Graphite oxide(GO) was prepared by the pressurized oxidation method and incorporated into polyimide(PI) matrix to fabricate high-k composite films by in-situ polymerization and subsequent thermal treatment. The results show that the as-prepared GO had good dispersion and compatibility in PI matrix due to the introduction of abundant oxygen-containing functional groups during the oxidation. The residual graphitic domains and the thermal treatment induced reduction of GO further enhanced the dielectric permittivity of the resulting GO–PI composites. The dielectric permittivity of the GO–PI composites exhibited a typical percolation behavior with a percolation threshold of 0.0347 of volume ratio and a critical exponent of 0.837. Near the percolation threshold, the dielectric permittivity of the GO–PI composite increased to 108 at 10~2 Hz and was 26 times that of the pure PI.
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