In Situ Insights into Cathode Calcination: A multimodal Assessment of the Crystallization Process of LiNiO₂

Calcination is a crucial step in the solid-state synthesis of metal oxides, finding applications not only in manufacturing of cathode materials for batteries but also across various industrial sectors. However, the inherent complexity associated with the process, involving elusive kinetic intermediates, hindering in-depth understanding and predictive control over the production of high-performance metal oxide materials. In this presentation, we report our in-situ analysis of the calcination process of LiNiO2, a potential high-performance cathode for Li-ion battery, to assess the course of crystallization and phase progression vs temperature and time. The composition phase evolution diagrams derived from quantitation Rietveld analysis over in-situ XRD patterns, extracted with multivariate curve resolution (MCR) fitting of the in-situ XAS data, simulated with a phase-field based continuum model, and constructed by using a cosine similarity based automated data analysis as an in-line tool for process monitoring, are examined individually and compared with each other to draw new insights over the calcination process in order to establish optimized processing parameters.