Co-Sputtered Thin Film Consisting of Platinum Nanoparticles Embedded in Graphite-Like Carbon and Its High Electrocatalytic Properties for Electroanalysis Tianyan You, † Osamu Niwa,* ,† Tsutomu Horiuchi, † Masato Tomita, † Yuzuru Iwasaki, † Yuko Ueno, † and Shigeru Hirono ‡ NTT Lifestyle and Environmental Technology Labs, 3-1 Morinosato, Wakamiya, Atsugi, Kanagawa 243-0198, Japan, and NTT Afty Corporation, 4-16-30 Shimorenjyaku, Mitaka, Tokyo 181-0013 Japan Received June 5, 2002. Revised Manuscript Received September 26, 2002 The radio frequency (RF) sputtering method was used to prepare nanoscale platinum (0) particles highly dispersed in a graphite-like carbon film (Pt-NEGCF) by co-sputtering platinum and carbon. The preparation is very simple, controllable, and reproducible. We studied this film with respect to its structural characterization and electrocatalytic properties. The XPS spectrum reveals that the platinum state in the Pt-NEGCF is platinum (0). TEM images show that the structure of the carbon in the film is graphite-like and that the platinum particles are highly dispersed in the carbon matrix. The electrochemical properties of the Pt-NEGCF electrode were evaluated. Compared with Pt bulk electrode, this film electrode is highly electrocatalytic as regards hydrogen evolution, dioxygen reduction, and hydrogen peroxide oxidation with good stability. 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