Microstructure and compression behavior of chip consolidated magnesium

Chips produced by turning a commercial purity magnesium billet were cold compacted and then hot extruded at four different temperatures: 250, 300, 350, and 400 degrees C. Cast billets, of identical composition, were also extruded as reference material. Chip boundaries, visible even after 49: 1 extrusion at 400 degrees C, were observed to suppress grain coarsening. Although 250 degrees C extruded chip-consolidated product showed early onset of yielding and lower ductility, fully dense material (extruded at 400 degrees C) had nearly 40% reduction in grain size with 22% higher yield strength and comparable ductility as that of the reference. The study highlights the role of densification and grain refinement on the compression behavior of chip consolidated specimens.

Low temperature charge transport and microwave absorption of carbon coated iron nanoparticles-polymer composite films

In this paper, the low temperature electrical conductivity and microwave absorption properties of carbon coated iron nanoparticles-polyvinyl chloride composite films are investigated for different filler fractions. The filler particles are prepared by the pyrolysis of ferrocene at 980 degrees C and embedded in polyvinyl chloride matrix. The high resolution transmission electron micrographs of the filler material have shown a 5 nm thin layer graphitic carbon covering over iron particles. The room temperature electrical conductivity of the composite film changes by 10 orders of magnitude with the increase of filler concentration. A percolation threshold of 2.2 and an electromagnetic interference shielding efficiency (EMI SE) of similar to 18.6 dB in 26.5-40 GHz range are observed for 50 wt% loading. The charge transport follows three dimensional variable range hopping conduction. (C) 2012 Elsevier Ltd. All rights reserved.

Synthesis, characterization, thermo- and photoluminescence properties of Bi3+ co-doped Gd2O3:Eu3+ nanophosphors

Gd2O3:Eu3+ (4 mol%) co-doped with Bi3+ (Bi = 0, 1, 3, 5, 7, 9 and 11 mol%) ions were synthesized by a low-temperature solution combustion method. The powders were calcined at 800A degrees C and were characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), Fourier transform infrared and UV-Vis spectroscopy. The PXRD profiles confirm that the calcined products were in monoclinic with little cubic phases. The particle sizes were estimated using Scherrer's method and Williamson-Hall plots and are found to be in the ranges 40-60 nm and 30-80 nm, respectively. The results are in good agreement with TEM results. The photoluminescence spectra of the synthesized phosphors excited with 230 nm show emission peaks at similar to 590, 612 and 625 nm, which are due to the transitions D-5(0)-> F-7(0), D-5(0)-> F-7(2) and D-5(0)-> F-7(3) of Eu3+, respectively. It is observed that a significant quenching of Eu3+ emission was observed under 230 nm excitation when Bi3+ was co-doped. On the other hand, upon 350 nm excitation, the luminescent intensity of Eu3+ ions was enhanced by incorporation of Bi3+ (5 mol%) ions. The introduction of Bi3+ ions broadened the excitation band of Eu3+ of which a new strong band occurred ranging from 320 to 380 nm. This has been attributed to the 6s(2)-> 6s6p transition of Bi3+ ions, implying a very efficient energy transfer from Bi3+ ions to Eu3+ ions. The gamma radiation response of Gd2O3:Eu3+ exhibited a dosimetrically useful glow peak at 380A degrees C. Using thermoluminescence glow peaks, the trap parameters have been evaluated and discussed. The observed emission characteristics and energy transfer indicate that Gd2O3:Eu3+, Bi3+ phosphors have promising applications in solid-state lighting.

Synthesis of BiFeO by carbonate precipitation

Magnetoelectric multiferroic BiFeO3 (BFO) was synthesized by a simple carbonate precipitation technique of metal nitrate solutions. X-ray powder diffraction and thermo-gravimetric analysis (TGA) revealed that the precipitate consists of an intimate mixture of crystalline bismuth carbonate and an amorphous hydroxide of iron. The precipitate yielded BiFeO3 at an optimal calcination temperature of similar to 560A degrees C. Energy dispersive X-ray (EDX) analysis showed 1:1 ratio between Bi and Fe in the oxide. X-ray photoelectron spectroscopy (XPS) studies confirmed that Fe to be in +3 oxidation states both in the precipitated powder and BiFeO3. The synthesized BFO exhibits a very weak ferromagnetic correlation at room temperature and the degree of which increases slightly on cooling down to 10 K suggesting alteration in the long range spatial modulation of the spins arrangement as compared to the bulk BiFeO3.

