Systematic experiments were performed on the synthesis of nano-structured LiFePO4 by the solvothermal route using different reaction times of 2, 8, 16, and 36 h at a moderate temperature of 240. C. The physical, chemical and electrochemical properties of the LiFePO4 samples were investigated by powder X-ray Diffraction, field-emission SEM/TEM, inductively coupled plasma atomic emission spectrometry (ICP-AES), particle size distribution measurement, and galvanostatic tests. The crystal growth mechanism during the solvothermal reaction was deemed to consist of four stages, viz. the dissolution of the precursor and nucleation, growth and aggregation, partial dissolution, and complete crystallization. (C) 2012 The Electrochemical Society. [DOI: 10.1149/2.108204jes] All rights reserved.