AI 中文总结
本文提出一种自动化开源Python程序，用于分析非均匀多晶器件的微米级同步辐射衍射数据，以固体氧化物电解池为案例验证，该协议经修改可应用于多种电化学器件。
AI 中文摘要
电化学与光伏器件的一种新颖尸检表征方法是空间分辨衍射，采用超聚焦的微米级X射线束来检测降解产物与应变的分布，该技术称为μ-XRD。除了光束聚焦和样品制备本身的重大实验困难外，所得数据的分析也复杂且具有挑战性，文献中很少尝试进行完整的Rietveld分析。困难在于数据规模，其可能包含数百甚至数千个衍射图谱，根据器件内位置的不同，具有截然不同的结晶相组成；还在于数据拟合的难度，因为同一位置存在多个相，包括可能难以索引并归为已知相的降解产物。本文中，我们提出了一种完全自动化的开源Python程序，用于对在微米级位置采集的衍射图谱二维数据集进行相识别和Rietveld分析，这些数据集是在具有多晶相的化学非均匀器件横截面上测量的。固体氧化物电解池（SOEC）是一种有前景的绿色制氢技术，可利用废热分解水，效率高于聚合物电解质膜等低温电解技术，但因高工作温度表现出多种降解模式。我们使用我们的分析协议对包含空气电极、阳离子扩散阻挡层、电解质和燃料电极的SOEC碎片进行案例研究。经修改后，该协议可应用于其他器件，如全固态电池、湿电解质电池电极、固体氧化物燃料电池、光伏器件和金属氧化物赝电容器。
英文摘要
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.
CommentsIn review