Synthesis of one-dimensional N-doped Ga2O3 nanostructures: different morphologies and different mechanisms

N-doped monoclinic Ga2O3 nanostructures of different morphologies have been synthesized by heating Ga metal in ambient air at 1150 degrees C to 1350 degrees C for 1 to 5 h duration. Neither catalyst nor any gas flow has been used for the synthesis of N-doped Ga2O3 nanostructures. The morphology was controlled by monitoring the curvature of the Ga droplet. Plausible growth mechanisms are discussed to explain the different morphology of the nanostructures. Elemental mapping by electron energy loss spectroscopy of the nanostructures indicate uniform distribution of Ga, O and N. It is interesting to note that we have used neither nitride source nor any gas flow but the synthesis was carried out in ambient air. We believe that ambient nitrogen acts as the source of nitrogen. Unintentional nitrogen doping of the Ga2O3 nanostructures is a straightforward method and such nanostructures could be promising candidates for white light emission.

Fabrication of Transparent BaNaB9O15 Glass-Microcrystal Composites

Transparent glasses in the BaO-Na2O-B2O3 (BNBO) system were fabricated via the conventional melt-quenching technique. The amorphous and the glassy nature of the as-quenched samples were confirmed by x-ray powder diffraction (XRD) and differential thermal analysis (DTA), respectively. Cyclic heat treatment of the as-quenched glasses yielded transparent glass-microcrystal composites. The volume fraction of the crystallites and their sizes could be easily controlled by this process. Heat-treated samples were highly transparent owing to the minimum mismatch between the refractive indices of the crystallites and the glass residual matrix. BNBO samples that were heat treated at 540A degrees C for 4 h for 10 cycles were found to be 60% to 70% transparent in the 500 nm to 900 nm wavelength range.

Electrochemical, phosphate hydrolysis, DNA binding and DNA cleavage properties of new polyaza macrobicyclic dinickel(II) complexes

A new class of macrobicyclic dinickel(II) complexes Ni2L1,2 B](ClO4)(4) (1-6), where L-1,L-2 are polyaza macrobicyclic binucleating ligands, and B is a N,N-donor heterocyclic base (viz. 2,2'-bipyridine (bipy) and 1,10-phenanthroline (phen)) are synthesized and characterized. The redox, catalytic, DNA binding and DNA cleavage properties were studied. They exhibit two irreversible waves in the cathodic region around E-pc = -0.95 V and E-pa = -0.85 V vs. Ag/Ag+ in CH3CN-0.1 M TBAP, respectively. The first order rate constants for the hydrolysis of 4-nitrophenylphosphate to 4-nitrophenolate by the dinickel(II) complexes 1-6 are in the range from 3.36 x 10(-5) to 10.83 x 10(-5) Ms-1. The complexes 3 and 6 show good binding propensity to calf thymus DNA giving binding constant values (K-b) in the range from 3.08 x 10(5) to 5.37 x 10(5) M-1. The binding site sizes and viscosity data suggest the DNA intercalative and/or groove binding nature of the complexes. The complexes display significant hydrolytic cleavage of supercoiled pBR322DNA at pH 7.2 and 37 degrees C. The hydrolytic cleavage of DNA by the complexes is supported by the evidence from free radical quenching and T4 ligase ligation. The pseudo Michaelis-Menten kinetic parameters k(cat) = 5.44 x 10(-2) h(-1) and K-M = 6.23 x 10(-3) M for complex 3 were obtained. Complex 3 also shows an enormous enhancement of the cleavage rate, of 1.5 x 10(6), in comparison to the uncatalysed hydrolysis rate (k = 3.6 x 10(-8) h(-1)) of ds-DNA.

Surfactant solubility and micellization in ternary eutectic melt (acetamide plus urea plus ammonium nitrate)

Cationic surfactants such as dodecyltrimethylammonium bromide (DTAB), tetradecyltrimehtylammonium bromide (TTAB) and hexadecyltrimethylammonium bromide (HTAB); and anionic surfactants such as sodium decyl sulphate (SDeS), sodium dodecyl sulphate (SDS) and sodium tetradecyl sulphate (STDS) have been used to determine their solubility and micellization in ternary eutectic melt (acetamide + urea + ammonium nitrate) at 50 degrees C. We employed the electrical conductivity and the surface tension measurement techniques to determine the critical micelle concentration (CMC). The deviation in the slope of the specific conductance/surface tension against surfactant concentration plots indicated the aggregations of surfactants and hence, their CMC. CMC decreases with increase of alkyl chain length due to the increased van der Waals forces. The calculated increment in Gibb's energy per methylene group for cationic and anionic surfactants is about -6 kJ mol(-1) and -4 kJ mol(-1) respectively. It is found that, the CMCs of the surfactants in the ternary melt are higher than the CMCs of same surfactants in water (similar to 25 degrees C). (C) 2012 Elsevier B.V. All rights reserved.

