Microstructure Evolution During the Sintering of Freeze-Cast Alumina

Abstract

Reports on freeze-cast ceramic materials frequently focus on the study of the organized macroporosity and the properties of the materials. This study aims to describe the microstructure evolution of freeze-cast alumina during the sintering process, analyzing grain growth, densification, pore elimination and crystal structure at different sintering temperatures (1300-1500 °C). Aqueous suspensions with 20 vol% alumina were freeze-cast in liquid N2 and sintered. The microstructure was analyzed by stereological analysis, N2 adsorption and X-ray diffraction. Grain sizes varied within 237-500 nm, and the intergranular porosity decreased from 8.8% at 1300 °C to 1.4% at 1500 °C. N2 isotherm analysis revealed pore shrinking from the region of macro and mesopores (20-80 nm), to smaller residual mesopores (3.7-15 nm) at temperatures above 1400 °C. Rietveld refinement of the XRD diffractograms confirmed increased crystallite size and decreased lattice strain at higher sintering temperatures. This comprehensive description of microstructural evolution of the freeze-cast alumina contributes to understanding the sintering of highly porous ceramics produced via freeze-casting.

Keywords

• Sintering
• freeze-casting
• alumina
• microstructure