272 resultados para Scanning electron microscopic


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GaN films were grown on c-plane sapphire by plasma-assisted molecular beam epitaxy (PAMBE). The effect of N/Ga flux ratio on structural, morphological, and optical properties was studied. The dislocation density found to increase with increasing the N/Ga ratio. The surface morphology of the films as seen by scanning electron microscopy shows pits on the surface and found that the pit density on the surface increases with N/Ga ratio. The room temperature photoluminescence study reveals the shift in band-edge emission toward the lower energy with increase in N/Ga ratio. This is believed to arise from the reduction in compressive stress in the films as is evidenced by room temperature Raman study. The transport studied on the Pt/GaN Schottky diodes showed a significant increase in leakage current with an increase in N/Ga ratio and was found to be caused by the increase in pit density as well as increase in dislocation density in the GaN films. (C) 2011 American Institute of Physics. [doi:10.1063/1.3634116]

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In this study we have employed multiwall carbon nanotubes (MWCNT), decorated with platinum as catalytic layer for the reduction of tri-iodide ions in dye sensitized solar cell (DSSC). MWCNTs have been prepared by a simple one step pyrolysis method using ferrocene as the catalyst and xylene as the carbon source. Platinum decorated MWCNTs have been prepared by chemical reduction method. The as prepared MWCNTs and Pt/MWCNTs have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). In combination with a dye adsorbed TiO(2) photoanode and an organic liquid electrolyte, Pt/MWCNT composite showed an enhanced short circuit current density of 16.12 mA/cm(2) leading to a cell efficiency of 6.50% which is comparable to that of Platinum. (C) 2011 Elsevier Ltd. All rights reserved.

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Nanowires of Pr0.57Ca0.41Ba0.02MnO3 (PCBM) (diameter similar to 80-90 nm and length similar to 3.5 mu m) were synthesized by a low reaction temperature hydrothermal method. Single-phase nature of the sample was confirmed by XRD experiments. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the morphology and microstructures of the nanowires. While the bulk PCBM is known to exhibit charge order (CO) below 230 K along with a ferromagnetic transition at 110 K, SQUID measurements on the nanowires of PCBM show that the charge order is completely absent and a ferromagnetic transition occurs at 115 K. However, the magnetization in the nanowires is observed to be less compared to that in the bulk. This observation of the complete 'melting' of the charge order in the PCBM nanowires is particularly significant in view of the observation of only a weakening of the CO in the nanowires of Pr0.5Ca0.5MnO3. Electron paramagnetic resonance experiments were also carried out on the PCBM nanowires using an X-band EPR spectrometer. Characteristic differences were observed in the line width of nanowires when compared with that of the bulk.

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In the present investigation, various kinds of textures, namely, unidirectional, 8-ground, and random were attained on the die surfaces. Roughness of the textures was varied using different grits of emery papers or polishing powders. Then pins made of Al-4Mg alloys were slid against steel plates at various numbers of cycles, namely, 1, 3, 5, 10 and 20 using pin-on-plate reciprocating sliding tester. Tests were conducted at a sliding velocity of 2 minis in ambient conditions under both dry and lubricated conditions. A constant normal load of 35 N was applied in the tests. The morphologies of the worn surfaces of the pins and the formation of transfer layer on the counter surfaces were observed using a scanning electron microscope. Surface roughness parameters of the plates were measured using an optical profilometer. In the experiments, it was observed that the coefficient of friction and formation of the transfer layer depend on the die surface textures under both dry and lubricated conditions. More specifically, the coefficient of friction decreases for unidirectional and 8-ground surfaces while for random surfaces it increases with number of cycles. However, the coefficient of friction is highest for the sliding perpendicular to the unidirectional textures and least for the random textures under both dry and lubricated conditions. The difference in friction values between these two surfaces decreases with increasing number of cycles. The variation in the coefficient of friction under both dry and lubrication conditions is attributed to the change in texture of the surfaces during sliding. (C) 2011 Elsevier B.V. All rights reserved.

