Real-time X-ray analytical micro-furnace technique for in situ phase formation analysis during material synthesis

Abstract

The monitoring of real-time reaction mechanisms can provide authentic structural information related to the prepared materials. This study reports the development of a novel real-time X-ray analytical micro-furnace (RT-XAMF) technique, which is applied during the synthesis of LiNi0.8Co0.15Al0.05O2 to monitor the phases present between 30 and 850 degrees C. To ensure stable temperature control during heating and ensure the practicality of the RT-XAMF technology, an insulating block was developed that allowed a small temperature tolerance of +/- 0.5 degrees C up to 1000 degrees C. Detailed information was gathered regarding the optimal heat treatment conditions for layered structure formation, and in the Li-excess LiNi0.8Co0.15Al0.05O2 electrode material, high charge and discharge capacities were obtained. The formation of a layered structure was monitored upon mixing various lithium salts (LiOH center dot H2O, Li2CO3, LiNO3, and LiF) with the Ni0.8Co0.15Al0.05(OH)(2) precursor. Our results indicate that this RT-XAMF technology can be applied in the development of metal oxides and ceramic materials.