Reduction Behavior and Characteristics of Metal Oxides in the Nanoscale

The development of nanomaterials and nanotechnology enables the production of nanosized metallic alloys with advanced characteristics from their oxides via a thermal reduction technique. The aim of the present work was to produce metallic iron, nickel, and tungsten through the gaseous reduction of nanosized metal oxide powders as a preliminary step towards the fabrication of nanosized heavy tungsten alloys with unique properties. Nanosized NiO, Fe2O3, and WO3 were isothermally and non-isothermally reduced with H2, and the oxygen weight loss was continuously recorded as a function of time. The Thermogravimetric TG-DTA technique was applied in the non-isothermal reduction up to 1000 °C. The reduction extents were calculated from the TG curve, whereas the accompanying heat of the reaction was measured from the DTA curve. The results revealed that NiO was reduced at <420 °C, Fe2O3 was reduced at <600 °C, and WO3 was reduced at >950 °C. In the isothermal process, metal oxides were reduced with H2 at 700–1000 °C; a micro-force balance was used and the O2 weight loss was continuously recorded. At a given temperature, the rate of reduction increased in the order NiO > Fe2O3 > WO3. The nano-oxide powders and the reduced products were physically and chemically characterized. The activation energy (Ea) values were computed from the isothermal reduction in the initial and later stages to elucidate the corresponding reduction mechanism. The Ea values indicated that the reduction of metal oxides was controlled by the gas diffusion mechanism at both the initial and later stages of reduction. The results of the present study determined the optimal operation parameters at which the thermal gaseous reduction technique could be applied for preparing metallic alloys from nanosized metal oxides.