%0 Journal Article %T One-step route to a hybrid TiO2/TixW1 xN nanocomposite by in situ selective carbothermal nitridation %A Zo£¿ Schnepp %A Martin J Hollamby %A Masahiko Tanaka %A Yoshitaka Matsushita %A Yoshio Katsuya and Yoshio Sakka %J Science and Technology of Advanced Materials %D 2012 %I Institute of Physics, National Institute for Materials Science %X Metal oxide/nitride nanocomposites have many existing and potential applications, e.g. in energy conversion or ammonia synthesis. Here, a hybrid oxide/nitride nanocomposite (anatase/TixW1 xN) was synthesized by an ammonia-free sol¨Cgel route. Synchrotron x-ray diffraction, complemented with electron microscopy and thermogravimetric analysis, was used to study the structure, composition and mechanism of formation of the nanocomposite. The nanocomposite contained nanoparticles (<5 nm diameter) of two highly intermixed phases. This was found to arise from controlled nucleation and growth of a single oxide intermediate from the gel precursor, followed by phase separation and in situ selective carbothermal nitridation. Depending on the preparation conditions, the composition varied from anatase/TixW1 xN at low W content to an isostructural mixture of Ti-rich and W-rich TixW1 xN at high W content. In situ selective carbothermal nitridation offers a facile route to the synthesis of nitride-oxide nanocomposites. This conceptually new approach is a significant advance from previous methods, which generally require ammonolysis of a pre-synthesized oxide. %U http://dx.doi.org/10.1088/1468-6996/13/3/035001