Reduced graphene oxide and nickel oxide composite was prepared by homogeneous coprecipitation and subsequent annealing. Characterizations show that NiO particles have a nanosheet-based microsphere structure and anchor uniformly on the surface of reduced graphene oxide platelets. As an anode for Li ion batteries, the composite has 1641mAhg−1 and 1097mAhg−1 specific capacities for the first discharge and charge, respectively, higher than the theoretical capacity of NiO. It shows an excellent cycling performance with a discharge capacity of 1041mAhg−1 after 50 cycles at a current of 100mAg−1, and has a good rate capacity with 727mAhg−1 at a current of 1600mAg−1. The results show a synergistic effect of nanosheet-based NiO microspheres and reduced graphene oxide platelets in the composite for improved electrochemical performance.