ZnCo2O4 nanocluster particles (NCPs) were prepared through a designed hydrothermal method, with the assistance of a surfactant, sodium dodecyl benzene sulfonate. The crystalline structure and surface morphology of ZnCo2O4 were investigated by XRD, XPS, SEM, TEM, and BET analyses. The results of SEM and TEM suggest a clear nanocluster particle structure of cubic ZnCo2O4 (~100 nm in diameter), which consists of aggregated primary nanoparticles (~10 nm in diameter), is achieved. The electrochemical behavior of synthesized ZnCo2O4 NCPs was investigated by galvanostatic discharge/charge measurements and cyclic voltammetry. The ZnCo2O4 NCPs exhibit a high reversible capacity of 700 mAh g−1 over 100 cycles under a current density of 100 mA g−1 with an excellent coulombic efficiency of 98.9% and a considerable cycling stability. This work demonstrates a facile technique designed to synthesize ZnCo2O4 NCPs which show great potential as anode materials for lithium ion batteries. ; Graphical Abstract :