Transcript Document 7437445
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 Detection limits improve: 10x or better (vs. SEM-EDS) X-rays are penetrating (microns to millimeters)
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
Non-Destructive Testing 100x Eagle Video (color) Small Fracture in Diamond Table ? Glass-Filled ?
Conclusion: Yes!
* Rh Tube * Aperture/Rh filter 10x Eagle Video (B/W)
“As Delivered” Sample Analysis
Chemical Residues from suspected drug lab X-ray Excitation minimizes sample preparation Qualitative answer in < 2 minutes
High Sensitivity Reduced background
Eagle System Schematic
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 mm 2 Si(Li) detector Genesis 2000 (Windows XP) Vision32 version 4 software (patented FP and Comb32)
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 mm 2 Si(Li) detector rotation table
OR
sample backlighting LineScan, Mapping & Image processing software
Sample Illumination: White LEDs
Directionally adjustable LED arrays Individual arrays for both Low- & High-mag image views Individual light output adjustment to both arrays at both magnification views Low-mag High-mag
Color Low-Magnification Image (single)
$20 banknote (US)
Color Low-Magnification Image (montage)
$20 banknote (US)
Hi-Magnification Image - Montage 5 × 5
Hi-Magnification Image - Montage 3 × 3
Hi-Magnification Image (Single) + Digital Zoom Blue security-fibre in banknote
Normal (100 × ) Digital Zoom (2 × “normal”)
Transmission Sample Backlighting
Fine “Hi-Purity” Silica particles Reflective lighting Transmission lighting
Transmission Sample Backlighting
Transmission lighting (Low Mag View) Transmission lighting (High Mag View)
Si(Li) Detector properties
Active area (mm 2 ) Be
(coated)
window Processing TC (µsec) Countrate (cps) Resolution @MnKa (eV) 30 80
nominal
8µm 35 5000 10 15000 35 5000
nominal
12µm 10 15000
100,000cps processing capability Absolute intensities: I 30 ≈ I 80
×
55%
≤145 ≤165 ≤155 ≤185
Detector’s relative low energy performances 30mm 2 80mm 2
Glass sample (srm620) Spectra normalised to CaK (3690eV) NaK a MgK a AlK a SiK a 500 700 900 1100 1300 1500 1700 1900 (eV)
Si(Li) Cooling
Standard: Liquid Nitrogen • • • • 30 mm 2 or 80 mm 2 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.
Capillary X-ray Optics
J
c = f(1/E) “Total” Reflection of X-rays inside glass capillary
Incident X-Ray Spectral Distribution (Modified Excitation Spectrum)
Multilevel Sample Analysis
Filter Benefits
Improve Limits of Detection Make analysis possible This is accomplished by … Remove Tube Characteristic Lines Reduce Bremsstrahlung in limited region Eliminate Bragg Diffraction Peaks in limited region
Example: Ni Filter
Filter Band Pass High Sensitivity Region Useful Region Ni Absorption Edge
Example: Ni Filter – Improve Limits of Detection
“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
“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
“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
Manual Control and Analysis
Automated Multiple Point Analyses Navigate to Feature Save Coordinates in Stage Table
Automated Multi-Point Analysis: Example: Foreign Particulates
Foreign Particulates in Silica Transmission lighting (Low Mag View) Transmission lighting (High Mag View)
FP “Standardless” Analysis: Particle 1 Element: Cr (K) Mn (K) Fe (K) Ni (K) Particle 1 Wt% 18.88
0.44
69.47
11.21
Particle 1 = Stainless Steel
FP “Standardless” Analysis: Accuracy Bulk Compositional Standard: Stainless 310
Element:
Si(K) Cr(K) Mn(K) Fe(K) Ni(K) Mo(K) Total
Measured Wt%
0.53
24.97
1.44
53.03
19.7
0.32
100
Given Wt%
0.51
24.88
1.39
52.8
19.6
0.23
99.41
Note: Measured with Poly-capillary lens % Error
3.9
0.4
3.6
0.4
0.5
39.1
Foreign Particulates in Silica Particle “2” Particles “3” and “4”
Foreign Particulates in Silica Particle 2 Particle 1
“Stainless” Steels Same Alloy
Foreign Particulates in Silica Particle 3
Silica particles with impurities
Multi-Point Analysis: Chemical Distribution
• Automated Matrix Point Collection • Data ported into Excel
Y Position (mm)
45.82
42.6
43.14
43.67
44.21
45.28
44.75
X Position (mm)
86.1
85.69
85.28
84.86
84.45
Y Position (mm)
84.04
83.63
83.22
82.81
X Position (mm)
Spectral Mapping Definition
Collect and save XRF spectrum at each map pixel Database correlating each spectrum to position
(X, Y)
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
Spectral Mapping: Mapping Examples
Elemental Spatial Distribution Maps: Paper Fe X-rays penetrate paper Mg Map Al Map
• Generation of BMP Elemental Maps
Fe Map
Spatial Distribution Maps: Facial Tissue
• Tissue masked with carbon tape for Si-free zone • Mapping region 15.6 mm x 11.3 mm
Spatial Distribution Maps: Facial Tissue
• Recall spectra from mapped pixels • Hot Si spots hide low-level Silicone coverage
Spatial Distribution Maps: Facial Tissue
• 3 individual color logarithmic scales (NIST) • Low level Silicone distribution exposed in Green
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
Quantitative Mapping: Geological Sample
FeK Intensity Fe 2 O 3 Wt%
Quantitative Mapping: Geological Sample
SiK Intensity SiO 2 Wt%
Multi-Field Mapping: Geological Sample
• 7 adjacent High Mag Camera FOV • Map more layers in shorter time • Maps are stitched together in SW utility while adjusting map intensities
Spectral Mapping - Bone Fossilization
Fe K P Si Na
Map Image Overlays: Bone Fossilization Fe – Red K – Blue Si – Yellow P – Gray Na Green
Metal Analysis: Coins (Non-Destructive) * Rare Coin (2 Reichsmark - 1927?) *
Pixels: 64 x 50 Map * Dwell time: 0.3 s/pixel * Total time ~ 20 minutes
Conclusion: Counterfeit Coin
Eagle Applications
Glass, Ceramics (inhomogeneity, inclusions, particles) Metal alloys (inhomogeneity, particles, wire filament) Inorganic contaminants, residues, deposits (ex. Corrosion) Inorganic additives polymers, paints, inks Inclusions in plastics, “light element” materials Coating thickness and distribution of coating thickness