Effect of Thermal Treatment on the Textural Properties of CeO2 Powders Synthesized in Near‐ and Supercritical Alcohols

CeO₂ nanocrystals (NCs) have attracted increasing interest over the past few years, in particular for their use in catalytic reactions. Syntheses mediated by near‐ and supercritical alcohols have proven to be innovative ways to obtain CeO₂ NCs with controlled crystallite sizes (from 3 to 8 nm depending on the alcohol) and surface functionalities, with alcohol moieties. When submitted to a thermal treatment at 500 °C, required to desorb/degrade surface organic species, these powders displayed different behaviors depending on the alcohol used during the synthesis. Cerium oxide powders synthesized in sc‐MeOH, sc‐EtOH and sc‐iPrOH undergo sintering during treatment at 500 °C, with a decrease of their specific surface area. Conversely, those synthesized in sc‐BuOH, nc‐PentOH and nc‐HexOH keep their initial crystallite sizes and morphology, but show a great enhancement of their specific surface area (up to 200 m² g^?1), which is unprecedented after such a thermal treatment.