Vol. 337 No. 10 (2026)
DOI https://doi.org/10.18799/24131830/2026/10/5716
Rheological characteristics and features of thermal shrinkage during dilatometry of commercial powders of partially stabilized zirconia
Relevance. Partially stabilized zirconia is a sought-after ceramic material for medical application, which is widely used as dental implants, crowns, permanent dentures, etc. Medical products made of partially stabilized zirconia have high biological compatibility, good mechanical and optical properties, and their disadvantage, which leads to a shorter service life, is the degradation of properties in a humid environment and at elevated temperatures (partly consistent with the operating conditions of implants in the body). The full cycle of technology for manufacturing products of partially stabilized zirconia consists in the following main stages: processing of natural raw materials (baddeleyite or zircon), synthesis and preparation of powder, powder compaction and high-temperature processing, which makes it advisable to study the rheological characteristics and processes of thermal shrinkage of partially stabilized zirconia powders. Aim. To investigate rheological characteristics of commercial zirconium dioxide powders, as well as their thermal shrinkage by determining the constants of the Ivensen equation and the apparent activation energy of isothermal sintering. Objects. Partially stabilized zirconia powders of commercial brands: TZ-3YS (Tosoh Corp., Japan) and VK-R80Y3R (MSE Supplies LLC, USA). Methods. The rheological characteristics of partially stabilized zirconia powders were determined based on the provisions of the mechanistic pressing model according to the method of constructing compaction curves with successive discharges during their compaction in closed rigid molds. The processes of thermal shrinkage were studied using optical dilatometry in air. Powder compacts for dilatometry were pre-manufactured by cold static uniaxial single-sided pressing in steel molds. The microstructure and phase composition of the samples after dilatometry were studied by scanning electron microscopy and X-ray phase analysis. Results and conclusions. It is shown that the rheological properties of powder materials during their compaction in closed rigid molds can be determined with high reliability using the method of constructing compaction curves with successive discharges, which allows determining the dependence of its deformation on a single sample (after recalculation – density) from the applied pressing pressure. According to dilatometry data, the authors determined the coefficients of the Ivensen equation, and calculated the apparent activation energy of isothermal sintering during dilatometry.
For citation: Deulina D.E., Shevchenko I.N., Dvilis E.S., Paygin V.D., Tolkachev O.S., Stepichev D.A. Rheological characteristics and features of thermal shrinkage during dilatometry of commercial powders of partially stabilized zirconia. Bulletin of the Tomsk Polytechnic University. Geo Assets Engineering, 2026, vol. 337, no. 10, pp. 7–18. http://doi.org/10.18799/24131830/2026/10/5716
Keywords:
Partially stabilized zirconium dioxide, PSZ, cold uniaxial static pressing, rheological characteristics, dilatometry
References:
1. Lyamina G.V., Ilela A.E., Dvilis E.S., Petyukevich M.A., Tolkachev O.S. Medical ceramics from powders of the system Al2O3–ZrO2–Y2O3 obtained on an installation of nanospray drying. Nanotechnologies in Russia, 2018, vol. 13, pp. 337–343.
2. Thamaraiselvi T.V., Rajeswari S. Biological evaluation of bioceramic materials. Trends Biomater. Artificial Organs, 2004, vol. 18, pp. 9–17.
3. Sathish S., Geetha M. Comparative study on corrosion behavior of plasma sprayed Al2O3, ZrO2, Al2O3/ZrO2, and ZrO2/Al2O3 coatings. Transactions of Nonferrous Metals Society of China, 2016, vol. 26, pp. 1336–1344. DOI: 10.1016/S1003-6326(16)64236-X.
4. Yousry M., Hammad I., Halawani M.E., Aboushelib M. Translucency of recent zirconia materials and material-related variables affecting their translucency: a systematic review and meta-analysis. BMC Oral Health, 2024, vol. 24, pp. 309. DOI: 10.1186/s12903-024-04070-7.
