Practical Spectrum Imaging - Bruker...Sep 09, 2007 · NMR, EPR, MRI Bruker BioSciences Corporation...
Transcript of Practical Spectrum Imaging - Bruker...Sep 09, 2007 · NMR, EPR, MRI Bruker BioSciences Corporation...
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Practical Spectrum Imaging:Rapid Collection for Routine Analysis
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Welcome
Don BeckerWebinar Host
Today’s TopicsIntroductionX-ray Detectors for MicroanalysisHyperMap ApplicationsμXRF Instrument Design - ARTAXARTAX Element Mapping in Forensics and IndustryQ&A
Guest SpeakersTed Juzwak – Applications Lab Manager, Ewing, NJArmin Gross – International Sales Manager, Berlin, Germany
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Bruker Companies
Bruker AXSAdvanced X-ray Solutions
XRF, Diffraction, Single Crystal, Microanalysis
Bruker DaltonicsMass Spectrometry
Bruker OpticsFTIR, NIR, Raman
Bruker BioSpin(Affiliated privately held not part of Bruker BioSciences)
NMR, EPR, MRI
Bruker BioSciences Corporation(NASDAQ: BRKR)
The innovative ultraflex™ III mass spectrometer
S4 Pioneer
D8 Discover
Recombinase Fragment with 3 DNA Strand – Dr. Yu Lau, University of Saskatchewan
XFlash 4010
TENSOR 27 & HYPERION FT-IR Microscope
AVANCE III
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Bruker AXS Microanalysis
MicroanalysisEst. 2006
Est. 1965
Est. 1991
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MicroanalysisQUANTAX with XFlashQUANTAX with XFlash®
Ted JuzwakBruker AXS Microanalysis USA
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UHV Dewar Si(Li) Detector XFlash® Detector
Conventional EDS Detector
Cooling with LN2 (ca. -190°C)
2 hours to cool down
Technology from 1960’s
Weight approx. 8 kg
SDD Technology
no LN2 (Peltier cooling, ca. -25°C)
30 seconds to cool down
Up to 10 times faster
High efficiency
Stable resolution, reliable quantification
Weight 2.5 kg
X-ray Detectors for Microanalysis
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History of the SDD
2nd generation
XFlash®20002000
2007: 10th anniversaryof the XFlash® Detector!
XFlash®30012002
3rd generation
1st generation
XFlash®10001997
4th generation
XFlash®4010July 2006
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4th generation high resolution detector
10 mm² active area
Energy resolution: ≤ 125 eV,
specification at MnKα, 100 000 cps
Detection of beryllium (4)
Input count-rate: > 700,000 cps
2-stage Peltier cooler
Vibration-free
Maintenance-free
XFlash® Detector 4010
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129eV Resolution at Mn: XFlash vs Si(Li)
0-2 129 1292-8 131 1298-14 133 12914-20 138 12920-42 149 12942-62 161 12962-110 191 129110-150 NP 129150-200 NP 130200-300 NP 131
Count Rate (Kcps) Si(Li) XFlash®
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XFlash 4010 SDDResolution vs Count Rate
Resolution vs. Count Rate100
120
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2405 10 20 40 63 100 140
Count Rate [kcps]
Reso
lutio
n [e
V]
Si(Li)Xflash
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0
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0 50 100FWHM, elektronic [eV]
FWHM [eV]
CuNiCoFeMnCrVTiScCaKArClSPSiAlMgNaNeFONCBBe
-8 eV at
Mn/Kα
-17 eV at
C/Kα
Theoretical energy resolution ofKα lines for Si-based detectors
Mn/Kα=133 eVMn/Kα=125 eV
C/Kα =65 eV
C/Kα=48 eV
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XFlash SDD at 5K, 10K, 20K, 50K, 100K cps
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5K, 10K, 20K, 50K, 100K cps –No peak shift with count rate!
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Output Count Rate vs Input Count Rate
Output Count Rate (OCR) versus Input Count Rate (ICR)for selected shaping times (SVE III)
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Input Count Rate [kcps]
Output Count Rate[kcps]
"275kcps"
"130kcps"
"60 kcps"
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XFlash® Family Of Detectors
XFlash 4010: 10mm2, 125eV, Be DetectionXFlash 4030: 30mm2, 133eV, B Detection
XFlash Quad 4040: 4 x 10mm2, 125eV, Be Detection
XFlash Multi- Detectors
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Multiple Detector Systems
Internal view chamber
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Si(Li) detector (30 mm2)• 138 eV resolution• 20,000 cps input• 60% dead time • Duration: 6.25 hours
XFlash® QUAD 4040• 138 eV resolution• 720,000 cps input• 40% dead time• Duration: 7 minutes
Mineralogical sample, 15 keV, 600 x 450 Pixel
The 30 mm2 Si(Li) needs 50x longer for the same result!
