Abstract: Silver iodide nanoclusters were successfully prepared in the channels of NaZSM-5 zeolite by a thermal diffusion method. Chemical analysis, powder X-ray diffraction, nitrogen adsorption technique, and infrared spectroscopy were used to characterize the prepared samples. The solid diffuse reflectance absorption spectra and luminescence properties were studied. Chemical analysis showed that the guest silver iodide was incorporated into the host NaZSM-5. Powder X-ray diffraction analysis showed that the framework of NaZSM-5 still remained in the (NaZSM-5)-AgI samples. Infrared spectra indicate that the vibration of the framework of NaZSM-5 had little variation attributable to the encapsulation of AgI in the host. This phenomenon is due to the incorporation of silver iodide into NaZSM-5. Investigation of the absorption revealed that the guest silver iodide was encapsulated in the channels of NaZSM-5. Solid diffuse reflectance absorption spectra indicated that the absorption of prepared (NaZSM--5)-AgI host-gust samples had nothing with the host NaZSM-5. The absorption spectra of the (NaZSM-5)-AgI samples were influenced by the size of AgI nanoclusters. Luminescence investigation showed that the prepared samples had a high energy band gap and a strong radiation process. The (NaZSM-5)-AgI samples are luminescient composite materials.