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In this work, we studied the impact of post-metallization annealing (PMA) on interfacial and bulk dielectric properties of AlSiO/β-Ga2O3 metal–oxide–semiconductor capacitors (MOSCAPs). Annealing at 300 °C improved the reverse operational stability within the test operation range from −10 V to −42 V. The near-interface fast and slow traps were both suppressed by PMA at 300 °C and 350 °C, leading to a negligible flat-band voltage hysteresis. The low gate leakage region was extended from 3.7 MV cm−1 to 4 MV cm−1 and the breakdown strength was improved from 7.8 MV cm−1 to 8.2 MV cm−1 for AlSiO/β-Ga2O3 MOSCAPs with PMA at 300 °C compared with not-annealed samples. The superior operational reliability demonstrated in this work is useful for future high-performance and reliable MOS-based Ga2O3 transistors. [ABSTRACT FROM AUTHOR]