Preparation of Freestanding Zn Nanocrystallites by Combined Milling at Cryogenic and Room Temperatures

The present investigation reports the preparation of freestanding nanocrystalline Zn by combined mechanical milling at cryogenic and room temperatures. The cryomilling is used as an effective means of rapid fracturing. The detailed scanning electron microscopy and transmission electron microscopy observations indicate that the minimum crystallite size is 6 +/- A 2 nm after 3 hours of cryomilling. The crystallite size increases to 30 +/- A 2 nm after 3 hours of room temperature milling of the cryomilled powder due to deformation-induced sintering. Detailed theoretical analysis allows us to obtain a diagram of size of the nanoparticles formed vs temperature to explain the experimental findings.

Effect of stress orientation on microstructural evolution during creep of near-lamellar Ti-47Al-2Cr-2Nb

Microstructural evolution was studied in a near-lamellar two phase (alpha(2) + gamma) Ti-47Al-2Cr-2Nb alloy under high temperature creep and exposure conditions. The aim of this study was to probe the role of stress orientation, with respect to lamellar plates, on microstructural changes during primary creep. Creep testing was complemented with SEM and TEM based microstructural characterization. It was observed that retention of excess alpha(2) resulted in an unstable microstructure. Under stress and temperature, excess alpha(2) was lost and Cr-rich precipitates formed. Depending on stress orientation, the sequence of precipitates formed was different. alpha(2) loss was accompanied by formation of the non-equilibrium C14 Laves phase when lamellar plates were oriented parallel to the stress axis. In contrast, alpha(2) loss did not result in formation of the C14 phase in perpendicular samples. It was concluded that C14 formed preferentially in certain test orientations because of its effectiveness in relieving residual stresses in alpha(2) that arose from lattice misfit and modulus mismatch. (c) 2012 Elsevier B.V. All rights reserved.

Microstructure and tensile properties of consolidated magnesium chips

In this study tensile properties of consolidated magnesium chips obtained from solid state re-cycling (SSR) has been examined and correlated with the microstructure. Chips machined from as-cast billet of pure magnesium were consolidated through SSR technique, comprising of compaction at ambient conditions followed by hot extrusion at four different temperatures viz., 250, 300, 350 and 400 degrees C. The extruded rods were characterized for microstructure and their room temperature tensile properties. Both ultimate tensile strength and 0.2% proof stress of these consolidated materials are higher by 15-35% compared to reference material (as cast and extruded). Further these materials obey Hall-Petch relation with respect to strength dependence of grain size. Strain hardening behavior, measured in terms of hardening exponent, hardening capacity and hardening rate was found to be distinctly different in chip consolidated material compared to reference material. Strength asymmetry, measured as a ratio of compressive proof stress to tensile proof stress was higher in chip consolidated material. (C) 2012 Elsevier B.V. All rights reserved.

The Fracture Characteristics of a Near Eutectic Al-Si Based Alloy Under Compression

The fracture of eutectic Si particles dictates the fracture characteristics of Al-Si based cast alloys. The morphology of these particles is found to play an important role in fracture initiation. In the current study, the effects of strain rate, temperature, strain, and heat treatment on Si particle fracture under compression were investigated. Strain rates ranging from 3 x 10(-4)/s to 10(2)/s and three temperatures RT, 373 K, and 473 K (100 A degrees C and 200 A degrees C) are considered in this study. It is found that the Si particle fracture shows a small increase with increase in strain rate and decreases with increase in temperature at 10 pct strain. The flow stress at 10 pct strain exhibits the trend similar to particle fracture with strain rate and temperature. Particle fracture also increases with increase in strain. Large and elongated particles show a greater tendency for cracking. Most fracture occurs on particles oriented nearly perpendicular to the loading axis, and the cracks are found to occur almost parallel to the loading axis. At any strain rate, temperature, and strain, the Si particle fracture is greater for the heat-treated condition than for the non-heat-treated condition because of higher flow stress in the heat-treated condition. In addition to Si particle fracture, elongated Fe-rich intermetallic particles are also seen to fracture. These particles have specific crystallographic orientations and fracture along their major axis with the cleavage planes for their fracture being (100). Fracture of these particles might also play a role in the overall fracture behavior of this alloy since these particles cleave along their major axis leading to cracks longer than 200 mu m.