5. Chevalier J. What future for zirconia as a biomaterial? Biomaterials, 2006, vol. 27, pp. 535–543. DOI: j.biomaterials.2005.07.034.
6. Christensen R. Focus on: monolithic crowns. Dentistry Today, 2013, vol. 32, no. 3, p. 22.
7. Rinke S., Fischer C. Range of indications for translucent zirconia modifications: clinical and technical aspects. Quintessence international, 2013, vol. 44, no. 8. DOI: 10.3290/j.qi.a29937.
8. Stober T., Bermejo J.L., Rammelsberg P., Schmitter M. Enamel wear caused by monolithic zirconia crowns after 6 months of clinical use. Journal of oral rehabilitation, 2014, vol. 41, pp. 314–322. DOI: 10.1111/joor.12139.
9. Filser F., Kocher P., Gauckler L.J. Net-shaping of ceramic components by direct ceramic machining. Assembly Autom, 2003, vol. 23, pp. 82–90. DOI: 10.1108/01445150310501217.
10. Fedorov P.P., Yarotskaya E.G. Zirconium dioxide. Review. Condensed Matter and Interphases, 2021, vol. 23, pp. 169–187. DOI: 10.17308/kcmf.2021.23/3427.
11. Fabris S., Paxton A.T., Finnis M.W. A stabilization mechanism of zirconia based on oxygen vacancies only. Acta Materialia, 2002, vol. 50, pp. 5171–5178. DOI: 10.48550/arXiv.cond-mat/0206080.
12. Smorokov A.A., Kantaev A.S., Yerzhanov A.B. Development of a low-temperature desiliconization method for zircon concentrate after activation with NH4HF2. Journal of Tomsk Polytechnic University. Geo Assets Engineering, 2022, vol. 333, pp. 27–36. (In Russ.) DOI: 10.18799/24131830/2022/4/3459
13. Denry I., Kelly J.R. State of the art of zirconia for dental applications. Dental materials, 2008, vol. 24, pp. 299–307. DOI: 10.1016/j.dental.2007.05.007.
14. Gupta T.K., Lange F.F., Bechtold J.H. Effect of stress-induced phase transformation on the properties of polycrystalline zirconia containing metastable tetragonal phase. Journal of Materials Science, 1978, vol. 13, pp. 1464–1470. DOI: 10.1007/BF00553200.
15. Zwahlen L., Karlin S., Venzin L., Rohr R. Speed-sintering protocol and blank type affect optical properties and strength of 3–5 mol % yttria-stabilized zirconia. Dental Materials, 2026, vol. 42, pp. 1057–1067. DOI: 10.1016/j.dental.2026.02.016.
16. Tolkachev O.S., Dvilis E.S., Alishin T.R., Khasanov O.L., Miheev D.A., Chzhan T. Assessment of the hydrothermal resistance of Y-TZP ceramics by the degree of tetragonality of major phases. Letters on Materials, 2020, vol. 10, pp. 416–421. DOI: 10.22226/2410-3535-2020-4-416-421.
17. Dyakonenko E.E., Sahabieva D.A., Akselrod I.B., Lebedenko I.Yu. Comparative evaluation of traditional and speed sintering of dental zirconia ceramics. Stomatology, 2022, vol. 101, no. 4, pp. 106–113. (In Russ.) DOI: 10.17116/stomat2022101021106.
18. Biesuz M., Beauvoir T.H., Bona E., Cassetta M., Maniere C., Sglavo V.M., Estournes C. Ultrafast high-temperature sintering (UHS) vs. conventional sintering of 3YSZ: microstructure and properties. Journal of the European Ceramic Society, 2024, vol. 44, pp. 4741–4750. DOI: 10.1016/j.jeurceramsoc.2024.01.064.
19. Lim C.H., Alves L.M.M., Vardhaman S., Bonfante E.A., Kim D.K., Zhang Y. Two-step sintering suppresses grain growth and improves flexural strength of dental zirconia. Dental Materials, 2025, vol. 41, pp. 194–202. DOI: 10.1016/j.dental.2024.11.008.
