 2008 All rights reserved EDAX Inc Figure 2 Screenshot of EDAX GUI interface with image showing analysis region in upper left corner WDS Spectrum is shown in upper right and EDS with WDS overlayed on bottom An important issue to consider is increasing beam spread with kV In semiconductor samples a low kV is required to keep the beam within the analysis area Figure 5 shows a comparison of 5kV vs 10kV Figure 3 Left image shows SEM cross section and right image shows WDS map resolving tungsten regions 2008 WDS NEWS Resolving EDS Overlaps Using WDS conta from rg At 5kV the beam is within 1000 while at 10kV the beam spread increases tenfold For this reason 5kV was used for this analysis With EDX mapping silicon and tungsten M lines cannot be resolved and both maps will look very much the
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