A broad pore size distribution mesoporous SnO2 as anode for lithium-ion batteries

We demonstrate here that mesoporous tin dioxide (abbreviated M-SnO2) with a broad pore size distribution can be a prospective anode in lithium-ion batteries. M-SnO2 with pore size ranging between 2 and 7.5 nm was synthesized using a hydrothermal procedure involving two different surfactants of slightly different sizes, and characterized. The irreversible capacity loss that occurs during the first discharge and charge cycle is 890 mAh g(-1), which is smaller than the 1,010-mAh g(-1) loss recorded for mesoporous SnO2 (abbreviated S-SnO2) synthesized using a single surfactant. After 50 cycles, the discharge capacity of M-SnO2 (504 mAh g(-1)) is higher than that of S-SnO2 (401 mAh g(-1)) and solid nanoparticles of SnO2 (abbreviated nano-SnO2 < 4 mAh g(-1)) and nano-SnO2. Transmission electron microscopy revealed higher disorder in the pore arrangement in M-SnO2. This, in turn imparts lower stiffness to M-SnO2 (elastic modulus, E (R) a parts per thousand aEuro parts per thousand 14.5 GPa) vis-a-vis S-SnO2 (E (R) a parts per thousand aEuro parts per thousand 20.5 GPa), as obtained using the nanoindentation technique. Thus, the superior battery performance of M-SnO2 is attributed to its intrinsic material mechanical property. The fluidity of the internal microstructure of M-SnO2 resulted in a lower degree of aggregation of Sn particles compared to S-SnO2 and nano-SnO2 structural stabilization and long-term cyclability.

Stress and texture development during sputtering of yttria, zirconia, and yttria stabilized zirconia films on Si substrates

Understanding and controlling growth stress is a requisite for integrating oxides with Si. Yttria stabilized zirconia (YSZ) is both an important functional oxide and a buffer layer material needed for integrating other functional oxides. Stress evolution during the growth of (100) and (111) oriented YSZ on Si (100) by radio frequency and reactive direct current sputtering has been investigated with an in-situ monitor and correlated with texture evolution. Films nucleated at rates <5 nm/min are found to be (111) oriented and grow predominantly under a compressive steady state stress. Films nucleated at rates >20 nm/min are found to be (100) oriented and grow under tension. A change in growth rate following the nucleation stage does not change the orientation. The value of the final steady state stress varies from -4.7 GPa to 0.3 GPa. The in-situ studies show that the steady state stress generation is a dynamic phenomenon occurring at the growth surface and not decided at film nucleation. The combination of stress evolution and texture evolution data shows that the adatom injection into the grain boundaries is the predominant source of compressive stress and grain boundary formation at the growth surface is the source of tensile stress. (C) 2012 American Institute of Physics. http://dx.doi.org/10.1063/1.4757924]

Microstructure and mechanical properties of oxidation resistant suction cast Nb-Si-Al alloy

In this paper, we report a significant improvement in mechanical and oxidation properties of near eutectic Nb-Si alloys by the addition of aluminum (Al) and control of microstructural length scale. A comparative study of two alloys Nb-18.79at%Si and Nb-12.3at%Si-9at%Al were carried out. The processing for microstructure refinements were carried out by vacuum suction casting in water cooled thick copper mould. It is shown that addition of Al suppresses Nb3Si phase and promotes beta Nb5Si3 phase under nonequilibrium solidification condition. The microstructural length scale and in particular eutectic spacing reduces significantly to 50-100 nm in suction cast ternary alloy. A detailed TEM study shows the presence of delta-Nb11Si4 phase in Nb matrix. The hardness of Nb solid solution can be increased as a consequence to a level observed in Nb3Si intermetallic due to the well oriented precipitates. Compression test yields the ultimate strength of 1.8 +/- 0.1 GPa and engineering strain of 2.3 +/- 0.03%. In comparison, the binary Nb-18.79 at% Si alloy possesses an ultimate strength of 1.35 +/- 0.1 GPa and strain of 0.2 +/- 0.01% when processed under identical conditions. The latter exhibits coarser microstructural length scale (300-400 nm) and a brittle behavior. The indentation fracture toughness of Al containing suction cast alloy shows a value of 20.2 +/- 0.5 MPa root m which represents a major improvement over bulk Nb-Si eutectic alloy. The detailed thermal studies confirm a multifold improvement in oxidation resistance up to 1000 degrees C. (C) 2012 Elsevier B.V. All rights reserved.