Tailoring the Magnetic and Optical Characteristics of Nanocrystalline BiFeO3 by Ce Doping

The Ce-doped BiFeO3 (BFO) nanoparticles (NPs) were synthesized using a facile solgel route with varying Ce concentrations in the range of 15 mol%. Ferroelectric transition temperature was found to shift from 723 degrees C +/- 5 degrees C for pristine BFO NPs to 534 degrees C +/- 3 degrees C for 5 mol% Ce-doped BFO NPs. UVVis absorption spectra of BFO NPs showed a significant blue shift of similar to 100 nm on Ce doping. The Fourier transformed infrared (FTIR) spectrum centered similar to 550 cm(-1) becomes considerably broadened on Ce doping which is due to additional closely spaced vibrational peaks as revealed by the second derivative FTIR analysis. High-frequency EPR measurements indicated that clustering occurs at high dopant levels, and that Fe is present as Fe(3+)corroborating Mossbauer measurements. The values of saturation and remanent magnetization for 3% Ce-doped BFO NPs are 3.03 and 0.49 emu/g, respectively, which are quite significant at room temperature, making it more suitable for technological applications.

Transition due to base roughness in a dense granular flow down an inclined plane

Particle simulations based on the discrete element method are used to examine the effect of base roughness on the granular flow down an inclined plane. The base is composed of a random configuration of fixed particles, and the base roughness is decreased by decreasing the ratio of diameters of the base and moving particles. A discontinuous transition from a disordered to an ordered flow state is observed when the ratio of diameters of base and moving particles is decreased below a critical value. The ordered flowing state consists of hexagonally close packed layers of particles sliding over each other. The ordered state is denser (higher volume fraction) and has a lower coordination number than the disordered state, and there are discontinuous changes in both the volume fraction and the coordination number at transition. The Bagnold law, which states that the stress is proportional to the square of the strain rate, is valid in both states. However, the Bagnold coefficients in the ordered flowing state are lower, by more than two orders of magnitude, in comparison to those of the disordered state. The critical ratio of base and moving particle diameters is independent of the angle of inclination, and varies very little when the height of the flowing layer is doubled from about 35 to about 70 particle diameters. While flow in the disordered state ceases when the angle of inclination decreases below 20 degrees, there is flow in the ordered state at lower angles of inclination upto 14 degrees. (C) 2012 American Institute of Physics. http://dx.doi.org/10.1063/1.4710543]

Stabilization of O-Mn-O clusters (Mn-5) in three dimensionally extended MOF structures: synthesis, structure and properties

Four new three-dimensional Mn2+ ion-containing compounds have been prepared by employing a hydrothermal reaction between Mn(CH3COO)(2)center dot 4H(2)O, sulfodibenzoic acid (H(2)SDBA), imidazole, alkali hydroxide and water at 220 degrees C for 1 day. The compounds have Mn-5 (1-4) clusters connected by SDBA, forming the three-dimensional structure. A time and temperature dependent study on the synthesis mixture revealed the formation of a one-dimensional compound, Mn(SDBA)(H2O)(2), at lower temperatures (T <= 180 degrees C). The stabilization of the fcu related topology in the compounds is noteworthy. Magnetic studies indicate strong anti-ferromagnetic interactions between the Mn2+ ions within the clusters in the temperature range 75-300 K. The rare participation of a sulfonyl group in the bonding is important and can pave way for the design of new structures.

Infrared Spectra of Dimethylphenanthrenes in the Gas phase

Infrared spectra of atmospherically and astronomically important dimethylphenanthrenes (DMPs), namely 1,9-DMP, 2,4-DMP, and 3,9-DMP, were recorded in the gas phase from 400 to 4000 cm(-1) with a resolution of 0.5 cm(-1) at 110 degrees C using a 7.2 m gas cell. DFT calculations at the B3LYP/6-311G** level were carried out to get the harmonic and anharmonic frequencies and their corresponding intensities for the assignment of the observed bands. However, spectral assignments could not be made unambiguously using anharmonic or selectively scaled harmonic frequencies. Therefore, the scaled quantum mechanical (SQM) force field analysis method was adopted to achieve more accurate assignments. In this method force fields instead of frequencies were scaled. The Cartesian force field matrix obtained from the Gaussian calculations was converted to a nonredundant local coordinate force field matrix and then the force fields were scaled to match experimental frequencies in a consistent manner using a modified version of the UMAT program of the QCPE package. Potential energy distributions (PEDs) of the normal modes in terms of nonredundant local coordinates obtained from these calculations helped us derive the nature of the vibration at each frequency. The intensity of observed bands in the experimental spectra was calculated using estimated vapor pressures of the DMPs. An error analysis of the mean deviation between experimental and calculated intensities reveal that the observed methyl C-H stretching intensity deviates more compared to the aromatic C-H and non C-H stretching bands.

