Na3V2(PO4)3/C (NVP/C) in aqueous Zn-ion batteries cathode material was prepared by spray drying method and studied by changing the calcination temperature and calcination time. The effects of different calcination temperature and calcination time on the performance of NVP/C were investigated. The structure and morphology of NVP/C were characterized by XRD, SEM and BET, and the electrochemical performance of the sample was analyzed by cyclic voltammetry and charge and discharge test. The results show that all the samples obtained at different calcination temperature and calcination time are pure NVP/C, and do not change the crystal structure of NVP/C. Higher calcination temperatures or longer calcination times can lead to the particle size enlarges and the performance decays rapidly. The calcination temperature of 700 ℃ and calcination time of 8 h are optimal synthesis conditions of NVP/C materials. The samples synthesized in this condition possess a regular appearance, good crystallinity, low impedance and excellent ion diffusion, thus showing the best electrochemical performance. It exhibits the best discharge specific capacity of 122.4 mA·h/g at 0.1 A/g. Moreover, the capacity still reaches 103.9 mA·h/g after 200 cycles at 1.0 A/g.