Cobalt nanoparticles were synthesized on silica thin films by heat treating Co/silica films spun on thermally oxidized Si substrates. The as-deposited films were calcined in vacuum (∼0.03 Torr) for 2 h at 500 °C, followed by reduction in hydrogen at 650 °C for up to 15 h. The reduction process is characterized as one of time-dependent evolution of nanoparticles in both physical appearance and phase nature, eventually leading to the formation of well-dispersed Co nanoparticles, as ascertained by x-ray photoelectron spectroscopy and scanning electron microscopy. Slow conversion of Co ions into metallic Co observed in this study is ascribed to the absence of a Co3O4 phase that forms predominantly during calcination in air. Atomic force microscopy revealed a marked increase in the surface roughness of the film due to the development of nanoparticles. A distinct duplex-layer structure was observed in the reduced film, which consisted of the upper layer laden with nanoparticles and the lower layer essentially particle-free. The growth of the upper layer appears to be controlled by the upward diffusion of Co2+ in the film during the reduction process.
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Park, S.M., Ki, W., Yu, J. et al. Sol-gel synthesis of highly dispersed cobalt nanoparticles on silica thin films. Journal of Materials Research 20, 3094–3101 (2005). https://doi.org/10.1557/JMR.2005.0390