Journal
JOURNAL OF PHYSICAL CHEMISTRY LETTERS
Volume 2, Issue 15, Pages 1874-1878Publisher
AMER CHEMICAL SOC
DOI: 10.1021/jz2008209
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Funding
- U.S. Department of Energy (DOE) with Laboratory Directed Research and Development at Brookhaven National Laboratory (BNL) [DE-AC02-98CH10886]
- U.S. DOE, Office of Basic Energy Sciences
- U.S. DOE, Office of EERE through the ORNL's High Temperature Materials Laboratory
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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 LiFePO4 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 LiFePO4, which occurs at temperatures as low as 105 degrees 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.
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