143 resultados para Nano-indentation


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Titania (TiO2) nano-photocatalysts, with different phases, prepared using a modified sol-gel process were employed in the degradation of rhodamine at 10 mg L-1 concentration. The degradation efficiency of these nano-photocatalysts was compared to that of commercial Degussa P25 titania. It was found that the nanocatalysts calcined at 450 degrees C and the Degussa P25 titania had similar photoreactivity profiles. The commercial Degussa P25 nanocatalysts had an overall high apparent rate constant of (K-app) of 0.023 min(-1). The other nanocatalyst had the following rate constants: 0.017, 0.0089, 0.003 and 0.0024 min(-1) for 450, 500, 550 and 600 degrees C calcined catalysts, respectively. This could be attributed to the phase of the titania as the anatase phase is highly photoactive than the other phases. Furthermore, characterisation by differential scanning calorimetry showed the transformation of titania from amorphous to anatase and finally to rutile phase. SEM and TEM characterisations were used to study the surface morphology and internal structure of the nanoparticles. BET results show that as the temperature of calcinations was raised, the surface area reduced marginally. X-ray diffraction was used to confirm the different phases of titania. This study has led to a conclusion that the anatase phase of the titania is the most photoactive nanocatalyst. It also had the highest apparent rate constant of 0.017 min(-1), which is similar to that of the commercial titania.

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Deformation and recrystallization textures in nano-crystalline nickel with average grain size of 20 nm were investigated using X-ray diffraction, electron microscopy and differential scanning calorimetry. The deformation behaviour of nano-crystalline nickel is quite complicated due to intervention of other deformation mechanisms like grain boundary sliding and restoration mechanisms like grain growth and grain rotation to dislocation mediated slip. Recrystallization studies carried out on the deformed nano-crystalline nickel showed that the deformation texture was retained during low temperature annealing (300 degrees C), while at higher temperature (1000 degrees C), the texture got randomised. The exact mechanism of texture formation during deformation and recrystallization has been discussed.

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It is generally known that addition of conducting or insulating particles to mineral transformer oil, lowers its breakdown strength, E-d. However, if the particulates are of molecular dimensions, or nanoparticles, (NPs), as they are called, the breakdown strength is seen to increase considerably. Recent experiments by the authors on oil cooled power equipment such as transformers showed that, nanofluids comprising NPs of selected oxides of iron, such as Fe(3)o(4), called magnetite, added to transformer oil increased the breakdown voltage of the virgin oil and more importantly a remarkable enhancement in the thermal conductivity and the viscosity and hence an increased loadability of the transformer for a given top oil temperature (TOT).

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The existence of an indentation size effect (ISE) in the onset of yield in a Zr-based bulk metallic glass (BMG) is investigated by employing spherical-tip nanoindentation experiments. Statistically significant data on the load at which the first pop-in in the displacement occurs were obtained for three different tip radii and in two different structural states (as-cast and structurally relaxed) of the BMG. Hertzian contact mechanics were employed to convert the pop-in loads to the maximum shear stress underneath the indenter. Results establish the existence of an ISE in the BMG of both structural states, with shear yield stress increasing with decreasing tip radius. Structural relaxation was found to increase the yield stress and decrease the variability in the data, indicating ``structural homogenization'' with annealing. Statistical analysis of the data was employed to estimate the shear transformation zone (STZ) size. Results of this analysis indicate an STZ size of similar to 25 atoms, which increases to similar to 34 atoms upon annealing. These observations are discussed in terms of internal structure changes that occur during structural relaxation and their interaction with the stressed volumes in spherical indentation of a metallic glass. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

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In submitted research; nanocrystalline powders having elements Ni0.5Cu0.25Zn0.25Fe2 xInxO4 with varied amounts of indium ( x = 0.0, 0.1, 0.2, 0.3 and 0.4) were grown-up by modified citrate to nitrate alchemy. The realism of single phase cubic spinel creation of the synthesized ferrite samples was studied by the DTA-TGA, XRD, SEM, EDX, FT-IR, VSM and dielectric measurements. SEM was applied to inspect the morphological variations and EDX was used to determine the compositional mass ratios. The studies on the dielectric constant (epsilon'), dielectric loss (epsilon `'), loss tangent (tan delta), ac conductivity (sigma(ac)), resistive and reactive parts of the impedance analysis (Z' and Z `') at room temperature were also carried out. The saturation magnetizations (Ms) were determined using the vibrating sample magnetometer (VSM). Ms. decreased with the increase In3+ doping content, as Fe3+ of 5(mu B) ions are replaced by In3+ of 5 mu(B) ions. (C) 2012 Elsevier B. V. All rights reserved.

