Showing papers by "L. John Kennedy published in 2014"

Synthesis, characterization of nickel aluminate nanoparticles by microwave combustion method and their catalytic properties

Abstract: Microwave combustion method (MCM) is a direct method to synthesize NiAl 2 O 4 nanoparticles and for the first time we report the using of Sesame ( Sesame indicum L.) plant extract in the present study. Solutions of metal nitrates and plant extract as a gelling agent are subsequently combusted using microwave. The structure and morphology of NiAl 2 O 4 nanoparticles are investigated by X-ray diffraction (XRD), Fourier transforms infrared spectra (FT-IR), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis (EDX), high resolution transmission electron microscopy (HR-TEM), diffuse reflectance spectroscopy (DRS) and photoluminescence (PL) spectroscopy, Brunauer–Emmett–Teller (BET) analysis and vibrating sample magnetometer (VSM). XRD pattern confirmed the formation of cubic phase NiAl 2 O 4 . The formation of NiAl 2 O 4 is also confirmed by FT-IR. The formation of NiAl 2 O 4 nanoparticles is confirmed by HR-SEM and HR-TEM. Furthermore, the microwave combustion leads to the formation of fine particles with uniform morphology. The magnetic properties of the synthesized NiAl 2 O 4 nano and microstructures were investigated by vibrating sample magnetometer (VSM) and their hysteresis loops were obtained at room temperature. Further, NiAl 2 O 4 prepared by MCM using Sesame ( S. indicum L.) plant extract is tested for the catalytic activity toward the oxidation of benzyl alcohol.

Comparative investigation of structural, optical properties and dye-sensitized solar cell applications of ZnO nanostructures.

Abstract: Dye-sensitized solar cells (DSSCs) based on ZnO nanostructures with two different morphologies, such as nanowires (ZNWs) and nanoparticles (ZNPs), were synthesized by microwave combustion (MCM) and conventional combustion (CCM) method. The obtained ZnO nanostructures were characterized by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), high resolution transmission electron microscopy (HR-TEM), energy dispersive X-ray analysis (EDX), diffuse reflectance (DRS) and photoluminescence (PL) spectroscopy. The XRD results confirmed the formation of hexagonal wurtzite ZnO. The crystallite size of the ZnO nanostructures was calculated using Sherrer's formula. The formation of ZNWs and ZNPs was confirmed by HR-SEM and HR-TEM. The optical absorption and PL emissions were determined by DRS and PL spectra respectively. ZnO nanostructures with band gap energies of 3.36 eV (MCM) and 3.25 eV (CCM) were obtained. The dye-sensitized ZnO nanowire arrays exhibit much stronger optical absorption as compared with ZnO nanoparticle arrays, suggesting that the larger surface area improves light harvesting. The dye-sensitized solar cell based on the optimized ZnO nanowires array reaches a conversion efficiency of 1.73%, which is higher than that obtained from ZnO nanoparticles (0.69%) under the light radiation of 1000 W/m2. As-prepared ZNWs have potential applications in fabricating next generation nanodevices.

Optical and magnetic properties of Co-doped CuO flower/plates/particles-like nanostructures.

Abstract: In this study, pure and Co-doped CuO nanostructures (0.5, 1.0, 1.5, and 2.0 at wt% of Co) were synthesized by microwave combustion method. The prepared samples were characterized by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis (EDX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometry (VSM). Powder X-ray diffraction patterns refined by the Rietveld method indicated the formation of single-phase monoclinic structure. The surface morphology and elemental analysis of Co-doped CuO nanostructures were studied by using HR-SEM and EDX. Interestingly, the morphology was found to change considerably from nanoflowers to nanoplates then to nanoparticles with the variation of Co concentration. The optical band gap calculated using DRS was found to be 2.1 eV for pure CuO and increases up to 3.4 eV with increasing cobalt content. Photoluminescence measurements also confirm these results. The magnetic measurements indicated that the obtained nanostructures were ferromagnetic at room temperature with an optimum value of saturation magnetization at 1.0 wt.% of Co-doped CuO, i.e., 970 micro emu/g.

Enhanced selectivity to benzaldehyde in the liquid phase oxidation of benzyl alcohol using nanocrystalline ZSM-5 zeolite catalyst

Abstract: In the present paper, nanocrystalline hierarchical ZSM-5 zeolites were successfully synthesized by the hydrothermal method in the presence of tetrapropylammonium hydroxide as a single template with the gel composition of 58SiO2:Al2O3:20TPAOH:1,500H2O. The prepared zeolite catalysts were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Nitrogen adsorption–desorption (BET), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HR-TEM) techniques. The formation of pure and highly crystalline ZSM-5 zeolite phase is confirmed by XRD. The IR vibration band at 550 cm−1 is assigned to the double 5-rings of MFI-type zeolites. N2 adsorption–desorption isotherms showed that the synthesized product had high BET surface area and possessed composite pore structures with both micro and mesopores. The catalytic performance of hierarchical ZSM-5 zeolite was investigated in the selective oxidation of benzyl alcohol (BzOH) with hydrogen peroxide (H2O2) under mild conditions. The results showed that the conversion of BzOH and the selectivity to benzaldehyde were about 94 and about 99 % respectively, when using 0.08 g ZSM-5 catalyst with acetonitrile as the solvent and H2O2 as the oxidant at 90 °C. This catalyst can be retrieved and reprocessed for five times without a significant loss in its activity and selectivity.

