| Summary: | The unique properties and numerous applications of nanocrystalline titanium dioxide (TiO<sub>2</sub>) are stimulating research on improving the existing and developing new titanium dioxide synthesis methods. In this work, we demonstrate for the first time the possibilities of the extraction–pyrolytic method (EPM) for the production of nanocrystalline TiO<sub>2</sub> powders. A titanium-containing precursor (extract) was prepared by liquid–liquid extraction using valeric acid C<sub>4</sub>H<sub>9</sub>COOH without diluent as an extractant. Simultaneous thermogravimetric analysis and differential scanning calorimetry (TGA–DSC), as well as the Fourier-transform infrared (FTIR) spectroscopy were used to determine the temperature conditions to fabricate TiO<sub>2</sub> powders free of organic impurities. The produced materials were also characterized by X-ray diffraction (XRD) analysis and transmission electron microscopy (TEM). The results showed the possibility of the fabrication of storage-stable liquid titanium (IV)-containing precursor, which provided nanocrystalline TiO<sub>2</sub> powders. It was established that the EPM permits the production of both monophase (anatase polymorph or rutile polymorph) and biphase (mixed anatase–rutile polymorphs), impurity-free nanocrystalline TiO<sub>2</sub> powders. For comparison, TiO<sub>2</sub> powders were also produced by the precipitation method. The results presented in this study could serve as a solid basis for further developing the EPM for the cheap and simple production of nanocrystalline TiO<sub>2</sub>-based materials in the form of doped nanocrystalline powders, thin films, and composite materials.
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