detector technology
DESCRIPTION
Detector_technologyTRANSCRIPT
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Detector Technology, Tips, Tricks
Innovation with Integrity
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X-Ray Powder Diffraction (XRPD) –Bragg-Brentano Geometry
14-15/12/2011 Advanced XRD Workshop 2
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X-ray Detector – From X-Ray Photon Energy h⋅ν to CPS
Sen
sor
Pre
-am
plifi
catio
n
Photonsh⋅⋅⋅⋅νννν
Am
plifi
catio
n
Sig
nal
proc
essi
ng
Cou
ntin
g
14-15/12/2011 Advanced XRD Workshop 3
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Point detectors (0-D)
• Scintillation counter
• Proportional counter
• Si(Li) solid state detector
• Ge solid state detectors
• Silicon pin diodes
• Silicon drift detectors
• Ionization chambers
Commonly Used X-Ray Detectors
Linear detectors (1-D)
• MikroGap detector
• Compound silicon strip
detector
• Single wire
proportional counter
• Image plate detector
(IP)*
• Linear CCD*
• Photographic film*
Area detectors (2-D)
• CCD camera*
• Multi wire
proportional counter
(MWPC)
• MikroGap detector
• Image plate detector
(IP)*
• Photographic film*
• Pixel detectors
• CMOS detectors* Integrating (analog) detectors, of little use for XRD
14-15/12/2011 Advanced XRD Workshop 4
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Point detectors (0-D)
• Scintillation counter
• Proportional counter
• Si(Li) solid state detector
• Ge solid state detectors
• Silicon pin diodes
• Silicon drift detectors
• Ionization chambers
Point Detectors
Linear detectors (1-D)
• MikroGap detector
• Compound silicon strip
detector
• Single wire
proportional counter
• Image plate detector
(IP)
• Linear CCD
• Photographic film
Area detectors (2-D)
• CCD camera
• Multi wire
proportional counter
(MWPC)
• MikroGap detector
• Image plate detector
(IP)
• Photographic film
• Pixel detectors
• CMOS detectors
14-15/12/2011 Advanced XRD Workshop 5
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Scintillation Counter
Sodium-IodideCrystal
Photocathode
Optical Window
-Pulse
MeasuringDevice
Light Photon Photomultiplier Tube
Dynode Anode
X-Rays
14-15/12/2011 Advanced XRD Workshop 6
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Scintillation Counter
• Active Area: 30 mm Ø• Sensitivity: from Cr- to Mo-radiation• Energy resolution: 30% - 45% (2.5 keV at 8 keV e.g.)
• NaI(Tl) scintillation:• Maximum count rate >2x106 cps• Noise: < 0.3 cps
• Infinite life time• Maintenance free• Routine detector for all applications• Potential angular resolution: no limit! (typical 0.037° for Bragg-Brentano geometry)
14-15/12/2011 Advanced XRD Workshop 7
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X-Ray Powder Diffraction with Scintillation Counter
D8 ADVANCE diffractometer
• Cu-radiation• 40 kV, 50 mA• 0.3 ° divergence and anti-scatter slit
• 2.5° axial Soller slits• 20µm Ni Cu-Kß filter• 0.05mm receiving slit• Scintillation counter• 0.006° step size• 10 seconds per step• NIST 1976 Corundum sample
• FWHM at 100% reflection 0.04°
• Angular position accuracy certified ±0.01°
14-15/12/2011 Advanced XRD Workshop 8
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Solid State DetectorSOL-XE Detector
• Active area: 4 x 15 mm2
• Si(Li) solid state energy dispersive detector• Energy resolution < 350 eV(4.5%) at 50.000 cps
• Suppression of e.g. Fe-fluorescence and Cu-Kß radiation
• Linearity up to 75.000 cps integral events
• Wavelength range: 2 keV up to 30 keV (Cr-…Mo-radiation)
14-15/12/2011 Advanced XRD Workshop 9
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Solid State DetectorFunctional Principle
Lithium drifteddepletion region~ 0.5 – 3 mm
AmplifierSignal processing
counting
Au Cathode~ - 500 V~ 200 nm
