Abstract: Organic reagents can be used as a driving agent to synthesize a wide spectrum of nanomaterials.  In this work, nickel molybdate (NiMoO4) nanoparticles with a pure monoclinic crystalline phase were synthesized by using a facile one step microwave heating technique in solid state within a few minutes. Ammonium hepta molybdate tetrahydrate and nickel nitrate hexahydrate as initial materials were mixed to each other without any solvent and put into a domestic microwave oven with one step scheduled run. We introduced an alternative route of power input into chemical reactions in solid state by using microwave radiation.  In fact, the obtained results can draw an outlook of the effectiveness and feasibility of this technique for the synthesis of various nanoparticles. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion of x-ray spectrometry (EDX) were used to characterize the prepared product.  The study of photocatalytic behaviour of the resulting product indicated a high capability on the removal of Methylene Blue (MB) from aqueous solution.