Effect of Ce doping on structural, optical and photocatalytic properties of ZnO nano-structures.

Abstract: A novel self-assembled pure and Ce doped ZnO nano-particles (NPs) were successfully synthesized by a simple low temperature co-precipitation method. The prepared photocatalysts were characterized by X-ray diffraction (XRD), High resolution scanning electron microscopy (HR-SEM), High resolution transmission electron microscopy (HR-TEM), diffuse reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The results indicated that the prepared photocatalysts shows a novel morphology, high crystallinity, uniform size distribution, and more defects. Photocatalytic degradation (PCD) of nonylphenol, a potent endocrine disrupting chemical in aqueous medium was investigated. Higher amount of oxygen defects exhibits enhanced PCD of nonylphenol. In addition, the influence of the Ce contents on the structure, morphology, absorption, emission and photocatalytic activity of ZnO nanoparticles (NPs) were investigated systematically. The relative PCD efficiency of pure ZnO, Ce-doped ZnO NPs and commercial TiO2 (Degussa P-25) have also been discussed.

Biominerals doped nanocrystalline nickel oxide as efficient humidity sensor: A green approach

Abstract: The simple and green method is adopted for the preparation of biominerals (derived from the Hygrophila spinosa T. Anders plant seeds) doped nanocrystalline NiO. The prepared samples were subjected to instrumental analysis such as XRD, FT-IR, HR-SEM, EDX, UV–vis–DRS techniques. The surface area of all the samples was calculated from the Williamson–Hall's plot. The humidity sensitivity factor ( S f ) of the prepared samples was evaluated by two probe dc electrical resistance method at different relative humidity levels. The change in the resistance was observed for the entire sensor samples except pure NiO (NH0). Compared to all the other composition, HST of 0.5% in NiO (NH2 sample) enhances the sensitivity factor ( S f ) of about 90,000. The NH2 sample exhibited good linearity, reproducibility and response and recovery time about 210 ± 5 s and 232 ± 4 s, respectively. It is found that the sensitivity largely depends on composition, crystallite size and surface area.

Studies on the Structural, Morphological, Optical, and Magnetic Properties of α -Fe 2 O 3 Nanostructures by a Simple One-Step Low Temperature Reflux Condensing Method

Abstract: Uniform hematite (α-Fe2O3) nanoparticles have been successfully synthesized through a simple one-step low temperature reflux condensing method which requires no surfactants or templates. The crystallite size was calculated by using Debye–Sherrer formula, and it showed the range of 4–27 nm. The lattice parameters of the samples were measured by Rietveld analysis. The morphology of the products was studied by high resolution scanning electron microscopy (HR-SEM), and it was confirmed by high resolution transmission electron microscopy (HR-TEM). The HRTEM images exhibit the well defined lattice fringes of α-Fe2O3 particles that confirm their high crystallinity. The formation of pure α-Fe2O3 was further confirmed by using energy dispersive X-ray (EDX) analysis. The optical properties and the bandgap energy were measured by UV-Visible diffuse reflectance spectra (DRS) and photoluminescence (PL) spectra. The bandgap energy was measured by using Kubelka–Munk method, and the value was found to be 2.26 eV. Magnetic hysteresis (M–H) loops revealed that the as-prepared α-Fe2O3 samples displayed ferromagnetic behavior. These results show that the prepared hematite possess good magnetic properties.

Structural, Morphological, Optical, and Magnetic Properties of Fe-Doped CuO Nanostructures

Abstract: Pure and Fe-doped CuO nanostructures with different weight ratios (0.5, 1.0, 1.5, and 2.0 at wt% of Fe) were prepared by a facile and fast microwave combustion method. The structure and morphology of the samples were investigated by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometry (VSM). The XRD patterns refined by the Rietveld method indicated the formation of single-phase monoclinic structure and also confirm that the Fe ions are successfully incorporated into the CuO crystal lattice by occupying Cu ionic sites. Interestingly, the morphology was found to change considerably from nanoflowers to nanorod and disk-shaped then to nanoparticles with the variation of Fe content. The optical band gap calculated using DRS was found to be 2.8 eV for pure CuO and increases up to 3.4 eV with increasing Fe content. Photoluminescence measurements also confirm these results. The magnetic measurements indicated that the obtained nanostructures are found to show a room temperature ferromagnetism (RTF) with an optimum value of saturation magnetization at 2.0 wt.% of Fe-doped CuO, i.e.1.2960 x 10 -3 emu/g.