Continuous flow hydrothermal synthesis of phase pure rutile TiO2 nanoparticles with a rod-like morphology

Abstract

Titania nanocrystals are used in numerous applications but specific polymorphs (anatase, rutile, brookite) are typically required in specific applications making synthesis control over the crystal phase essential. Supercritical continuous flow reactors constitute fast, scalable alternatives to conventional autoclave hydrothermal synthesis. They provide outstanding control over nanoparticle characteristics such as size, crystallinity, and morphology but previous studies have always resulted in anatase products. Here we report, for the first time, a continuous hydrothermal flow method for obtaining phase pure rutile nanoparticles thereby significantly broadening the crystal design space for large scale titania applications. Through variation of the reactor temperature, the dimensions of the rod-like rutile crystallites are tunable in a range of 35 to 60 nm in length and 10 to 35 nm in width (maximum aspect ratio of ∼3.5) leading to a tunable band gap (3.2–3.5 eV) and high specific surface areas exceeding 200 m² g⁻¹.