New high-throughput X-ray powder diffraction system on ID31

X-ray powder diffraction (XRPD) is one of the essential techniques for the structural characterisation of materials and, in particular, is fundamental for scientists researching advanced battery materials. Thanks to the ESRF’s Extremely Brilliant Source (EBS), the acquisition time for XRPD measurements can be reduced down to seconds (depending on the sample), compared to one day using conventional laboratory sources. In this context, an automated, high-throughput sample treatment system was necessary to adapt to faster experiments.

Within the STREAMLINE project (funded by the European Commission under grant agreement no. 870313 / Sustainable research at micro and nano X-ray beamlines) and in collaboration with an industrial partner (BASF Ludwigshafen, Germany), the ESRF Business Development Office, Sample Environment group and beamline scientists, a robotic sample-changing system has been developed for high-throughput XRPD measurements (Figure 1), making it possible to measure several thousand samples a day.
 

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Fig. 1: The high-throughput XRPD sample system installed at beamline ID31.

To take full advantage of the ESRF-EBS and to satisfy the demand from industry, the sample changer was designed with the following specifications: fast change from one sample to the next; an automatic identification labelling system for each sample and its results; fluidisation of the powder and the capacity to run up to 1056 samples autonomously. The device was created, assembled and installed at beamline ID31.

 A standardised, lightweight sample holder was designed and produced as a low-cost, injection-moulded part. The holder can contain 16 samples in small, individual chambers, each with its own QR code. Each sample can be moved inside its chamber when a vibration is applied to fluidise the powder during data acquisition. Injection-moulded clips hold two 50-µm Kapton window foils to sufficiently seal each chamber so that no powder can escape while the holder is transported and shaken.

The sample holder is inserted into the device's charging mechanism with all the samples organised and identifiable. A motor moves the sample holder into place as a QR code camera recognises the samples, applies vibration and initiates data acquisition all at once. It takes about 95 ms to move the sample and read the QR code while the sample holder is vibrating. The sample holder is ejected into a tray after the 16 samples are measured (18 seconds for a 1-second acquisition time per sample), and the subsequent samples are loaded. In this way, the system can fully automatically measure up to 66 sample holders (1056 samples) within less than one hour, depending on the chosen acquisition time.

The video below illustrates the process.

After collecting the raw data, an automated azimuthal integration is applied, and everything is stored in a folder within a hdf5 file with a name generated automatically from the sample QR code, allowing the user to download it remotely after the experiment.

In addition to the new, high-throughput system, a mail-in sample service will be established in order to speed up the experiments even further. The service is already in demand, with industrial user BASF planning to send up to 1000 samples per week to be analysed for its recently launched battery research laboratory.