Nanoparticles of CoFe2O4 and CoIn0.15Fe1.85O4 ferrites were prepared by citrate gel route and characterized to understand their structural, electrical, and magnetic properties. X-ray diffraction and Raman spectroscopy were used to confirm the formation of single phase cubic spinel structure. The average grain sizes from the Scherrer formula were below 50 nm. Microstructural features were obtained by scanning electron microscope and compositional analysis by energy dispersive spectroscopy. The hysteresis curve shows enhancement in coercivity while reduction in saturation magnetization with the substitution of In3+ ions. Enhancement of coercivity is attributed to the transition from multidomain to single domain nature. Electrical properties, such as dc resistivity as a function of temperature and ac conductivity as a function of frequency and temperature were studied for both the samples. The activation energy derived from the Arrhenius equation was found to increase in the doped sample. The dielectric constant (ε′) and dielectric loss (tan δ) are also studied as a function of frequency and temperature. The variation of dielectric properties ε′, tan δ, and ac conductivity (σac) with frequency reveals that the dispersion is due to Maxwell–Wagner type of interfacial polarization in general and the hopping of charge between Fe2+ and Fe3+ as well as between Co2+ and Co3+ ions at B-sites. Magnetization and electrical property study showed its dominant dependence on the grain size.
We report the synthesis and characterization of Nd doped ZnO thin films grown on Si (1 0 0) substrates by the spray pyrolysis method. The surface morphology of these thin films was investigated by scanning electron microscopy and shows the presence of randomly distributed structures of nanorods. Grazing angle x-ray diffraction studies confirm that the doped Nd ions occupied Zn sites and these samples exhibited a wurtzite hexagonal-like crystal structure similar to that of the parent compound, ZnO. The micro-photoluminescence measurement shows a decrease in the near band edge position with Nd doping in the ZnO matrix due to the impurity levels. The near-edge x-ray absorption fine structure (NEXAFS) measurements at the O K edge clearly exhibit a pre-edge spectral feature which evolves with Nd doping, suggesting incorporation of more charge carriers in the ZnO system and the presence of strong hybridization between O 2p–Nd 5d orbitals. The Nd M5 edge NEXAFS spectra reveal that the Nd ions are in the trivalent state.
We report on synthesis of spherical Au nanoparticles at the surface and embedded in carbonaceous matrix by 150 keV Ar ion irradiation of thin Au film on polyethyleneterepthlate (PET). The pristine and irradiated samples are characterized by Rutherford backscattering spectrometry (RBS), atomic force microscopy, scanning electron microscopy and transmission electron microscopy (TEM) techniques. RBS spectra reveal the sputtering of Au film and interface mixing, increasing with increasing fluence. Surface morphology shows that at the fluence of 5 × 1015 ions cm−2, dewetting of thin Au film begins and partially connected nanostructures are formed whereas, at the higher fluence of 5 × 1016 ions cm−2, isolated spherical Au nanoparticles (45 ± 20 nm) are formed at the surface. Cross-sectional TEM observations also evidence the Au nanoparticles at the surface and mixed metal–polymer region indicating the formation of nanocomposites with small Au nanoparticles. The results are explained by the crater formation, sputtering followed by dewetting of the thin Au film and interdiffusion at the interface, through molten zones due to thermal spike induced by Ar ions.
An electrochemical reactor with anode and cathode chambers separated by a composite perfluoro polymer cation exchange membrane was designed, fabricated and used for the reduction of dissolved carbon dioxide under ambient conditions to formate. The flow reactor enhanced the mass transfer of carbon dioxide compared to the batch reactor and maximum current efficiency of 93% for formate formation was obtained. A formate concentration of 1.5 Â 10 )2 mol dm )3 was obtained. Experiments were conducted using two different perfluoro polymer membranes -Nafion 961 and Nafion 430. Optimum values of flow rate and current density were evaluated for the energy efficient formation of formate in aqueous phosphate buffer solutions.
This study performs O K-and Ti L 3,2-edge x-ray absorption near-edge structure ͑XANES͒ measurements and first-principles pseudopotential calculations for the electronic structures of ABO 3-type Pb 1Ϫx Ca x TiO 3 (xϭ0-1) perovskites. The features in the O K-edge XANES spectra are found to be contributed primarily by hybridization between O 2p and Ti 3d, Pb 6p, and Ca 3d orbitals. The O K-edge XANES spectra reveal that partial substitution of A cations, Pb, by Ca not only decreases O 2p-Pb 6p but also O 2p-Ti 3d hybridization. The Ti L 3,2-edge measurements find that the off-center displacement of Ti, and hence, ferroelectricity persist up to a Ca concentration between 0.3 and 0.4.
