The unique properties and numerous applications of nanocrystalline titanium dioxide (TiO₂) 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 TiO₂ powders. A titanium-containing precursor (extract) was prepared by liquid–liquid extraction using valeric acid C₄H₉COOH 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 TiO₂ 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 TiO₂ 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 TiO₂ powders. For comparison, TiO₂ 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 TiO₂-based materials in the form of doped nanocrystalline powders, thin films, and composite materials.

Nanolayered coatings are proposed for use in microelectronic devices where the size/performance ratio is becoming increasingly important, with the aim to achieve existing quality requirements while reducing the size of the devices and improving their ability to perform stably over multiple cycles. Si-SiO₂-W structures have been proposed as a potential material for the fabrication of microelectronic devices. However, before such materials can be implemented in devices, their properties need to be carefully studied. In this study, Si-SiO₂-W nanolayered structures were fabricated and subjected to numerous thermal treatment cycles at 150 °C. A total of 33 heating cycles were applied, resulting in a cumulative exposure of 264 h. The changes in chemical bonds and microstructure were monitored using Fourier Transform Infrared spectrometry (FTIR) and scanning electron microscopy (SEM). The FTIR signal at 960 cm⁻¹, indicating the presence of W deposited on SiO₂, was selected to characterize the thermal stability during the heating cycles. The estimated signal intensity variation closely resembled the normal inhomogeneity of the nanolayers. The increase in slope intensity was estimated to be 1.7 × 10⁻⁵.