en Research Paper Research Paper <p style="text-align: justify;">In this work, we report the synthesis of silver decamolybdate, Ag₆Mo₁₀O₃₃, nanostructure by a simple mechanohemical process followed by calcination treatment using acetamide as driving agent. Morphological study by scanning electron microscopy (SEM) images revealed bundles of rods grown closely together with an average diameter of 92 nm for Ag₆Mo₁₀O₃₃sample. Ni-substituted Ag₆Mo₁₀O₃₃ compound was prepared <em>via</em> introducing nickel cation to precursor system in mechanical milling step. The particle size decreased to 87 nm by incorporating nickel units in substituted polymolybdate. It was concluded that the suitable selection of reagents can direct solid phase reaction towards producing nanostructured products. This technique is easy and simple for preparation of various mixed metal oxides without using any solvents and or complex procedures. In addition, the photocatalytic activity of the prepared products was studied on the removal of 4-nitro phenol (4-NP) as organic pollutant from water. The obtained results were also discussed in detail.</p> Mechanochemical reaction, Polyoxometalate, Nanostructure, Photocatalytic characteristic. 48 53 http://ijmse.iust.ac.ir/browse.php?a_code=A-10-399-1&slc_lang=en&sid=1 A. Tadjarodi tajarodi@iust.ac.ir 180031947532846005547 180031947532846005547 Yes Research Laboratory of Inorganic Materials Synthesis, Department of Chemistry, Iran University of Science and Technology, Tehran, 16846-13114, Iran M. Imani mimani@chem.iust 180031947532846005548 180031947532846005548 No Research Laboratory of Inorganic Materials Synthesis, Department of Chemistry, Iran University of Science and Technology, Tehran, 16846-13114, Iran A. Iraji zad iraji@sharif.edu 180031947532846005549 180031947532846005549 No Department of Physics, Sharif University of Technology, Tehran, Iran 2Institute for Nanoscience and Nanotechnology (INST), Sharif University of Technology, Tehran 11155-9161, Iran