Here, we present the low-temperature (∼600 °C) solution combustion method for the fabrication of CoFe₂O₄, NiFe₂O₄, and Co_0.5Ni_0.5Fe₂O₄ nanoparticles (NPs) of 12-64 nm range in pure cubic spinel structure, by adjusting the oxidant (nitrate ions)/reductant (glycine) ratio in the reaction mixture. Although nitrate ions/glycine (N/G) ratios of 3 and 6 were used for the synthesis, phase-pure NPs could be obtained only for the N/G ratio of 6. For the N/G ratio 3, certain amount of Ni²⁺ cations was reduced to metallic nickel. The NH₃ gas generated during the thermal decomposition of the amino acid (glycine, H₂NCH₂COOH) induced the reduction reaction. X-ray diffraction (XRD), Raman spectroscopy, vibrating sample magnetometry, and X-ray photoelectron spectroscopy techniques were utilized to characterize the synthesized materials. XRD analyses of the samples indicate that the Co_0.5Ni_0.5Fe₂O₄ NPs have lattice parameter larger than that of NiFe₂O₄, but smaller than that of CoFe₂O₄ NPs. Although the saturation magnetization (M _s) of Co_0.5Ni_0.5Fe₂O₄ NPs lies in between the saturation magnetization values of CoFe₂O₄ and NiFe₂O₄ NPs, high coercivity (H _c, 875 Oe) of the NPs indicate their hard ferromagnetic behavior. Catalytic behavior of the fabricated spinel NPs revealed that the samples containing metallic Ni are active catalysts for the degradation of 4-nitrophenol in aqueous medium.

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