Magnetic nanoparticles of NiFe2O4 were successfully prepared by utilizing the sol–gel techniques. The prepared samples were investigated through various techniques such as X-ray diffraction (XRD), transmission electron microscopy (TEM), dielectric spectroscopy, DC magnetization and electrochemical measurements. XRD data analysed using Rietveld refinement procedure inferred that NiFe2O4 nanoparticles displayed a single-phase nature with face-centred cubic crystallinity with space group Fd-3m. Average crystallite size estimated using the XRD patterns was observed to be ~10 nm. The ring pattern observed in the selected area electron diffraction pattern (SAED) also confirmed the single-phase formation in NiFe2O4 nanoparticles. TEM micrographs confirmed the uniformly distributed nanoparticles with spherical shape and an average particle size of 9.7 nm. Raman spectroscopy showed characteristic bands corresponding to NiFe2O4 with a shift of the A1g mode, which may be due to possible development of oxygen vacancies. Dielectric constant, measured at different temperatures, increased with temperature and decreased with increase in frequency at all temperatures. The Havrilliak–Negami model used to study the dielectric spectroscopy indicated that a NiFe2O4 nanoparticles display non-Debye type relaxation. Jonscher’s power law was utilized for the calculation of the exponent and DC conductivity. The exponent values clearly demonstrated the non-ohmic behaviour of NiFe2O4 nanoparticles. The dielectric constant of the nanoparticles was found to be >300, showing a normal dispersive behaviour. AC conductivity showed an increase with the rise in temperature with the highest value of 3.4 × 10−9 S/cm at 323 K. The M-H curves revealed the ferromagnetic behaviour of a NiFe2O4 nanoparticle. The ZFC and FC studies suggested a blocking temperature of ~64 K. The saturation of magnetization determined using the law of approach to saturation was ~61.4 emu/g at 10 K, corresponding to the magnetic anisotropy ~2.9 × 104 erg/cm3. Electrochemical studies showed that a specific capacitance of ~600 F g−1 was observed from the cyclic voltammetry and galvanostatic charge–discharge, which suggested its utilization as a potential electrode for supercapacitor applications.
The presence of heavy metals in increased concentrations in the environment has become a global environmental concern. This rapid increase in heavy metals in the environment is attributed to enhanced industrial and mining activities. Metal ions possess a lengthy half-life and property to bioaccumulate, are non-biodegradable and, thus, are a threat to the human health. A number of conventional spectroscopic and chromatographic techniques are being used for the detection of heavy metals, but these suffer from various limitations. Nano-based sensors have emerged as potential candidates for the sensitive and selective detection of heavy metals. Thus, the present study was focused on the synthesis of selenium nanoparticles (SeNPs) by using selenite-reducing bacteria in the development of a heavy metal toxicity biosensor. During the biosynthesis of selenium nanoparticles, supernatants of the overnight-grown culture were treated with Na2SeO32− and incubated for 24 h at 37 °C. The as-synthesized nanoparticles were characterized by UV–Vis spectroscopy, X-ray diffraction (XRD), Fourier transform infrared (FTIR) and transmission electron microscopy (TEM) analyses. XRD and TEM results confirmed the formation of SeNPs in sizes ranging from 35 to 40 nm, with face-centered cubic (FCC) structures. The bioreduction process and validation of the formation of SeNPs was further confirmed by FTIR studies. The reduction in the biosynthesis of SeNPs using bacterial metabolite due to heavy metal cytotoxicity was analyzed by the colorimetric bioassay (SE Assay). The inhibition of selenite reduction and loss of red color in the presence of heavy metals may serve as a biosensor for heavy metal toxicity analysis. Thus, this biosensor development is aimed at improving the sensitivity and specificity of analytic detection.
Magnetic nanostructures of CoFe2O4 were synthesized via a microwave-assisted hydrothermal route. The prepared nanostructures were investigated using X-ray diffraction (XRD), field emission electron microscopy (FE-SEM), energy dispersive X-ray (EDX) spectroscopy, high-resolution transmission electron microscopy (HR-TEM), selective area electron diffraction (SAED) pattern, DC magnetization, and dielectric spectroscopy measurements. The crystal structure studied using HR-TEM, SAED, and XRD patterns revealed that the synthesized nanostructures had a single-phase nature and ruled out the possibility of any secondary phase. The lattice parameters and unit cell volume determined from the XRD data were found to be 8.4821 Å and 583.88 Å3. The average crystallite size (~7.0 nm) was determined using Scherrer’s equation. The FE-SEM and TEM micrographs revealed that the prepared nanostructures had a spherical shape morphology. The EDX results showed that the major elements present in the samples were Co, Fe, and O. The magnetization (M) versus temperature (T) measurements specified that the CoFe2O4 nanostructures showed ferromagnetic ordering at room temperature. The blocking temperature (TB) determined using the M-T curve was found to be 315 K. The magnetic hysteresis (M-H) loop of the CoFe2O4 nanostructures recorded at different temperatures showed the ferromagnetic behavior of the CoFe2O4 nanostructures at temperatures of 200 K and 300 K, and a superparamagnetic behavior at 350 K. The dielectric spectroscopy studies revealed a dielectric constant (ε′) and loss tangent (tanδ) decrease with the increase in the frequency, as well as demonstrating a normal dispersion behavior, which is due to the Maxwell–Wagner type of interfacial polarization. The values of ε′ and tanδ were observed to increase with the increase in the temperature.
