A multi-sample automatic system for in situ electrochemical X-ray diffraction synchrotron measurements

J Synchrotron Radiat. 2007 Nov;14(Pt 6):487-91. doi: 10.1107/S0909049507039209. Epub 2007 Oct 13.

Abstract

An automatic system that allows continuous in situ electrochemical X-ray diffraction measurements has been developed and implemented at the MS-X04SA beamline at the Swiss Light Source. The system consists of an automatic sample changer, improved ;coffee bag' electrochemical cells, and simple control software. The sample changer can sequentially move up to 32 electrochemical cells into the beam. For each cell an independent electrochemical program is possible. The MYTHEN microstrip detector at the beamline enables parallel detection of diffracted X-ray beams and, thus, fast data acquisition, along with a high 2theta resolution. In this communication the set-up is presented on two typical examples from the field of lithium-ion batteries, (i) structural changes in a layered LiCoO(2) positive electrode upon battery charging and (ii) the effect of co-intercalation of ionic liquids into the graphite negative electrode.