X-ray diffraction and scattering measurements can be carried out on a range of samples types – powders, single crystals, thin films and in some cases non-crystalline samples (SAXS). These data can be used to identify the crystalline phases present (material characterisation, mineralogy, comparison of bulk sample with single crystal data), crystallography to determine and/or refine structures. Thin films can be studied for phase identification, grazing incidence XRD for thickness of layers, X-ray reflectometry (XRR). Reciprocal space mapping of epitaxial samples. Changes in structure can also be monitored with in-situ non-ambient studies.
Both single crystal and powder X-ray diffraction facilities are available to researchers across the University through a mix of a service and open access to trained users.
A Rigaku XtaLAB Synergy-ED electron diffractometer will be installed early in 2024 adding electron diffraction facilities.
The powder diffraction facilities consist of a Malvern Panalytical Empyrean multi-purpose platform equipped with Cu sealed tube X-ray source, multicore iCore/dCore motorised optics, hybrid monochromator, focussing mirror and PIXcel3D detector.
Many configurations are available including:
Reflection and transmission geometry with 45-position sample changer
Grazing Incidence XRD , X-ray reflectometry (thin films)
Anton-Paar XRK900 non ambient chamber 25 <T <900 °C under gas flow
Basic SAXS measurements
We also have a Rigaku MiniFlex benchtop diffractometer equipped with Cu sealed tube X-ray source and 6-position sample changer and an X’Pert PRO MPD also with Cu sealed tube source and monochromator.
In general, these instruments are used by research workers collecting and analysing their own data, booked through an online booking system but we’re also happy to collect data and assist with analysis where there are small numbers of samples or infrequent use.
Single Crystal X-ray diffraction
Single crystal diffraction can be used to experimentally determine the solid state structure of a crystalline material – molecular or non-molecular e.g. molecular compounds, inorganic materials, framework materials such as MOFs. The precise coordinates of the atoms in the structure allow calculation of bond lengths and angles, torsion angles and also information on the crystal packing and intermolecular interactions present in the structure. The relative configuration for structures can structures containing stereo centres can be routinely determined and we can determine the absolute configuration of enantiomerically pure material, including lighter atom materials (using Cu radiation where necessary). For less frequent users a full structural analysis service is provided – carrying out all steps beyond crystal submission through data collection, structure solution and refinement to the production of publication materials where possible. For researchers who routinely need single crystal data, training and support is provided to allow collection and analysis of their own structures.
We have a Bruker D8 Venture kappa geometry diffractometer equipped with a Photon-II CPAD detector and dual (Cu and Mo) ImS 3.0 microfocus sources equipped with an Oxford Cryosystem Cryostream 1000 low temperature device (80-500K).
In addition to the facilities in the School of Chemistry we have an allocation with the National Crystallography Service, based in Southampton (http://www.ncs.ac.uk/) which has very powerful in-house equipment and regular access to synchrotron facilities at Diamond Light Source, allowing data to be collected from much smaller and/or weakly diffracting samples.
Please contact Dr Claire Wilson Claire.email@example.com (Room B2-27b, 0141-330-3214) if you are interested in using the crystallography/diffraction facilities, would like further details or access to any these facilities.