In Situ Gas Supply System on the Powder Diffraction Beamline I11 at Diamond Light Source

Abstract:

Beamline I11 at Diamond began accepting users for high resolution powder diffraction experiments in Oct 2008. We present the design, key specifications, performance and the hardware of this new beamline which receives an intense and highly collimated x-ray beam generated by an in-vacuum undulator. With the simple optics (a double-crystal monochromator, harmonic rejection mirrors and slits), a high purity beam of low energy-bandpass X-rays optimised at 15 keV is delivered at the sample. The heavy duty diffraction instrument is designed to have the flexibility to house a variety of sample environments and holds two detection systems to collect high quality diffraction data, i.e. multi-analysing crystals (MAC) for high angular resolution experiments and a fast position sensitive detector (PSD) for time-resolved studies. A recent addition to the beamline capabilities is the installation of a specifically designed gas control system. This allows the in-situ dosing of a powder sample with gases such as hydrogen and carbon dioxide, at low (~10 mbar) and high pressures (<100 bar). In addition a low pressure capillary sample cell is described which is now available to users of the beamline.

• Periodical: Materials Science Forum (Volumes 706-709)
• Pages: 1707-1712
• DOI: https://doi.org/10.4028/www.scientific.net/MSF.706-709.1707
• Online since: January 2012
• Authors: J.E. Parker, J. Potter, S.P. Thompson, A.R. Lennie, C.C. Tang
• Keywords: Gas Adsorption, In Situ, Powder Diffraction, Sample Environment, Synchrotron, X-Ray

References

[1] Davis, M.E., Ordered porous materials for emerging applications. Nature, 2002. 417: pp.813-821.

DOI: 10.1038/nature00785

[2] Schlapbach, L. and A. Zuttel, Hydrogen-storage materials for mobile applications. Nature, 2001. 414: pp.353-358.

DOI: 10.1038/35104634

[3] Clausen, B.S., et al., In situ cell for combined XRD and on-line catalysis tests: Studies of Cu-based water gas shift and methanol catalysis. Journal of Catalysis, 1991. 132: pp.524-535.

DOI: 10.1016/0021-9517(91)90168-4

[4] Norby, P., et al., A reaction cell for in-situ studies of hydrothermal titration. Journal of Applied Crystallography, 1998. 31: pp.481-483.

[5] Brunelli, M. and A.N. Fitch, A glass capillary cell for in-situ powder X-ray diffraction of condensed volatile compounds. Solid HCFC-123a and HCFC-124. Journal of Synchrotron Radiation, 2003. 10: pp.337-339.

DOI: 10.1107/s0909049503007969

[6] Chupas, P.J., et al., A versatile sample-environment cell for non-ambient X-ray scattering experiments. Journal of Applied Crystallography, 2008. 41: pp.822-824.

DOI: 10.1107/s0021889808020165

[7] Jensen, T.R., et al., Versatile in-situ powder X-ray diffractions cells for solid-gas investigations. Journal of Applied Crystallography, 2010. 43: pp.1456-1463.

[8] Tang, C.C., et al., Design of powder diffraction beamline (BL-I11) at Diamond. Zeitschrift fur Kristallographie Supplements, 2007. 26: pp.153-158.

DOI: 10.1524/zksu.2007.2007.suppl_26.153

[9] Thompson, S.P., et al., Beamline I11 at Diamond: A new instrument for high resolution powder diffraction. Review of Scientific Instruments, 2009. 80(7).

DOI: 10.1063/1.3167217

[10] Parker, J.E., et al., High-throughput powder diffraction on beamline I11 at Diamond. Journal of Applied Crystallography, 2011. 44: pp.102-110.

[11] Hodeau, J. -L., et al., Nine crystal multi-analyser stage for high-resolution powder diffraction between 6 and 40 keV. SPIE Proceedings, 1998. 3448: pp.353-361.

[12] Thompson, S.P., et al., A Position Sensitive Detector for Fast X-ray Powder Diffraction Experiments Journal of Synchrotron Radiation, 2011 submitted.

[13] Schmitt, B., et al., Mythen detector system. Nuclear Instruments and Methods in Physics Research A, 2003. 501: pp.267-273.

[14] Vitorica-Yrezabel, I.J., et al., Synthesis and polymorphism of (4-ClpyH)2[CuCl4]: solid–gas and solid–solid reactions. CrystEngComm, 2011 accepted.

DOI: 10.1039/c0ce00628a