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Joe Hriljac, Science Group Leader

The Crystallography Science Group comprises the High Resolution Powder Diffraction beamline (I11), the Extreme Conditions beamline (I15), the X-ray Pair Distribution Function (XPDF) beamline (I15-1), and the Small-Molecule Single-Crystal Diffraction beamline (I19). Bringing these beamlines together into one science group means we can fully exploit the technical and scientific expertise within its teams to provide the basis for future development and pioneering experiments. The coming year will see many beamline upgrade projects, with the aim to further develop our tools, data analysis pipelines and strategic planning for the Diamond-II upgrade.

I11 update

: Senior Support Scientist Sarah Day working on the LDE battery pouch cell experiment on I11.

The high brightness beamline uses monochromatic X-rays in the range of 6 - 25 keV for high-resolution and time-resolved powder diffraction experiments in the first Experimental Hutch (EH1) or for Long Duration Experiments (LDEs) in EH2. Thanks to our dedicated beamline staff, I11 has continued to efficiently deliver beamtime, facilitating experiments to the busy user programme throughout the year, in particular for non-ambient applications and experiments requiring unusual hardware setups such as toxic/corrosive gas absorption studies at cryogenic temperatures, resonant diffraction at high temperature and time-resolved in operando lithium-ion (Li-ion) battery work. The continued success in terms of high quality research is clearly evidenced from record publications output, with an increase of 40% compared to the previous period.

As the I11 facility has now been running for more than 10 years, the main components of the original design such as the monochromator (DCM), diffractometer and X-ray source (in vacuum undulator), are starting to show signs of wear. We have therefore developed an upgrade plan, endorsed by the Scientific Advisory Committee (SAC) and the Diamond Industrial Science Committee (DISCo) at the end of 2017 to replace these components in order to maintain our competitiveness. The construction of the new high stability DCM and the high-energy cryo-cooled undulator have already started and should be complete and ready for installation next year. We have also completed the design/specification for a new diffractometer, which will be delivered for installation late autumn. Finally, improvements of the detection systems (MAC and PSD) and the replacements of existing sample environments are also included in the project.

Bringing these beamlines together into one science group means we can fully exploit the technical and scientific expertise within its teams to provide the basis for future development and pioneering experiments.

I15 update

: Joe Hriljac, appointed Crystallography Science Group Leader in March 2019.

The Extreme Conditions beamline, I15, employs high energy X-rays to explore the structure of materials at high pressures, high and low temperatures, as well at other in situ and in operando conditions. The beamline receives an X-ray continuum from the superconducting wiggler; this allows for experiments which require monochromatic X-rays between 20 and 80 keV, as well as polychromatic beam. I15 was originally designed to serve the mineral physics community, which it has while also assisting material scientists, chemists and solid state physicists with their structural investigations, at pressure or otherwise.

I15 continues to offer capabilities and support that few extreme conditions beamlines do. I15 users have pre–experiment access to bespoke assistance and training from our highly skilled staff in diamond anvil cell (DAC) preparation and loading, as well as the loaning of DACs for I15 experiments. The high pressure gas loader available at I15 offers users the choice of many possible gases to use as their pressure transmitting media (PTM), allowing them to optimise for hydrostaticity with helium or neon, or choosing a PTM based on desired interactions with the sample at pressure. The recent addition of the laser heating system adds a further unique capability – the I15 system is capable of quickly ramping the laser power to perturb a sample without delivering too much heat to the bulk. The I15 team are actively working on the future development plans for the beamline.

I15-1 update

: The I15 and I15-1 beamlines team and support group, clockwise from top left: Annette Kleppe, Maria Diaz Lopez, Philip Chater, Stuart Gurney, Dean Keeble, Dominik Daisenberger, Christine Beavers (PBS), Lawrence Gammond, Allan Ross, Volodymyr Khotkevych.; The I15 and I15-1 beamlines team and support group, clockwise from top left: Annette Kleppe, Maria Diaz Lopez, Philip Chater, Stuart Gurney, Dean Keeble, Dominik Daisenberger, Christine Beavers (PBS), Lawrence Gammond, Allan Ross, Volodymyr Khotkevych.

The XPDF beamline, I15-1, is dedicated to producing high quality X-ray scattering data for Pair Distribution Function (PDF) analysis. Operational since 2017, I15-1 has illuminated samples from diverse fields, from Earth sciences to pharmaceuticals, as well as material science and chemistry. XPDF receives X-rays from the inside edge of the wiggler fan, and this light is monochromated and directed to the end station in three energies: 40, 65 and 76 keV. PDF data are collected at high energies to produce the low sample absorption and high Q range required for successful interpretation. Gaining structural information on amorphous samples is a primary goal of many XPDF experiments, but crystalline samples can also display local structure variations such as defects and disorder, which can be observed with PDF analysis.

Consisting of a sample position, with an optional sample changing magazine, and two large area detectors, the end station is highly flexible and has been adapted to many in situ and in operando experiments, including variable temperature, gas flow, hydrothermal synthesis and electrochemical cycling. For more routine measurements, the 15 position sample changer has been a popular choice, allowing automatic data collection. A further automation improvement is currently underway; in spring 2020, a sample changing robot and an upgraded detector will be installed on I15-1. This upgrade will be a synergistic addition to the existing auto processing infrastructure, and will allow users to collect better data with less manual intervention.

I19 update

The Small-Molecule Single-Crystal Diffraction beamline, I19, uses X-rays in the 5 – 25 keV energy range to determine the structures of small-molecule systems with single-crystal diffraction techniques. This can be for characterisation of novel molecular materials or for investigating the variation in the structure of a crystalline material under an external physical influence such as change in temperature, the exposure to a gas, photo-excitation or through the application of high-pressure.

The use of the robotic sample changer, and remote access, is now well established in Experimental Hutch 1 (EH1) of the beamline, where pre-mounted samples are sent to Diamond under cryogenic storage and users then run their beamtime from their home institutions. This mode of operation makes it possible to carry out chemical crystallography studies in a more responsive manner as beamtime can be scheduled in more regular, and shorter, periods. From AP25 we will schedule individual shifts, rather than whole one-day (three shifts) blocks of beamtime, for those wishing to run their beamtime via the remote access route. For Experimental Hutch 2 (EH2) we have recently developed a cell which allows a high static electric field to be applied to the sample crystal. The application of electric fields to materials can result in a variety of responses that may have important technological applications, spanning electronic and ionic conductivity to piezo- and ferro-electricity.

In the near future, the control system for the Newport 4-circle diffractometer, housed in EH2, will be changed. This will not only improve the reliability of the instrument but will provide the foundation of further developments which will improve ease of use and allow better integration into the beamline’s infrastructure. More significantly, perhaps, at the start of AP25 we will upgrade the monochromator to provide greater beam stability and allow data collections to be performed more quickly. The monochromator upgrade also promises a more automated approach to wavelength changes and will provide users a more direct control of this for the first time.

Diamond Light Source is the UK's national synchrotron science facility, located at the Harwell Science and Innovation Campus in Oxfordshire.

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Diamond House
Harwell Science & Innovation Campus
Didcot
Oxfordshire
OX11 0DE

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