FEATURES OF THE PHASE COMPOSITION AND MICROSTRUCTURE OF CERAMIC MATERIALS BASED ON THE ZrO2–TiO2 SYSTEM
DOI:
https://doi.org/10.30857/2786-5371.2026.4.8Keywords:
phase formation, ceramics, microstructure, solid-state interaction, heat treatmentAbstract
Purpose. To establish the features of phase formation and microstructure development in ceramic compositions of the ZrO₂–TiO₂ system under high-temperature synthesis conditions, taking into account the phase transformations of the initial components and their interactions.
Methodology. Monoclinic ZrO2 with a purity of 99.99% and TiO2 with a purity of 99.65% were used to prepare the experimental samples. The starting components were mixed in ratios corresponding to the stoichiometric compositions of ZrTiO4 and ZrTi2O6. After preparing the batch mixture, the specimens were formed by double-sided uniaxial pressing at 120 MPa. Heat treatment was carried out at 1300 °C with a heating rate of 8 °C/min, a holding time of 5 min at the maximum temperature, followed by slow cooling in the furnace. The microstructure was examined by electron microscopy, and the phase composition was determined by X-ray diffraction.
Findings. The phase formation and microstructural features of materials based on the ZrO2–TiO2 system with ZrTiO4 and ZrTi2O6 compositions, synthesized at 1300 °C under rapid-firing conditions, were investigated. It was established that variations in the ratio of the starting components affect the phase composition of the materials and promote the formation of ZrTiO4-based phases that partially remain in a metastable state upon cooling to room temperature. X-ray diffraction analysis confirmed the presence of the initial TiO2 and ZrO2 oxides, as well as the ZrTiO4 (zirconium titanate) phase, in the samples. Electron microscopy revealed the formation of a characteristic microstructure associated with solid-state interactions in the ZrO2–TiO2 system.
Originality. The phase formation behavior of ZrO2–TiO2 compositions under rapid-firing conditions was established, and the effect of the starting-component ratio on the phase composition and microstructure of the materials was demonstrated.
Practical value. The results obtained can be used to optimize the composition and processing parameters for producing ceramic materials in the ZrO2–TiO2 system.
Downloads
References
Patil S., Chikkatti B. S., Sajjan A. M., Banapurmathet N. R. Development of ZrO2-TiO2 binary nanocomposites for enhanced energy storage in supercapacitors. Discover Electrochemistry. 2025. Vol. 2. Art. 13. DOI: https://doi.org/10.1007/s44373-025-00029-7.
Repnin A., Sotov A., Popovich A., Masaylo D. Development of TiO2/ZrO2 Multi-Material Obtained from Ceramic Pastes for Material Extrusion. Micromachines. 2023. Vol. 14, No. 12. Art. 2177. DOI: https://doi.org/10.3390/mi14122177.
Kumari P., Saha R., Saikia G., Bhujel A., Choudhury M. G., Jagdale P., Paul S. Synthesis of Mixed-Phase TiO2–ZrO2 Nanocomposite for Photocatalytic Wastewater Treatment. Toxics. 2023. Vol. 11, No. 3. Art. 234. DOI: https://doi.org/10.3390/toxics11030234.
Kong L., Karatchevtseva I., Wei T., Veliscek-Carolan J. Synthesis of Mesoporous Tetragonal ZrO2, TiO2 and Solid Solutions and Effect of Colloidal Silica on Porosity. Molecules. 2024. Vol. 29, No. 14. Art. 3278. DOI: https://doi.org/10.3390/molecules29143278.
Troitzsch U. TiO2-Doped Zirconia: Crystal Structure, Monoclinic-Tetragonal Phase Transition, and the New Tetragonal Compound Zr3TiO8. Journal of the American Ceramic Society. 2006. Vol. 89, No. 10. Р. 3201–3210. DOI: https://doi.org/10.1111/j.1551-2916.2006.01200.x.
Zhang X., Wu X., Shi J. Additive manufacturing of zirconia ceramics: a state-of-the-art review. Journal of Materials Research and Technology. 2020. Vol. 9. Р. 9029–9048. DOI: https://doi.org/10.1016/j.jmrt.2020.05.131.
Zhu H., Chiang C.-C., Craciun V., Deane G., Ren F., Esquivel-Upshaw J. Yttrium Ion Release and Phase Transformation in Yttria-Stabilized Zirconia Under Acidic Conditions: Implications for Dental Implant Durability. Materials. 2025. Vol. 18. Art. 3311. DOI: https://doi.org/10.3390/ma18143311.