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We report a simple, template free and low-temperature hydrothermal reaction pathway using Cu(II) - thiourea complex (prepared in situ from copper (II) chloride and thiourea as precursors) and citric acid as complexing agent to synthesize two-dimensional hierarchical nano-structures of covellite (CuS). The product was characterized with the help of X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive analysis of X-ray spectroscopy (EDAX) and X-ray photoelectron spectroscopy (XPS). The concentration of citric acid in the hydrothermal precursor solution was seen to have a profound effect on the nanostructure of the product generated. Based on the outcoming product nano-architecture at different concentration of the ionic surfactant in the hydrothermal precursor solution a possible mechanism suited for reaction and further nucleation is also discussed. (C) 2012 Elsevier B.V. All rights reserved.

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The combustion synthesis has been utilized to prepare nanophased powders of cobalt spinel ferrite using ODH and glycine fuels. The product was characterized by X‐ray diffraction; Fourier transformed spectroscopy, scanning electron microscopy, UV‐Vis absorption etc. The XRD patterns reveal spinal cubic structure. SEM profiles show the product is porous, agglomeration, irregular in shape. The crystallite size was estimated using Scherer’s formula and W‐H plots and show nano in size (13 nm: ODH & 36 nm: Glycine). The UV‐Vis absorption shows at ∼430 nm in both the samples.

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The authors studied the formation of a wafer-scale network of connected colloidal beads by reactive ion etching. The dimensions of the connections have been studied as a function of etching time for colloidal beads of different sizes, and could be well controlled. The authors have found that the nano-network forms and disappears for the same time of etching independent of the diameter of the polystyrene beads. With recent interest of connected colloidal networks in various optical sensing applications, such as photonic crystals, as surface-enhanced Raman scattering substrates, the studies have potential uses in the development of wafer-scale nanophotonic sensors.

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Here, we report for the first time a simple thermal oxidation strategy for the large area synthesis of Ge/GeO2 nanoholes from Ge and studied the luminescence of Ge/GeO2 and hole formation mechanism through phase and luminescence mapping. Photoluminescence mapping reveals that the emission in the visible range is only from the hole region, which provokes the necessity of the nanoholes. Such materials can also be used to convert ultraviolet to visible radiation for detection by conventional phototubes and to coat blue or ultraviolet diodes to obtain white light.

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Reports on the alloys formed from immiscible atoms when they are contained in a nano-sized system have initiated several research activities in the recent years. Bridging of the miscibility gap at nanoscale is significant as it has the potential to produce novel alloy materials with useful technological applications. Although the literature contains noticeable number of reports on the formation of solid solution between bulk immiscible atoms, several issues related to phase stability and microstructure remain unaddressed. This article discusses some of these issues using examples from the work done by the author's research group on isolated nanoparticles of bulk immiscible binary systems such as Ag-Ni, Ag-Fe and Ag-Co.

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Uniform La0.6Sr0.4MnO3 (LSMO) nanotubes of an average diameter 180 nm were synthesized by a modified sol-gel method employing nanochannel porous anodic alumina templates. The nanotubes were characterized chemically and structurally by XRD, SEM, EDX, and TEM. Postannealed (700 degrees C for 1 h hour) nanotubes were found to be polycrystalline from XRD and SAED studies. To get further insight into the nanotube structure, HRTEM studies were done, which revealed that obtained LSMO nanotubes were structurally constituted with nanoparticles of 3-12 nm size. These constituent nanoparticles were randomly aligned and self-knitted to build the nanotube wall. Investigation of magnetic properties at this structured nanoscale revealed remarkable irreversibility between the zero field cooling (ZFC) and field cooling (FC) magnetization curves accompanied with a peak in the ZFC curve indicating spin-glass-like behavior. Structural defects and compositional variations at surfaces and grain-boundaries of constituent nanoparticles might be responsible for this anomalous magnetic behavior.

