Synthesis of novel Zr-rich 312-type solid-solution MAX phase in the Zr-Ti-Si-C system

• Published in: Journal of the European Ceramic Society 2023-07, Vol.43 (8), p.3122-3130
• Main Authors: Istomin, P.V., Istomina, E.I., Nadutkin, A.V., Grass, V.E., Karateev, I.A., Makeev, B.A.
• Format: Article
• Language: English
• Subjects: Carbosilicothermic reduction; MAX phase; Out-of-plane ordering; Solid solution; Zr2TiSiC2
• ISSN: 0955-2219; 1873-619X
• DOI: 10.1016/j.jeurceramsoc.2023.02.049

A novel 312-type MAX-phase solid solution series in the Zr-Ti-Si-C system has been synthesized by the vacuum carbosilicothermic reduction method using mixtures of TiO2, ZrO2, SiC, and Si powders as starting materials. The upper limit for Zr content in metal sublattice of the synthesized (Zr,Ti)3SiC2 MAX phase solid solutions was found to be as much as approximately 66 at%, closely corresponding to a hypothetical quaternary Zr2TiSiC2 MAX phase. A wide miscibility gap inside the interval of Zr content in metal sublattice ranging between 22 at% and 55 at% was found. Crystal structure of the synthesized MAX-phase solid solutions was studied by HR-STEM/HAADF and XRD Rietveld analyses. The lattice constants were determined to be linearly correlated with Zr content as predicted by Vegard's law. A significant inhomogeneity in distribution of metal atoms similar to that of out-of-plane ordered quaternary MAX phases has been established for both Ti-rich and Zr-rich MAX-phase solid solutions.