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Detector Technology, Tips, Tricks - S. N. Bose National Centre for
Transcript of Detector Technology, Tips, Tricks - S. N. Bose National Centre for
X-ray Detector – From X-Ray Photon Energy h⋅ν to CPS
Sen
sor
Pre
-am
plifi
catio
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Photonsh⋅⋅⋅⋅νννν
Am
plifi
catio
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Sig
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proc
essi
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Cou
ntin
g
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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
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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
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Scintillation Counter
Sodium-IodideCrystal
Photocathode
Optical Window
-Pulse
MeasuringDevice
Light Photon Photomultiplier Tube
Dynode Anode
X-Rays
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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)
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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°
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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)
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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
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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
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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
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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
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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
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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
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)
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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
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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
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10000
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40000
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60000
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2-Theta [deg]
25 30 40 50 60 70
Inte
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[co
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10000
20000
30000
40000
50000
60000
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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
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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%
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
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500
µµ µµm
Compound Si Strip DetectorFor Hard X-rays
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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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• Optimized discriminator settings• Improve peak-to-background ratio
Compound Si Strip DetectorFluorescence DiscriminationN
orm
aliz
edto
max
.Inte
nsity
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
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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
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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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