Comparison: XFlash® with Si(Li)
Note: For an XFlash 4030 a 30mm2 SD, Duration = ~ 8.75 minutesand for an XFlash 4010 a 10mm2 SD, Duration = ~ 26.25 minutes
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SD Detectors have become the EDS detectors of choice
No liquid nitrogenNo vibrationReady to use in 30 secondsDoes not have to be warm to vent chamberBetter resolution than the traditional Si(Li)No change in resolution with count rate to 100,000 cpsCount rates of up to 1,000,000 cpsHigh resolution maps - Real time analysis of HyperMap Makes traditional mapping obsoleteFaster survey of sampleEasily moved to a new microscope – No Dewar!10 mm sq., 30 mm sq. active areasQUAD: 4 x 10mm sq. arrayMultiple XFlash detectors: up to four SDDs together
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Sample: Steel with Inclusions
Overall Spectrum15kV, 35oΨ, 20nA80Kcps @ 40%DT
50 µmMAG: 500X HV: 15.0 kV WD: 10.0 mm
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ESPRIT: Multi-Point Analysis
Region 1
Region 2
Region 3
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Multi-Point Analysis
50 µmMAG: 500X HV: 15.0 kV WD: 10.0 mm
Region 3
Region 2
Region 1
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HyperMap: Collection
50 µmMAG: 500X HV: 15.0 kV WD: 10.0 mm
Region 3
Region 2
Region 1
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50 µmMAG: 500X HV: 15.0 kV WD: 10.0 mm
HyperMap: SEI, Composite and Individual Maps
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Maximum Pixel Spectrum
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Verification of Maximum Pixel Spectrum
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HyperMaps: SEI and Individual Maps
50 µmMAG: 500X HV: 15.0 kV WD: 10.0 mm
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HyperMap: SEI and Composite
50 µmMAG: 500X HV: 15.0 kV WD: 10.0 mm
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Counts Area SE Fe-KA Al-K S-KA Ti-KA Mg-K P0 94.1 % -- 64.11 4.01 3.45 2.50 2.81 P1 2.5 % -- 37.45 64.09 2.75 2.15 5.18 P2 1.8 % -- 58.89 7.72 3.23 5.41 2.73 P3 1.5 % -- 46.07 39.47 3.20 2.64 3.45
AutoPhase
Counts Area SE Fe-KA Al-K S-KA Ti-KA Mg-K P0 94.1 % -- 64.11 4.01 3.45 2.50 2.81 P1 2.5 % -- 37.45 64.09 2.75 2.15 5.18 P2 1.8 % -- 58.89 7.72 3.23 5.41 2.73 P3 1.5 % -- 46.07 39.47 3.20 2.64 3.45
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AutoPhase Extracted Spectra
Area Fraction = 94.1%
Area Fraction = 2.5%
Area Fraction = 1.8%
Area Fraction = 1.5%
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XFlash®, QUANTAX & ESPRIT
XFlash SDD • No maintenance• High speed data acquisition• Maintain spectral resolution• Maintain sensitivity for all elements
Not limited to low resolution imagesCompositional image in secondsID phases that backscatter cannot separateImmediate verification of data while collecting• Meaningful Maps available in seconds• Extract spectra to verify identification and phase• Maximum pixel calculation• Phase Analysis
Full Quantification of any data
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Micro-XRF SpectrometerARTAXARTAX
A portable spectrometeroffering µm resolution
Armin Gross
Bruker AXS Microanalysis GmbH
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Contents
1. Introduction to µXRF
2. ARTAX instrument design
3. Line scan of solar cells
4. Element mapping in forensics
5. Element mapping in industry
6. Summary and outlook
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XRF TechnologiesµXRF vs EDS and XRF
Technology X-ray Microanalysis(EDS)
Micro X-rayFluorescence Analysis
(µXRF)
X-ray FluorescenceAnalysis (XRF)
Capability
Limitation
High resolution element mapping in the sub-µm range
Non-destructive spatial investigation of element distribution
Elemental analysis of bulk samples
Sample size limited by chamber
Analytical range of 10 µm to 10 mm
No information about spatial element distribution
nm - µm µm – mm mm - cm
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ARTAXIntroduction to µXRF
Micro X-ray fluorescence analysis (µXRF)
• Spatial resolved multi-element analysis
• Non-destructive analysis of the element composition
• Analysis at the location of the object
• Scan range 50 x 50 mm
• Target market art and conservation
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XFlash detector
Sample illumination
He purge
CCD camera
Collimator / Polycapillary lens
ARTAX Instrument DesignDetail of the Measuring Head
Tube housing
Red LED
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Beam focusing by polycapillary lensEnsemble of several thousand glass capillariesEach capillary ~1 µm in diameter
Advantages for fast mappingMinimal focal spot sizeabout 70 µmOutstanding intensity gain> 1000 compared to collimator
Instrument DesignExcitation Source
Metal-ceramic X-ray tubeMo, W or Rh target
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Instrument DesignExcitation Source
High precision coupling for fast exchange of excitation source
A source contains:
• tube housing incl. shutter
• X-ray tube (Mo, Rh, W target etc.)
