A liquid approach for the synthesis of M phase VO2 nanocrystals: Facile synthesis, characterization and reaction mechanism

Vanadium dioxide is considered to be a promising material in most fields because of its special reversible metal-insulator transition (MIT) near ambient temperature. Pure VO2(M) is usually synthesized by a hydrothermal method combined with a subsequent annealing process or one-step hydrothermal synthesis. Both synthetic routes have the disadvantages of long reaction times. In this report, a new synthesis method of VO2(M) nanoparticles was established under liquid conditions. First, the V2O4·2H2O precursor was prepared successfully by using N2H4·2HCl-reduced V2O5 under thermostatic stirring without any reagent auxiliary. Second, the V2O4·2H2O suspension in water transformed into VO2(M) nanocrystals under hydrothermal synthesis. The intermediate and final products were characterized by XRD, SEM, HRTEM, XPS and DSC. The morphology of prepared VO2(M) exhibits a snowflake-like structure (approximately 1.0–4.0 μm in length, 0.5–3.0 μm in width and 50–200 nm in thickness). The phase-transition temperature is 65.49 °C. In addition, the reaction route of "V2O4·2H2O →V2O4·xH2O → VO2(B) → VO2(M) transformation" and reaction mechanism were established by testing the precipitate at different times at the hydrothermal stage.