Nanomechanical and optical properties of highly a-axis oriented AlN films

This paper reports optical and nanomechanical properties of predominantly a-axis oriented AlN thin films. These films were deposited by reactive DC magnetron sputtering technique at an optimal target to substrate distance of 180 mm. X-ray rocking curve (FWHM = 52 arcsec) studies confirmed the preferred orientation. Spectroscopic ellipsometry revealed a refractive index of 1.93 at a wavelength of 546 nm. The hardness and elastic modulus of these films were 17 and 190 GPa, respectively, which are much higher than those reported earlier can be useful for piezoelectric films in bulk acoustic wave resonators. (C) 2012 American Institute of Physics. http://dx.doi.org/10.1063/1.4772204]

Effect of Mg addition on microstructural, mechanical and environmental properties of Nb-Si eutectic composite

The paper reports the effect of addition of small amount of Mg on the mechanical and oxidation properties of Nb-Nb3Si eutectic composites in Nb-Si system under the condition of suction casting. Mg addition increases the volume fraction of primary dendrites of Nb solid solution. This phase contains significant amount of strengthening precipitates. Two different precipitates are identified. The large plate shaped precipitates are that of hcp phase, while fine coherent precipitates have the structure similar to recently identified delta-Nb11Si2 phase. The Mg addition improves both the strength and ductility of the composite at room temperature (similar to 1.4 GPa and similar to 5% engineering strain) as well as at 700 degrees C(similar to 1.2 GPa and similar to 7% engineering strain). The presence of Mg results in a complex barrier layer which significantly increases the oxidation resistance up to a temperature of at least 1000 degrees C. (C) 2012 Elsevier B.V. All rights reserved.

Structural and mechanical properties of room temperature sputter deposited CrN coatings

Chromium nitride (CrN) thin films were deposited at room temperature on silicon and glass substrates using DC reactive magnetron sputtering in Ar + N-2 plasma. Structure and mechanical properties of these films were examined by using XRD, FESEM and nanoindentation techniques. XRD studies revealed that films are of mixed phase at lower nitrogen partial pressure (P-N2) and single phase at higher (P-N2). Microscopy results show that the films were composed of non-equiaxed columns with nanocrystallite morphology. The hardness and elastic modulus of the films increase with increasing nitrogen partial pressure (P-N2). A maximum hardness of similar to 29 GPa and elastic modulus of 341 GPa were obtained, which make these films useful for several potential applications. (C) 2012 Elsevier Ltd. All rights reserved.

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.

Pressure induced structural phase transformation in TiN: a first-principles study

Titanium nitride (TiN), which is widely used for hard coatings, reportedly undergoes a pressure-induced structural phase transformation, from a NaCl to a CsCl structure, at similar to 7 GPa. In this paper, we use first-principles calculations based on density functional theory with a generalized gradient approximation of the exchange correlation energy to determine the structural stability of this transformation. Our results show that the stress required for this structural transformation is substantially lower (by more than an order of magnitude) when it is deviatoric in nature vis-a-vis that under hydrostatic pressure. Local stability of the structure is assessed with phonon dispersion determined at different pressures, and we find that CsCl structure of TiN is expected to distort after the transformation. From the electronic structure calculations, we estimate the electrical conductivity of TiN in the CsCl structure to be about 5 times of that in NaCl structure, which should be observable experimentally. (C) 2013 American Institute of Physics. http://dx.doi.org/10.1063/1.4798591]

Influence of physical structure and chemistry of diesel soot suspended in hexadecane on lubrication of steel-on-steel contact

Soot generated from the combustion process in diesel engines affect engine tribology. In this paper, two diesel soot samples; from engine exhaust and oil filter are suspended in hexadecane oil and the suspension is used to lubricate a steel ball on steel flat sliding contact at a contact pressure of 1.3 GPa. The friction and wear of the steel flat are recorded. The data are compared with those recorded when the soot is generated by burning ethylene gas. The rationale for the comparatively poor tribology of diesel soot is explored by quantifying the size and shape of primary particles and agglomerates, hardness of single primary soot particles, the crystallinity and surface and near surface chemistry of soot and interparticle adhesion.

