Preliminary leaching of rice husks with a solution of hydrochloric acid before their combustion at 600°C is shown to be required to obtain relatively pure silica (∼99.5%) with a high specific surface area (∼260 m2/g) that is maintained even after heating at 800°C. Transmission electron microscopy observations indicate that this material has a homogeneous size distribution of nanometric particles. However, if the leaching with HCl is performed on the white ashes obtained by combustion of the rice husks at 600°C, an amorphous silica with the same purity also is obtained, but its specific surface area decreases to 1 m2/g. This behavior is due to a strong interaction between the silica and the potassium contained in the rice husks, which leads to a dramatic decrease of the specific surface area if K+ cations are not removed prior to the heat treatment at 600°C. This finding leads to a better understanding of the effect of potassium on the morphology of silica.

A planetary ball-mill device that enables one to perform solid-gas reactions at constant pressure was developed. Titanium powders were ball milled under nitrogen at a spinning rate of 960 rpm. The influence of the nitrogen pressure on the mechanochemical reactivity of titanium was analyzed at 1.5 and 11 bars. A spontaneous combustion took place during the grinding process, leading to a high yield of TiN for short milling times. The conversion of titanium into titanium nitride was facilitated by increasing the nitrogen pressure. At 11 bars, full conversion was reached for grinding times shorter than 5 h. Titanium nitride obtained in this way exhibited a high sintering activity.

Titanium carbonitride (TiC x N 1Àx ) powders were obtained by high-energy ball milling of elemental titanium and carbon (activated carbon or graphite) in a nitrogen atmosphere. The formation of the carbonitride phase was controlled by adequately choosing the experimental conditions of the milling process. The stoichiometry of TiC x N 1Àx powders was modified by adjusting the titanium-to-carbon molar ratio. The composition and cell parameters of the carbonitride phases were determined. Microstructural characterization of these phases showed a nanocrystalline nature.

Niobium, tantalum, and hafnium carbonitride nanopowders were obtained by high-energy ball milling of elemental metal and graphite in a nitrogen atmosphere. By adjusting milling parameters, a mechanically induced self-propagating reaction was observed during the formation of carbonitride phases. The stoichiometry of transition metal carbonitrides was controlled by fixing the starting metal-to-carbon molar ratio. Ignition of the reactant mixture was determined by the combined effect of nitrogen and carbon, gas, and solid reagents, respectively. The composition and lattice parameters were determined by X-ray diffraction measurements. Microstructural characterization showed a nanophase structure with a homogeneous chemical composition.