In this work, industrial waste hexafluorosilicic acid (H 2 SiF 6 or FSA) has been proven to be a low-cost alternative to silicate esters for the synthesis of high-quality MCM-41 (high surface area, high degree of order, narrow pore size distribution, high thermal stability) through a head-to-head comparison between the most common silica precursor, tetraethylorthosilicate (TEOS), and FSA. The effect of different parameters such as temperature, time, hydrothermal treatment, and the presence of ethyl acetate has been explored by studying the textural, structural, and morphological features. On the most promising samples, thermal and hydrothermal stability has been assessed, indicating a higher thermal stability for the FSA-derived sample, due to the thicker walls, and comparable hydrothermal stability. The mother solution treatment has allowed the obtainment of nanostructured fluorite as an additional valuable product and a CTAB-rich ammonia solution for successive synthesis with FSA. Recovery processes for the templating agent entrapped in the MCM-41 mesostructure have also been explored for both FSA-and TEOS-derived samples, showing an easier removal in the case of FSA-MCM-41. Moreover, mesostructured silica derived from FSA has also been proven to be an ideal support to design efficient and regenerable mesostructured iron oxide-based sorbents for H 2 S removal from syngas, showing similar performance to that of the corresponding nanocomposite prepared from TEOS.
The electric field has a large effect on the stoichiometry and grain growth of UO2+x during Spark Plasma Sintering. UO2+x is gradually reduced to UO2.00 as a function of sintering temperature and time. A gradient in the oxidation state within the pellets is observed in intermediate conditions. The shape of the gradient depends unequivocally on the direction of the electrical field. The positive surface of the pellet shows a higher oxidation state compared to the negative one. An area with larger grain size is found close to the positive electrode, but not in contact with it. We interpret these findings with the redistribution of defects under an electric field, which affect the stoichiometry of UO2+x and thus the cation diffusivity. The results bear implications for understanding the electric field assisted sintering of UO2 and non-stoichiometric oxides in general.
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