960 resultados para Energy dispersive spectrometry
Resumo:
A direct borohydride-hydrogen peroxide fuel cell employing carbon-supported Prussian Blue (PB) as mediated electron-transfer cathode catalyst is reported. While operating at 30 °C, the direct borohydride-hydrogen peroxide fuel cell employing carbon-supported PB cathode catalyst shows superior performance with the maximum output power density of 68 mW cm−2 at an operating voltage of 1.1 V compared to direct borohydride-hydrogen peroxide fuel cell employing the conventional gold-based cathode with the maximum output power density of 47 mW cm−2 at an operating voltage of 0.7 V. X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and Energy Dispersive X-ray Analysis (EDAX) suggest that anchoring of Cetyl-Trimethyl Ammonium Bromide (CTAB) as a surfactant moiety on carbon-supported PB affects the catalyst morphology. Polarization studies on direct borohydride-hydrogen peroxide fuel cell with carbon-supported CTAB-anchored PB cathode exhibit better performance with the maximum output power density of 50 mW cm−2 at an operating voltage of 1 V than the direct borohydride-hydrogen peroxide fuel cell with carbon-supported Prussian Blue without CTAB with the maximum output power density of 29 mW cm−2 at an operating voltage of 1 V.
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Thin films of Cd1−xMnxS (0<=x<=0.5) were deposited on glass substrates by thermal evaporation. All the films were deposited at 300 K and annealed at 373, 473, and 573 K for 1 h in a high vacuum in the range 10−4 Pa. The as-deposited and the annealed films were characterized for composition, structure, and microstructure by using energy-dispersive X-ray, X-ray diffraction, scanning electron microscopy, and atomic force microscopy (AFM). The electrical properties were studied by Hall effect measurement. Electrical conductivity was studied in the temperature range 190–450 K. AFM studies showed that all the films were in nanocrystalline form with grain size varying in the range between 36 and 82 nm. Grain size studies showed a definite increase with annealing temperature. All the films exhibited wurtzite structure of the host material. The lattice parameter varied linearly with composition, following Vegard's law in the entire composition range. Grain size, electrical conductivity, Hall mobility, carrier concentration, and activation energy varied, exhibiting either maxima or minima at x=0.3.
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Alum-impregnated activated alumina (AIAA) was investigated in the present work as an adsorbent for the removal of As(V) from water by batch mode. Adsorption study at different pH values shows that the efficiency of AIAA is much higher than as such activated alumina and is suitable for treatment of drinking water. The adsorption isotherm experiments indicated that the uptake of As(V) increased with increasing As(V) concentration from 1 to 25 mg/l and followed Langmuir-type adsorption isotherm. Speciation diagram shows that in the pH range of 2.8–11.5, arsenate predominantly exists as H2AsO4− and HAsO42− species and hence it is presumed that these are the major species being adsorbed on the surface of AIAA. Intraparticle diffusion and kinetic studies revealed that adsorption of As(V) was due to physical adsorption as well as through intraparticle diffusion. Effect of interfering ions revealed that As(V) sorption is strongly influenced by the presence of phosphate ion. The presence of arsenic on AIAA is depicted from zeta potential measurement, scanning electron microscopy (SEM) and energy-dispersive analysis of X-ray (EDAX) mapping study. Alum-impregnated activated alumina successfully removed As(V) to below 40 ppb (within the permissible limit set by WHO) from water, when the initial concentration of As(V) is 10 mg/l.
Resumo:
Polymeric outdoor insulators are being increasingly used for electrical power transmission and distribution in the recent years. One of the current topics of interest for the power transmission community is the aging of such outdoor polymeric insulators. A few research groups are carrying out aging studies at room temperature with wet period as an integral part of multistress aging cycle as specified by IEC standards. However, aging effect due to dry conditions alone at elevated temperatures and electric stress in the presence of radiation environment has probably not been explored. It is interesting to study and understand the insulator performance under dry conditions where wet periods are either rare or absent and to estimate the extent of aging caused by multiple stresses. This paper deals with the long-term accelerated multistress aging on full-scale 11 kV distribution class composite silicone rubber insulators. In order to assess the long-term synergistic effect of electric stress, temperature and UV radiation on insulators, they are subjected to accelerated aging in a specially designed multistress-aging chamber for 3800 hours. All the stresses are applied at an accelerated level. Using a data acquisition system developed for the work, leakage current has been monitored in LabVIEW environment. Chemical changes due to degradations have been studied using Energy Dispersive X-Ray analysis, Scanning Electron Microscope and Fourier transform Infrared Spectroscopy. Periodically different parameters like low molecular weight (LMW) molecular content, hydrophobicity, leakage current and surface morphology were monitored. The aging study is under progress and only intermediate results are presented in this paper.