Micro-focus tubee.g. Mo-target
Line-focus tubee.g. W-target
Polycapillary lens
Collimator
coupling
Filter device
• X-ray optics (polycapillary lens, collimator)
• Filter device
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Glass Standard BR E2Spectrum section above 20 keV
22 24 26 28 30 32 34- keV -
0.0
1.0
2.0
3.0
4.0x 1E3 Pulses
Ag
Sn
Sb
Ba
In
blue = W
green = Mo
red = Cr
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Glass Standard CRM 610Low energy range
1.00 1.50 2.00- keV -
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200
400
600
PulsesNa_K Al_K
Na
Al Si
blue = W
green = Mo
red = Cr
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Specifications• Si drift chamber detector (SDD)• 10 mm² active area, Be window• Electro-thermal cooling
Advantages• Energy resolution < 160 eV
(Mn-Kα line, 100 kcps)
• Highest throughput (> 100 kcps)
• No liquid nitrogen required
Upgrade option• Energy resolution < 145 eV
Instrument DesignXFlash® Silicon Drift Detector
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Instrument DesignCCD Camera and Sample Illumination
• Camera image of sample area under investigation Magnification about 20
White LED for optimization of the image qualitycan be dimmed
One red laser diode - can be dimmed
Red spot in center of crosshair
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Instrument DesignHelium Purging
SpecificationsDetection of light elementsNa(11) to Ar(18)
AdvantagesNo vacuum required,avoids damage of fragile samples
Hardly limitations in form and size of the sample
Small time effort
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• 15th to 17th century: peak in the painting of enamels in thefrench city Limoges
• End of 19th century:Limoges style replicas
• Line thickness of paintings about 150 µm
• Classification initially done by EDS
Art ApplicationsLimoges Painted Enamels
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Line Scan ApplicationInvestigation of Solar Cells
Production of solar cellsTypical layer structure of a CdTe solar cellDuring production the homogenity is tested routinely
Measurement parametersARTAX line scan48 measurements50 kV, 600 µA15 s
Glass body
CdTe3000 nm
Mo 5 – 15 nm
Al 200 nm
Cr 5 nm
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ApplicationsInvestigation of Solar Cells
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ApplicationsInvestigation of Solar Cells
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X-axis (mm)
Net
are
a co
unts
Al K12 Si K12 Cr K12 Mo L1 Cd L1 Te L1
Si: lower absorbance
Cd > 90% removedTe almost unchanged
Mo ?
