The low-cost sol-gel combustion method is used to create nickel-doped copper ferrite (NixCu1-xFe2O4 where x = 0, 0.5 and 1.0) nanoparticles with di-ethanolamine as a size-reducing agent. The temperature effect on X-ray Diffraction (XRD), combined with the Jana2006 refinement result suggested that 500 0C is an optimum temperature for obtaining phase pure CuFe2O4 and NiFe2O4 nanoparticles. The phase fraction, lattice parameters, unit cell volume, micro strain, crystallite size and dislocation density are also reported. Strain-induced broadening of the structural properties of CuFe2O4 and NiFe2O4 nanoparticles is analysed using the Williamson–Hall plot. Activation energy analysis revealed that 4.93 kJ/mol and 4.45 kJ/mol of energy are required to produce the CuFe2O4 and NiFe2O4 nanoparticles, respectively. Indistinguishable particle morphology with partial agglomeration was observed in the SEM results. Direct and indirect band gap values are found to decreases with increasing x values. Biological Oxygen Demand (BOD) and Chemical Oxygen Demand (COD) results revealed that reductions for COD and TOC vary from 93 to 95%, while the BOD/COD rate changes from 0.13 to 0.57. The 18-fold increase in the BOD/COD ratio led to a significant improvement in the biodegradability of the industrial wastewater.