Single ZnIn₂S₄ or Zn-In-S composites were synthesized by a simple low temperature (80 °C) method assisted by the presence of NaCl. The products were characterized by XRD, SEM, TEM, TG/DTA, ICP-AES, BET and UV-Vis absorption spectrometry. The decomposition of thioacetamide (TAA) at low temperature was investigated by UV-Vis absorption spectrometry. The decomposition rate of TAA and NaCl concentration influenced the composition, structure, morphology and grain size of the products. The obtained samples are marigold-like microspheres consisting of nanosheets. Loading 0.10 wt% Pt on the samples by in situ photoreduction, allowed the photocatalytic activity of the prepared samples to be evaluated by hydrogen evolution from aqueous solution containing triethanolamine as the electron donor under visible light (λ ≥ 420 nm) irradiation. The activity of the sample obtained in the presence of 0.50 mol L⁻¹ NaCl is ca. 5 times higher than samples without NaCl. Thus, a photocatalyst with layered structure is beneficial for photoactivity. A possible mechanism is discussed.