The growth of the textile industry results in a massive accumulation of dyes on water. This enormous rise in pigments is the primary source of water pollution, affecting the aquatic lives and our ecosystem balance. This study aims to notify the fabrication of neodymium incorporated copper oxide (Nd2O3 doped CuO) nanoparticles by combustion method for effective degradation of dye, methylene blue (MB). X-ray diffraction (XRD), Field emission Scanning electron microscopy (FESEM), Zeta potential have been applied for characterization. Photocatalyst validity has been evaluated for methylene blue degradation (MB). Test conditions such as time of contact, H2O2, pH, and photo-Fenton have been modified to identify optimal degradation conditions. Noticeably, 7.5% Nd2O3 doped CuO nanoparticle demonstrated the highest photocatalytic efficiency, up to 90.8% in 80 min, with a 0.0227 min−1 degradation rate. However, the photocatalytic efficiency at pH 10 becomes 99% with a rate constant of 0.082 min−1. Cyclic experiments showed the Nd2O3 doped CuO nanoparticle’s stability over repeated use. Scavenge hydroxyl radical species responsible for degradation using 7.5% Nd2O3 doped CuO nanoparticles have been investigated under visible irradiation.