Evolution of microhardness and microstructure in a cast Al–7 % Si alloy during high-pressure torsion

Disks of a cast Al-7 % Si alloy were processed through high-pressure torsion (HPT) for 1/4, 1/2, 1, 5, and 10 revolutions under a pressure of 6.0 GPa and at temperatures of 298 and 445 K. The hardness of the samples after processing was significantly higher than in the cast sample, and the hardness profiles across the samples became more uniform with increasing numbers of turns. Processing at higher temperature gave lower hardness values. Experiments were conducted to examine the effects of HPT processing on various microstructural aspects of the cast Al-7 % Si alloy such as the grain size, the Taylor factor, and the fraction of high-angle grain boundaries. The results demonstrate that there is a correlation between trends in the microhardness values and the observed microstructures.

A new approach for understanding ion transport in glasses; example of complex alkali diborate glasses containing lead, bismuth and tellurium oxides

Mechanism of ion transport in glasses continues to be incompletely understood. Several of the theoretical models in vogue fail to rationalize conductivity behaviour when d.c. and a.c. measurements are considered together. While they seem to involve the presence of at least two components in d.c. activation energy, experiments fail to reveal that feature. Further, only minor importance is given to the influence of structure of the glass on the ionic conductivity behaviour. In this paper, we have examined several general aspects of ion transport taking the example of ionically conducting glasses in pseudo binary, yNa(2)B(4)O(7)center dot(1-y) M (a) O (b) (with y = 0 center dot 25-0 center dot 79 and M (a) O (b) = PbO, TeO2 and Bi2O3) system of glasses which have also been recently characterized. Ion transport in them has been studied in detail. We have proposed that non-bridging oxygen (NBO) participation is crucial to the understanding of the observed conductivity behaviour. NBO-BO switching is projected as the first important step in ion transport and alkali ion jump is a subsequent event with a characteristically lower barrier which is, therefore, not observed in any study. All important observations in d.c. and a.c. transport in glasses are found consistent with this model.

Synthesis, microstructure and thermal expansion studies on Ca0 center dot 5+x/2Sr0 center dot 5+x/2Zr4P6-2x Si-2x O-24 system prepared by co-precipitation method

We report on the synthesis, microstructure and thermal expansion studies on Ca0 center dot 5 + x/2Sr0 center dot 5 + x/2Zr4P6 -aEuro parts per thousand 2x Si-2x O-24 (x = 0 center dot 00 to 1 center dot 00) system which belongs to NZP family of low thermal expansion ceramics. The ceramics synthesized by co-precipitation method at lower calcination and the sintering temperatures were in pure NZP phase up to x = 0 center dot 37. For x a parts per thousand yen 0 center dot 5, in addition to NZP phase, ZrSiO4 and Ca2P2O7 form as secondary phases after sintering. The bulk thermal expansion behaviour of the members of this system was studied from 30 to 850 A degrees C. The thermal expansion coefficient increases from a negative value to a positive value with the silicon substitution in place of phosphorous and a near zero thermal expansion was observed at x = 0 center dot 75. The amount of hysteresis between heating and cooling curves increases progressively from x = 0 center dot 00 to 0 center dot 37 and then decreases for x > 0 center dot 37. The results were analysed on the basis of formation of the silicon based glassy phase and increase in thermal expansion anisotropy with silicon substitution.

A soluble-lead redox flow battery with corrugated graphite sheet and reticulated vitreous carbon as positive and negative current collectors

A soluble-lead redox flow battery with corrugated-graphite sheet and reticulated-vitreous carbon as positive and negative current collectors is assembled and performance tested. In the cell, electrolyte comprising of 1 center dot 5 M lead (II) methanesulfonate and 0 center dot 9 M methanesulfonic acid with sodium salt of lignosulfonic acid as additive is circulated through the reaction chamber at a flow rate of 50 ml min (-aEuro parts per thousand 1). During the charge cycle, pure lead (Pb) and lead dioxide (PbO2) from the soluble lead (II) species are electrodeposited onto the surface of the negative and positive current collectors, respectively. Both the electrodeposited materials are characterized by XRD, XPS and SEM. Phase purity of synthesized lead (II) methanesulfonate is unequivocally established by single crystal X-ray diffraction followed by profile refinements using high resolution powder data. During the discharge cycle, electrodeposited Pb and PbO2 are dissolved back into the electrolyte. Since lead ions are produced during oxidation and reduction at the negative and positive plates, respectively there is no risk of crossover during discharge cycle, preventing the possibility of lowering the overall efficiency of the cell. As the cell employs a common electrolyte, the need of employing a membrane is averted. It has been possible to achieve a capacity value of 114 mAh g (-aEuro parts per thousand 1) at a load current-density of 20 mA cm (-aEuro parts per thousand 2) with the cell at a faradaic efficiency of 95%. The cell is tested for 200 cycles with little loss in its capacity and efficiency.

