A versatile one-step pyrolysis method is successfully employed to fabricate hollow carbon nanospheres (HCNs, ca. 60 nm in diameter) supported with metallic nanoparticle catalyst. The resultant catalyst hybrid was characterized by using TEM, FTIR, TGA measurements. It is confirmed that,
as the carbon precursor and hollow core/shell structure template, hollow chitosan nanospheres provide the important adsorption sites for the metallic precursor. The one-step pyrolysis process at 750 °C under nitrogen atmosphere results in the simultaneous decomposition of the chitosan
nanospheres to HCNs and the adsorbed metal salt complex to metallic nanoparticles. It is found that metallic nanoparticles with an average diameter of ca. 4 nm highly dispersed in the carbon shell of HCNs, and no aggregation phenomenon occurs under the high deposition temperature. As a demonstration,
the HCNs-supported Pt catalyst for the electrochemical methanol oxidation was studied.