The paper presents comparative characteristics of ZnFe LDH obtained by co-precipitation and plasma treatment of colloidal solutions of zinc and iron oxides. Obtained layered structure were analyzed by XRD, TG and UV–vis characterizations, and evaluated by mixture of three dyes (Rhodamine B, Reactive Red 6C, and Methylene Blue) degradation under UV light irradiation. Obtained Zn
Fe layered structures exhibited improved photocatalytic activity for all three dyes. The use of underwater discharge plasma has broad prospects for obtaining new photocatalysts.