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Materials Chemistry- EH3
The materials chemistry hutch at ID15A is devoted to operando and time resolved diffraction and imaging, total scattering, and diffraction computed tomography. The station is optimised for rapid alternation between the different techniques during a single operando experiment in order to collect complementary data on working systems. The high available energy (up to 120 keV) means that even bulky and highly absorbing systems may be studied. The combination of the beamline's optimised focusing optics and a photon counting CdTe pixel detector allows for both unprecedented data quality at high energy, and for very rapid triggered experiments.
Key points
- Energy range, monochromatic 40 < E < 120 KeV
- Beam sizes from 0.3 µm to 8 mm
Techniques
- Angular dispersive diffraction using area detectors
- Pair distribution function experiments
- X-ray imaging, fast tomography, diffraction tomography
Experimental hutch overview
As shown below, EH3 contains four main elements mounted on highly stable granite platforms. From right to left, these are 1) Secondary focusing using compound refractive lenses; 2) A sample stage containing both heavy and light duty sample towers; 3) A detector stage with long translations; and 4) An ancillary table offering the ability to mount a SAXS detector.
The following experimental configurations are available in standard operation:
|
XRD-/PDF-/SAXS-CT |
Abs-/Phase-Contrast-CT |
High Precision Total Scattering |
High Frequency Time-Resolved |
Energy (keV) |
20 – 140 |
20 – 140 |
60 – 140 |
20 – 140 |
Primary Optics |
LLM/DMLM |
LLM/DMLM/Pink |
LLM/DMLM |
LLM/DMLM |
Secondary Optics |
TF/CRL/KB |
- |
TF |
TF/CRL/KB |
Beam size |
|
|
|
|
Vertical (µm) |
0.3 – 20 |
< 6 |
100 – 200 |
15 – 200 |
Horizontal (µm) |
0.3 – 50 |
< 8 |
100 – 200 |
20 – 200 |
Spatial Resolution |
|
|
|
|
Vertical (µm) |
> 0.3 µm |
0.6/1.4/3.1 |
- |
|
Horizontal (µm) |
> 0.3 µm |
0.6/1.4/3.1 |
- |
|
Detector |
Pilatus/Maxipix |
Imaging Detectors |
Pilatus |
Pilatus/Maxipix |
Goniometer |
HR |
HR |
HR/HL |
HR/HL |
X-ray diffraction detectors
EH3 is equipped with a Dectris Pilatus3 X 2M utilising a CdTe sensor. This detector gives unprecedented data quality at high energy, as can be seen in the comparison of its characteristics with respect to a conventional flat panel detector such as the commonly used Perkin Elmer XRD 1621, and in the comparison between data taken in identical conditions with the two detectors.
|
Pilatus3 X CdTe 2M |
Perkin Elmer XRD 1621 |
Detection technology |
Hybrid photon counting |
Flat panel |
Sensor material |
CdTe |
CsI |
Pixel size [µm2] |
172⨯172 |
200⨯200 |
Total number of pixels (H ⨯ V) |
1475⨯1679 |
2024⨯2024 |
Maximum frame rate (Hz) |
250 (500 with ROI) |
15 (30 with 2⨯2 binning) |
Point Spread Function (FWHM) |
1 pixel |
2 pixels |
Energy threshold (keV) |
8 – 40 |
none |
Maximum count rate (ph/s/pixel) |
5⨯106 |
Integrating detector |
Non linearity |
< 2% at 106 counts/s/pixel |
|
Counter depth |
20 bit |
16 bit |
Dynamic range |
20 bit |
12.8 bit |
Minimum exposure (ns) |
200 |
3.3⨯107 |
Image lag |
0 |
~1% after 100ms |
Readout time |
0.95 ms |
|
File format |
CBF, HDF5 |
Multiframe EDF |
X-ray imaging detectors
A range of imaging cameras are available for experiments which require complimentary absorption tomography. These detectors are permanently mounted and can be used sequentially with the diffraction and/or SAXS detector and one another. The detectors system characteristics are listed below.