The synthesis of microsized carbon spheres supporting the semiconductor platinum diphosphide, PtP 2 , was conducted by the thermal decomposition of an organometallic precursor. This novel reaction was carried out using the reaction under autogenic pressure at elevated temperature (RAPET) method by dissociating Pt(PPh 3 ) 4 at 1000°C. The product was characterized using methods of electron microscopy (scanning electron microscope (SEM), transmission electron microscope (TEM), selected area energy dispersive spectroscopy (SAEDS), elemental analyzer (EA) and energy dispersive X-ray analysis (EDX)) and powder-XRD. Transmission electron microscope images indicate that the particle size of the nanoparticles of PtP 2 coated on the carbon spheres is 50nm.