Supercritical fluids offer fast and facile routes toward well-crystallized tailor-made cerium oxide nanoparticles. However, the use of surfactants to control morphology and surface properties remains essential. Therefore, although water, near-critical (nc) or supercritical (sc), is a solvent of choice, the poor water solubility of some surfactants could require other solvent systems such as alcohols, which could themselves behave as surface modifiers. In here, the influence of seven different alcohols, MeOH, EtOH, PrOH, iPrOH, ButOH, PentOH, and HexOH, in alcothermal conditions (300 °C, 24.5 MPa) over CeO(2) nanocrystals (NCs) size, morphology, and surface properties was investigated. The crystallite size of the CeO(2) nanocrystals can be tuned in the range 3-7 nm depending on the considered alcohol, and their surface has been modified by these solvents without the use of surfactants. Mechanisms are proposed for the interaction of primary and secondary alcohols with CeO(2) surface and its functionalization during the synthesis based on FTIR and TGA-MS studies. This study allows apprehending the role of alcohols during the synthesis and may lead to an informed choice of solvent as a function of the required size and surface properties of CeO(2) NCs. It also opens new route to CeO(2) functionalization using supercritical alcohol derivatives.
Herein we introduce a powerful and fast method to produce nanominerals using a bottom up approach. The supercritical hydrothermal flow synthesis is exploited to produce model nanominerals by mimicking natural environments at high temperatures under pressure. This innovative concept is demonstrated with the talc synthesis; this represents a major technical breakthrough since it allows decreasing the mineral-synthesis time from tens of hours to tens of seconds. Through this example, we show these nanominerals exhibit new crystal-chemistry signals and new properties. This approach provides a means to reproduce the early stages of formation of minerals in different natural environments from sedimentary environments (low temperature and pressure) to hydrothermal/metamorphic environments (high temperature and high pressure).
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