LiCoPO4/C nanocomposites could be prepared by a combination of spray pyrolysis and wet ball-milling followed by heat treatment. The effect of spray pyrolysis temperature on physical and electrochemical properties of the LiCoPO4/C nanocomposites was investigated in the range of spray pyrolysis temperature from 200 to 500 degrees C. Single phase LiCoPO4 olivine structure could be identified by X-ray diffraction analysis for all samples. Scanning electron microscopy observation showed that all samples consisted of approximately 100 nm primary particles. The LiCoPO4/C nanocomposites were used as a cathode active material for lithium batteries, and the electrochemical tests were carried out using the cell Li[1 M LiPF6 in EC:DMC= 1:1] LiCoPO4/C at various charge/discharge rates in a cutoff potential between 2.5 and 5.0 V. The final LiCoPO4/C nanocomposite sample prepared at a spray pyrolysis temperature of 300 degrees C exhibited the best electrochemical performance mainly due to the largest specific surface area, the smallest primary particle size and a well distributed carbon in the composites. The cells exhibited initial discharge capacities of 134 mAh g(-1) 0.05 degrees C, 128 mAh g(-1) at 1 degrees C and 88 mAh g(-1) at 10 degrees C. (C) 2011 Elsevier B.V. All rights reserved.