Abstract: | Cube‐shaped CuInS2 nanoparticles were successfully prepared through a simple low‐temperature solution route. Mercaptoacetic acid was used as capping agent. The product was characterized by means of X‐ray diffraction (XRD), energy dispersive analysis of X‐rays (EDAX), transmission electron microscopy (TEM), and photoluminescence spectroscopy (PL). The CuInS2 nanocubes obtained were of a chalcopyrite structure. The EDAX analysis shows that as‐synthesized CuInS2 nanocubes were slightly Cu‐rich and nearly stoichiometric. |