Spark plasma sintering of magnesium titanate ceramics

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 (XR...

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Published inCeramics 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
LanguageEnglish
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
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Abstract 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.
AbstractList 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.
Author Filipović, Suzana
Fahrenholtz, William G.
Mirković, Miljana
Obradović, Nina
Peleš Tadić, Adriana
Đorđević, Antonije
Smith, Steven
Petrović, Jovana
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Oxygen vacancies relaxation
SEM
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Hardness
Magnesium titanate ceramics
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Snippet 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...
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SubjectTerms Ball milling
Hardness
Magnesium titanate ceramics
Oxygen vacancies relaxation
SEM
XRD
Title Spark plasma sintering of magnesium titanate ceramics
URI https://dx.doi.org/10.1016/j.ceramint.2024.02.004
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