%0 Journal Article
%T In situ neutron diffraction to investigate the solid-state synthesis of Ni-rich cathode materials.
%A Goonetilleke D
%A Suard E
%A Bergner B
%A Janek J
%A Brezesinski T
%A Bianchini M
%J J Appl Crystallogr
%V 56
%N 0
%D 2023 Aug 1
%M 37555229
暂无%R 10.1107/S1600576723004909
%X Studying chemical reactions in real time can provide unparalleled insight into the evolution of intermediate species and can provide guidance to optimize the reaction conditions. For solid-state synthesis reactions, powder diffraction has been demonstrated as an effective tool for resolving the structural evolution taking place upon heating. The synthesis of layered Ni-rich transition-metal oxides at a large scale (grams to kilograms) is highly relevant as these materials are commonly employed as cathodes for Li-ion batteries. In this work, in situ neutron diffraction was used to monitor the reaction mechanism during the high-temperature synthesis of Ni-rich cathode materials with a varying ratio of Ni:Mn from industrially relevant hydroxide precursors. Rietveld refinement was further used to model the observed phase evolution during synthesis and compare the behaviour of the materials as a function of temperature. The results presented herein confirm the suitability of in situ neutron diffraction to investigate the synthesis of batches of several grams of electrode materials with well-controlled stoichiometry. Furthermore, monitoring the structural evolution of the mixtures with varying Ni:Mn content in real time reveals a delayed onset of li-thia-tion as the Mn content is increased, necessitating the use of higher annealing temperatures to achieve layering.