Detector Technology

Detector Technology, Tips, Tricks
Innovation with Integrity
X-Ray Powder Diffraction (XRPD) Bragg-Brentano Geometry
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Advanced XRD Workshop
X-ray Detector From X-Ray Photon Energy h to CPS
Amplification
Preamplification
Signal processing
Counting
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Sensor
Photons h
Commonly Used X-Ray Detectors

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
Linear detectors (1-D) Area detectors (2-D)

MikroGap detector Compound silicon strip detector Single wire proportional counter Image plate detector (IP)* Linear CCD* Photographic film*
CCD camera* Multi wire

proportional counter (MWPC)
MikroGap detector Image plate detector

(IP)*
Photographic film* Pixel detectors
* Integrating (analog) detectors, of little use for XRD

14-15/12/2011 Advanced XRD Workshop
CMOS detectors
4
Point Detectors

MikroGap detector Compound silicon strip detector Single wire proportional counter Image plate detector (IP) Linear CCD Photographic film
CCD camera Multi wire


(IP)
Photographic film Pixel detectors CMOS detectors
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Scintillation Counter
X-Rays Light Photon Photomultiplier Tube Pulse Measuring Device Dynode Photocathode Optical Window
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Sodium-Iodide Crystal
Anode
Scintillation Counter
Active Area: 30 mm 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 BraggBrentano 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 20m Ni Cu-K 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 Detector SOL-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. Fefluorescence and Cu-K 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 Detector Functional Principle

Au contact ~ 20 nm Pre amplifier Bias voltage
X-Rays
h
Amplifier Signal processing counting

Au Cathode ~ - 500 V ~ 200 nm
e-
Be window P-type Region ~ 0.1m

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Lithium drifted depletion region ~ 0.5 3 mm
n-type Region ~ 0.1m

10
X-Ray Powder Diffraction with Energy Dispersive SOL-XE

SOL-XE: No Nickel filter, more than 2 times more intensity
D8 ADVANCE diffractometer Cu-radiation 40 kV, 50 mA 0.3 divergence and anti-scatter slit 2.5 axial Soller slits No Ni Cu-K 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
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11
Suppression of Fe-fluorescence
Measurement on Hematite/Muscovite composite with Cu-Radiation and scintillation counter
1500 1400 1300 1200 1100 1000 900 800 700 600 500 400 300 200 100 0 7 10 20 30 40 50
Ni-Filter
Lin (Counts)
2-Theta - Scale
Hematite/Muscovite, 2 Soller, 0,5 slits, 0,2 mm D S, Ni-Filter - Step: 0.020 - Step time: 1. s Hematite Muscovite
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12
Suppression of Fe-fluorescence
Measurement on Hematite/Muscovite composite with Cu-Radiation, SOL-XE detector
1000 900 800
Sol-X Detector
Lin (Counts)
700 600 500 400 300 200 100 0 7 10 20 30 40 50
2-Theta - Scale
Hematite/Muscovite, 2 Soller, 0,5 slits, 0,2 mm D S, Solid state Detektor - Step: 0.020 - Step time : 1. s Hematite Muscovite
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13
X-Ray Powder Diffraction with SOL-XE Monochromatic K-radiation

Energy dispersive SOLXE detector can be used with any radiation source, not only Cu. Park the detector on K line of corundum, collect a peak and calibrate with 8.9 KeV for K Very easy and fast way to switch between K and K radiation or between different radiation sources
Energy calibration window of SOL-XE detector
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14
X-Ray Powder Diffraction with SOL-XE Monochromatic K-radiation
700
600
500
400
300
NIST1976 corundum plate Bragg-Brentano geometry 0.5divergence 0.1 mm receiving slit Sol-XE detector K peaks of corundum K peaks of corundum
Lin (Cps)
200
100
0 46 50
60
2-Theta - Scale
File: NIST 1976_1sec kbeta.raw - Step: 0.010 - St ep time: 1. s 00-046-1212 (*) - Corundum, syn - Al2O3 - WL: 1.5406 00-046-1212 (*) - Corundum, syn - Al2O3 - WL: 1.39222
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Commonly Used X-Ray Detectors


MikroGap detector Compound silicon strip detector Single wire proportional counter Image plate detector (IP) Linear CCD Photographic film
CCD camera Multi wire


(IP)
Photographic film Pixel detectors CMOS detectors
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Compound Si Strip Detector LYNXEYE 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 Detector How Does it Work