20. Ouyang R.F., Chen Y.X., Li L. Preparation of denser and stronger 3YSZ ceramics by cold sintering assisted pressure – less sintering at reduced temperature from 100 nm powder. Ceramics International, 2026, vol. 52, pp. 11701–11708. DOI: 10.1016/j.ceramint.2026.01.328.
21. Bhandari S., Manière C., Sedona F., De Bona E., Sglavo V.M., Colombo P., Fambri L., Biesuz M., Franchin G. Ultra-rapid debinding and sintering of additively manufactured ceramics by ultrafast high-temperature sintering Journal of the European Ceramic Society, 2024, vol. 44, pp. 328–340. DOI: 10.1016/j.jeurceramsoc.2023.08.040.
22. Oglezneva S.A., Portal M.N. Investigation of the kinetics of isothermal sintering of crushed and mechanically alloyed iron powders. Izvestiya vuzov. Powder metallurgy and functional coatings, 2015, vol. 1, pp. 9–16. (In Russ.)
23. Dvilis E.S. Patterns of processes of consolidation of powder systems under changing conditions of deformation and physical effects. Dr. Diss. Tomsk, 2014. 386 p. (In Russ.)
24. Ivensen V.A. Phenomenology of sintering and some questions of theory. Moscow, Metallurgiya Publ., 1985. 246 p. (In Russ.)
25. Laberty-Robert C., Ansart F., Deloget C., Gaudon M., Rousset A. Dense yttria stabilized zirconia: sintering and microstructure. Ceramics international, 2003, vol. 29, pp. 151–158. DOI: 10.1016/S0272-8842(02)00099-8.
26. Dvilis E.S., Khasanov O.L., Sokolov V.M. The relationship between the parameters of the state of the pressed powder body and the properties of ceramics sintered from it. Fundamental Research, 2016, vol. 11, pp. 691–697. (In Russ.)
27. Dvilis E.S., Khasanov O.L., Paygin V.D., Tolkachev O.S. Production of light–transmitting YSZ ceramics by cold static uniaxial and ultrasonic pressing followed by free sintering. Fundamental Research, 2017, vol. 12–4, pp. 268–276. (In Russ.)
28. Tolkachev O.S., Dvilis E.S., Alishin T.R., Leonov A.A., Paygin V.D., Mikheev D.A. Consolidation processes, structure and properties of composite material based on ZrO2 nanoparticles and Al2O3 nanofibers. Structures made of composite materials, 2019, vol. 3, pp. 30–36. (In Russ.)
29. Marcomini R. F., Arantes V. L. Sintering mechanisms of partially stabilized zirconia (TZ3Y) with ZnO and Co3O4 as sintering additives. Cerâmica, 2021, vol. 67, pp. 244–249. DOI: 10.1590/0366-69132021673823099.
30. Bernard‐Granger G., Guizard C. Apparent activation energy for the densification of a commercially available granulated zirconia powder. Journal of the American Ceramic Society, 2007, vol. 90, pp. 1246–1250. DOI: 10.1111/j.1551-2916.2006.01415.
31. Kumagai T. Mechanism for densification of yttria-stabilized tetragonal zirconia powder by electric current-activated/assisted sintering. Materials Transactions, 2011, vol. 52, pp. 2098–2105. DOI: 10.2320/matertrans.M2011104.
32. Chatchay D. Structure and mechanical properties of composites based on zirconium dioxide and wollastonite. Cand. Diss. Tomsk, 2021. 167 p. (In Russ.)
33. Vartanyan M.A., Akinshin D.V., Vershinin D.I., Speshilov I.O. Development of a firing mode for ceramics based on aluminum oxide with a eutectic sintering additive for metallization by chemical method. Modern methods and technologies of creation and processing of materials, 2018, vol. 1, pp. 37–46. (In Russ.)


