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SIC synchrotrons

Electrocatalysis experiments at PETRA III

Dorotea, Harald and Lindsay were at the PETRA III synchrotron in Hamburg last week, making high-energy surface X-ray diffraction measurements on model electrocatalysts – simplified materials that should help us understand how to improve the performance of electrolyzers and fuel cells. The experiments were part of a collaboration with Prof. Gary Harlow from the Oregon Center for Electrochemistry at the University of Oregon (go Huskies!). The X-ray measurements were made at the Swedish Materials Science beamline P21. Also joining the experiment was Andrea Grespi, PhD student from Lund University.

View across the “Max von Laue” ring hall at the PETRA III synchrotron, Hamburg, Germany.
Samples were initially prepared at the DESY Nanolab (thanks Heshmat and colleagues!) before transferring to the synchrotron for measurements. Dorotea was in charge of this part of the experiment. Here she is moving the freshly-prepared sample (which you can’t see) through the ultra-high vacuum system.
The samples are very delicate, so we try to avoid exposure to too much air. Here’s the improvised solution for this experiment: a bag sealed around the entry door to the vacuum system. The bag is filled with dry nitrogen and the sample transferred into an airtight jar, which we can then take to a proper glove box to load into the electrochemistry cell.
After getting the sample loaded into the electrochemistry cell (the beige thing on the pedestal here with tubes coming out), this is mounted at the X-ray beamline for measurements. Here you see the setup almost ready; Gary is adjusting the camera we use to monitor the surface of the sample during measurements.
Gary and Harald watching as the X-ray diffraction data come in.
X-ray diffraction pattern from the sample, which is a material only a few atomic layers thick. The pattern of spots tells us about the atomic structure, and we can follow changes in real time while we change the conditions.

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