Nanostructured As2Ni3O8 samples were synthesized via facile solid state reactions at 850 and 950 °C for 8h using As2O3, Ni(CH3COO)2.2H2O and Ni(NO3)2.6H2O raw materials. The synthesized nanomaterials were characterized by powder X-ray diffraction (PXRD) technique and fourier-transform infrared (FTIR) spectroscopy. The rietveld analyses showed that the obtained materials were crystallized well in monoclinic crystal structure with the space group P121/c1. The lattice parameters of the targets were about a = 5.76 Å, b = 9.54 Å and c = 10.18 Å with β = 92.95 °. It was found that nickel nitrate created a highly crystalline and pure As2Ni3O8 structure. However, nickel acetate created the target with lower purity and crystal phase growth; it produced the samples with smaller crystallite sizes. Reaction temperature changing showed that the parameter affected on the crystal growth of the obtained materials. The morphologies of the synthesized materials were studied by field emission scanning electron microscopy (FESEM) technique. Ultraviolet-visible spectra showed that the synthesized As2Ni3O8 nanomaterials had strong light absorption in the ultraviolet - visible light region. The direct optical band gaps were 2.6 and 2.5 eV for S1 and S3, respectively. The data showed that the band gaps were decreased by increasing the reaction temperature. This is due to the increasing the crystallite sizes of the obtained materials. تفاصيل المقالة