Demirci S., Sunol A. K., Sahiner N. Catalytic activity of amine functionalized titanium dioxide nanoparticles in methanolysis of sodium borohydride for hydrogen generation. Applied Catalysis B: Environmental. 2020. Vol. 261. Art. 118242. DOI: https://doi.org/10.1016/j.apcatb.2019.118242.
Eddy D. R., Permana M. D., Sakti L. K., Sheha G. A., Solihudin N., Hidayat S., Takei T., Kumada N., Rahayu I. Heterophase Polymorph of TiO2 (Anatase, Rutile, Brookite, TiO2 (B)) for Efficient Photocatalyst: Fabrication and Activity. Nanomaterials. 2023. Vol. 13, No. 4. Art. 704. DOI: https://doi.org/10.3390/nano13040704.
Moulson A. J., Herbert J. M. Electroceramics: Materials, Properties, Applications. John Wiley & Sons Ltd., New York, 2003. DOI: https://doi.org/10.1002/0470867965.
Biermann H., Martin U., Aneziris C. G., Kolbe A., Müller A., Schärfl W., Herrmann M. Microstructure and compression strength of novel TRIP-steel/Mg-PSZ composites. Advanced Engineering Materials. 2009. Vol. 11, No. 12. Р. 1000–1006. DOI: https://doi.org/10.1002/adem.200900210.
Martin S., Richter S., Decker S., Martin U., Krüger L., Rafaja D. Reinforcing Mechanism of Mg-PSZ Particles in Highly-Alloyed TRIP Steel. Steel Research International. 2011. Vol. 82, No. 9. Р. 1133–1140. DOI: https://doi.org/10.1002/srin.201100099.
Weigelt C., Berek H., Aneziris C. G., Wolf S., Eckner R., Krüger L. Effect of minor titanium additions on the phase composition of TRIP steel/magnesia partially stabilised zirconia composite materials. Ceramics International. 2015. Vol. 41, No. 2. Р. 2328–2335. DOI: https://doi.org/10.1016/j.ceramint.2014.10.040.
Dondi M., Matteucci F., Cruciani G. Zirconium titanate ceramic pigments: Crystal structure, optical spectroscopy and technological properties. Journal of Solid State Chemistry. 2006. Vol. 179, No. 1. Р. 233–246. DOI: https://doi.org/10.1016/j.jssc.2005.10.032.
Azough F., Freer R., Wang C.-L., Lorimer G. W. The relationship between the microstructure and microwave dielectric properties of zirconium titanate ceramics. Journal of Materials Science. 1996. Vol. 31. Р. 2539–2549. DOI: https://doi.org/10.1007/BF00687279.
Saenko I., Ilatovskaya M., Savinykh G., Fabrichnaya O. Experimental investigation of phase relations and thermodynamic properties in the ZrO2–TiO2 system. Journal of the American Ceramic Society. 2017. Vol. 101. Р. 386–399. DOI: https://doi.org/10.1111/jace.15176.
Troitzsch U., Ellis J. The ZrO2-TiO2 phase diagram. Journal of Materials Science. 2005. Vol. 40. Р. 4571–4577. DOI: https://doi.org/10.1007/s10853-005-1116-7.
Logvinkov S. M., Borysenko O. M., Shumejko V. M., Shabanova H. M., Korohodska A. M., Kryvobok R. V. Features of the phase formation of materials of the ZrO2 – TiO2 system for microwave dielectric ceramics. Functional Materials. 2026. Vol. 33, No. 2. Р. 211–219. DOI: https://doi.org/10.15407/fm33.02.211.
Logvinkov S. M., Borysenko O. M., Klochko N. P., Shabanova H. М., Shumeiko V. М. Question of the ZrO2 – TiO2 phase diagram. Bulletin of the National Technical University «KhPI». Series: Chemistry, Chemical Technology and Ecology. 2025. No. 2 (14). Р. 33–38. DOI: https://doi.org/10.20998/2079-0821.2025.02.05.
Souza J. V. C., Castro P. J., Nono M. C. A., Mineiro S. L. Sintering temperature influence on microwave dielectric properties of TiO2-ZrO2 ceramics. Materials Science Forum. 2010. Vol. 660–661. Р. 646–651. DOI: https://doi.org/10.4028/www.scientific.net/MSF.660-661.