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The dry sliding wear and friction behaviour of A356 Al alloy and its composites containing 10 and 20 vol.% SiC(P) have been studied using pin-on-disc set up. In these tests, A356 Al alloy and its composites are used as disc whereas brake pad was used in the form of pins. Wear tests were carried out at a load of 192 N and the sliding speed was varied from 1 to 5 m/s. Tests were done for a sliding distance of 15 km. The effects of sliding velocity on the wear rate, coefficient of friction and nature of tribolayers formed on discs have been studied. Wear rates of composites as calculated by weight loss method, found to be negative at sliding speed of more than 2 m/s. Worn surfaces of pins and discs have been analyzed using scanning electron microscope. SEM and EDAX analysis of worn surfaces of composite discs showed formation of tribolayers, consisting of mixture of oxides of Al, Si, Cu, Ca, Ba, Mg, and Fe. In these layers, copper and barium content found to be increase with sliding speed in the case of composites. (C) 2011 Elsevier B.V. All rights reserved.

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Wear resistant coatings were produced on a permanent mould cast MRI 230D Mg alloy by (a) PEO in silicate based electrolyte, (b) PEO in phosphate based electrolyte, (c) hybrid coatings of silicate PEO followed by laser surface alloying (LSA) with Al and Al(2)O(3), and (d) hybrid coatings of phosphate PEO followed by LSA with Al and Al(2)O(3). Microstructural characterization of the coatings was carried out by scanning electron microscopy (SEM) and X(ray diffraction. The tribological behavior of the coatings was investigated under dry sliding condition using linearly reciprocating ball-on-flat wear test. Both the PEO coatings exhibited a friction coefficient of about 0.8 and hybrid coatings exhibited a value of about 0.5 against the AISI 52100 steel ball as the friction partner, which were slightly reduced with the increase in applied load. The PEO coatings sustained the test without failure at 2 N load but failed at 5 N load due to micro-fracture caused by high contact stresses. The hybrid coatings did not get completely worn off at 2 N load but were completely removed exposing the substrate at 5 N load. The PEO coatings exhibited better wear resistance than the hybrid coatings and silicate PEO coatings exhibited better wear resistance than the phosphate PEO coatings. Both the PEO coatings melted/decomposed on laser irradiation and all the hybrid coatings exhibited similar microstructure and wear behavior irrespective of the nature of the primary PEO coating or laser energies. SEM examination of worn surfaces indicated abrasive wear combined with adhesive wear for all the specimens. The surface of the ball exhibited a discontinuous transfer layer after the wear test. (C) 2011 Elsevier B.V. All rights reserved.

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In the present investigation, various kinds of surface textures were attained on the steel plates. Roughness of the textures was varied using various grinding or polishing methods. The surface textures were characterized in terms of roughness parameters using an optical profilometer. Then experiments were conducted using an inclined pin-on-plate sliding apparatus to identify the role of surface texture and its roughness parameters on coefficient of friction and transfer layer formation. In the experiments, a soft polymer (polypropylene) was used for the pin and hardened steel was used for the plate. Experiments were conducted at a sliding velocity of 2 minis in ambient conditions under both dry and lubricated conditions. The normal load was varied from 1 to 120 N during the tests. The morphologies of the worn surfaces of the pins and the formation of a transfer layer on the steel plate surfaces were observed using a scanning electron microscope. Based on the experimental results, it was observed that the transfer layer formation and the coefficient of friction along with its two components, namely adhesion and plowing, were controlled by the surface texture of the harder mating surfaces and were less dependent of surface roughness (R(a)) of the harder mating surfaces. The effect of surface texture on the friction was attributed to the variation of the plowing component of friction for different surfaces. Among the various surface roughness parameters studied, the mean slope of the profile, Delta(a), was found to most accurately characterize variations in the friction and wear behavior. (C) 2011 Elsevier B.V. All rights reserved.

