In the present paper,with CoCl2 x 6H2O used as precursor, Co-doped ZnO diluted magnetic semiconductor (DMS) crystals were synthesized by hydrothermal method with KOH as mineralizer. The morphology, and the relative content and distribution uniformity of the surface and inner Co element of synthesized crystals were investigated by scanning electron microscope (SEM) and X-ray energy dispersive spectrometry (XREDS), respectively. It was found that Co-doped ZnO crystals with different morphology were yielded, while the bigger crystals showed polar growth charactertistics, and the Co content in the crystal depended on its morphology. The exposed face also changed with crystal morphology. There was more Co in bigger crystals than in smaller ones. Moreover, more Co located in +c (10 11)compared to +c (10 10) exposed face, especially for cone crystals. In addition, it was observed that there was a little amount of cobalt oxide cluster in inner crystal,and the distribution of Co content was relative uniform in both the surface and inner part of the crystal. Cobalt oxide cluster may have effect on the magnetic properties of Co-doped ZnO diulted magnetic semiconductor since Co2+ possesses magnetic property.