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Application of GaAs-based metal-oxide-semiconductor (MOS) structures, as a “high carrier mobility” alternative to conventional Si MOS transistors, is still hindered due to difficulties in their preparation with low surface/interface defect states. Here, aluminum oxide as a passivation and gate insulator was formed by room temperature oxidation of a thin Al layer prepared in situ by metal-organic chemical vapor deposition. The GaAs-based MOS structures yielded two-times higher sheet charge density and saturation drain current, i.e., up to 4 × 1012 cm-2 and 480 mA/mm, respectively, than the counterparts without an oxide surface layer. The highest electron mobility in transistor channel was found to be 6050 cm2/V s. Capacitance measurements, performed in the range from 1 kHz to 1 MHz, showed their negligible frequency dispersion. All these results indicate an efficient suppression of the defect states by in situ preparation of the semiconductor structure and aluminum oxide used as a passivation and gate insulator.