Spark plasma sintering of magnesium titanate ceramics

• Published in: Ceramics international Vol. 50; no. 9; pp. 15283 - 15291
• Main Authors: Filipović, Suzana, Obradović, Nina, Fahrenholtz, William G., Smith, Steven, Mirković, Miljana, Peleš Tadić, Adriana, Petrović, Jovana, Đorđević, Antonije
• Format: Journal Article
• Language: English
• Published: Elsevier Ltd 01.05.2024
• Subjects: Ball milling; Hardness; Magnesium titanate ceramics; Oxygen vacancies relaxation; SEM; XRD; Ball milling; Oxygen vacancies relaxation; SEM; XRD; Hardness; Magnesium titanate ceramics
• ISSN: 0272-8842; 1873-3956
• DOI: 10.1016/j.ceramint.2024.02.004

Magnesium titanate ceramics were prepared by reactive spark plasma sintering (SPS) at 1200 °C for 5 min. Prior to sintering, MgO and TiO2 powders were mixed by high energy ball milling (HEBM) for 15, 30, or 60 min. The effect of milling time on phase composition was analyzed by X-ray diffraction (XRD) for milled powders and sintered specimens. The morphology of the sintered ceramics was investigated by scanning electron microscopy (SEM), while elemental distribution was determined by energy dispersive spectroscopy (EDS). The presence of the MgTi2O5 phase was detected in XRD and was confirmed by EDS analysis. Microcracking was observed for specimens prepared with longer milling times and attributed to the coefficient of thermal expansion (CTE) mismatch dominantly due to the anisotropic crystal structure of MgTiO3 phase. The sample milled for 15 min showed the highest Vickers hardness due to less or no microcracking and nearly full density. The dielectric measurements in the range of 10 Hz–250 MHz demonstrated extremely high dielectric permittivity, as high as 104 at 1 kHz. An increase in loss tangents was observed due to oxygen vacancy formation, which was promoted by the vacuum environment during SPS. Oxygen vacancy-related dielectric relaxation was also detected and explained.