Connolley Thomas, Magdysyuk Oxana V, Michalik Stefan, Allan Phoebe K, Klaus Manuela, Kamm Paul H, Garcia-Moreno Francisco, Nelson Jennifer A, Veale Matthew C, Wilson Matthew D
Diamond Light Source Ltd, Harwell Campus, Didcot, Oxfordshire OX11 0DE, United Kingdom.
School of Chemistry, University of Birmingham, Haworth Building, Edgbaston, Birmingham B15 2TT, United Kingdom.
J Appl Crystallogr. 2020 Oct 13;53(Pt 6):1434-1443. doi: 10.1107/S1600576720012078. eCollection 2020 Dec 1.
An experimental technique is described for the collection of time-resolved X-ray diffraction information from a complete commercial battery cell during discharging or charging cycles. The technique uses an 80 × 80 pixel 2D energy-discriminating detector in a pinhole camera geometry which can be used with a polychromatic X-ray source. The concept was proved in a synchrotron X-ray study of commercial alkaline Zn-MnO AA size cells. Importantly, no modification of the cell was required. The technique enabled spatial and temporal changes to be observed with a time resolution of 20 min (5 min of data collection with a 15 min wait between scans). Chemical changes in the cell determined from diffraction information were correlated with complementary X-ray tomography scans performed on similar cells from the same batch. The clearest results were for the spatial and temporal changes in the Zn anode. Spatially, there was a sequential transformation of Zn to ZnO in the direction from the separator towards the current collector. Temporally, it was possible to track the transformation of Zn to ZnO during the discharge and follow the corresponding changes in the cathode.
本文描述了一种实验技术，用于在商业电池单元的充放电循环过程中收集时间分辨的X射线衍射信息。该技术在针孔相机几何结构中使用一个80×80像素的二维能量分辨探测器，可与多色X射线源配合使用。这一概念在对商业碱性锌锰AA尺寸电池的同步加速器X射线研究中得到了验证。重要的是，无需对电池进行改装。该技术能够以20分钟的时间分辨率观察空间和时间上的变化（每次扫描收集5分钟数据，两次扫描之间等待15分钟）。由衍射信息确定的电池中的化学变化与对同一批次类似电池进行的互补X射线断层扫描相关联。最清晰的结果是关于锌阳极的空间和时间变化。在空间上，从隔膜到集流体的方向上，锌依次转变为氧化锌。在时间上，可以跟踪放电过程中锌向氧化锌的转变，并跟踪阴极中的相应变化。
