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Abstract : In this present study, pure and Ni2+ (3, 7, and 10% mol.)-substituted SnO2 nanoparticles (NPs) were synthesized by sol-gel method. The prepared samples were characterized by powder XRD, FT-IR, FE-SEM, HR-TEM, EDX, UV-visible spectra, room temperature (RT) photoluminescence (PL) spectroscopy, and VSM techniques. XRD study revealed the polycrystalline tetragonal rutile structure of pure and Ni2+-substituted SnO2 NPs. Crystallite size of pure and Ni2+-substituted SnO2 NPs were found to be 26 to 34 nm in range. FT-IR study confirmed the presence of metal-oxide (M-O) bond vibrations for pure and Ni-substituted SnO2 NPs. FE-SEM, EDX, HR-TEM, and SAED pattern indicated that pure and Ni2+-substituted SnO2 NPs are well-defined formation of spherical-sized nanocrystallites, with diameter of about 10–40 nm of grain size. UV-Vis spectrum specified a sharp absorption peak ~ 425 nm representing the band to band transition. RT-PL study showed the peak ~ 467 nm for all samples, indicating the band gap of 2.65 eV. The higher value of Ms is found to be 0.0429 emu/g for Ni-substituted SnO2 NPs. Magnetic study revealed that the Ni-substituted SnO2 NPs presented ferromagnetism. Photocatalytic degradation (PCD) of methylene blue (MB) was analyzed using photo-catalytic reactor and obtained the maximum of PCD efficiency of 3% Ni-substituted SnO2 NPs under the visible light irradiation.