Metal-insulator-semiconductor structures are fabricated by depositing SiO2 films on an MOCVD-grown n-type GaN epitaxial layer and a GaN/Al0.4Ga0.6N/GaN double heterojunction. The SiO2 films are grown by plasma-enhanced chemical vapor deposition. High-frequency C-V characteristics show the agreement of the measured C-V curve of SiO2/n-GaN with an ideal curve in deep depletion and the very small hysteresis, which indicates that the interface traps concentration in the sample is low. However, for SiO2/GaN/Al0.4Ga0.6N/GaN, the measured C-V curves show a notable flat-band shift of about 9.2 V and a typical polarization hysteresis window. These show the influence of the polarization charges in this structure. The capacitance on SiO2/GaN/Al0.4Ga0.6N/GaN reaches a minimum value under around –5V bias. The saturation at a minimum value of the C-V curve indicates the presence of holes accumulation in the MIS structure. These results imply that the piezoelectric effect in GaN/Al0.4Ga0.6N/GaN play an important role for the formation of the p-channel.