An investigation on the thermally induced interface degradation of Si3N4/Si/p-GaAs metal– insulator–semiconductor (MIS) structures is presented. We characterize the mutation of chemical identities by in situ angle-resolved x-ray photoelectron spectroscopy and the nature of an insulator and interface by a variable angle spectroscopic ellipsometry after high temperature annealing. The minimum interface state density of the Si3N4/Si/p-GaAs MIS capacitor as determined by capacitance–voltage and conductance loss measurements was about 8×1010 eV−1 cm−2 near GaAs midgap after rapid thermal annealing at 550 °C in N2. However, this density increased to 5×1011 eV−1 cm−2 after annealing at 750 °C in N2. The underlying mechanisms responsible for this degradation are described.

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