We investigate the effect of blend host polymer on solid polymer electrolyte (SPE) films doped with ammonium iodide (NH4I) salt using a variety of experimental techniques. Structural studies on the composite SPEs show that the blending of Poly(ethylene oxide) (PEO)–Poly(vinylidene fluoride) (PVDF) polymers in a suitable ratio enhances the amorphous fraction of the polymer matrix and facilitates fast ion conduction through it. We observe that the addition of a small amount of PVDF in the PEO host polymer enhances the ion – polymer interaction leading to more ion dissociation. As a result, the effective number of mobile charge carriers within the polymer matrix increases. Systematic investigation in these blend SPEs shows that the maximum conductivity (1.01 × 10–3 S/cm) is obtained for PEO – rich (80 wt. % PEO, 20 wt. % PVDF) composites at 35 wt. % NH4I concentration at room temperature. Interestingly, at higher salt concentrations (above 35 wt. %), the conductivity is found to decrease in this system. The reduction of conductivity at higher salt concentrations is the consequence of decrease in the carrier concentration due to the formation of an ion pair and ion aggregates. PVDF–rich compositions (20 wt. % PEO and 80 wt. % PVDF), on the other hand, show a very complex porous microstructure. We also observe a much lower ionic conductivity (maximum ∼ 10–6 S/cm at 15 wt. % salt) in these composite systems relative to PEO-rich composites.
We report O and Ca K-edges x-ray absorption near edge structure (XANES) spectra of Ba 1−x Ca x TiO 3 (x = 0.01 and 0.08), BaTiO 3 and CaTiO 3 and the electronic structure of Ba 0.875 Ca 0.125 TiO 3 obtained by first-principles calculation. The characteristic features in the O K-edge XANES spectra of these ferroelectric perovskites are influenced by the Ca concentration. They differ substantially from those of the reference TiO 2 . The O K-edge spectra suggest that the combination of the alkaline-earth-metal oxides, CaO and/or BaO, with TiO 2 enhance the effective charge of the O ions. Thus, a large dipole moment may result from the displacement of the Ti ion from the centre of the TiO 6 octahedron leading to collective displacement of Ti ions through attractive dipole-dipole couplings and may give rise to ferroelectricity. In the Ca K-edge XANES spectra there is a pre-edge feature similar to those found in other 3d transition-metal perovskites, which may provide information about hole doping.
Au nanoparticles (NPs) on the surface and embedded in a matrix have been the subject of studies dealing with a variety of spectroscopic and sensing applications. Here, we report on low energy Ar ion induced evolution of the morphology of a thin Au film on a polyethylene terephthalate (PET) substrate along with thermodynamic interpretations, and corresponding unique surface plasmon resonance (SPR) and photoluminescence (PL) properties. These properties are linked to the variation of surface nanostructures and the surface enhanced Raman scattering (SERS) effect of methyl orange (MO) dye molecules adsorbed on the surface. Ion induced thermal spike and sputtering resulted in dewetting of the film with subsequent formation of spherical NPs. This was followed by embedding of the NPs in the modified PET due to the thermodynamic driving forces involved. The surface and interface morphologies were studied using atomic force microscopy and cross-sectional transmission electron microscopy. X-ray photoelectron spectroscopy was used to study the chemical changes in the system upon irradiation. The optical properties were studied by diffuse reflectance UV-Vis spectroscopy and PL using a 325 nm He-Cd laser. The red shift of the SPR absorption and the blue shift of the PL emission have been correlated with the surface morphology. The blue PL emission bands at around 3.0 eV are in good agreement with the literature with respect to the morphological changes and the blue shift is attributed to compressive strain on the embedded Au NPs. Enhancement of the SERS signals is observed and found to be correlated with the SPR response of the Au nanostructures. The SERS analyses indicate that MO molecules may be adsorbed with different orientations on these surfaces i.e. Au NPs located on the surface or embedded in the modified PET. These polymeric substrates modified by NPs can have a potential application in solid-state light emitting devices and can be applied in SERS based sensors for the detection of organic compounds.
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