We report herein a simple strategy for fabricating two-dimensional (2D) petal-like NixCd1-xS/octadecylamine (ODA) hybrids exhibiting both photoluminescent and superhydrophobic properties via a facile liquid-liquid interfacial self-assembly technique. First, thioglycolic acid stabilized CdS quantum dots (QDs) doped with nickel were synthesized in aqueous solution. Then, relying on the facile H2O/CHCl3 interfacial platform, through the electrostatic interactions between positively charged amino groups of ODA and negatively charged carboxyl groups of a QD surface, we have successfully fabricated petal-like NixCd1-xS/ODA hybrids. These NixCd1-xS/ODA hybrids present enhanced photoluminescence compared with Ni(x)Cd(1-x)SQDs, especially in high quantum yield, which is enhanced from 3% to 50%. Moreover, the NixCd1-xS/ODA hybrid film has a water contact angle of 152.7 degrees, leading to its excellent hydrophobic property. Finally, by virtue of their excellent polymer compatibility and optical properties, we extended the robust QDs as "fluorescent ink" to print elegant photoluminescent patterns by silk-screen printing.