Sketch taken from: from Kemmer et al., Phys. Bl., vol. 41, p117 (1985)
h+ e-
LYNXEYE: Compound Silicon Strip Detector

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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19

150000 140000 130000 120000 110000
LYNXEYE: 138,000 counts
Intensity [counts]
100000 90000 80000 70000 60000 50000 40000 30000
Scinti: 1100 counts
150000 140000 130000 120000 110000
20000 10000 0 34.71 34.8 34.9 35.0 35.1 35.2 35.3 35.4 35.5 35.6 35.7
Intensity [counts]
100000 90000 80000 70000 60000 50000 40000 30000 20000 10000 0 25 30 40 50
2-Theta [deg]
60
70
2-Theta [deg]
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20

I rel 100.00
SRM 660a
Scinti LynxEye
80.00
Normalised Intensity!
60.00
40.00
20.00
0.00 115.50 116.00 116.50 2 deg

117.00
117.50
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21
High-Resolution XRPD on NIST 660a Resolution

Counts 100000
SRM 660a
LynxEye
80000
FWHM = 0.0365 2
60000
40000
With standard slit settings, Using small slits and sollers resolution can be even improved!
20000
0 29.90 30.10 30.30 2 deg

30.50
30.70
30.90
High-Resolution XRPD on NIST 660a: LYNXEYE vs. Scintillation Counter

FWHM 0.14 0.12 0.10 0.08 0.06 0.04 0.02 0.00 0.00 40.00 80.00 2 deg
SRM 660a
Scinti LynxEye
120.00
160.00
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XRPD on NIST 660a Resolution

I rel 100
SRM 660a
Scinti LynxEye
80
60
40
20
0 20.90 21.10 21.30 2 deg

21.50
21.70
21.90
Bragg-Brentano Geometrie Flat Detector Error

the 1-D Detector is tangential to goniometer circle, which causes shifts and 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 LYNXEYE Ag-Behenate

D8 ADVANCE 35 kV, 50 mA 500 mm 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
Compound Si Strip Detector Optimized for Cu Radiation

LYNXEYE: Compound Silicon Strip Detector

Compound Si Strip Detector Optimized for Cu Radiation
Wavelength
Linear absorption coefficient for Si (cm-1) 439.3
Efficiency (300m sensor) > 99%
Cr
Co
216.4
> 99%
Cu
139.4
> 98%
Mo
14.25
~ 35%
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Compound Si Strip Detector For Hard X-rays

500 m LYNXEYE: Compound Silicon Strip Detector

Compound Si Strip Detector For Hard X-rays
Wavelength
Linear absorption coefficient for Si (cm-1) 439.3 216.4 139.4 14.25 7.09
Efficiency (500m sensor) > 99% > 99% > 99%
Cr Co Cu Mo Ag
~ 50%
~ 30%
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Compound Si Strip Detector Fluorescence Discrimination

Optimized discriminator settings Improve peak-to-background ratio
Normalized to max.Intensity
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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 2-D HI-STAR Limited maximum count rate due to long ion drift times (6 sec) l (typically <103 counts/mm2/sec) Permanent detection gas flow required
MBRaun PSD mounted on D8 ADVANCE With capillary sample stage

Functional Principle of Conventional Gas Filled Proportional Detector Voltage Source + + + + + - - Anode + Electrical Current Measuring Device
X-Rays
Cathode Detection Gas

MicroGap Detector Technology VNTEC-1TM Detector

Large active area of 50x16 mm Capture angle >12 2 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 Moradiation No operating gas purge required, maintenance free Radiation hard
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MicroGap Detector Technology How Does it Work

MikroGapTM technology with resistive anode: shortens drift time of ions fast electrons induce charge on readout strips Adjusted surface resistance (105 - 107 / area): high enough to limit discharges low enough to support high count rates
US Patent US 6,340,819 B1
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VNTEC-1 Scanning Diffraction Measurements

Count rates: 0.85 kcps 1.7 kcps 3.9 kcps 6.6 kcps
Conventional proportional counter Angular resolution 0.05 0.12 Strong function of count rate
MikroGapTM, VNTEC-1 Angular resolution <0.05 Independent of count rate
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VNTEC-1 in SNAPSHOT Mode Kinetic Studies of Phase Transition

