Abstract. LiFePO 4 precursor is produced in planetary milling with LiOH·H 2 O, H 3 PO 4 , Fe 2 O 3 and sucrose, which is characterized by X-ray diffraction, scanning electron microscope(SEM), laser particle size analyzer (LPSA). The results showed that the particle size was submicron level, the LPSA data showed that there was double peak of the sample, which the big one appeared around 0.66 ȝm and the small one appeared around 1.71 ȝm and the positions did not change with the change of parameters. The mixture was conductive to obtain narrow-size-range LiFePO 4 .