Abstract: Carboxymethyl hemicellulose was modified by the carboxymethylation reaction which extracted from bamboo. The hemicellulose/chitosan/graphene oxide composite films were prepared from the obtained carboxymethyl hemicelluloses, chitosan and grapheme oxide, which possessed excellent mechanical and oxygen barrier properties. The properties of the composite films were analyzed by FT-IR, XRD, SEM, TGA, mechanical strength and oxygen barrier tests. The different contents of graphene oxide were detected to analyze the effects of structure and properties of the composite films. The matrix of CMH, CS, GO were combined mainly through ion bond and hydrogen bond, and the GO was dispersed uniformly in CMH/CS matrix. Therefore, the surface of the film was smooth and dense with regular layered structure. The mechanical properties and thermal stability of the composite films were obviously improved by the addition of GO, which was due to the enhancement of GO in the whole composite system. The oxygen barrier ability of the composite film was also increased. The best mechanical properties of composite membranes were as follows:the tensile stress was 73.63 MPa, the tensile strain was 20.24%, and Young's modulus was 2.28 GPa when the content of graphene oxide was 0.5%. Meanwhile, it performed the best oxygen barrier property when the content of graphene oxide was 0.5%, and the gas permeation coefficient of the film was reached to 3.793 cm³·cm/(m²·s·Pa). The initial decomposition and maximum loss ratio temperature of the FG_0.5 were 242.4 and 274.5℃, respectively.