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.
The effect of phosphate on the anatase-+rutile transformation has been studied. The conclusion has been reached that the polymorphic transformation takes place through the nucleation of rutile on the surface of TiO, when the oxide undergoes either thermal or mechanical treatment. The phosphate strongly inhibits the anatase + rutile conversion through a mechanism that implies its chemisorption on TiO, as a bidentate ligand which hinders the surface ionic mobility.
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.
The formation of ZnSe via a mechanically-induced self-sustaining reaction (MSR) from a Zn/Se mixture showed that only size reduction and mixing of the reactants without product formation occurred during the induction period prior to ignition. Therefore, all mechanical energy supplied by the planetary mill during this time, called the ignition time (t ig ), was used exclusively in the activation of the reactants. This system was chosen to study the dependence of t ig on the main parameters characterising the milling intensity of planetary mills. The variation of the ignition time with the process conditions reflected changes in the mechanical dose rate of the planetary mill. A direct relationship between the inverse of the ignition time and the power of the planetary mill was established, which allows the validation of theoretical models proposed in the literature for the energy transfer in milling devices and the comparison of milling equipment efficiencies.
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