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Abstract: Porous spheres of CuSCN nanoparticles with an average diameter of 0.4–0.6 μm have been prepared by a simple reaction between CuO suspension, NH2OH and KSCN in the presence of gelatin at 10 °C. Gelatin played a decisive role as an inhibitor of the direct attack of NH2OH, KSCN to CuO surfaces and coagulation of the growing CuSCN in producing porous spheres. The products were characterized by X-ray powder diffraction, transmission electron microscopy, and X-ray photoelectron spectra techniques. [Copyright &y& Elsevier]