Kohei Kasuya, Md. Shahiduzzaman, Makoto Kobayashi, Shu Yin, Masato Kakihana, and Koji Tomita “Synthesis of brookite-type TiO2 nanoparticles by emulsion-assisted hydrothermal method using titanium glycolate complex”, Journal of the Ceramic Society of Japan, 129, 720–724 (2021).
We present a method for synthesizing brookite-type titanium dioxide (TiO2) using an emulsion-assisted hydrothermal approach and a water-soluble titanium complex with glycolic acid as a complexing agent. In this study, stirred hydrothermal synthesis was used to synthesize water-in-oil emulsions with titanium glycolate complex in the aqueous phase. The resulting brookite-type TiO2 was investigated using Raman spectroscopy for crystal polymorph identification, X-ray Diffraction to identify crystal polymorphs and crystallite size, Transmission Electron Microscope for primary particle size, and crystal shape, and Dynamic Light Scattering for TiO2 secondary particle size in aqueous dispersion. The synthesized brookite-type TiO2 was a needle-like crystal with a width between 20 and 30 nm and a length of more than 70 nm, growing in the b-axis direction at an angle of about 70° from the (120) plane. Furthermore, compared to the conventional synthesis method, the secondary particle size was smaller, and the dispersibility in water was improved. The results show that the brookite-type TiO2 dispersion obtained using the emulsion-assisted hydrothermal method can facilitate the formation of uniform films and can be applied to the electron transport layer of organic perovskite solar cells.