A VARIETY OF METHODS ARE AVAILABLE FOR THE PREPARATION OF NANOPARTICLES: SOL-GEL, THERMAL DECOMPOSITION, VAPOR CONDENSATION, REVERSE MICELLE OR MICRO EMULSION, HIGH-ENERGY BALL MILLING, ULTRASONIC SHOT PEENING, LITHOGRAPHY, VAPOR DEPOSITION AND electrochemical SYNTHESIS. ELECTROCHEMISTRY HAS NOT BEEN EMPLOYED AS A MEANS OF PREPARING LARGE NUMBERS OF METAL NANOPARTICLES, BUT SOME ADVANTAGES OF electrochemical METHODS OVER CHEMICAL ONES IN SYNTHESIS OF SMALL METAL PARTICLES ARE THE HIGH PURITY OF THE PARTICLES, THE POSSIBILITY OF A PRECISE PARTICLE SIZE CONTROL, DIRECT SYNTHRSIS ON ELECTRODE.IN THE PRESENT WORK, MOLYBDENUM OXIDE NANOPARTICLES WERE SYNTHESIZED BY DIFFERENT electrochemical METHODS INCLUDING GALVANOSTATIC, POTENTIOSTATIC AND CYCLIC VOLTAMMETRIC METHODS FROM AQUEOUS MOLYBDATE SOLUTION ON POLYPYRROLE, PPY. PPY WAS SYNTHESIZED FROM PYRROLE, GALVANOSTATICALLY ON ST-12 STEEL. THE RESULTING NANOPARTICLES WERE CHARACTERIZED BY SCANNING ELECTRON MICROSCOPY, SEM, AND ENERGY-DISPERSIVE X-RAY SPECTROSCOPY, EDX.THE CATALYTIC PERFORMANCE OF THESE LAYER BY LAYER ASSEMBLIES ON METHANOL ELECTRO-OXIDATION REACTION WAS STUDIED BY electrochemical METHODS.