BiFe1−xCrxO3, (0 ≤ x ≤ 10) nanoparticles were prepared through the sol–gel technique. The synthesized nanoparticles were characterized using various techniques, viz., X-ray diffraction, high-resolution field emission scanning electron microscopy (HRFESEM), energy dispersive spectroscopy (EDS), UV–Vis absorption spectroscopy, photoluminescence (PL), dc magnetization, near-edge X-ray absorption spectroscopy (NEXAFS) and cyclic voltammetry (CV) measurements, to investigate the structural, morphological, optical, magnetic and electrochemical properties. The structural analysis showed the formation of BiFeO3 with rhombohedral (R3c) as the primary phase and Bi25FeO39 as the secondary phase. The secondary phase percentage was found to reduce with increasing Cr content, along with reductions in crystallite sizes, lattice parameters and enhancement in strain. Nearly spherical shape morphology was observed via HRFESEM with Bi, Fe, Cr and O as the major contributing elements. The bandgap reduced from 1.91 to 1.74 eV with the increase in Cr concentration, and PL spectra revealed emissions in violet, blue and green regions. The investigation of magnetic field (H)-dependent magnetization (M) indicated a significant effect of Cr substitution on the magnetic properties of the nanoparticles. The ferromagnetic character of the samples was found to increase with the increase in the Cr concentration and the increase in the saturation magnetization. The Fe (+3/+4) was dissolved in mixed-valence states, as found through NEXAFS analysis. Electrochemical studies showed that 5%-Cr-doped BFO electrode demonstrated outstanding performance for supercapacitors through a specific capacitance of 421 F g−1 measured with a scan rate of 10 mV s−1. It also demonstrated remarkable cyclic stability through capacitance retention of >78% for 2000 cycles.
Herein, we present an electrocatalyst constructed by zinc oxide hexagonal prisms/phosphorus-doped carbon nitride wrinkles (ZnO HPs/P-CN) prepared via a facile sonochemical method towards the detection of nitrofurantoin (NF). The ZnO HPs/P-CN-sensing platform showed amplified response and low-peak potential compared with other electrodes. The exceptional electrochemical performance could be credited to ideal architecture, rapid electron/charge transfer, good conductivity, and abundant active sites in the ZnO HPs/P-CN composite. Resulting from these merits, the ZnO HPs/P-CN-modified electrode delivered rapid response (2 s), a low detection limit (2 nM), good linear range (0.01–111 µM), high sensitivity (4.62 µA µM−1 cm2), better selectivity, decent stability (±97.6%), and reproducibility towards electrochemical detection of NF. We further demonstrated the feasibility of the proposed ZnO HPs/P-CN sensor for detecting NF in samples of water and human urine. All the above features make our proposed ZnO HPs/P-CN sensor a most promising probe for detecting NF in natural samples.
Herein, for the first time, the growth of ZnO nanorods directly on aluminum (Al) substrate via a low temperature (80 °C) wet chemical method, and used as binder-free electrode for supercapacitors were reported. XRD pattern and HRTEM images showed that high crystalline nanorods grown on Al substrate with c-axis orientation. Morphological studies revealed that the nanorods possessed well defined hexagon phase with length and diameter of ~2 µm and 100–180 nm, respectively. Raman spectrum of ZnO nanorods showed that the characteristic E2H mode corresponds to the vibration associated with the oxygen atoms of ZnO. The optical properties of ZnO nanorods studied using Room-temperature PL spectra revealed a near-band-edge (NBE) peak at ~388 nm emission and deep level (DLE) at ~507 nm. Electrochemical measurements showed that ZnO nanorods on Al substrate exhibited remarkably enhanced performance as electrode for supercapacitors with a value of specific capacitance of 394 F g−1 measured with scan rate of 20 mV s−1. This unique nanorods structures also exhibited excellent stability of >98% capacitance retention for 1000 cycles that were measured at 1A g−1. The presented easy and cost-effective method might open up the possibility for the mass production of binder-free electrodes for efficient electrochemical energy storage devices.