New solvothermal flow synthesis of strontium titanate nanoparticles based on the use of acetylacetonate precursors in water/ethanol mixture

Abstract

In this study, strontium titanate (SrTiO₃) nanoparticles were obtained utilizing a one-step supercritical continuous solvothermal synthesis process involving acetylacetonate precursors for both strontium and titanium cations instead of the historical alkoxide ones. These precursors are expensive, difficult to access (especially for strontium isopropoxyde) and inadequately stable, forcing the use of a glove box and controlled atmospheres, which is not the case for acetylacetonates. Pure SrTiO₃ nanoparticles with a crystallite size of roughly 20 nm were successfully synthesized. In addition to the cubic structure of SrTiO₃, FTIR revealed surface functions that are typical of "wet" processes, while Raman spectroscopy showed the activation of non-centrosymmetric modes brought on by non-linear contributions. The nanoparticles show a faceted shape and are stable at elevated temperatures (up to 800 °C), according to in-situ high temperature XRD measurements. However, due to a chemical deficiency in strontium, titanium dioxide (TiO₂) phases are formed at higher temperatures. In-situ high temperature HRTEM investigations showed the existence of two populations of particles, with a better stability for the bigger-sized particles after thermal treatment as well as the sintering and restructuring of the smallest ones. Also, the microscopy results suggest the possibility of a chemical inhomogeneity within the crystallites. Overall, this study offers important new knowledge on the physicochemical characteristics of the synthesized SrTiO₃ nanoparticles and their thermal stability using a novel supercritical continuous solvothermal approach based on the use of acetylacetonate precursors.