A novel homoleptic bismuth(III) beta-diketonate (dibenzoylmethane - dbm) complex [Bi(dbm)(3)](2) has been used as a precursor to thin films of crystalline beta-Bi2O3, and hexachloroplatinic acid (H2PtCl6 center dot 6H(2)O) has been demonstrated as a suitable precursor for deposition of platinum nanoparticles, both deposited via aerosol-assisted chemical vapour deposition (AACVD). Thin films of Pt-Bi2O3 were co-deposited from a mixture of [Bi(dbm)(3)](2) and H2PtCl6 center dot 6H(2)O; the introduction of Pt particles into beta-Bi2O3 causes hydrogen to be evolved during photolysis of water over the composite material, a property not found for Pt particles or beta-Bi2O3 alone.