Lithium cobalt phosphate (LiCoPO₄, LCP), having a high operating potential (4.8 V vs. Li/Li+), a flat voltage profile and a good theoretical capacity (167 mAh/g), is considered a promising cathode material for improving the energy density of lithium-ion batteries (LIBs) [1] [2]. Here we report a category of method for synthesizing LCP, the solvothermal (ST) method with a binary solvent (deionized water: ethyl alcohol = 1:1), controlling the concentration of cobalt ion in 0.05 mol/L (ST-0.05) and 0.25mol/L (ST-0.25). The material phase was apparently identified via X-ray diffraction (XRD). Observed by scanning electron microscopy (SEM), the grain size of LCP powders synthesizing by solvothermal method with two kinds of the concentration of cobalt ion were 400 × 400 × 1000 nm cuboids (ST-0.05) and 150 × 150 × 250 nm hexagonal prisms containing nanoparticles (ST-0.25), respectively. Discharge capacities of LCP were 76.0 mAh/g (ST-0.05) and 94.5 mAh/g (ST-0.25), in the first cycle at 0.1 C, respectively.