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Carbonaceous nickel oxide powder samples have been synthesized from an adducted nickel beta-ketoester complex used as a ``single source precursor'' through a solution-based microwave-assisted chemical route. Comprehensive analysis of the resulting powder material has been carried out using various characterization techniques. These analysis reveal that, depending on the solvent used, either NiO/C or Ni/NiO/C composites are formed, wherein Ni and/or NiO nanocrystals are enveloped in amorphous carbon. As the components emerge from the same molecular source, the composites are homogeneous on a fine scale, making them promising electrode materials for supercapacitors. Electrochemical capacitive behavior of these oxide composites is studied in a three-electrode configuration. With a specific capacitance of 113 F g(-1), Ni/NiO/C is superior to NiO/C as capacitor electrode material, in 0.1 M Na2SO4 electrolyte. This is confirmed by impedance measurements, which show that charge-transfer resistance and equivalent series resistance are lower in Ni/NiO/C than in NiO/C, presumably because of the presence of metallic nickel in the former. The cyclic voltammograms are nearly rectangular and the electrodes display excellent cyclability in different electrolytes: Na2SO4, KOH and Ca(NO3)(2)center dot 4H(2)O. Specific capacitance as high as 143 F g(-1), is measured in Ca(NO3)(2)center dot 4H(2)O electrolyte.

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The deformation behaviour of macrocrystalline and nanocrystalline nickel shows a striking similarity in terms of higher intragranular misorientation and a texture with dominant Brass component on rolling. This is in contrast to microcrystalline nickel, with lower intragranular misorientation and typical Copper type texture. This has been attributed to the free surfaces in macrocrystalline sample and grain boundaries in nanocrystalline sample. Experimental evidence of `Grain Boundary Affected Zone' (GBAZ) showing multi-slip in contrast to limited slip in the grain interiors has been provided. The similarity in evolution of texture and intragranular misorientation is explained on the basis of reduced contribution from the GBAZ at the two extreme length scales.

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In this work, the effect of hybridizing micro-Ti with nano-SiC particulates on the microstructural and the mechanical behaviour of Mg-5.6Ti composite were investigated. Mg materials containing micron-sized Ti particulates hybridized with different amounts of nano-size SiC particulates were synthesized using the disintegrated melt deposition method followed by hot extrusion. The microstructural and mechanical behaviour of the developed Mg hybrid composites were studied in comparison with Mg-5.6Ti. Microstructural characterization revealed grain refinement attributed to the presence of uniformly distributed micro-Ti particles embedded with nano-SiC particulates. Electron back scattered diffraction (EBSD) analyses of Mg-(5.6Ti + 1.0SiC)(BM) hybrid composite showed relatively more localized recrystallized grains and lesser tensile twin fraction, when compared to Mg-5.6Ti. The evaluation of mechanical properties indicated that the best combination of strength and ductility was observed in the Mg-(5.6Ti + 1.0SiC)(BM) hybrid composites. The superior strength properties of the Mg-(5.6Ti + x-SiC)(BM) hybrid composites when compared to Mg-5.6Ti is attributed to the presence of nano-reinforcements, the uniform distribution of the hybridized particles and the better interfacial bonding between the matrix and the reinforcement particles, achieved by nano-SiC addition.

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Instrumented microindentation (IM) on two Ni-Ti shape memory alloys (SMAs), where one is austenitic and the other is martensitic at room temperature, were conducted from 40 to 150 degrees C. Results show that the depth and work recovery ratios, eta(d) and eta(w) respectively, are complementary to each other. While eta(d) decreases gradually with temperature for austenite, it drops markedly for the martensite in the martensite-to-austenite transformation regime. These results affirm the utility of IM for characterizing SMAs.