Here,
we present the low-temperature (∼600 °C) solution combustion method for the fabrication
of CoFe
2
O
4
, NiFe
2
O
4
, and
Co
0.5
Ni
0.5
Fe
2
O
4
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
Ni
2+
cations was reduced to metallic nickel. The NH
3
gas generated during the thermal decomposition of the amino
acid (glycine, H
2
NCH
2
COOH) 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
0.5
Ni
0.5
Fe
2
O
4
NPs have lattice parameter larger than that
of NiFe
2
O
4
, but smaller than that of CoFe
2
O
4
NPs. Although the saturation magnetization (
M
s
) of Co
0.5
Ni
0.5
Fe
2
O
4
NPs lies in between the saturation magnetization
values of CoFe
2
O
4
and NiFe
2
O
4
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.