Chitosan/Boron nitride (BN) composites were prepared by solution method using CuSO4/glycine chelate complex as the catalysis with variable percentage of boron nitride loading. The dispersion of BN with the chitosan polymer was achieved with sonication at power of 120 W and frequency of 80 kHz. The chemical interactions of chitosan and BN were studied by Fourier transform infrared spectroscopy. The structure of chitosan and BN composites were investigated by XRD and TEM. It was observed that the BN were dispersed with chitosan matrix through intercalation. The quantitative identification of composites was investigated by Energy Dispersive X-ray Spectroscopy and Selected Area Electron Diffraction. Thermal stabilities of chitosan/BN composites were studied by thermogravimetric analysis. It was found that, the thermal stability of the chitosan/BN composites was increased compare with virgin chitosan. The oxygen barrier properties of chitosan/BN composites were measured using gas permeameter. A substantial reduction in oxygen permeability was observed increasing boron nitride concentrations by which the synthesized composite materials may applicable in packaging industry.