The invention discloses a preparation method of a three-dimensional flower-cluster-shaped CdS QDs (at) ZnS / ZnO composite photocatalyst, belongs to the field of preparation of photocatalytic materials, and aims to solve the problem of relatively low photocatalytic efficiency. The preparation method comprises the following steps: 1, preparing
zinc oxide: dissolving Zn (CH3COO) 2.2 H2O in deionized water, stirring until Zn (CH3COO) 2.2 H2O is completely dissolved, adding NaOH, stirring to form an
emulsion, transferring the mixed
emulsion into a
polytetrafluoroethylene reaction kettle, and treating at 160 DEG C for 10 hours; 2, preparation of
cadmium sulfide quantum dots (CdS QDs): dropwise adding
thioacetamide (TAA) into a Cd (NO3) 2.4 H2O
aqueous solution, continuously stirring and dropwise adding a NaOH solution, adjusting the pH value of the solution to 10.5, then adding a Na2S solution, stirring at 65 DEG C for 1 h, cooling to
room temperature, and aging for 24 h; and 3, dissolving Zn (CH3COO) 2.2 H2O and TAA in deionized water, adding ZnO
powder, adding CdS QDs, and carrying out rapid stirring. Putting into a
microwave reaction instrument, reacting at 160 DEG C for 45 minutes, washing and
drying. The three-dimensional flower-cluster-shaped CdS QDs (at) ZnS / ZnO composite photocatalyst is prepared through a
microwave-assisted hydrothermal method, and the photocatalytic oxidation performance is effectively improved.