Developing the most
straightforward, cheapest, and eco-friendly
approaches for synthesizing nanostructures with well-defined morphology
having the highest possible surface area to volume ratio is challenging
for design and process. In the present work, nanosheets of NiO and
β-Ni(OH)
2
/Co
3
O
4
, and nanorods
of Co
3
O
4
have been synthesized at a large scale
via the microwave-assisted chemical coprecipitation method under low
temperature and atmospheric pressure. X-ray absorption spectroscopy
(XAS) measurements, which comprises both X-ray absorption near-edge
structure (XANES) and extended X-ray absorption fine structure (EXAFS)
techniques, have been carried out at Co and Ni K-edges to probe the
electronic structure of the samples. Also, the local atomic structural,
chemical bonding, morphological, and optical properties of the sample
were systematically investigated using XAS, synchrotron X-ray diffraction
(SXRD), Raman spectroscopy, FTIR, transmission electron microscopy
(TEM), and UV–visible spectroscopy. The normalized XANES spectra
of the β-Ni(OH)
2
/Co
3
O
4
nanosheets
show the presence of Ni
2+
and a mixed oxidation state of
Co. The disorder factor decreases from β-Ni(OH)
2
/Co
3
O
4
to Co
3
O
4
with increasing
Co–O bond length. The SXRD pattern analyzed using Rietveld
refinement reveals that NiO has a face-centered cubic phase, Co
3
O
4
has the standard spinal structure, and β-Ni(OH)
2
/Co
3
O
4
has a mixed phase of hexagonal
and cubic structures. TEM images revealed the formation of nanosheets
for NiO and β-Ni(OH)
2
/Co
3
O
4
samples and nanorods for Co
3
O
4
samples. FTIR
and Raman spectra show the formation of β-Ni(OH)
2
/Co
3
O
4
, which reveals the fingerprints of Ni–O
and Co–O.