NiFe.O./SiO./NiO magnetic was successfully synthesized using NiFe.O., SiO,, and NiO as the core, interlayer, and shell, respectively. NiFe.O./SiO./NiO under UV light irradiation was used for photocatalytic degradation of methyl orange dye with different pH, catalyst dose, and initial dye concentration. This composite was characterized by X- ray Diffraction (XRD), Fourier Transform Infra-Red (FTIR), Scanning Electron Microscopy-Electron Dispersive X- ray Spectroscopy (SEM-ED), Vibrating Sample Magnetometer (VSM), UV-Vis Diffuse Reflectance Spectroscopy (UV-Vis DRS), and Point of Zero Charge (pHpzc). The results showed that the composite is a superparamagnetic material with a saturation magnetization value of 44.13 emu/g. It also has a band gap of 2.67 eV with a pHpze of 6.33. The optimum conditions for photocatalytic degradation were at pH of 4; 0.50 g/L catalyst dose, and 10 mg/L initial concentration. NiFe.O./SiO./Nio degradation efficiency to methyl orange dye was 95.76%. The photocata- lytic degradation in different concentrations follows the pseudo-first-order, where the greater the concentration, the smaller the constant rate (k). After five cycles of repeated usage, NiFe.O./SiO./NiO has good catalytic perfor- mance as well as efficient and favourable of a recyclable photocatalystCopyright (c) 2022 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0).