Eagle III — Micro-EDXRF System

Eagle System Schematic

XRF Advantages

Non-destructive: No beam damage or coating of sampleMinimal Sample Preparation:• conductivity not required• sample shape can be irregular

Low Vacuum (~ 100 mTorr) or No Vacuum (Air)Navigation by Optical MicroscopeDetection 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 systemOrders 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

10x Eagle Video (B/W)

100x Eagle Video (color) Small Fracture in Diamond Table? Glass-Filled ?

* Rh Tube* Aperture/Rh filter

Conclusion: Yes!

“As Delivered” Sample Analysis

Chemical Residues from suspected drug labX-ray Excitation minimizes sample preparationQualitative answer in < 2 minutes

High Sensitivity

Reduced background

Eagle System Schematic

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)

Configuration — Standard Eagle III

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

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

$20 banknote (US)

Color Low-Magnification Image (single)

$20 banknote (US)

Color Low-Magnification Image (montage)

Hi-Magnification Image - Montage 5×5

Hi-Magnification Image - Montage 3×3

Hi-Magnification Image (Single) + Digital Zoom

Normal (100×) Digital Zoom (2× “normal”)

Blue security-fibre in banknote

Transmission Sample Backlighting

Reflective lighting Transmission lighting

Fine “Hi-Purity” Silica particles

Transmission Sample Backlighting

Transmission lighting (Low Mag View)

Transmission lighting (High Mag View)

Si(Li) Detector properties

Active area(mm2)

Be(coated)

windowProcessing TC

(µsec)Countrate

(cps)Resolution

@MnKa (eV)

30nominal

8µm

35 5000 ≤145

10 15000 ≤165

80nominal

12µm

35 5000 ≤155

10 15000 ≤185

100,000cps processing capabilityAbsolute intensities: I30 ≈ I80× 55%

30mm2

80mm2

NaK MgK AlK SiK

500 700 900 1100 1300 1500 1700 1900 (eV)

Glass sample (srm620)Spectra normalised to CaK (3690eV)

Detector’s relative low energy performances

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.

Capillary X-ray Optics

“Total” Reflection of X-rays inside glass capillary

c = f(1/E)

Incident X-Ray Spectral Distribution(Modified Excitation Spectrum)

Multilevel Sample Analysis

Filter Benefits

Improve Limits of DetectionMake analysis possible

Remove Tube Characteristic LinesReduce Bremsstrahlung in limited regionEliminate Bragg Diffraction Peaks in limited region

This is accomplished by …

Example: Ni Filter

High Sensitivity Region

Useful Region

Ni Absorption Edge

Filter Band Pass

Example: Ni Filter – Improve Limits of Detection

“Vision” Software: Modes of Operation

Manual point to pointAutomated multiple point, lines or matricesAnalyze within an area and add spectra togetherLine 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 ScanElemental 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

  Particle 1

Element: Wt%

Cr (K) 18.88

Mn (K) 0.44

Fe (K) 69.47

Ni (K) 11.21

Particle 1 = Stainless Steel

FP “Standardless” Analysis: Accuracy

Bulk Compositional Standard: Stainless 310 

Element:   Measured Wt%   Given Wt%   % Error

Si(K)   0.53   0.51   3.9

Cr(K)   24.97   24.88   0.4

Mn(K)   1.44   1.39   3.6

Fe(K)   53.03   52.8   0.4

Ni(K)   19.7   19.6   0.5

Mo(K)   0.32   0.23   39.1

Total   100   99.41    

Note: Measured with Poly-capillary lens

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 3Particle 4

Silica particles with impurities

Multi-Point Analysis: Chemical Distribution73

.24

72.7

72.1

7

71.6

3

71.0

9

70.5

6

70.0

2 45.82

45.28

44.75

44.21

43.67

43.14

42.6

Y Position (mm)X Position (mm)

86.1

85.69

85.28

84.86

84.45

84.04

83.63

83.22

82.81

46.7

7

46.3

6

45.9

5

45.5

3

45.1

2

44.7

1 44.3

43.8

9

43.4

8

Y Position (mm)

X Position (mm)

• Automated Matrix Point CollectionAutomated Matrix Point Collection• Data ported into ExcelData ported into Excel

Spectral Mapping Definition

Collect and save XRF spectrum at each map pixelDatabase 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 significanceQuantitative mapping

Spectral Mapping:

Mapping Examples

Elemental Spatial Distribution Maps: Paper

Mg Map Al Map Fe Map

• Generation of BMP Elemental Maps

Fe X-rays penetrate paper

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 Fe2O3 Wt%

Quantitative Mapping: Geological Sample

SiK Intensity SiO2 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

Na

K

Si

P

Map Image Overlays: Bone Fossilization

Fe – RedK – BlueSi – YellowP – GrayNa - 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