The new nanocrystalline composition was synthesized using NiSO 4 and MoO 3 and PPDA (p-phenylenediamine) via the hydrothermal method. The structure, morphology and photoluminescence property of nanocrystal were studied using X-ray diffraction (XRD), Fourier transform infra red (FT-IR) spectroscopy, scanning electron microscopy (SEM), photoluminescence (PL) spectra, thermogravimetric analysis (TGA-DTA) and energy-dispersive X-ray spectroscopy (EDX). The effect of factors such as type and concentration of initial materials, pH values, temperature and reaction duration on the structure and morphology of nanocrystals was investigated in the preparation of composition. The results show that the pH of the initial solution affects the size of the prepared nanocrystals; the size of the crystals is increased and the morphology of the nanostructures is changed with the increment in pH value. According to the obtained results, neutral or low alkaline conditions of pH are more favorable for the formation of the nanocrystals. The obtained nanocrystal shows an intense PL emission at room temperature with a maximum peak at 461 nm and excitation at the wavelength of 300 nm. TGA and DTA analysis display a total weight loss of 13.42%.

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