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Eagle III — Micro-EDXRF System

Eagle III — Micro-EDXRF System. Eagle System Schematic. XRF Advantages. Non-destructive: No beam damage or coating of sample Minimal Sample Preparation: conductivity not required sample shape can be irregular Low Vacuum (~ 100 mTorr) or No Vacuum (Air) Navigation by Optical Microscope

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Eagle III — Micro-EDXRF System

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  1. Eagle III — Micro-EDXRF System

  2. Eagle System Schematic

  3. XRF Advantages • Non-destructive: No beam damage or coating of sample • Minimal Sample Preparation: • conductivity not required • sample shape can be irregular • Low Vacuum (~ 100 mTorr) or No Vacuum (Air) • Navigation by Optical Microscope • Detection limits improve: 10x or better (vs. SEM-EDS) • X-rays are penetrating (microns to millimeters)

  4. Advantages to EDS (Matt’s addition) • Cheaper to add EDS to a microscope than to buy an XRF system • Orders of magnitude better image quality • CCD camera in XRF has magnification of 150 – 200X • Resolution comparable to XRF: about 10 nm • SEM image quality can be orders of magnitude better • Smaller analytical volume • One order of magnitude always • Another order of magnitude if you can live with lower voltage

  5. Non-Destructive Testing 10x Eagle Video (B/W) 100x Eagle Video (color) Small Fracture in Diamond Table ? Glass-Filled ? Conclusion: Yes! * Rh Tube * Aperture/Rh filter

  6. “As Delivered” Sample Analysis • Chemical Residues from suspected drug lab • X-ray Excitation minimizes sample preparation • Qualitative answer in < 2 minutes

  7. High Sensitivity Reduced background

  8. Eagle System Schematic

  9. Configuration — Standard Eagle III • Standard features • Rh or Mo tube (40kV, 40W) • 300µm monocapillary • Video: 10× colour; 100× colour (plus 2× digital zoom) • Sapphire™ 80 mm2 Si(Li) detector • Genesis 2000 (Windows XP) • Vision32 version 4 software (patented FP and Comb32)

  10. Configuration — Eagle III - OPTIONS • Options • 100µm monocapillary in lieu of the 300µm • collimators (1 & 2mm) • manually interchangeable filters (for collimator only) • 40kV, 20W Cr-anode X-ray tube • 50 kV, 50W X-ray tube (Mo, Rh or W anodes) • 30 mm2 Si(Li) detector • rotation table OR sample backlighting • LineScan, Mapping & Image processing software

  11. Sample Illumination: White LEDs Low-mag High-mag • Directionally adjustable LED arrays • Individual arrays for both Low- & High-mag image views • Individual light output adjustment to both arrays at both magnification views

  12. Color Low-Magnification Image (single) $20 banknote (US)

  13. Color Low-Magnification Image (montage) $20 banknote (US)

  14. Hi-Magnification Image - Montage 5×5

  15. Hi-Magnification Image - Montage 3×3

  16. Hi-Magnification Image (Single) + Digital Zoom Blue security-fibre in banknote Normal (100×) Digital Zoom (2× “normal”)

  17. Transmission Sample Backlighting Fine “Hi-Purity” Silica particles Reflective lighting Transmission lighting

  18. Transmission Sample Backlighting Transmission lighting (Low Mag View) Transmission lighting (High Mag View)

  19. Si(Li) Detector properties

  20. Detector’s relative low energy performances 30mm2 80mm2 NaKa MgKa AlKa SiKa 500 700 900 1100 1300 1500 1700 1900 (eV) Glass sample (srm620) Spectra normalised to CaK (3690eV)

  21. Si(Li) Cooling • Standard: Liquid Nitrogen • 30 mm2 or 80 mm2 • 5 L dewar • ≥ 3 day hold time • Detector can be allowed to warm when not in use. Detector High Voltage bias is switched off when detector warms.

  22. Capillary X-ray Optics “Total” Reflection of X-rays inside glass capillary Jc= f(1/E)

  23. Incident X-Ray Spectral Distribution(Modified Excitation Spectrum)

  24. Multilevel Sample Analysis

  25. Filter Benefits • Improve Limits of Detection • Make analysis possible • Remove Tube Characteristic Lines • Reduce Bremsstrahlung in limited region • Eliminate Bragg Diffraction Peaks in limited region This is accomplished by …

  26. Example: Ni Filter Filter Band Pass High Sensitivity Region Useful Region Ni Absorption Edge

  27. Example: Ni Filter – Improve Limits of Detection

  28. “Vision” Software: Modes of Operation • Manual point to point • Automated multiple point, lines or matrices • Analyze within an area and add spectra together • Line Scan (generates a plot) • Elemental Imaging and Spectral Mapping

  29. “Vision” Software: Applications • Qualitative Analysis (what elements and where) • Quantification: • Fundamental Parameter Modeling Quantification without standards and with type standard(s) {Patented} • Semi-empirical quantification with type standards

  30. “Vision” Software: Applications (cont’d) • Coating thickness • FP modeling • FP modeling with standards correction • Spectral Match (Known alloys - ID unknown) • Line Scan • Elemental Imaging and Spectral Mapping • Image Manipulation and Overlay

  31. Manual Control and Analysis

  32. Automated Multiple Point Analyses Navigate to Feature Save Coordinates in Stage Table

  33. Automated Multi-Point Analysis: Example: Foreign Particulates

  34. Foreign Particulates in Silica Transmission lighting (Low Mag View) Transmission lighting (High Mag View)

  35. FP “Standardless” Analysis: Particle 1  Particle 1 = Stainless Steel

  36. FP “Standardless” Analysis: Accuracy Note: Measured with Poly-capillary lens

  37. Foreign Particulates in Silica Particle “2” Particles “3” and “4”

  38. Foreign Particulates in Silica Particle 2 Particle 1 • “Stainless” Steels • Same Alloy

  39. Foreign Particulates in Silica Particle 3 Particle 4 • Silica particles with impurities

  40. Multi-Point Analysis: Chemical Distribution • Automated Matrix Point Collection • Data ported into Excel

  41. Spectral Mapping Definition (X, Y) Collect and save XRF spectrum at each map pixel Database correlating each spectrum to position

  42. Spectral Mapping: Search and Use of Data • Spectral Display: • Point by point • Summation of selected region or total map • Display of Linear Distributions • Return to Sample using Map for collection of spectrum with improved statistical significance • Quantitative mapping

  43. Spectral Mapping: Mapping Examples

  44. Elemental Spatial Distribution Maps: Paper Mg Map Al Map Fe Map Fe X-rays penetrate paper • Generation of BMP Elemental Maps

  45. Spatial Distribution Maps: Facial Tissue • Tissue masked with carbon tape for Si-free zone • Mapping region 15.6 mm x 11.3 mm

  46. Spatial Distribution Maps: Facial Tissue • Recall spectra from mapped pixels • Hot Si spots hide low-level Silicone coverage

  47. Spatial Distribution Maps: Facial Tissue • 3 individual color logarithmic scales (NIST) • Low level Silicone distribution exposed in Green

  48. Quantitative Mapping: Geological Sample • Sedimentary rock • Epoxy-embedded “puck” • used to make thin • sections • Map area defined by • 5x5 Hi-Mag montage Map Image: Total XRF counts in each map pixel

  49. Quantitative Mapping: Geological Sample FeK Intensity Fe2O3 Wt%

  50. Quantitative Mapping: Geological Sample SiK Intensity SiO2 Wt%

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