Equimolar concentrations
of Zr4+ and Bi3+ were chelated with ethylenediaminetetraacetic
acid ligand with the purpose of using it as a precursor to generate
pyrochlore-like Bi2Zr2O7. When the
X-ray amorphous precursor was calcined at 750 °C for 3 h in air,
pyrochlore-like product with superstructure reflections was identified
by powder X-ray diffraction (PXRD) along with one minor reflection
due to β-Bi2O3. This phase was found to
be metastable from additional experiments conducted by varying calcination
conditions. Structural refinement of PXRD pattern by Le Bail method
in Fd3̅m space group yielded
cubic lattice constant of 10.8421(27) Å. Flower-petal-like morphology
of the sample was evident in its field-emission scanning electron
microscopy image and energy-dispersive X-ray analysis performed at various locations of the specimen
confirmed nearly equal concentration of zirconium and bismuth. Six
bands at 260, 320, 448, 531, 597, and 828 cm–1 were
observed for this sample in its Raman spectrum and supported our claim
of pyrochlore-like structure. Indexation of bright spots present in
selected area electron diffraction pattern and observed distances
of lattice fringes in high-resolution transmission electron microscopy
image were in conformity with the results from PXRD measurements.
Absorbance maxima at 312, 372, and 423 nm with a broad tailing stretching
up to visible region was noticed in the UV–visible spectrum
of this sample. Direct band gap of 2 eV was estimated for this sample
from Tauc plot. The oxygen ion conductivity of the sample in the temperature
range of 333–773 K was examined, and the highest conductivity
at 773 K was 3.071 × 10–6 S/cm. From activation
energy estimation and dielectric loss analysis, thermally activated
process related to the mobility of oxygen ion vacancy was found responsible
for the observed ionic conductivity. A similar conclusion was reached
after careful analysis of dielectric spectroscopy data of this sample.
High surface area (125.04 m2/g) and mesoporosity (pore
diameter of 3.81 nm) were possessed by this sample, which paved way
for studying its catalytic role in the reduction of nitroaromatics
and carcinogenic Cr6+. Cyclability experiments showed the
retainment of catalytic activity up to five cycles by the sample without
undergoing any structural change.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.