Al: almost removed
Cr: removed
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ApplicationsElement Mapping in Forensics
Section of a bullet
• Area 1.8 x 1.8 mm• Meas. points 100• Meas. time 5 s• Total time 23 min
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ApplicationsElement Mapping in Forensics
Section of a bullet
• Spectrum
5 10 15 20- keV -
0
2
4
6
x 1E3 Pulses
Fe Cu Zn Sr Sr Ba Pb
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ApplicationsElement Mapping in Forensics
Section of a bullet• Distribution of
Fe, Cu, Pb, Ba
39,80 39,60 39,40 39,20 39,00 38,80 38,60 38,40 38,20 38,00
33,62
33,42
33,22
33,02
32,82
32,62
32,42
32,22
32,02
31,82
198000-220000
176000-198000154000-176000
132000-154000
110000-13200088000-110000
66000-88000
44000-66000
22000-440000-22000
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39,80 39,60 39,40 39,20 39,00 38,80 38,60 38,40 38,20 38,00
33,62
33,42
33,22
33,02
32,82
32,62
32,42
32,22
32,02
31,82
198000-220000
176000-198000154000-176000
132000-154000
110000-13200088000-110000
66000-88000
44000-66000
22000-440000-22000
ApplicationsElement Mapping in Forensics
Section of a bullet• Distribution of
Fe, Cu, Pb, Ba
39,80 39,60 39,40 39,20 39,00 38,80 38,60 38,40 38,20 38,00
33,62
33,42
33,22
33,02
32,82
32,62
32,42
32,22
32,02
31,82
135000-150000
120000-135000105000-120000
90000-105000
75000-9000060000-75000
45000-60000
30000-45000
15000-300000-15000
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39,80 39,60 39,40 39,20 39,00 38,80 38,60 38,40 38,20 38,00
33,62
33,42
33,22
33,02
32,82
32,62
32,42
32,22
32,02
31,82
135000-150000
120000-135000105000-120000
90000-105000
75000-9000060000-75000
45000-60000
30000-45000
15000-300000-15000
ApplicationsElement Mapping in Forensics
Section of a bullet• Distribution of
Fe, Cu, Pb, Ba
39,80 39,60 39,40 39,20 39,00 38,80 38,60 38,40 38,20 38,00
33,62
33,42
33,22
33,02
32,82
32,62
32,42
32,22
32,02
31,82
32400-36000
28800-32400
25200-28800
21600-25200
18000-21600
14400-18000
10800-14400
7200-10800
3600-7200
0-3600
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39,80 39,60 39,40 39,20 39,00 38,80 38,60 38,40 38,20 38,00
33,62
33,42
33,22
33,02
32,82
32,62
32,42
32,22
32,02
31,82
32400-36000
28800-32400
25200-28800
21600-25200
18000-21600
14400-18000
10800-14400
7200-10800
3600-7200
0-3600
ApplicationsElement Mapping in Forensics
Section of a bullet• Distribution of
Fe, Cu, Pb, Ba
39,80 39,60 39,40 39,20 39,00 38,80 38,60 38,40 38,20 38,00
33,62
33,42
33,22
33,02
32,82
32,62
32,42
32,22
32,02
31,82
12600-14000
11200-12600
9800-112008400-98007000-8400
5600-7000
4200-56002800-4200
1400-2800
0-1400
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ApplicationsElement Mapping in Industry
Polymer mould with metal structures
• Area 2.9 x 2.9 mm• Meas. points 900• Meas. time 5 s• Total time 5 h 10 min
5 10 15- keV -
0
100
200
300
400
Pulses
Ca Ti Fe Cr Cu Sr Mo
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ApplicationsElement Mapping in Industry
Polymer mould with metal structures
• Distribution of Cr and Ca
41,1
0
40,9
0
40,7
0
40,5
0
40,3
0
40,1
0
39,9
0
39,7
0
39,5
0
39,3
0
39,1
0
38,9
0
38,7
0
38,5
0
38,3
0
31,94
31,54
31,14
30,74
30,34
29,94
29,54
29,14
8900-92008600-89008300-86008000-83007700-80007400-77007100-74006800-71006500-68006200-6500
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ApplicationsElement Mapping in Industry
Polymer mould with metal structures
• Distribution of Cr and Ca
41,1
0
40,9
0
40,7
0
40,5
0
40,3
0
40,1
0
39,9
0
39,7
0
39,5
0
39,3
0
39,1
0
38,9
0
38,7
0
38,5
0
38,3
0
31,94
31,54
31,14
30,74
30,34
29,94
29,54
29,14
8900-92008600-89008300-86008000-83007700-80007400-77007100-74006800-71006500-68006200-6500
41,1
0
40,9
0
40,7
0
40,5
0
40,3
0
40,1
0
39,9
0
39,7
0
39,5
0
39,3
0
39,1
0
38,9
0
38,7
0
38,5
0
38,3
0
31,94
31,54
31,14
30,74
30,34
29,94
29,54
29,14
6540-68006280-65406020-62805760-60205500-57605240-55004980-52404720-49804460-47204200-4460
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Summary and Outlook
The µXRF Spectrometer ARTAX features a fast multi-element mapping in the mm range for industrial and forensic samples
The fast exchange of the excitation source (X-ray tube, collimator, polycap lens) allows optimization of spatial resolution and detection limits
Bruker AXS continuous its development in the field of µXRF spectrometry
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Thank you for attending!
Please type any questions you may have in the Q&A panel to the right of
your screen and click Send.
Copies of this presentation and related microanalysis resource
materials will be emailed to you.
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www.bruker-axs.com