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Analyticalsem

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  • 1. Materials Characterization Lab www.mri.psu.edu/mcl Analytical SEM Mark S. Angelone MCL msa3@psu.edu June 22, 2005
  • 2. Materials Characterization Lab www.mri.psu.edu/mcl Summer Characterization Open Houses Technique Time Date Location Thermal analysis (TGA, DTA, DSC) 9:45 AM June 8 250 MRL Bldg. Transmission Electron Microscopy (TEM/STEM) 9:45 AM June 15 114 MRI Bldg Scanning electron microscopy (SEM) 9:45 AM June 22 541 Deike Bldg. Analytical SEM 11:00 AM June 22 541 Deike Bldg. X-ray Diffraction (XRD) 9:45 AM June 29 250 MRL Bldg. Dielectric Characterization (25 min lecture only) 9:45 AM July 6 250 MRL bldg. High temperature sintering lab (20 min lecture only) 10:15 AM July 6 250 MRL Bldg. Focused Ion Beam (FIB) 9:45 AM July 13 114 MRI Bldg TEM sample preparation 11:00 AM July 13 114 MRI Bldg Orientation imaging microscopy (OIM/EBSD) 9:45 AM July 20 250 MRL Bldg. Chemical analysis (ICP, ICP-MS) 9:45 AM July 27 541 Deike Bldg. Atomic Force Microscopy (AFM) 9:45 AM August 3 114 MRI Bldg Small angle x-ray scattering (SAXS) 9:45 AM August 10 541 Deike Bldg. Particle Characterization 9:45 AM August 17 250 MRL X-ray photoelectron spectroscopy (XPS/ESCA) 9:45 AM August 24 114 MRI Bldg Auger Electron Spectroscopy (AES) 11:00 AM August 24 114 MRI Bldg NOTE LOCATIONS: The MRI Bldg is in the Innovation Park near the Penn Stater Hotel; MRL Bldg. is on Hastings Road. More information: www.mri.psu.edu/mcl
  • 3. Materials Characterization Lab www.mri.psu.edu/mcl Materials Characterization Lab Locations MRI Bldg: XPS/ESCA, FIB SIMS, TEM, HR- TEM, FE-Auger, MRL Bldg: Hosler Bldg: AFM, XRD SEM, XRD, OIM, DTA, SEM,AFM,ESEM, DSC, TGA, FTIR, Penn Stater FE-SEM, EPMA, ICP, Hotel Raman, AFM, Powder, E&ES Bldg: ICP-MS,BET, SAXS dielectric, prep, shop, SEM IC, UV-Vis Route 322 Steidle Bldg: Atherton Street Nanoindenter (322 Business) I-99 Park Ave. 0 0 0 0 0 0 0 Ave. 0 0 0 0 0 Park 0 Beaver 0 0 Stadium 0 0 0 Centre 0 0 Porter Road Community Univ Shortlidg Hospital 0 0 Burrowes Road ersi ty D e Pollock Road Road rive North Hastin Deike Bldg: gs Ro ad College Ave.
  • 4. Materials Characterization Lab www.mri.psu.edu/mcl ANALYTICAL SEM • Mostly X-ray Micro Analysis •EDS •WDS/EPMA • BSED/OIM July20 9:45am 250MRL •Cathodoluminescence
  • 5. Materials Characterization Lab www.mri.psu.edu/mcl
  • 6. Materials Characterization Lab www.mri.psu.edu/mcl
  • 7. Materials Characterization Lab www.mri.psu.edu/mcl MONTE CARLO
  • 8. Materials Characterization Lab www.mri.psu.edu/mcl Comprehensive energy-level diagram showing all electron transitions which Moseley’s relation between λ give rise to K, L and M x-rays. and Z for the Kα1, Lα1 and Mα1 characteristic x-ray lines.