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α-Manganese dioxide is synthesized in a microemulsion medium by a redox reaction between KMnO4 and MnSO4 in presence of sodium dodecyl sulphate as a surface active agent. The morphology of MnO2 resembles nanopetals, which are spread parallel to the field. The material is further characterized by powder X-ray diffraction, energy dispersive analysis of X-ray, and Brunauer–Emmett–Teller surface area. Supercapacitance property of α-MnO2 nanopetals is studied by cyclic voltammetry and galvanostatic charge–discharge cycling. High values of specific capacitance are obtained.
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Wear of etched near-eutectic aluminium silicon alloy slid against a steel ball under ambient is explored. The sliding velocity is kept low (0.01 m/s) and the nominal contact pressure is varied in a 15-40 MPa range. Four stages of wear are identified; ultra mild wear, mild wear, severe wear and post severe oxidative wear. The first transition is controlled by the protrusions of silicon particles, projecting out of the aluminium alloy matrix. Once these protrusions disappear under pressure and sliding, oxidation and bulk energy dissipation mechanisms take over to institute transitions to other stages of wear. The phenomenological characteristics of wear stages are explored using a variety of techniques including nanoindentation, focused ion beam milling, electron microscopy, X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDS) and optical interferometry. (c) 2010 Elsevier B.V. All rights reserved.
Resumo:
This thesis comprises four intercomplementary parts that introduce new approaches to brittle reaction layers and mechanical compatibility of metalloceramic joints created when fusing dental ceramics to titanium. Several different methods including atomic layer deposition (ALD), sessile drop contact angle measurements, scanning acoustic microscopy (SAM), three-point bending (TPB, DIN 13 927 / ISO 9693), cross-section microscopy, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS) were employed. The first part investigates the effects of TiO2 layer structure and thickness on the joint strength of the titanium-metalloceramic system. Samples with all tested TiO2 thicknesses displayed good ceramics adhesion to Ti, and uniform TPB results. The fracture mode was independent of oxide layer thickness and structure. Cracking occurred deeper inside titanium, in the oxygen-rich Ti[O]x solid solution surface layer. During dental ceramics firing TiO2 layers dissociate and joints become brittle with increased dissolution of oxygen into metallic Ti and consequent reduction in the metal plasticity. To accomplish an ideal metalloceramic joint this needs to be resolved. The second part introduces photoinduced superhydrophilicity of TiO2. Test samples with ALD deposited anatase TiO2 films were produced. Samples were irradiated with UV light to induce superhydrophilicity of the surfaces through a cascade leading to increased amount of surface hydroxyl groups. Superhydrophilicity (contact angle ~0˚) was achieved within 2 minutes of UV radiation. Partial recovery of the contact angle was observed during the first 10 minutes after UV exposure. Total recovery was not observed within 24h storage. Photoinduced ultrahydrophilicity can be used to enhance wettability of titanium surfaces, an important factor in dental ceramics veneering processes. The third part addresses interlayers designed to restrain oxygen dissolution into Ti during dental ceramics fusing. The main requirements for an ideal interlayer material are proposed. Based on these criteria and systematic exclusion of possible interlayer materials silver (Ag) interlayers were chosen. TPB results were significantly better in when 5 μm Ag interlayers were used compared to only Al2O3-blasted samples. In samples with these Ag interlayers multiple cracks occurred inside dental ceramics, none inside Ti structure. Ag interlayers of 5 μm on Al2O3-blasted samples can be efficiently used to retard formation of the brittle oxygen-rich Ti[O]x layer, thus enhancing metalloceramic joint integrity. The most brittle component in metalloceramic joints with 5 μm Ag interlayers was bulk dental ceramics instead of Ti[O]x. The fourth part investigates the importance of mechanical interlocking. According to the results, the significance of mechanical interlocking achieved by conventional surface treatments can be questioned as long as the formation of the brittle layers (mainly oxygen-rich Ti[O]x) cannot be sufficiently controlled. In summary in contrast to former impressions of thick titanium oxide layers this thesis clearly demonstrates diffusion of oxygen from sintering atmosphere and SiO2 to Ti structures during dental ceramics firing and the following formation of brittle Ti[O]x solid solution as the most important factors predisposing joints between Ti and SiO2-based dental ceramics to low strength. This among other predisposing factors such as residual stresses created by the coefficient of thermal expansion mismatch between dental ceramics and Ti frameworks can be avoided with Ag interlayers.
