The synthesis of microsized carbon spheres supporting the semiconductor platinum diphosphide, PtP2, 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(PPh3)(4) at 1000 degrees 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 PtP2 coated on the carbon spheres is 50 nm. (c) 2006 Elsevier Ltd. All rights reserved.