A simple, two-step method using activated carbon (AC) as a support/scaffold was developed to synthesize metal oxide nanocrystalline materials (NCMs). In the first step, metal nitrate precursors were deposited by wet impregnation onto the AC, then heated in argon at 350 °C to immobilize the metal oxides. In the second step, the AC was removed by calcination in air at 500 °C, to obtain the unsupported metal oxide NCMs. Characterization by N2-sorption isotherms, TGA, XPS and EXAFS reveals that the metal oxide particles are crystalline and nanometre-sized, with surface areas up to 148 m2 g−1. Moreover, the TEM images show particle sizes in the range 5–10 nm, even after calcination at 500 °C for 2 h. Their thermal stability and high surface areas, together with the nanometre-sized structures, make them promising materials for catalytic applications (e.g., CO oxidation).
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