Scientists working at the ESRF and BASF have teamed up to co-develop a new service for automated characterisation of solid-state materials such as battery materials. This development aims to enable routine analysis of hundreds of samples per shipment.
Amongst its many activities, the Horizon2020 “Streamline” project is helping the ESRF to develop new services for its users aiming to take advantage of the ESRF’s new Extremely Brilliant source (ESRF-EBS). The capacity at the beamlines could be increased through automation of experiments for fast characterisation methods by using sample changers, workflows to control the beamline and eventually automated data analysis. Such developments have already been proven at the structural biology beamline MASSIF-1 (ID30-A1), which routinely analyses hundreds of protein crystal samples per day.
Scientists at BASF are implementing automation for sample preparation and analysis for their in-house characterisation techniques. Bernd Hinrichsen, responsible for the X-ray diffraction laboratory at BASF, saw the need for a service going beyond their in-house capabilities and that combined X-ray powder diffraction and PDF analysis and started discussions with the ESRF to learn about feasibility.
Bernd told us about the origin of the idea, “BASF produces lots of samples for analysis, and I noticed the demand for characterisation increasing in particular for battery materials and nano-materials such as catalysts. Although we have extensive characterisation facilities in our labs, I thought we could get better results by using synchrotron techniques that provide higher resolution.”
Within Streamline, three X-ray characterisation techniques had already been earmarked for development into high-throughput services, one of which was powder diffraction. A focus group was organised early in 2020 to discuss combining the ambitions of Streamline with BASF’s understanding of the real needs of industry researchers, with Bernd as the invited expert. With colleagues at BASF, Bernd has defined the specifications for the powder diffraction service, targeting samples in batches of 100, with expectations of a characterisation series reaching up to 500 samples per shipment, thus setting a target for the capacity of a sample changer.
Beamlines ID11, ID22 and ID31 were tested for data collection using a predefined set of samples. Carlotta Giacobbe, Scientist at ID11, took in charge the series of tests. Carlotta reported, “All beamlines provided very high-quality data, and finally we chose beamline ID31 for further development based on the rapidity of data collection revealed by the tests and the ease of building automation within its open and flexible sample environment”.
Designs and prototype sample holders have been produced by the engineers of the ESRF Sample Environment Group in collaboration with BASF. Bernd commented, “the final model is very small compared to those previously used in our labs, and the need for less than 100 mg of sample will be welcomed by the researchers making the materials”. An equivalent commercially-available model has been identified to ensure a reliable supply that would be available to all users.
A design prototype for the sample changer has also been made by ESRF’s Johannes Frey and his intern Laura Jarnias. This will be tested shortly at the beamline to see how well it performs. The design had to fulfil multiple requirements: ensure reproducible positioning of the sample at the beam position in an easy and quick manner, exchange samples at the speed of about one per second. Bernd is very positive about the design, and gave his outlook for the tests, “The beamline tests will prove the quality that we will be able to achieve with the EBS, the beamline’s optics and the EIGER detector. Although powder diffraction does not pose the biggest experimental challenges, the synchrotron’s high monochromaticity and a tiny beam footprint on the detector will improve significantly on typical home lab capabilities. Our goal is to achieve data quality that is better in all respects to a home lab setup, paired with easy accessibility. I believe that, by the end of the year, we will be able to collect hundreds or even thousands of powder diffraction patterns within an hour.”
The sample changer will be optimised and thoroughly tested within the Streamline project. Eventually, a new mail-in service will be created for the benefit of all users, both academic and industrial.
BASF at the ESRF on 28 January 2020 (From left to right, upper row: A. Fitch, E. Capria, P. Welter, Y. Watier, V. Honkimaki; lower row: E. Mitchell, B. Hinrichsen, J. Kieffer, C. Giacobbe).