CuS microcrystals were successfully prepared through a mild solvothermal reaction in ethylene glycol （EG） with the assistance of cationic surfactant cetyltrimethylammonium bromide （CTAB）. An interesting morphology evolution from flower-like microspheres to hollow microspheres, and finally to smooth nanoflakes was observed when increasing the amount of CTAB. The products were characterized by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, and UV-vis spectroscopy. It was found that the amount of CTAB played an important role in determining the morphology of the CuS microcrystals. Electrical measurement reveals that the as-prepared CuS microspheres were of high conductivity, which might favor their device applications. It is expected that CuS microcrystals with controlled morphologies and structures will have important applications in solar cells. This simple but effective method could also be extended to the controlled growth of other inorganic microcrystals.
