Journal article

Publication year: 2023

Pages: 1066-1075

Journal: Journal of Applied Crystallography

Volume number: 56

Issue number: 4

ISSN: 1600-5767

Open access status: Hybrid

DOI Link: https://doi.org/10.1107/S1600576723004909

Publisher: International Union of Crystallography

Abstract: 
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 lithiation as the Mn content is increased, necessitating the use of higher annealing temperatures to achieve layering.

Harvard Citation style: Goonetilleke, D., Suard, E., Bergner, B., Janek, J., Brezesinski, T. and Bianchini, M. (2023) In situ neutron diffraction to investigate the solid-state synthesis of Ni-rich cathode materials, Journal of Applied Crystallography, 56(4), pp. 1066-1075. https://doi.org/10.1107/S1600576723004909

APA Citation style: Goonetilleke, D., Suard, E., Bergner, B., Janek, J., Brezesinski, T., & Bianchini, M. (2023). In situ neutron diffraction to investigate the solid-state synthesis of Ni-rich cathode materials. Journal of Applied Crystallography. 56(4), 1066-1075. https://doi.org/10.1107/S1600576723004909