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Corrosion of SAE 310 stainless steel in H2-H2O-H2S gas mixtures was studied at a constant temperature of 1150 K. Reactive gas mixtures were chosen to yield a constant oxygen potential of approximately 6 × 10-13 Nm-2 and sulfur potentials ranging from 0.19 × 10-2 Nm-2 to 33 × 10-2 Nm-2. The kinetics of corrosion were determined using a thermobalance, and the scales were analyzed using metallography, scanning electron microscopy, and energy dispersive X-ray analysis. Two corrosion regimes, which were dependent on sulfur potential, were identified. At high sulfur potentials (P S 2 ± 2.7 × 10-2 Nm-2) the corrosion rates were high, the kinetics obeyed a linear rate equation, and the scales consisted mainly of sulfide phases similar to those observed from pure sulfidation. At low sulfur potentials (P S 2 ± 0.19 × 10-2 Nm-2) the corrosion rates were low, the kinetics obeyed a parabolic rate equation, and scales consisted mainly of oxide phases. Thermochemical diagrams for the Fe-Cr-S-O, Fe-Ni-S-O, Cr-Ni-S-O, and Si-Cr-S-O systems were constructed, and the experimental results are discussed in relation to these diagrams. Based on this comparison, reasonable corrosion mechanisms were developed. At high sulfur potentials, oxide and sulfide phases initially nucleate as separate islands. Overgrowth of the oxide by the sulfide occurs and an exchange reaction governs the corrosion process. Preoxidation at low oxygen potentials and 1150 K is beneficial in suppressing sulfidation at high sulfur potentials.

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Large single crystal of triglycine sulphate (dimension 100 mm along monoclinic b-axis and 15 mm in diameter) was grown using the unidirectional solution growth technique. The X-ray diffraction studies confirmed the growth/long axis to be b-axis (polar axis). The dielectric studies were carried out at various temperatures to establish the phase transition temperature. The frequency response of the dielectric constant, dielectric loss and impedance of the crystal along the growth axis, was monitored. These are typically characterized by strong resonance peaks in the kHz region. The piezoelectric coefficients like stiffness constant (C), elastic coefficient (S), electromechanical coupling coefficient (k) and d (31) were calculated using the resonance-antiresonance method. Polarization (P)-Electric field (E) hysteresis loops were recorded at various temperatures to find the temperature-dependent spontaneous polarization of the grown crystal. The pyroelectric coefficients were determined from the pyroelectric current measurement by the Byer and Roundy method. The ferroelectric domain patterns were recorded on (010) plane using scanning electron microscopy and optical microscopy.

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A methodology for evaluating the reactivity of titanium with mould materials during casting has been developed. Microhardness profiles and analysis of oxygen contamination have provided an index for evaluation of the reactivity of titanium. Microhardness profile delineates two distinct regions, one of which is characterised by a low value of hardness which is invariant with distance. The reaction products are uniformly distributed in the metal in this region. The second is characterised by a sharp decrease in microhardness with distance from the metal-mould interface. It represents a diffusion zone for solutes that dissolve into titanium from the mould. The qualitative profiles for contaminants determined by scanning electron probe microanalyser and secondary ion mass spectroscopy in the as-cast titanium were found to be similar to that of microhardness, implying that microhardness can be considered as an index of the contamination resulting from metal-mould reaction.

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Metal-mold reaction during Ti casting in zircon sand molds has been studied using scanning electron microscope, energy and wave length dispersive analysis of X-rays, X-ray diffraction, microhardness measurements, and chemical analysis. Experimental results suggest that oxides from the mold are not fully leached out by liquid Ti, but oxygen is preferentially transferred to liquid Ti, leaving behind metallic constituents in the mold as lower oxides or intermetallics of Ti. The electron microprobe analysis has revealed the depth profile of contaminants from the mold into the cast Ti metal. The elements Si, Zr and O were found to have diffused to a considerable distance within the Ti metals. A possible mechanism has now been evolved in regard to the reactions that occur during casting of Ti in zircon sand molds.

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A solid state galvanic cell incorporating yttria-stabilized zirconia electrolyte and ruthenium(IV) oxide electrodes has been used to measure the equilibrium chemical potential of oxygen corresponding to the decomposition of CuCrO4 in the range 590–760 K. For the reaction CuO(tenorite) + CuCr2O4(spinel) + 1.5O2(g)→2CuCrO4(orth), ΔGXXX = −183540 + 249.6T(±900) J mol−1. The decomposition temperature of CuCrO4 in pure oxygen at a pressure of 1.01 × 105 Pa is 735(±1) K. By combining the results obtained in this study with data on the Gibbs energy of formation of CuCr2O4 and CuCrO2 reported earlier, the standard Gibbs energy of formation of CuCrO4 and the phase relations in the system Cu-Cr-O at temperatures below 735 K have been deduced. Electron microscopic studies have indicated that the decomposition of CuCrO4 to CuCr2O4 is topotactic.

