In this research, Ag2ZnI4/AgI nanopowders were synthesized by a novel and easy way. To find the optimal conditions for the synthesis of nanopowders, the influence of some synthesis factors was studied. The results of this investigation indicated that the grain size and morphology of Ag2ZnI4/AgI nanopowders were appreciably affected via the studied factors. The as-synthesized Ag2ZnI4/AgI were characterized with FT-IR, FESEM, EDS and XRD. The obtained outcomes revealed that with the aid of this new method can be prepared the sphere-like Ag2ZnI4/AgI nanopowders with desirable uniformity. Also, the photocatalyst performance of as-synthesized Ag2ZnI4/AgI nanopowders was examined via elimination of the organic contamination under UV illumination.