LIFEPO4 WITH AN OLIVINE STRUCTURE HAS ATTRACTED EXTENSIVE INTEREST AS A POTENTIAL CATHODE MATERIAL FOR LITHIUM-ION BATTERIES. BECAUSE LIFEPO4 IS AN ENVIRONMENTALLY FRIENDLY AND SAFE LITHIUM-ION BATTERY CATHODE MATERIAL, HIGH STABILITY, LOW COST AND THEORETICAL CAPACITY (170 MA.H G-1) IT IS ALSO MUCH LESS TOXIC THAN LICOO2 OR LINIO2. LIFEPO4 WITH AN OLIVINE STRUCTURE IS DIFFICULT TO ATTAIN ITS FULL CAPACITY BECAUSE ITS ELECTRONIC CONDUCTIVITY IS VERY LOW, WHICH LEADS TO INITIAL CAPACITY LOSS AND POOR RATE CAPABILITY, AND DIFFUSION OF LI+ION IN THE OLIVINE STRUCTURE IS SLOW. THERE ARE TWO METHODS TO IMPROVE THE ELECTRONIC CONDUCTIVITY. ONE METHOD IS TO INTRODUCE CONDUCTIVE ADDITIVES INCLUDING CARBON COATING AND SUPERVALENT CATION DOPING. ANOTHER METHOD IS TO CONTROL THE PARTICLE SIZE BY OPTIMIZING THE SYNTHESIS CONDITIONS. THE MAIN OBJECTIVE OF THIS RESEARCH IS TO PREPARE LIFEPO4 NANOPARTICLES WITH HIGH CRYSTALLINITY AND PROPER ELECTRONIC CONDUCTIVITY BY THE PULSED CURRENT ELECTROCHEMICAL METHOD AS A CONFIDENT WAY FOR CONTROLLING PARTICLES SIZES BY OPTIMIZING THE SYNTHESIS CONDITIONS. THE EFFECTS OF CURRENT AMPLITUDE, PULSE TIME, RELAXATION TIME, AMMONIUM PHOSPHATE CONCENTRATION, LITHIUM NITRATE CONCENTRATION, AND SYNTHESIS TEMPERATURE WERE INVESTIGATED AND OPTIMIZED TO OBTAIN A UNIFORM LIFEPO4 NANOPOWDER. AT FIRST, THE SOLUTION INCLUDING LINO3 AND NH4H2PO4 WITH DIFFERENT MOLAR RATIOS WERE PREPARED. IRON (II) IONS WERE HOMOGENOUSLY INTERRED INTO THE SOLUTION BY DIRECT OXIDATION OF IRON ANODE BY EXERTING CURRENT PULSES TO FORM LIFEPO4. THE MORPHOLOGY, PARTICLES SIZES AND THE COMPOSITION OF THE SAMPLES WERE ANALYZED BY SEM AND XRD. THE OBTAINED RESULTS SHOWED THAT THE OPTIMIZED LIFEPO4 SAMPLE INCLUDES UNIFORM CRYSTALLINE NANOPARTICLES WITH 20 NM AVERAGE DIAMETER.