Detector Technology, Tips, Tricks
Innovation with Integrity
X-Ray Powder Diffraction (XRPD) Bragg-Brentano Geometry
14-15/12/2011
Advanced XRD Workshop
X-ray Detector From X-Ray Photon Energy h to CPS
Amplification
Preamplification
Signal processing
Counting
14-15/12/2011
Advanced XRD Workshop
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
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 CMOS detectors
14-15/12/2011
Advanced XRD Workshop
Scintillation Counter
X-Rays Light Photon Photomultiplier Tube Pulse Measuring Device Dynode Photocathode Optical Window
14-15/12/2011 Advanced XRD Workshop 6
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)
14-15/12/2011
Advanced XRD Workshop
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
14-15/12/2011
Advanced XRD Workshop
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)
14-15/12/2011
Advanced XRD Workshop
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
14-15/12/2011
Lithium drifted depletion region ~ 0.5 3 mm
n-type Region ~ 0.1m
10
Advanced XRD Workshop
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
14-15/12/2011
Advanced XRD Workshop
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
14-15/12/2011
Advanced XRD Workshop
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
14-15/12/2011
Advanced XRD Workshop
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
14-15/12/2011
Advanced XRD Workshop
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
14-15/12/2011
Advanced XRD Workshop
15
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 CMOS detectors
14-15/12/2011
Advanced XRD Workshop
16
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
14-15/12/2011
Advanced XRD Workshop
17
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
14-15/12/2011 Advanced XRD Workshop 18
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
14-15/12/2011
Advanced XRD Workshop
19
High Resolution XRPD in NIST 1976, LYNXEYE vs. Scintillation Counter
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]
14-15/12/2011
Advanced XRD Workshop
20
High Resolution XRPD in NIST 1976, LYNXEYE vs. Scintillation Counter
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
Advanced XRD Workshop
117.00
117.50
14-15/12/2011
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
14-15/12/2011 Advanced XRD Workshop 22
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
Advanced XRD Workshop
SRM 660a
Scinti LynxEye
120.00
160.00
14-15/12/2011
23
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
14-15/12/2011 Advanced XRD Workshop 24
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
14-15/12/2011
Advanced XRD Workshop
25
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
14-15/12/2011 Advanced XRD Workshop 26
Compound Si Strip Detector Optimized for Cu Radiation
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 27
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%
14-15/12/2011
Advanced XRD Workshop
28
Compound Si Strip Detector For Hard X-rays
Sketch taken from: from Kemmer et al., Phys. Bl., vol. 41, p117 (1985)
500 m LYNXEYE: Compound Silicon Strip Detector
14-15/12/2011 Advanced XRD Workshop 29
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%
14-15/12/2011
Advanced XRD Workshop
30
Compound Si Strip Detector Fluorescence Discrimination
Optimized discriminator settings Improve peak-to-background ratio
Normalized to max.Intensity
14-15/12/2011
Advanced XRD Workshop
31
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
14-15/12/2011 Advanced XRD Workshop 32
Functional Principle of Conventional Gas Filled Proportional Detector Voltage Source + + + + + - - Anode + Electrical Current Measuring Device
X-Rays
Cathode Detection Gas
14-15/12/2011 Advanced XRD Workshop 33
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
14-15/12/2011
Advanced XRD Workshop
34
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
14-15/12/2011
Advanced XRD Workshop
35
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
14-15/12/2011
Advanced XRD Workshop
36
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)
14-15/12/2011
Advanced XRD Workshop
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
14-15/12/2011 Advanced XRD Workshop 38
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
14-15/12/2011
Advanced XRD Workshop
39
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
14-15/12/2011 Advanced XRD Workshop 41
Innovation with Integrity
Copyright Bruker Corporation. All rights reserved.
