INDUSTRY

December 2022 ESRFnews

High photon-flux inspires the chemical company BASF to analyse battery samples at unprecedented speed. It was just before the coronavirus pandemic that a battery specialist at BASF cornered Bernd Hinrichsen about X-ray diffraction at the German multinational s Ludwigshafen headquarters. He said, how could we cope with 1000 samples a week? recalls Hinrichsen, BASF s research manager. It was not something we wanted to do with our lab instrumentation. But I had been following the EBS upgrade at the ESRF, and the higher X-ray brilliance. I thought, this could be one killer application for all those photons coming out of the tube. Although he has been at BASF for

12 years, Hinrichsen himself has a PhD in X-ray diffraction, and spent his early career running the company s X-ray diffraction laboratory. He approached the ESRF s head of the Business Development Office (BDO), Edward Mitchell, who proposed a first meeting with BASF s specialist in automation, Peter Welter, as well as several ESRF staff: Yves Watier of the Sample Environment Support Service (SESS); Jérôme Kieffer of the Instrumentation Services and Development Division; Veijo Honkimäki, Andy Fitch and Carlotta Giacobbe of the ID31, ID22 and ID11 beamlines, respectively; and Ennio Capria, also of the BDO. Now, after less than three years development during a global pandemic, driven by the ESRF s sample environment service, ID31 team and BDO, and with help from the STREAMLINE project (funded by the European Commission), they have a solution and it is better than Hinrichsen had expected.

Bespoke design It consists of a 3D-printed motorised sample changer and a number of holders, designed by Johannes Frey of the SESS for the ID31 beamline (which Hinrichsen jokes resembles the Parthenon of Greece, due to the granite pillars supporting the detector for wide-angle X-ray scattering). The

holders look like short rulers, and can hold up to 16 samples each. In tests, it took just one second to collect data via X-ray powder diffraction (XRPD) for each sample, and less than one- tenth of a second to switch between samples. Collecting data of similar noise-to-signal quality would take a week back at the lab, according to Hinrichsen. The speed, the low level of noise, is astounding, he says. Hinrichsen expects that BASF

scientists will be able to collect data for 1000 samples in an hour or two. Ultimately it will be a mail-in service,

Industry asks, ESRF delivers

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whereby his battery colleagues package their samples securely, post by courier, and download the data remotely when they are ready. The BASF researchers are particularly interested in nickel-manganese- cobalt cathodes for high-energy, high- power batteries. There are a lot of synthesis parameters that they want to optimise, Hinrichsen explains. We re on the verge of doing this routinely, perhaps once a week, or once every other week. 

Jon Cartwright

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The motorised sample changer on ID31 should help BASF collect data for 1000 samples in less than two hours.

The speed, the low level of noise, is astounding