Automating the analysis of micron-scale synchrotron diffraction data on inhomogeneous polycrystalline samples: a solid oxide electrolysis cell case study
A novel approach to post mortem characterisation of electrochemical and photovoltaic devices is spatially-resolved diffraction using a hyper-focused, micron-width x-ray beam to examine the distribution of degradation products and strain, a technique called $μ$-XRD. Aside from the experimental difficulties associated with beam focusing and sample preparation, which are themselves non-trivial, the analysis of resulting data is complex and challenging, with full Rietveld analysis rarely attempted in literature. The difficulty lies in the size of the data, which may consist of hundreds or even thousands of diffraction patterns with very different crystallographic phase compositions depending on position within the device, and the difficulty in fitting the data due to the presence of many phases at the same position, including possible degradation products which may be difficult to index and assign to known phases. In this paper, we present a fully-automated open access Python routine for performing phase identification and Rietveld analysis on 2D datasets of diffraction pattern taken at micron-scale positions, measured over the cross-section of a chemically inhomogeneous device with polycrystalline phases. Solid oxide electrolyser cells are a promising technology for green hydrogen production which can utilise waste heat to split water at higher efficiencies than low-temperature electrolysis techniques such as polymer electrolyte membranes, but exhibit many degradation modes due to the high operating temperatures. We present a case study using our analysis protocol on an SOEC fragment encompassing the air electrode, cation diffusion barrier, electrolyte, and fuel electrode. With modification, this protocol could be applied to other devices such as all-solid-state batteries, wet-electrolyte battery electrodes, solid oxide fuel cells, photovoltaic devices, and metal-oxide pseudocapacitors.