10.1021/jz2008209.s001
Jiajun Chen
Jiajun
Chen
Jianming Bai
Jianming
Bai
Haiyan Chen
Haiyan
Chen
Jason Graetz
Jason
Graetz
In Situ Hydrothermal Synthesis of LiFePO<sub>4</sub> Studied by Synchrotron X-ray Diffraction
American Chemical Society
2015
reaction conditions
synthesis reactions
lithium battery materials
battery electrodes
reaction kinetics
LiFePO 4 Studied
Situ Hydrothermal Synthesis
hydrothermal conditions
LiFePO 4
formation
Li battery electrode materials
particle size
lattice parameters
synthesis procedures
Bragg reflections
synthesis conditions
antisite defects
2015-12-16 19:40:05
Journal contribution
https://acs.figshare.com/articles/journal_contribution/In_Situ_Hydrothermal_Synthesis_of_LiFePO_sub_4_sub_Studied_by_Synchrotron_X_ray_Diffraction/2016552
The development of high capacity, safe lithium battery materials requires new tools to better understand how reaction conditions affect nucleation and crystallization, particle size, morphology, and defects. We present a general approach for studying the synthesis of Li battery electrode materials in real time. The formation of LiFePO<sub>4</sub> was investigated by time-resolved in situ synchrotron X-ray diffraction under hydrothermal conditions, and the reaction kinetics were determined by changes of the Bragg reflections. We provide the first evidence in support of a dissolution–reprecipitation process for the formation of LiFePO<sub>4</sub>, which occurs at temperatures as low as 105 °C and appears to be a three-dimensional diffusion-controlled process. Lattice parameters and their evolution were monitored in situ, as well as the formation of antisite defects and their subsequent elimination under various synthesis conditions. The ability to characterize and tailor synthesis reactions in situ is essential for rapid optimization of the synthesis procedures and, ultimately, the development of new battery electrodes.