Tension-compression asymmetry in an extruded Mg alloy AM30: temperature and strain rate effects

The effect of strain rate, (epsilon) over dot, and temperature, T, on the tension-compression asymmetry (TCA) in a dilute and wrought Mg alloy, AM30, over a temperature range that covers both twin accommodated deformation (below 250 degrees C in compression) as well as dislocation-mediated plasticity (above 250 degrees C) has been investigated. For this purpose, uniaxial tension and compression tests were conducted at T ranging from 25 to 400 degrees C with (epsilon) over dot varying between 10(-2) and 10 s(-1). In most of the cases, the stress-strain responses in tension and compression are distinctly different; with compression responses `concaving upward,' due to {10 (1) over bar2} tensile twinning at lower plastic strains followed by slip and strain hardening at higher levels of deformation, for T below 250 degrees C. This results in significant levels of TCA at T < 250 degrees C, reducing substantially at high temperatures. At T=150 and 250 degrees C, high (epsilon) over dot leads to high TCA, in particular at T=250 degrees C and (epsilon) over dot=10 s(-1), suggesting that twin-mediated plastic deformation takes precedence at high rates of loading even at sufficiently high T. TCA becomes negligible at T=350 degrees C; however at T=400 degrees C, as (epsilon) over dot increases TCA gets higher. Microscopy of the deformed samples, carried out by using electron back-scattered diffraction (EBSD), suggests that at T > 250 degrees C dynamic recrystallization begins between accompanied by reduction in the twinned fraction that contributes to the decrease of the TCA.

Effect of indium addition on microstructural, mechanical and oxidation properties of suction cast Nb-Si eutectic alloy

The paper reports effect of small ternary addition of In on the microstructure, mechanical property and oxidation behaviour of a near eutectic suction cast Nb-19.1 at-%Si-1.5 at-%In alloy. The observed microstructure consists of a combination of two kinds of lamellar structure. They are metal-intermetallic combinations of Nb-ss-beta-Nb5Si3 and Nb-ss-alpha-Nb5Si3 respectively having 40-60 nm lamellar spacings. The alloy gives compressive strength of 3 GPa and engineering strain of similar to 3% at room temperature. The composite structure also exhibits a large improvement in oxidation resistance at high temperature (1000 degrees C).

Deformation mechanisms during superplastic testing of Ti-6Al-4V-0.1B alloy

Superplastic tensile tests on warm rolled and optimally annealed boron modified alloy Ti-6Al-4V-0.1B at a temperature of 850 degrees C and initial strain rate of 3 x 10(-4) s(-1) results in a higher elongation (similar to 500%) compared to the base alloy Ti-6Al-4V (similar to 400%). The improvement in superplasticity has been attributed to enhanced contribution from interfacial boundary sliding to the overall deformation for the boron modified alloy. The boundary sliding was facilitated by the starting microstructure which predominantly contains small equiaxed primary a grains with narrow size distribution. Dynamic processes such as coarsening and globularization of primary a phase occur under the test condition but do not significantly contribute to the observed difference in superplasticity between the two alloys. In spite of cavitation takes place around the TiB particles during deformation, they do not cause macroscopic cracking and early fracture by virtue of the cavities being extremely localized. Localized cavitation is found to correlate with increased material transfer due to faster diffusion.

Composition, structure and electrical properties of DC reactive magnetron sputtered Al2O3 thin films

Thin films of alumina (Al2O3) were deposited over Si < 1 0 0 > substrates at room temperature at an oxygen gas pressure of 0.03 Pa and sputtering power of 60 W using DC reactive magnetron sputtering. The composition of the as-deposited film was analyzed by X-ray photoelectron spectroscopy and the O/Al atomic ratio was found to be 1.72. The films were then annealed in vacuum to 350, 550 and 750 degrees C and X-ray diffraction results revealed that both as-deposited and post deposition annealed films were amorphous. The surface morphology and topography of the films was studied using scanning electron microscopy and atomic force microscopy, respectively. A progressive decrease in the root mean square (RMS) roughness of the films from 1.53 nm to 0.7 nm was observed with increase in the annealing temperature. Al-Al2O3-Al thin film capacitors were then fabricated on p-type Si < 1 0 0 > substrate to study the effect of temperature and frequency on the dielectric property of the films and the results are discussed.

