MicroEDXRF System XRF Advantages Nondestructive No beam damage or coating of sample Minimal Sample Preparation conductivity not required sample shape can be irregular Detection limits improve 10x or better vs SEMEDS ID: 502612
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ORBIS — Micro-EDXRF SystemSlide2
XRF AdvantagesNon-destructive: No beam damage or coating of sampleMinimal Sample Preparation: conductivity not requiredsample shape can be irregular
Detection limits improve: 10x or better (vs. SEM-EDS)
Navigation by Optical Microscope
Low Vacuum (~ 300 mTorr) or No Vacuum (Air)
More appropriate than SEM for larger scale features
X-rays are penetrating (microns to millimeters)Slide3
Sample Chamber / XYZ StageChamber DoorWidth ~ 500 mmHeight ~ 515 mmCan be set up to swing:
Right to left (as shown)
Left to Right
Open access to sample chamberSlide4
Manual Control and AnalysisSlide5
Spectral Mapping: Mapping ExamplesSlide6
Elemental Spatial Distribution Maps: Paper
Mg Map
Al Map
Fe Map
Generation of BMP Elemental Maps
Fe X-rays penetrate paperSlide7
Mapping 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 CoinSlide8
Cl Mapping of Cement Core: Filtered Excitation
Surface Treatment
Cross Section
Cement Core
Goal:
To access diffusion of Cl into cement from deicing agent where Cl could corrode supporting steel
Cores are cross-sectioned
Rough cut
(often there is a desire to avoid polishing to minimize sample preparation or corruption of the sample)
Acquisition of data with Rh-tube, poly-capillary optic and Al(thin) filter to remove interfering scatter from Rh(L) tube lineSlide9
Cement Chemistry – Road Salt: Filtered ExcitationData courtesy of J.M. Davis, Microanalysis Research Group – NISTMap images processed and displayed using Lispix SW
Surface TreatmentSlide10
Spectral Mapping - Bone Fossilization
Fe
Na
K
Si
P
Data courtesy of George Havrilla, LANLSlide11
Map Tool: Substitution Map Image Overlay Fe – Red
K –
Blue
Si –
Yellow
P –
Gray
Na -
Green
Bone FossilizationSlide12
Map Tool: Elemental Image Overlay – RGB Phase AnalysisBone fossilization Ca – RedBone
Si – Green
mineral
P – Blue
Bone
Substitution Overlay Image: Ca-Si-PSlide13
Map Tool: Elemental Image Overlay – RGB Phase Analysis
Bone fossilization
Bone – purple (Ca, P)
New mineral – orange (Ca, Si)Slide14
Spatial Distribution Maps: Facial Tissue Tissue masked with carbon tape for Si-free zone Mapping region 15.6 mm x 11.3 mmSlide15
Map Tool: Data Mining
Recall spectra from mapped pixels
Hot Si spots hide low-level Silicone coverageSlide16
Map Tool: 3-Log Band Image Scaling 3 individual color logarithmic scales (NIST) Low level Silicone distribution exposed in
GreenSlide17
Spectral Mapping with Poly-capillary and Filter – Alumina supported Catalysts Ag supported on Alumina Spheres
Pd supported on Alumina pellets
Objective:
Measure metal distribution in ceramic support
Samples: Embedded in epoxy and cross-sectioned on one side (no polish)
Ag(L), Pd(L) versus Ag(K), Pd(K)
L-lines probe ~ 20
m
m into ceramic; no need to make a thin section
K-lines probe ~ 4 mm into ceramic; interference from opposite surface
Map Acquisition: Rh tube excitation requires filter to remove Rh(L) interference
Poly-capillary: ~ 55 mm FWHM lateral resolution at Ag(L), Pd(L)
Thin Al filter to remove Rh(L) from exciting spectrum
True Analytical flexibility in micro-XRF beamSlide18
Spectral Mapping – Alumina supported Catalysts
Ag(L) Map: Thermal Image Scaling
Pd(L) Map: Thermal Image Scaling
Objective:
Measure metal distribution in ceramic support
Samples: Embedded in epoxy and cross-sectioned on one side (no polish)
Metal is concentrated in the exterior shell of the ceramic supportSlide19
Spectral Mapping – Alumina supported Catalysts
Ag(L) Map: 3 Log Band Image Scaling
Pd(L) Map: 3 Log Band Image Scaling
Objective:
Measure metal distribution in ceramic support
Samples: Embedded in epoxy and cross-sectioned on one side (no polish)
Specialized Image Scaling reveals important distributional details
Ag(L) map shows interior ring of Ag at weaker concentration, but no internal Ag
Pd(L) map shows the interior pellet has weak, uniform concentration of Pd Slide20
High Resolution Spectral Mapping – Odessa Meteorite (20mm x 16 mm)Area ~ 20 mm x 16 mm
RGB Merge
Fe – Red
Ni – Green
P - Blue
Elemental Image Overlay
Total Spectral Count Image
(TSC Image)
Fe – green
Ni – blue
Cr – cyan
S – magenta
Cl – yellow
P - redSlide21
High Resolution Spectral Mapping – Odessa Meteorite (20mm x 16 mm)
Elemental Image Overlay
P
Cl
Fe
S
Ni
FeSlide22
High Resolution Spectral Mapping –
Odessa Meteorite (20mm x 16 mm)
RGB Merge
Fe – Red
Ni – Green
P - Blue
Fe:Ni (Kamacite) Fe:Ni (Taenite) Fe:Ni:P(
*
) (Schreibersite)
*
*
*
*
*
*
*
*
*
*Slide23
High Resolution Spectral Mapping –
Odessa Meteorite (20mm x 16 mm)
RGB Merge
Fe – Red
Ni – Green
S - Blue
Fe:Ni (Kamacite) Fe:Ni (Taenite) FeS (Troilite)