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A facile one-pot heating process without any injection has been developed to prepare different Cu-Zn-S-based nanocrystals.The composition of the products evolves from Cu(Ⅰ)-doped ZnS (ZnS∶Cu(Ⅰ)) nanocrystals to Cu1.94S-ZnS heterostructured nanocrystals, and finally to digenite nanocrystals just by controlling the molar ratios of zinc acetylacetonate (Zn(acac)2) to copper acetylacetonate (Cu(acac)2).Accompanying the composition transformation, the crystal phase of ZnS is changed from cubic zinc blende to hexagonal wurtzite.