MoS₂ nanomaterials with different morphologies such as nanoplates, nanowalls, and 3D microspheres composed of ultrathin nanoflakes were synthesized via a simple solid-phase reaction process. The structure and morphology of these samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer–Emmett–Teller analysis (BET). The electrochemical test behavior of the as-prepared MoS₂ nanostructure electrodes were also investigated and the results indicated that the 3D MoS₂ microsphere electrode exhibits a high discharge capacity of 850.9 mA h g⁻¹ at 100 mA g⁻¹ after 50 cycles, which displays higher specific capacity and cycling stability than other as-prepared samples. Moreover, the reversible capacity for the 3D MoS₂ microspheres can still be maintained at 783.5 mA g⁻¹ at 800 mA g⁻¹. The enhanced electrochemical performance of the 3D MoS₂ microspheres could be attributed to their spherical structure, the ultrathin nanoflakes, high specific surface area and their unique layered structure.