Thermoluminescence, photoluminescence and EPR studies on Mn2+ activated yttrium aluminate (YAlO3) perovskite

Thermoluminescence (TL) measurements were carried out on undoped and Mn2+ doped (0.1 mol%) yttrium aluminate (YAlO3) nanopowders using gamma irradiation in the dose range 1-5 kGy. These phosphors have been prepared at furnace temperatures as low as 400 degrees C by using the combustion route. Powder X-ray diffraction confirms the orthorhombic phase. SEM micrographs show that the powders are spherical in shape, porous with fused state and the size of the particles appeared to be in the range 50-150 nm. Electron Paramagnetic Resonance (EPR) studies reveal that Mn ions occupy the yttrium site and the valency of manganese remains as Mn2+. The photoluminescence spectrum shows a typical orange-to-red emission at 595 nm and suggests that Mn2+ ions are in strong crystalline environment. It is observed that TL intensity increases with gamma dose in both undoped and Mn doped samples. Four shouldered TL peaks at 126, 240, 288 and 350 degrees C along with relatively resolved glow peak at 180 degrees C were observed in undoped sample. However, the Mn doped samples show a shouldered peak at 115 degrees C along with two well defined peaks at similar to 215 and 275 degrees C. It is observed that TL glow peaks were shifted in Mn doped samples. The kinetic parameters namely activation energy (E), order of kinetics (b), frequency factor (s) of undoped, and Mn doped samples were determined at different gamma doses using the Chens glow peak shape method and the results are discussed in detail. (C) 2012 Elsevier B.V. All rights reserved.

Structural and phase dependent thermo and photoluminescent properties of Dy(OH)(3) and Dy2O3 nanorods

Hexagonal Dy(OH)(3) and cubic Dy2O3 nanorods were prepared by hydrothermal method. Dy(OH)(3) nanorods was directly obtained at 180 degrees C for 20 h after hydrothermal treatment whereas subsequently heat treatment at 750 degrees C for 2 h gives pure cubic Dy2O3. SEM micrographs reveal that needle shaped rods with different sizes were observed in both the phases. TEM results also confirm this. The TL response of hexagonal Dy(OH)(3) and cubic Dy2O3 nanorods have been analyzed for gamma-irradiation over a wide range of exposures (1-5 kGy). TL glow peak intensity increases with gamma dose in both the phases. The activation energy (E), order of kinetics (6), and frequency factor (s) for both the phases have been determined using Chen's peak shape method. The simple glow curve shape, structure and linear response to gamma-irradiation over a large span of exposures makes the cubic Dy2O3 as a useful dosimetric material to estimate high exposures of gamma-rays. (c) 2012 Elsevier Ltd. All rights reserved.

Structural, EPR, optical and Raman studies of Nd2O3:Cu2+ nanophosphors

Nanocrystalline Nd2O3:Cu2+ (2 mol %) phosphors have been prepared by a low temperature solution combustion technique. Powder X-ray diffraction (PXRD) results confirm that hexagonal A-type Nd2O3 (900 degrees C, 3 h) and the lattice parameters have been evaluated by Rietveld refinement. Surface morphology of as-formed and Cu2+ doped Nd2O3 phosphors show that the particles are irregular in shape and porous in nature. TEM results also confirm the nature and size of the particles. The EPR spectrum exhibits two resonance signals with effective g values at g(parallel to) approximate to 2.12 and g(perpendicular to) approximate to 2.04. The g values indicate that the site symmetry of Cu2+ ions is octahedral symmetry with elongated tetragonal distortion. Raman studies show major peaks, which are assigned, to F-g and combination of A(g) + E-g modes. It is observed that the Raman peaks and intensity have been reduced in Cu2+ doped samples. UV-Visible absorption spectra exhibit a strong and broad absorption band at similar to 240 nm. Further, the absorption peak shifts to similar to 14 nm in Cu2+ doped samples. The optical band gap is estimated to be 5.28 eV for Cu doped Nd2O3 nanoparticles which are higher than the bulk Nd2O3 (4.7 eV). This can be attributed to the quantum confinement effect of the nanoparticles. (C) 2012 Elsevier B.V. All rights reserved.