Advanced design of a x-ray absorption spectroscopy setup for measuring transition metals speciation in molten carbonates, hydroxides and hydrogenosulfates

Abstract

Battery recycling is currently becoming a crucial issue. One possible treatment path involves the use of molten salts. A mechanistic understanding of the underlying processes requires being able to analyze in situ speciation in molten salts at various temperatures. This can be advantageously achieved using x-ray absorption spectroscopy, the use of Quick-EXAFS facilities being particularly appropriate. Consequently, this paper presents the design and development of a new setup allowing carrying out Quick-EXAFS experiments in oxidizing molten salts at high temperatures. We describe the different components of a cell and the performance of the heating device. We illustrate the capabilities of the setup by analyzing the temperature evolution of Co speciation upon dissolution of LiCoO₂, a typical battery electrode material, in molten carbonates, hydroxides, and hydrogenosulphates.