Currently, the primary method for preparing alumina fiber-reinforced alumina ceramic (Al2O3f/Al2O3) composites is the slurry impregnation (SI) process. However, this technique is plagued by the challenge of necessitating a high sintering temperature. Hence, an attempt was initiated to prepare Al2O3f/Al2O3 composites through the polymer impregnation and pyrolysis (PIP) method, with the objective of reduce thermal damage to the fibers during the preparation process. The high-temperature inorganic processing of the Al2O3 precursor was studied, ultimately leading to the selection of 900 °C as the optimal pyrolysis temperature for the PIP process. The microstructure and high-temperature mechanical properties of the obtained composites were studied. The results indicated that the composites maintained microstructure stability up to 1000 °C. The flexural strength almost unchanged (from 37.20 ± 4.09 MPa to 37.03 ± 2.01 MPa). At 1200 °C, the formation of mullite greatly increased the defect density in the matrix, leading to a decrease in the flexural strength (28.42 ± 5.50 MPa). After heat treatment at 1400 °C, some of the blocky matrix dissolved and filled partial pores, improving the flexural strength (42.60 ± 1.95) of the composites. The continuous increases in flexural modulus meant that the brittleness of the composites became stronger with increasing temperature.
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