• An aqueous hybrid battery with Li 3 V 2 (PO 4 ) 3 @C as cathode and Zn as anode is proposed. • A uniform and dispersed morphology of Li 3 V 2 (PO 4 ) 3 @C was fabricated by freeze-drying assisted sol-gel method. • The effects of carbon content on morphology, structure and electrochemical properties of the materials were explored. In this paper, fast ion and electron delivery inside electrode materials, which is very crucial to the aqueous zinc-ion hybrid batteries (AZHBs), has been studied in order to achieve the excellent electrochemical performance. The Li 3 V 2 (PO 4 ) 3 @C (LVP@C) composites were successfully fabricated by freeze-drying assisted sol-gel method, and the effects of carbon content on the structure, morphology and electrochemical performance of LVP@C composites were investigated. XRD results suggested that the products were made up of an ideal monoclinic structure of LVP, and the structural changes of Li + intercalation and de-intercalation during charge-discharge process were verified. Particularly, the LVP@C-05 sample exhibits excellent crystallinity. SEM images presented that with the increase of carbon content, the size of particles is smaller, and the distribution of particles is more uniform and dispersed. Especially, the LVP@C-05 sample has the smallest and the most uniform dispersed particles. The charging-discharging results indicated that the LVP@C-05 sample delivers the highest initial capacity of 95mAh g −1 at the current density of 2C, and the capacity retention after 50th cycles is 91%. Even at 20C current density, the LVP@C-05 also shows an attractive discharge capacity as high as 67mAh g −1 . CV results presented that the ionic diffusion coefficient of the LVP@C-05 sample is the highest (2.59×10 −12 cm 2 s −1 ), compared to the value of LVP@C-0, LVP@C-03, LVP@C-07 sample. Besides, EIS and Nyquist plots fitting results indicated that the R ct of LVP@C-05 sample is the lowest (189.5 Ω), showing a lower charge transfer resistance and increasing the kinetics of the reaction.