  • 9. Materials Characterization Lab www.mri.psu.edu/mcl IZ1α (WFZ1)
  • 10. Materials Characterization Lab www.mri.psu.edu/mcl TOOLS FOR XRAY ANALYSIS •XRF/Microfocus •EDS/SEM/TEM •WDS/SEM •EPMA
  • 11. Materials Characterization Lab www.mri.psu.edu/mcl EDS/SEM (Energy Dispersive Spectrometer) • Fast/easy – high collection efficiency and simultaneous • Low focusing – rough samples, tilt • Common
  • 12. Materials Characterization Lab www.mri.psu.edu/mcl DETECTOR CRYSTAL
  • 13. Materials Characterization Lab www.mri.psu.edu/mcl SOLID STATE PROCESS
  • 14. Materials Characterization Lab www.mri.psu.edu/mcl
  • 15. Materials Characterization Lab www.mri.psu.edu/mcl
  • 16. Materials Characterization Lab www.mri.psu.edu/mcl
  • 17. Materials Characterization Lab www.mri.psu.edu/mcl QUANT PITFALLS • SAMPLE RELATED • Beam Sensitivity • Overlaps
  • 18. Materials Characterization Lab www.mri.psu.edu/mcl
  • 19. Materials Characterization Lab www.mri.psu.edu/mcl QUANT PITFALLS • SAMPLE RELATED • Beam Sensitivity • Overlaps • MATRIX EFFECTS • GEOMETRY RELATED • Tilt • WD
  • 20. Materials Characterization Lab www.mri.psu.edu/mcl
  • 21. Materials Characterization Lab www.mri.psu.edu/mcl Sample: K919 NIST test RM Oxygen by stoichiometry (Normalised) All results in Atomic Percent Spectrum Label Si Mn Fe Co Ni Cu Zn Ba Ce O K919flat10m 21.40 1.16 1.15 1.26 1.35 3.54 0.02 9.32 0.08 60.72 k919tilt15d 24.39 N/A 1.06 0.94 1.12 1.75 0.05 8.09 0.33 62.28 k919lat15m 21.58 1.16 0.97 1.41 1.40 3.09 -0.17 9.41 0.29 60.86 Cert Assay 19.8 2.14 2.10 1.78 2.04 2.27 NA 7.87 2.54 NA
  • 22. Materials Characterization Lab www.mri.psu.edu/mcl QUANT PITFALLS • Sample Related • Beam Sensitivity • Overlaps • MATRIX EFFECTS • GEMETRY RELATED • Tilt • WD • ROUGHNESS
  • 23. Materials Characterization Lab www.mri.psu.edu/mcl Tilt/WD CHANGE IN “FLAT” SAMPLES ē ē ē EDS
  • 24. Materials Characterization Lab www.mri.psu.edu/mcl QUANT PITFALLS •INSTRUMENTAL • SAMPLE RELATED •Beam Drift • Beam Sensitivity •Window Ice, Contamination • Overlaps •Spectral Artifacts •Sum/Escape Peaks •Count related processing errors • MATRIX EFFECTS •Background • GEMETRY RELATED • Tilt • WD • ROUGHNESS
  • 25. Materials Characterization Lab www.mri.psu.edu/mcl
  • 26. Materials Characterization Lab www.mri.psu.edu/mcl QUANT PITFALLS •INSTRUMENTAL • SAMPLE RELATED •Beam Drift • Beam Sensitivity •Window Ice, Contamination • Overlaps •Spectral Artifacts •Sum/Escape Peaks •Count related processing errors • MATRIX EFFECTS •Background •Stray Radiation • GEMETRY RELATED • Tilt • WD • ROUGHNESS
  • 27. Materials Characterization Lab www.mri.psu.edu/mcl EDS/SEM APPLICATIONS Contaminates •
  • 28. Materials Characterization Lab www.mri.psu.edu/mcl Automotive Ball Studs
  • 29. Materials Characterization Lab www.mri.psu.edu/mcl EDS/SEM APPLICATIONS Contaminates • • Defects
  • 30. Materials Characterization Lab www.mri.psu.edu/mcl
  • 31. Materials Characterization Lab www.mri.psu.edu/mcl EDS/SEM APPLICATIONS Contaminates • • Defects • Phase/Mineral ID • Fast (large scale) mapping • EDS/ESEM • Quant with care → 5% accuracy/0. 5% Sensitivity •Z ≥ 5 ????
  • 32. Materials Characterization Lab www.mri.psu.edu/mcl EPMA ELECTRON PROBE MICRO ANALYZER • Ebeam built for Quant • Stability • Controlled Geometry • WDS Resolution/Sensitivity
  • 33. Materials Characterization Lab www.mri.psu.edu/mcl The basic layout of the Cameca MBX electron microprobe. Electron gun with mechanical 1. alignment. 2. Adjustable anode to Wehnelt distance. 3. Condenser lens in electron column with beam current regulator. 4. WDS spectrometer. 5. Minicoil probe-forming objective lens. 6. Specimen chamber with mechanical stage. 7. Coaxial light optical system. 8. Scanning coils. 9. Sample airlock 10. vacuum system.
  • 34. Materials Characterization Lab www.mri.psu.edu/mcl
  • 35. Materials Characterization Lab www.mri.psu.edu/mcl
  • 36. Materials Characterization Lab www.mri.psu.edu/mcl
  • 37. Materials Characterization Lab www.mri.psu.edu/mcl EPMA ELECTRON PROBE MICRO ANALYZER • Ebeam built for Quant • Stability • Controlled Geometry • WDS Resolution/Sensitivity • Intensity
  • 38. Materials Characterization Lab www.mri.psu.edu/mcl Efficiency of XRAY Microanalysis 1 nA of beam electrons = 10-9 coulomb/sec 1 electron’s charge = 1.6x 10-19 coulomb ergo, 1 nA = 1010 electrons/sec Probability that an electron will cause an ionization: 1 in 1000 to 1 in 10,000 ergo, 1 nA of electrons in one second will yield 106 ionizations/sec Probability that ionization will yield characteristic X-ray (not Auger electron): 1 in 10 to 4 in 10. ergo, our 1 nA of electrons in 1 second will yield 105 xrays. Probability of detection: for EDS, solid angle < 0.01 (1 in 100). WDS, <.001 ergo 103 X-rays/sec detected by EDS, and 102 by WDS. These are for pure elements. For EDS, 10 wt%, 102 X-rays; 1 wt% 10 X-rays; 0.1 wt % 1 X-ray/sec.
