A binary heterostructure of Au/ZnO nanocomposite is prepared in a novel way based on successive pulsed laser ablation of the two targets in an aqueous solution with varied pulse time. The development of the method allows generating a noble metal (Au) and metal oxide (ZnO) one after one to produce a novel heterostructure with a tunable shell applicable as a catalytic degradable material. The nanocomposite samples are tested to study their optical, morphological, and structural properties. The photocatalytic degradation study demonstrates a significant decrease in the absorbance intensity of Rohdamin B (RhB) dye as the irradiation time increases. It indicates a reduction in dye concentration with a remarkable improvement in contact time. Besides, the degradation percentage against pH value is investigated. It reveals an increasing trend as the pH value rises with a maximum percentage at pH 10. The study is also concerned with the influence of the initial concentration of RhB dye on the degradation efficiency of the nanocomposite. Higher initial concentrations of the dye lead to a decrease in the degradation efficiency of the catalysts. Finally, the kinetic analysis of RhB photodegradation reveals that the Langmuir-Hinshelwood first-order kinetic model accurately describes RhB's adsorption onto the nanocomposites.