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Thermal gravimetric analysis (TGA) and differential thermal analysis (DTA) are employed to investigate the thermal decomposition behaviour of zinc nitride powder, which indicated that the thermal oxidation of zinc nitride powder in air follows the two-step reaction model.When the temperature is between 200 and 500℃,compact ZnO or ZnxOyNz layers in the surface of zinc nitride powder will begin to form, and prevent the interior of zinc nitride powder from the thermal oxidation.When the temperature is higher than 500 ℃, fast thermal oxidation occurs in the interior of zinc nitride powder.Over 750 ℃, all the zinc nitride will tu into zinc oxide.The x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) of the zinc nitride powder annealed at different temperature in air are consistent with the two-step reaction model.