Pre amplifierAu contact~ 20 nm
X-Rays
Be window
P-typeRegion~ 0.1µm
n-typeRegion~ 0.1µm
Bias voltage
h
e-
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X-Ray Powder Diffraction with Energy Dispersive SOL-XE
D8 ADVANCE diffractometer
• Cu-radiation• 40 kV, 50 mA• 0.3 ° divergence and anti-scatter slit
• 2.5° axial Sollerslits
• No Ni Cu-Kß filter• 0.05° receiving slit• Sol-XE detector• 0.006° step size• 2.8 seconds per step
• NIST 1976 Corundum sample
• FWHM at 100% reflection 0.04°
SOL-XE: No Nickel filter, more than 2 times
more intensity
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MuscoviteHematiteHematite/Muscovite, 2° Soller, 0,5° slits, 0,2 mm D S, Ni-Filter - Step: 0.020 ° - Step time: 1. s
Lin
(Cou
nts)
0
100
200
300
400
500
600
700
800
900
1000
1100
1200
1300
1400
1500
2-Theta - Scale
7 10 20 30 40 50
Ni-Filter
• Measurement on Hematite/Muscovite composite with Cu-Radiation and scintillation counter
Suppression of Fe-fluorescence
14-15/12/2011 Advanced XRD Workshop 12
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MuscoviteHematiteHematite/Muscovite, 2° Soller, 0,5° slits, 0,2 mm D S, Solid state Detektor - Step: 0.020 ° - Step time : 1. s
Lin
(Cou
nts)
0
100
200
300
400
500
600
700
800
900
1000
2-Theta - Scale
7 10 20 30 40 50
Sol-X Detector
• Measurement on Hematite/Muscovite composite with Cu-Radiation, SOL-XE detector
Suppression of Fe-fluorescence
14-15/12/2011 Advanced XRD Workshop 13
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X-Ray Powder Diffraction with SOL-XEMonochromatic Kβ-radiation
• Energy dispersive SOL-XE detector can be used with any radiation source, not only Cu.
• Park the detector on Kβ line of corundum, collect a peak and calibrate with 8.9 KeVfor Kβ
• Very easy and fast way to switch between Kαand Kβ radiation or between different radiation sources
Energy calibration window of SOL-XE detector
14-15/12/2011 Advanced XRD Workshop 14
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X-Ray Powder Diffraction with SOL-XEMonochromatic Kβ-radiation
• NIST1976 corundum plate
• Bragg-Brentano geometry• 0.5°divergence• 0.1 mm receiving slit
• Sol-XE detector
• Kβ peaks of corundum
• Kα peaks of corundum
00-046-1212 (*) - Corundum, syn - Al2O3 - WL: 1.392 2200-046-1212 (*) - Corundum, syn - Al2O3 - WL: 1.540 6File: NIST 1976_1sec kbeta.raw - Step: 0.010 ° - St ep time: 1. s
Lin
(Cps
)
0
100
200
300
400
500
600
700
2-Theta - Scale
46 50 60
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Point detectors (0-D)
• Scintillation counter
• Proportional counter
• Si(Li) solid state detector
• Ge solid state detectors
• Silicon pin diodes
• Silicon drift detectors
• Ionization chambers
Commonly Used X-Ray Detectors
Linear detectors (1-D)
• MikroGap detector
• Compound silicon strip
detector
• Single wire
proportional counter
• Image plate detector
(IP)
• Linear CCD
• Photographic film
Area detectors (2-D)
• CCD camera
• Multi wire
proportional counter
(MWPC)
• MikroGap detector
• Image plate detector
(IP)
• Photographic film
• Pixel detectors
• CMOS detectors
14-15/12/2011 Advanced XRD Workshop 16
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Compound Si Strip DetectorLYNXEYE Detector
• Active Area: 14.4 x 16 mm• Capture angle 3.7° 2theta for D8 ADVANCE
• Compound silicon strip detector technology• Maximum global count rate: >100,000,000 cps
• Maximum local count rate: 700,000 cps
• Dynamic range >7x106
• Energy resolution: 25% (2 keV)• Wavelength range: from Cr- to Cu-radiation
• Maintenance free
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Compound Si Strip DetectorHow Does it Work
h+
e-
Sketch taken from: from Kemmer et al., Phys. Bl., vol. 41, p117 (1985)
LYNXEYE: Compound Silicon Strip Detector