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An isothermal section of the phase diagram for the system Nd-Pd-O at 1350 K has been established by equilibration of samples representing 13 different compositions and phase identification after quenching by optical and scanning electron microscopy, x-ray diffraction, and energy dispersive analysis of x-rays. The binary oxides PdO and NdO were not stable at 1350 K. Two ternary oxides Nd4PdO7 and Nd2Pd2O5 were identified. Solid and liquid alloys, as well as the intermetallics NdPd3 and NdPd5, were found to be in equilibrium with Nd2O3. Based on the phase relations, three solidstate cells were designed to measure the Gibbs energies of formation of PdO and the two ternary oxides. An advanced version of the solid-state cell incorporating a buffer electrode was used for high-temperature thermodynamic measurements. The function of the buffer electrode, placed between reference and working electrodes, was to absorb the electrochemical flux of the mobile species through the solid electrolyte caused by trace electronic conductivity. The buffer electrode prevented polarization of the measuring electrode and ensured accurate data. Yttria-stabilized zirconia was used as the solid electrolyte and pure oxygen gas at a pressure of 0.1 MP a as the reference electrode. Electromotive force measurements, conducted from 950 to 1425 K, indicated the presence of a third ternary oxide Nd2PdO4, stable below 1135 (±10) K. Additional cells were designed to study this compound. The standard Gibbs energy of formation of PdO (†f G 0) was measured from 775 to 1125 Kusing two separate cell designs against the primary reference standard for oxygen chemical potential. Based on the thermodynamic information, chemical potential diagrams for the system Nd-Pd-O were also developed.

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An isothermal section of the phase diagram for the system Cu-Rh-O at 1273 K has been established by equilibration of samples representing eighteen different compositions, and phase identification after quenching by optical and scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy dispersive analysis of X-rays (EDX). In addition to the binary oxides Cu2O, CuO, and Rh2O3, two ternary oxides CuRhO2 and CuRh2O4 were identified. Both the ternary oxides were in equilibrium with metallic Rh. There was no evidence of the oxide Cu2Rh2O5 reported in the literature. Solid alloys were found to be in equilibrium with Cu2O. Based on the phase relations, two solid-state cells were designed to measure the Gibbs energies of formation of the two ternary oxides. Yttria-stabilized zirconia was used as the solid electrolyte, and an equimolar mixture of Rh+Rh2O3 as the reference electrode. The reference electrode was selected to generate a small electromotive force (emf), and thus minimize polarization of the three-phase electrode. When the driving force for oxygen transport through the solid electrolyte is small, electrochemical flux of oxygen from the high oxygen potential electrode to the low potential electrode is negligible. The measurements were conducted in the temperature range from 900 to 1300 K. The thermodynamic data can be represented by the following equations: {fx741-1} where Δf(ox) G o is the standard Gibbs energy of formation of the interoxide compounds from their component binary oxides. Based on the thermodynamic information, chemical potential diagrams for the system Cu-Rh-O were developed.

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An isothermal section of the phase diagram for (silver + rhodium + oxygen) at T = 1173 K has been established by equilibration of samples representing twelve different compositions, and phase identification after quenching by optical and scanning electron microscopy (s.e.m.), X-ray diffraction (x.r.d.), and energy dispersive analysis of X-rays (e.d.x.), Only one ternary oxide, AgRhO2, was found to be stable and a three phase region involving Ag, AgRhO2 and Rh2O3 was identified. The thermodynamic properties of AgRhO2 were measured using a galvanic cell in the temperature range 980 K to 1320 K. Yttria-stabilized zirconia was used as the solid electrolyte and pure oxygen gas at a pressure of 0.1 MPa was used as the reference electrode. The Gibbs free energy of formation of the ternary oxide from the elements, ΔfGo (AgRhO2), can be represented by two linear equations that join at the melting temperature of silver. In the temperature range 980 K to 1235 K, ΔfGo(AgRhO2)/(J . mol-1) = -249080 + 179.08 T/K (±120). Above the melting temperature of silver, in the temperature range 1235 K to 1320 K, ΔfGo(AgRhO2)/(J . mol-1) = -260400 + 188.24 T/K (±95). The thermodynamic properties of AgRhO2 at T = 298.15 K were evaluated from the high temperature data. The chemical potential diagram for (silver + rhodium + oxygen) at T = 1200 K was also computed on the basis of the results of this study.