Deposition and characterization of pure and Cd doped SnO2 thin films by the nebulizer spray pyrolysis (NSP) technique

Pure and cadmium doped tin oxide thin films were deposited on glass substrates from aqueous solution of cadmium acetate, tin (IV) chloride and sodium hydroxide by the nebulizer spray pyrolysis (NSP) technique. X-ray diffraction reveals that all films have tetragonal crystalline structure with preferential orientation along (200) plane. On application of the Scherrer formula, it is found that the maximum size of grains is 67 nm. Scanning electron microscopy shows that the grains are of rod and spherical in shape. Energy dispersive X-ray analysis reveals the average ratio of the atomic percentage of pure and Cd doped SnO2 films. The electrical resistivity is found to be 10(2) Omega cm at higher temperature (170 degrees C) and 10(3) Omega cm at lower temperature (30 degrees C). Optical band gap energy was determined from transmittance and absorbance data obtained from UV-vis spectra. Optical studies reveal that the band gap energy decreases from 3.90 eV to 3.52 eV due to the addition of Cd as dopant with different concentrations.

Pt-Ru decorated self-assembled TiO2-carbon hybrid nanostructure for enhanced methanol electrooxidation

Porous titanium oxide-carbon hybrid nanostructure (TiO2-C) with a specific surface area of 350 m(2)/g and an average pore-radius of 21 center dot 8 is synthesized via supramolecular self-assembly with an in situ crystallization process. Subsequently, TiO2-C supported Pt-Ru electro-catalyst (Pt-Ru/TiO2-C) is obtained and investigated as an anode catalyst for direct methanol fuel cells (DMFCs). X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM) have been employed to evaluate the crystalline nature and the structural properties of TiO2-C. TEM images reveal uniform distribution of Pt-Ru nanoparticles (d (Pt -aEuro parts per thousand Ru) = 1 center dot 5-3 center dot 5 nm) on TiO2-C. Methanol oxidation and accelerated durability studies on Pt-Ru/TiO2-C exhibit enhanced catalytic activity and durability compared to carbon-supported Pt-Ru. DMFC employing Pt-Ru/TiO2-C as an anode catalyst delivers a peak-power density of 91 mW/cm(2) at 65 A degrees C as compared to the peak-power density of 60 mW/cm(2) obtained for the DMFC with carbon-supported Pt-Ru anode catalyst operating under similar conditions.

Tensile flow and work hardening behavior of hot cross-rolled AA7010 aluminum alloy sheets

The present work describes the tensile flow and work hardening behavior of a high strength 7010 aluminum alloy by constitutive relations. The alloy has been hot rolled by three different cross-rolling schedules. Room temperature tensile properties have been evaluated as a function of tensile axis orientation in the as-hot rolled as well as peak aged conditions. It is found that both the Ludwigson and a generalized Voce-Bergstrom relation adequately describe the tensile flow behavior of the present alloy in all conditions compared to the Hollomon relation. The variation in the Ludwigson fitting parameter could be correlated well with the microstructural features and anisotropic contribution of strengthening precipitates in the as-rolled and peak aged conditions, respectively. The hardening rate and the saturation stress of the first Voce-Bergstrom parameter, on the other hand, depend mainly on the crystallographic texture of the specimens. It is further shown that for the peak aged specimens the uniform elongation (epsilon(u)) derived from the Ludwigson relation matches well with the measured epsilon(u) irrespective of processing and loading directions. However, the Ludwigson fit overestimates the epsilon(u) in case of the as-rolled specimens. The Hollomon fit, on the other hand, predicts well the measured epsilon(u), of the as-rolled specimens but severely underestimates the epsilon(u), for the peak aged specimens. Contrarily, both the relations significantly overestimate the UTS of the as-rolled and the peak aged specimens. The Voce-Bergstrom parameters define the slope of e Theta-sigma plots in the stage-III regime when the specimens show a classical linear decrease in hardening rate in stage-III. Further analysis of work hardening behavior throws some light on the effect of texture on the dislocation storage and dynamic recovery.