  • 39. Materials Characterization Lab www.mri.psu.edu/mcl EPMA ELECTRON PROBE MICRO ANALYZER • Ebeam built for Quant • Stability • Controlled Geometry • WDS Resolution/Sensitivity • Intensity • 1% Accuracy/ppm sensitivity •Z ≥ 5
  • 40. Materials Characterization Lab www.mri.psu.edu/mcl LIMITATIONS Solid polished specimens • • Beam sensitivity • Heating • Volume Limits • Thin Films • Particles • Small Phases • Trace Mapping
  • 41. Materials Characterization Lab www.mri.psu.edu/mcl Image Acquisition Times number of .1 1 10 pixel density 100 sec/pixel pixels sec/pixel sec/pixel sec/pixel 16 X 16 256 25.6 sec 4.2 min 42 min 7.1 hrs 64 X 64 4096 6.8 min 68 min 11.3 hrs 4.7 days 128 X 128 16384 27.3 min 4.5 hrs 1.9 days 18.9 days 256 X 256 65536 1.82 hrs 18.2 hrs 7.58 days 75.8 days 1024 X 1024 1048576 29.1 hrs 12.1 days 121.3 days 3.3 years
  • 42. Materials Characterization Lab www.mri.psu.edu/mcl APPLICATIONS
  • 43. Materials Characterization Lab www.mri.psu.edu/mcl GRAND Mg Upper Granite Gorge, Grand Canyon Mg Ka map from a garnet crystal, mile 83, Upper Granite Gorge, Grand Canyon (Green - garnet; red - chlorite; orange - biotite; dark blue - muscovite; dark colors - primarily quartz).
  • 44. Materials Characterization Lab www.mri.psu.edu/mcl GARNET Ca Kα
  • 45. Materials Characterization Lab www.mri.psu.edu/mcl BSE Fe Si Ca
  • 46. Materials Characterization Lab www.mri.psu.edu/mcl
  • 47. Materials Characterization Lab www.mri.psu.edu/mcl SiO2 – 64.3 K2O – 17.1 Al2O3 – 17.8 CaO – 54.1 P2O5 – 40.8 MgO – 0.7 SiO2 – 54.2 F2 – 2.9 CaO – 10.9 Na2O – 5.4 Al2O3 – 27.6 SiO2 – 51.4 Fe2O3 – 97.2 MgO – 16.1 TiO2 – 1.4 FeO - 13.6 MnO – 0.8 Al2O4 – 1.9 TiO2 – 0.8 CaO – 14.9
  • 48. Materials Characterization Lab www.mri.psu.edu/mcl SiO2 – 64.3 K2O – 17.1 Al2O3 – 17.8 CaO – 54.1 P2O5 – 40.8 MgO – 0.7 SiO2 – 54.2 F2 – 2.9 CaO – 10.9 Na2O – 5.4 Al2O3 – 27.6 Y – 1100 ppm Ce – 350 La – 480 Sr – 620 Sr - 690 Ba - 505 SiO2 – 51.4 Fe2O3 – 97.2 MgO – 16.1 TiO2 – 1.4 Ba - 680 ppm FeO - 13.6 MnO – 0.8 Mn - 920 Al2O4 – 1.9 Cu – 405 TiO2 – 0.8 Ni – 385 CaO – 14.9 Cr - 370
  • 49. Materials Characterization Lab www.mri.psu.edu/mcl
  • 50. Materials Characterization Lab www.mri.psu.edu/mcl Monazite Radiometric Dating
  • 51. Materials Characterization Lab www.mri.psu.edu/mcl Glass Dark Vortex Si 31.5 Si 25.8 Al 1.2 Al 12.5 Na 1.4 Na 12.5 Ca 4.4 Ca 0.9 Ba 1.5 Ba 0.8 K 0.6 K 0.8 Cu 1.8 Cu 0.4 Zr 0.1 Zr 1.4
  • 52. Materials Characterization Lab www.mri.psu.edu/mcl
  • 53. Materials Characterization Lab www.mri.psu.edu/mcl 3 Sn in Float Glass 2 WT 1 10 20 DEPTH (µm)
  • 54. Materials Characterization Lab www.mri.psu.edu/mcl ION EXCHANGE Na+ K+ 10 WT 5 10 40 20 30 DEPTH (µm)
  • 55. Materials Characterization Lab www.mri.psu.edu/mcl
  • 56. Materials Characterization Lab www.mri.psu.edu/mcl www.mri.psu.edu/mcl Mark Angelone 310 Hosler Bldg 883-9350 msa3@psu.edu John Cantolina 310 Hosler Bldg 883-9358 jjc16@psu.edu

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