The electrical characteristics and reliability of the aluminum oxide (Al 2 O 3 ) metal-oxide-semiconductor (MOS) capacitors were investigated under low-temperature process consideration. The simple cost-effective technique in preparing the Al 2 O 3 /SiO 2 bilayer structure as the high-k gate dielectrics was demonstrated in this paper. SiO 2 was prepared by roomtemperature anodic oxidation, and Al 2 O 3 was fabricated by room-temperature in situ natural oxidation during the dc sputtering of aluminum in Ar/O 2 ambient. Compared to the Al 2 O 3 MOS capacitors without nitric acid (HNO 3 ) compensation, significant improvements in electrical characteristics, reliability, and uniformity were achieved by utilizing HNO 3 to moderately oxidize the existing Al 2 O 3 layer. In addition, the charge trapping behaviors of our samples were also studied by time-dependent dielectric breakdown under the 1000-s constant voltage stress and constant current stress tests. It was found that the electron trapping is dominant under a low negative bias stress. However, under a high negative bias stress, the Al 2 O 3 MOS capacitors show hole trapping due to the impact ionization near the SiO 2 /Si interface. The in situ oxidation in sputtering with HNO 3 compensation is suitable for future low-temperature dielectric applications.Index Terms-Al 2 O 3 , anodic oxide, HNO 3 compensation, low temperature, metal-oxide-semiconductor (MOS) capacitor.