MoS2 with (001) plane supported on carbon nanospheres (CNs) has been successfully synthesized by a facile solvothermal process. The effect of solvent and temperature on the growth of MoS2/CNs has been investigated, respectively. XRD results show that (001) plane of MoS2 was synthesized when using mixture solvent of N, N-dimethylformamide (DMF) and H2O. The electrochemical measurements show that MoS2/CNs samples with (001) plane have the enhanced hydrogen evolution reaction (HER) activity than MoS2/CNs without (001) plane. The effect of solvothermal temperature on (001) plane of MoS2 has been investigated. XRD results demonstrate the different interlayer spacing of 9.7 angstrom, 9.8 angstrom and 9.4 angstrom of (001) plane corresponding to 160, 200 and 240 degrees C, respectively, which may affect the electronic structure of MoS2 and bring different HER activity. TEM reveals the good interface adhesion between MoS2 and CNs at 200 degrees C, which may provide better conductivity and faster electron transfer rate. MoS2/CNs with the largest (001) distance obtained at 200 degrees C has the better HER activity than other samples synthesized at other temperatures. Therefore, tuning (001) plane of MoS2 under optimized conditions including solvent and temperature may be a facile way to prepare excellent HER electrocatalysts. (C) 2016 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.