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Although utilization of diverse classes of metal oxides as hydrogen storage materials has been reported, but there is still a major need to introduce efficient materials. Herein, mesoporous Zn2V2O7 nanostructures were produced by a new sonochemical method using hydrazine, zinc nitrate, and ammonium vanadate as the starting reagents and then annealed at 700 °C. Prior to annealing, Zn3V3O8 was produced in the presence of ultrasonic waves, whereas in the absence of ultrasonic waves, Zn2(VO4)2 was the major product. In fact, ultrasonic waves interfered with the reaction mechanism and reduced V5+ to V4+ and V3+. Because of the proper composition and structure of these nanostructures, they were used for electrochemical storage of hydrogen. Storage of over 2899 mAh/g after 20 cycles by flower-like nanostructures revealed their high capability. The results also showed that morphology affects efficiency such that three-dimensional spherical nanostructures had a storage capacity of 2247 mAh/g after 20 cycles.