<![CDATA[NiFe2O4 nanoparticles had been successfully synthesized by solution combustion method using urea fuel (organic precursor). The synthesized NiFe2O4 were characterized by X-ray diffraction (XRD), Scanning electron microscopy-Electron Dispersive X-ray Spectroscopy (SEM-EDs), Transmission Electron Microscopy (TEM), Fourier Transform Infra-Red (FTIR), Vibrating Sample Magnetometer (VSM), UV-Vis Diffuse Reflectance Spectroscopy (UV-Vis DRS), and Point of Zero Charge (pHpzc). NiFe2O4 nanoparticles irradiated with visible light were employed to degrade Congo red dye with the following variable: solution pH (3–8), H2O2 concentration (0.5–3 mM), and Congo red concentration (100–600 mg/L). XRD analysis results showed that the NiFe2O4 nanoparticles had a cubic spinel structure. The particle sizes are in the range of 10–40 nm. The magnetic properties of NiFe2O4 nanoparticles determined using VSM showed a magnetization saturation value of 47.32 emu/g. UV-Vis DRS analysis indicated that NiFe2O4 nanoparticles had an optical band gap of 1.97 eV. The success of synthesis was also proven by the EDS analysis results, which showed that the synthesized NiFe2O4 nanoparticles composed of Ni, Fe, and O elements. The removal efficiency of Congo red dye was 96.80% at the following optimum conditions: solution pH of 5.0, H2O2 concentration of 2 mM, Congo red dye concentration of 100 mg/L, and contact time of 60 min. The study of the photodegradation kinetics follows a pseudo-first order reaction with a rate constant value of 0.0853 min−1. Copyright © 2021 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). ]]>
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