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The out-diffusion of germanium from the core of a photosensitive fiber under elevated temperature is exploited to form a Fabry-Perot filter within a single fiber Bragg grating, by subjecting the diffused region to a single exposure using the standard phase-mask technique. A key aspect of our work is the measurement of the out-diffusion through energy dispersive X-ray analysis. Furthermore, we demonstrate the use of the above single-grating filter for discrimination and simultaneous measurement of strain and temperature. The proposed technique provides a significant advantage over other existing methods that require at least two gratings.
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Single-step low-temperature solution combustion (LCS) synthesis was adopted for the preparation of LaMnO3+ (LM) nanopowders. The powders were well characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS),surface area and Fourier transform infrared spectroscopy (FTIR). The PXRD of as-formed LM showed a cubic phase but, upon calcination (900degrees C, 6 h), it transformed into a rhombohedral phase. The effect of fuel on the formation of LM was examined, and its structure and magnetoresistance properties were investigated. Magnetoresistance (MR) measurements on LM were carried out at 0, 1, 4 and 7 T between 300 and 10 K. LM (fuel-to-oxidizer ratio; = 1) showed an MR of 17% at 1 T, whereas, for 4 and 7 T, it exhibited an MR of 45 and 55%, respectively, near the TM-I. Metallic resistivity data below TM-I showed that the double exchange interaction played a major role in this compound. It was interesting to observe that the sample calcined at 1200 degrees C for 3 h exhibited insulator behavior.
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ZnO (core)/graphitic (shell) nanowires were successfully fabricated by a one-step method. Morphology of the as-grown nanowires was studied in detail by scanning electron microscopy, transmission electron microscopy (TEM), and energy dispersive X-ray analysis (EDS). High resolution TEM micrographs and selected area electron diffraction patterns reveal the core/shell morphology of the nanowires that grew along the c-axis of ZnO. EDS study of the nanowires confirms that there are no impurities within the detectable limit. Superconducting quantum interference device magnetometer measurements show room temperature ferromagnetic ordering in these core/shell nanowires. (C) 2010 Elsevier Ltd. All rights reserved.
Resumo:
Germanium nanowires were grown on Au coated Si substrates at 380 degrees C in a high vacuum (5 x 10(-5) Torr) by e-beam evaporation of Germanium (Ge). The morphology observation by a field emission scanning electron microscope (FESEM) shows that the grown nanowires are randomly oriented with an average length and diameter of 600 nm and 120 nm respectively for a deposition time of 60 min. The nanowire growth ratewas measured to be similar to 10 nm/min. Transmission electron microscope (TEM) studies revealed that the Ge nanowires were single crystalline in nature and further energy dispersive X-ray analysis(EDAX) has shown that the tip of the grown nanowires was capped with Au nanoparticles, this shows that the growth of the Ge nanowires occurs by the vapour liquid solid (VLS) mechanism. HRTEM studies on the grown Ge nanowire show that they are single crystalline in nature and the growth direction was identified to be along [110]. (C) 2010 Elsevier B.V. All rights reserved.
Resumo:
Monophasic Na0.5La0.5Bi4Ti4O15 powders were synthesized via the conventional solid-state reaction route. The X-ray powder diffraction (XRD), selected area electron diffraction (SAED) and high resolution transmission electron microscopy (HRTEM) studies carried out on the as synthesized powdered samples confirmed the phase to be a four-layer Aurivillius that crystallizes in an orthorhombic A2(1)am space group. The microstructure and the chemical composition of the sintered sample were examined by scanning electron microscope (SEM) equipped with an energy dispersive X-ray analyzer (EDX). The dielectric properties of the ceramics have been studied in the 27-700 degrees C temperature range at various frequencies (100 Hz to 1 MHz). A sharp dielectric anomaly was observed at 580 degrees C for all the frequencies corresponding to the ferroelectric to paraelectric phase transition. Saturated ferroelectric hysteresis loops were observed at 200 degrees C and the associated remnant polarization (P-r) and coercive field (E-c) were found to be 7.4 mu C/cm(2) and 34.8 kV/cm, respectively. AC conductivity analysis confirmed the existence of two different conduction mechanisms in the ferroelectric region. Activation energies calculated from the Arrhenius plots were similar to 0.24 eV and similar to 0.84 eV in the 300-450 degrees C and 450-580 degrees C temperature ranges, respectively. (C) 2010 Elsevier B.V. All rights reserved.
