The present work explores the structural,
microstructural, optical,
magnetic, and hyperfine properties of Co
0.3
Zn
0.7
Fe
2
O
4
microspheres, which have been synthesized
by a novel template-free solvothermal method. Powder X-ray diffraction,
electron microscopic, and Fourier transform infrared spectroscopic
techniques were employed to thoroughly investigate the structural
and microstructural properties of Co
0.3
Zn
0.7
Fe
2
O
4
microspheres. The results revealed that
the microspheres (average diameter ∼121 nm) have been formed
by self-assembly of nanoparticles with an average particle size of
∼12 nm. UV–vis diffuse reflectance spectroscopic and
photoluminescence studies have been performed to study the optical
properties of the sample. The studies indicate that Co
0.3
Zn
0.7
Fe
2
O
4
microspheres exhibit
a lower band gap value and enhanced PL intensity compared to their
nanoparticle counterpart. The outcomes of dc magnetic measurement
and Mössbauer spectroscopic study confirm that the sample is
ferrimagnetic in nature. The values of saturation magnetization are
76 and 116 emu g
–1
at 300 and 5 K, respectively,
which are substantially larger than its nanosized counterpart. The
infield Mössbauer spectroscopic study and Rietveld analysis
of the PXRD pattern reveal that Fe
3+
ions have migrated
from [B] to (A) sites resulting in the cation distribution: (Zn
2+
0.46
Fe
3+
0.54
)
A
[Zn
2+
0.24
Co
2+
0.3
Fe
3+
1.46
]
B
O
4
. Comparison of
electrochemical performance of the Co
0.3
Zn
0.7
Fe
2
O
4
microspheres to that of the Co
0.3
Zn
0.7
Fe
2
O
4
nanoparticles reveals
that the former displays greater specific capacitance (149.13 F g
–1
) than the latter (80.06 F g
–1
)
due to its self-assembled porous structure. Moreover, it was found
that Co
0.3
Zn
0.7
Fe
2
O
4
microspheres
possess a better electrochemical response toward H
2
O
2
sensing than Co
0.3
Zn
0.7
Fe
2
O
4
nanoparticles in a wide linear range.