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High Resolution XRPD in NIST 1976, LYNXEYE vs. Scintillation Counter
• D8 ADVANCE• 35 kV, 50 mA• 0.3° divergence• 2.5° Soller• 0.3° anti-scatter• 2.5° Soller• 0.5% Ni-filter• 0.1 mm receiving slit• 3° opening• 0.006° step size• 1 sec/step
~ 150,000 counts
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High Resolution XRPD in NIST 1976, LYNXEYE vs. Scintillation Counter
Inte
nsity
[cou
nts
]
0
10000
20000
30000
40000
50000
60000
70000
80000
90000
100000
110000
120000
130000
140000
150000
2-Theta [deg]
25 30 40 50 60 70
Inte
nsity
[co
unts
]
0
10000
20000
30000
40000
50000
60000
70000
80000
90000
100000
110000
120000
130000
140000
150000
2-Theta [deg]
34.71 34.8 34.9 35.0 35.1 35.2 35.3 35.4 35.5 35.6 35.7
Scinti:1100 counts
LYNXEYE:138,000 counts
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High Resolution XRPD in NIST 1976, LYNXEYE vs. Scintillation Counter
SRM 660a
115.50 116.00 116.50 117.00 117.50
2θ deg
0.00
20.00
40.00
60.00
80.00
100.00
Irel
ScintiLynxEye
Normalised Intensity!
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High-Resolution XRPD on NIST 660aResolution
SRM 660a
29.90 30.10 30.30 30.50 30.70 30.90
2θ deg
0
20000
40000
60000
80000
100000
Counts
LynxEye
FWHM = 0.0365° 2 θ
With standard slit settings,Using small slits and sollersresolution can be even improved!
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High-Resolution XRPD on NIST 660a: LYNXEYE vs. Scintillation Counter
SRM 660a
0.00 40.00 80.00 120.00 160.00
2θ deg
0.00
0.02
0.04
0.06
0.08
0.10
0.12
0.14
FWHM
ScintiLynxEye
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XRPD on NIST 660aResolution
SRM 660a
20.90 21.10 21.30 21.50 21.70 21.90
2θ deg
0
20
40
60
80
100
Irel
ScintiLynxEye
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Bragg-Brentano Geometrie Flat Detector Error
• the 1-D Detector is tangential to goniometer circle, which causes shiftsand asymmetries of the reflections
A narrower detector capture angle reduces the drawbacks for the price of smaller intensities
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XRPD at Low Angles with LYNXEYEAg-Behenate
• D8 ADVANCE • 35 kV, 50 mA• 500 mm Ø• 0.1 ° divergence slit• 2.5° Soller slits• Anti-scatter screen• Ni 0.5 % filter• 30 rpm• LYNXEYE 1° opening• Step size: 0.006°
• Step time: 0.1 sec/step
2Theta: 0.5 °
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Compound Si Strip DetectorOptimized for Cu Radiation
Sketch taken from: from Kemmer et al., Phys. Bl., vol. 41, p117 (1985)
LYNXEYE: Compound Silicon Strip Detector
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Compound Si Strip DetectorOptimized for Cu Radiation
14-15/12/2011 28Advanced XRD Workshop
Wavelength
Linear absorptioncoefficient for Si
(cm-1)
Efficiency (300µµµµm sensor)
Cr 439.3 > 99%
Co 216.4 > 99%
Cu 139.4 > 98%
Mo 14.25 ~ 35%
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Compound Si Strip DetectorFor Hard X-rays
Sketch taken from: from Kemmer et al., Phys. Bl., vol. 41, p117 (1985)
LYNXEYE: Compound Silicon Strip Detector
14-15/12/2011 Advanced XRD Workshop 29
500
µµ µµm
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Compound Si Strip DetectorFor Hard X-rays
14-15/12/2011 30Advanced XRD Workshop
Wavelength
Linear absorptioncoefficient for Si
(cm-1)
Efficiency (500µµµµm sensor)
Cr 439.3 > 99%
Co 216.4 > 99%
Cu 139.4 > 99%
Mo 14.25 ~ 50%
Ag 7.09 ~ 30%
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14-15/12/2011 31Advanced XRD Workshop
• Optimized discriminator settings• Improve peak-to-background ratio
Compound Si Strip DetectorFluorescence DiscriminationN
orm
aliz
edto
max
.Inte
nsity
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Functional Principle of Conventional Gas Filled Proportional Detector