Phase Transition of NH4NO3, T = 3 K, 58 Snapshots melted Phase I (cubic) D8 ADVANCE with Bragg-Brentano geometry Power: 40kV, 50 mA Optics: 0.5 divergence slit 4 Soller slit Ni Cu-K-filter Step size: 0.023 Time per Snapshot: 1 sec High temperature chamber, permanent heating
37
Phase II (tetragonal)
Phase IV (orthorhombic)
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VNTEC-1 in Scanning Mode Hot Humidity Investigations by XRD

Parallel beam Gbel Mirror Radial Soller slit VNTEC-1 detector
Line focus X-ray tube
Heated supply hose Hot Humidity Sample chamber

VNTEC-1 in Scanning Mode Humidification Investigations on Creatine by Fast Continuous Scans

2500
2000
Scan speed 30/minute 0.01 sec/step 0.0065 /step 50 C 0.5 % relative humidity
Lin (Counts)
1500
1000
500
0
5 10 20 30 40
2Theta [deg]
Type: 2Th/Th locked - Start: 5.000 - End: 40.005 - Step: 0.007 - Step time: 0. s - Anode: Cu 00-029-1649 (Q) - Creatine - C4H9N3O2 00-029-1650 (D) - Creatine hydrate - C4H9N3O2H2O
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VNTEC-1 in Scanning Mode Humidification Investigations on Creatine by Fast Continuous Scans

110 100 90
Creatine hydrate
intensity [cps]
80 70 60 50 40 30 20 10 0
Creatine
5 10 20 30 40
2-Theta [deg]
Measurement conditions: Scan speed 30/min 5 40 2theta Step size 0.007 71 seconds/scan
14-15/12/2011 Advanced XRD Workshop
50 C 80 % relative humidity
40
BAXS Detectors for XPRD
Dimension
GF >150
GF >500
Gain factor 3
Capabilities
Innovation with Integrity
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Detector Technology, Tips, Tricks

Innovation with Integrity

X-Ray Powder Diffraction (XRPD) Bragg-Brentano Geometry

Advanced XRD Workshop

X-ray Detector From X-Ray Photon Energy h to CPS

Advanced XRD Workshop

Commonly Used X-Ray Detectors

Linear detectors (1-D) Area detectors (2-D)

CCD camera* Multi wire

MikroGap detector Image plate detector

Photographic film* Pixel detectors

* Integrating (analog) detectors, of little use for XRD

Linear detectors (1-D) Area detectors (2-D)

CCD camera Multi wire

MikroGap detector Image plate detector

Photographic film Pixel detectors CMOS detectors

Advanced XRD Workshop

Advanced XRD Workshop

X-Ray Powder Diffraction with Scintillation Counter

Advanced XRD Workshop

Solid State Detector SOL-XE Detector

Advanced XRD Workshop

Solid State Detector Functional Principle

Amplifier Signal processing counting

Be window P-type Region ~ 0.1m

Lithium drifted depletion region ~ 0.5 3 mm

n-type Region ~ 0.1m

Advanced XRD Workshop

X-Ray Powder Diffraction with Energy Dispersive SOL-XE

Advanced XRD Workshop

Advanced XRD Workshop

1000 900 800

700 600 500 400 300 200 100 0 7 10 20 30 40 50

Advanced XRD Workshop

X-Ray Powder Diffraction with SOL-XE Monochromatic K-radiation

Energy calibration window of SOL-XE detector

Advanced XRD Workshop

X-Ray Powder Diffraction with SOL-XE Monochromatic K-radiation

Advanced XRD Workshop

Commonly Used X-Ray Detectors

Linear detectors (1-D) Area detectors (2-D)

CCD camera Multi wire

MikroGap detector Image plate detector

Photographic film Pixel detectors CMOS detectors

Advanced XRD Workshop

Compound Si Strip Detector LYNXEYE Detector

Advanced XRD Workshop

Compound Si Strip Detector How Does it Work

LYNXEYE: Compound Silicon Strip Detector

High Resolution XRPD in NIST 1976, LYNXEYE vs. Scintillation Counter

Advanced XRD Workshop

High Resolution XRPD in NIST 1976, LYNXEYE vs. Scintillation Counter

LYNXEYE: 138,000 counts

100000 90000 80000 70000 60000 50000 40000 30000

Scinti: 1100 counts

150000 140000 130000 120000 110000

Advanced XRD Workshop

High Resolution XRPD in NIST 1976, LYNXEYE vs. Scintillation Counter

0.00 115.50 116.00 116.50 2 deg

High-Resolution XRPD on NIST 660a Resolution