Resumo:
In EHV and UHV power transmission lines, corona could occur even on well designed transmission line hardware and insulators especially under wet conditions. Corona if allowed to occur continuously can significantly damage the polymeric insulators used in such lines in the long run. This paper presents the experimental results of corona aging studies conducted on unfilled silicone rubber as well as filled silicone rubber nanocomposites. Corona aging studies were conducted on silicone rubber samples with filler concentrations of 0, 1, 2 and 3 % by wt of nanosilica for 25 h and 50 h. Needle-plane electrode geometry has been used to create the corona on the samples. Different characterization techniques such as Scanning Electron Microscopy, Energy Dispersive X-ray analysis, Hydrophobicity, Fourier Transform Infrared Spectroscopy, and Optical Profilometry have been used to assess the relative performance of the samples with respect to corona aging. Results indicate that at 3 wt %, the performance of the nanocomposite is much better than the unfilled silicon rubber which can be attributed to the modifications in the material caused by the size factor of the filler.
Resumo:
Pb0.76Ca0.24TiO3 (PCT24) nanoparticles were synthesized by modified sal gel method and characterized by a number of experimental techniques such as X-ray diffraction, TGA-DTA, FTIR and transmission electron microscopy equipped with energy-dispersive X-ray spectroscopy (EDX). X-ray diffraction (XRD) and selected-area electron diffraction (SAED) investigations demonstrated that the postannealed (650 degrees C for 1 h) PCT24 nanoparticles have tetragonal perovskite crystal structure. TEM have been employed to characterize the morphology, structure and composition of the as prepared nanoparticles. Dielectric results indicates the evidence for relaxor type behavior while observed leaky ferroelectric loops may be because of the defects such as grain boundaries and the pores in the sample as the sample was not heated at higher temperature, to retain the nanosize dimension of the particles.
Resumo:
The formation and decomposition of quasicrystalline and crystalline phases in as-rapidly solidified and annealed commercial AISI 2024 aluminum alloy containing 2 wt% Li have been investigated by detailed transmission electron microscopy, including a combination of bright field and dark field imaging, selected area diffraction pattern analysis and energy dispersive X-ray microanalysis. The microstructure of as-melt spun 2024-2Li consists of alpha-Al cells, containing small coherent delta' precipitates, and particles or a continuous network of the icosahedral phase at the cell boundaries. After annealing at 300-degrees-C, the intercellular particles of the icosahedral phase coarsen progressively and assume a more faceted shape; after annealing at 400-degrees-C, particles of the decagonal and crystalline O phases precipitate heterogeneously on preexisting particles of the icosahedral phase; and after annealling at 500-degrees-C, the icosahedral and decagonal phases dissolve completely, and small particles of the crystalline O phase remain together with newly precipitated plates of the T1 phase. The icosahedral phase in melt spun and melt spun/annealed 2024-2Li belongs to the Al6CuLi3 class of icosahedral phases, with a quasilattice constant of 0.51 nm, a stoichiometry of (Al, Si)6(Cu, Mn, Fe) (Li, Mg)3 and an average composition of Al-24.1 at.% Cu-6.4 at.% Mg-1.7 at.% Si-0.3 at.% Mn-0.5 at.% Fe as-melt spun and Al-21.9 at.% Cu-6.3 at.% Mg-1.0 at.% Si-0.5 at.% Fe as-heat-treated. The decagonal phase in melt spun/annealed 2024-2Li belongs to the Al4Mn class of decagonal phases, with a periodicity of 1.23 nm along the 10-fold symmetry axis, a stoichiometry of Al3(Cu, Mn, Fe) and an average composition of Al-10.3 at.% Cu-13.8 at.% Mn-2.3 at.% Fe. The crystalline O phase in melt spun/annealed 2024-2Li has an orthorhombic structure with lattice parameters of a = 2.24 nm, b = 2.35 nm and c = 1.23 nm, a stoichiometry of Al3(Cu, Mn, Fe) and an average composition of Al-11.0 at.% Cu-14.8 at.% Mn-3.9 at.% Fe. Detailed analysis of selected area diffraction patterns shows a close similarity between the icosahedral, decagonal and crystalline O phases in melt spun and melt spun/annealed 2024-2Li. In particular, the decagonal phase and crystalline O phases have a similar composition, and exhibit an orientation relationship which can be expressed as: [GRAPHICS] suggesting that the orthorhombic O phase is an approximant structure for the decagonal phase.