Pros• High sensitivity, low noise due to high intrinsic amplification caused by avalanche multiplication of charges (1 to 2 orders higher than solid state detector)
• Big active area for affordable costs possible
Cons• Limited maximum count rate due to long ion drift times (6 µsec) l (typically <103 counts/mm2/sec)
• Permanent detection gas flowrequired
2-D HI-STAR
MBRaun PSD mounted on D8 ADVANCEWith capillary sample stage
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Functional Principle of Conventional Gas Filled Proportional Detector
Detection Gas
ElectricalCurrent
Measuring Device
X-Rays
Cathode -
Anode +
+ -Voltage Source
+
-
+ + +
- - -
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MicroGap Detector Technology VÅNTEC-1TM Detector
• Large active area of 50x16 mm• Capture angle >12° 2θ D8 ADVANCE
• 100 msec Snapshots• Super speed continuous scan mode
• MikroGap technology • Global count rate >106 cps • Detector background <0.01 cps/mm2
• Dynamic Range 108
• Very good energy resolution of <25%• Wavelength range: from Cr- to Mo-radiation
• No operating gas purge required, maintenance free
• Radiation hard
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• MikroGapTM technology with resistive anode: • shortens drift time of ions• fast electrons induce charge on readout strips
• Adjusted surface resistance (105 - 107 Ω/ area): • high enough to limit discharges
• low enough to support high count rates
MicroGap Detector TechnologyHow Does it Work
US Patent US 6,340,819 B1
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VÅNTEC-1 – Scanning DiffractionMeasurements
• Conventional proportional counter
• Angular resolution 0.05° -0.12°
• Strong function of count rate
• MikroGapTM, VÅNTEC-1
• Angular resolution <0.05°
• Independent of count rate
Count rates:• 0.85 kcps• 1.7 kcps• 3.9 kcps• 6.6 kcps
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VÅNTEC-1 in SNAPSHOT ModeKinetic Studies of Phase Transition
• D8 ADVANCE with Bragg-Brentano geometry
• Power: 40kV, 50 mA
• Optics:• 0.5°divergence slit
• 4° Soller slit• Ni Cu-Kß-filter
• Step size: 0.023°• Time per Snapshot: 1 sec
• High temperature chamber, permanent heating
Phase Transition of NH 4NO3, ∆∆∆∆T = 3 K, 58 Snapshots
Phase IV (orthorhombic)
Phase II (tetragonal)
Phase I (cubic)
melted
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VÅNTEC-1 in Scanning ModeHot Humidity Investigations by XRD
Parallel beamGöbel Mirror
Line focusX-ray tube
Hot HumiditySample chamber
VÅNTEC-1detector
Radial Sollerslit
Heated supplyhose
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VÅNTEC-1 in Scanning Mode Humidification Investigations on Creatine by Fast Continuous Scans
00-029-1650 (D) - Creatine hydrate - C4H9N3O2·H2O
00-029-1649 (Q) - Creatine - C4H9N3O2
Type: 2Th/Th locked - Start: 5.000 ° - End: 40.005 ° - Step: 0.007 ° - Step time: 0. s - Anode: Cu
Lin
(Cou
nts)
0
500
1000
1500
2000
2500
2Theta [deg]
5 10 20 30 40
• Scan speed 30°/minute• 0.01 sec/step• 0.0065 °/step
• 50 °C
• 0.5 % relative humidity
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VÅNTEC-1 in Scanning Mode Humidification Investigations on Creatine by Fast Continuous Scans
inte
nsity
[cps
]
0
10
20
30
40
50
60
70
80
90
100
110
2-Theta [deg]
5 10 20 30 40
Measurement conditions:• 5° – 40° 2theta• Step size 0.007°
• Scan speed 30°/min
• 71 seconds/scan
Creatine
Creatinehydrate
• 50 °C
• 80 % relative humidity
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BAXS Detectors for XPRDD
imen
sion
Capabilities
Gain factor 3
GF >150 GF >500
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Innovation with Integrity
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