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).

Densification kinetics, phase assemblage and hardness of spark plasma sintered Cu-10 wt% TiB2 and Cu-10 wt% TiB2-10 wt% Pb composites

The present work demonstrates the synthesis of Cu-10 wt% TiB2 composites with a theoretical density of more than 90% by tailoring the spark plasma sintering (SPS) conditions in the temperature range of 400-700 degrees C. Interestingly, 10 wt% Pb addition to Cu-10 wt% TiB2 lowers the sinter density and the difference in the densification behavior of the investigated compositions was discussed in reference to the current profile recorded during a SPS cycle. The sintering kinetics and phase assemblage were also discussed in reference to surface melting of the constituents prior to bulk melting temperature, temperature dependent wettability of Pb on Cu, diffusion kinetics of Cu as well as the formation of various oxides. An important result is that a high hardness of around 2 GPa and relative density close to 92% qtheoretical was achieved for the Cu-10 wt% TiB2-10 wt% Pb composite, and such a combination has never been achieved before using any conventional processing route.

On the densification mechanisms and properties of Cu-Pb and Cu-Pb-TiB2 nanocomposites densified using spark plasma sintering

The present paper is aimed to understand the sub-processes triggered by rapid heating during spark plasma sintering as well as to assess the extent to which densification and properties of metallic materials can be enhanced using such superfast consolidation process. Using nanocrystalline Cu-Pb as a model system, the influence of Pb as well as TiB2 addition on the densification mechanisms and properties are discussed. Importantly, a high hardness of 2 GPa is achieved in Cu-based nanocomposites. (C) 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Effect of Stress and Interface defects on Photo Luminescence of Si nano-crystals embedded in SiO2

Effect of stress and interface defects on photo luminescence property of a silicon nano-crystal (Si-nc) embedded in amorphous silicon dioxide (a-SiO2) are studied in this paper using a self-consistent quantum-continuum based modeling framework. Si-ncs or quantum dots show photoluminescence at room temperature. Whether its origin is due to Si-nc/a-SiO2 interface defects or quantum confinement of carriers in Si-nc is still an outstanding question. Earlier reports have shown that stresses greater than 12 GPa change the indirect energy band gap structure of bulk Si to a direct energy band gap structure. Such stresses are observed very often in nanostructures and these stresses influence the carrier confinement energy significantly. Hence, it is important to determine the effect of stress in addition to the structure of interface defects on photoluminescence property of Si-nc. In the present work, first a Si-nc embedded in a-SiO2 is constructed using molecular dynamics simulation framework considering the actual conditions they are grown so that the interface and residual stress in the structure evolves naturally during formation. We observe that the structure thus created has an interface of about 1 nm thick consisting of 41.95% of defective states mostly Sin+ (n = 0 to 3) coordination states. Further, both the Si-nc core and the embedding matrix are observed to be under a compressive strain. This residual strain field is applied in an effective mass k.p Hamiltonian formulation to determine the energy states of the carriers. The photo luminescence property computed based on the carrier confinement energy and interface energy states associated with defects will be analysed in details in the paper.

An early in-situ stress signature of the AlN-Si pre-growth interface for successful integration of nitrides with (111) Si

The integration of Metal Organic Chemical Vapor Deposition (MOCVD) grown group III-A nitride device stacks on Si (111) substrates is critically dependent on the quality of the first AlN buffer layer grown. A Si surface that is both oxide-free and smooth is a primary requirement for nucleating such layers. A single parameter, the AlN layer growth stress, is shown to be an early (within 50 nm), clear (<0.5 GPa versus > 1GPa), and fail-safe indicator of the pre-growth surface, and the AlN quality required for successful epitaxy. Grain coalescence model for stress generation is used to correlate growth stress, the AlN-Si interface, and crystal quality. (C) 2013 AIP Publishing LLC.

Bactericidal effect of silver-reinforced carbon nanotube and hydroxyapatite composites

Bacterial infection remains an important risk factor after orthopedic surgery. The present paper reports the synthesis of hydroxyapatite-silver (HA-Ag) and carbon nanotube-silver (CNT-Ag) composites via spark plasma sintering (SPS) route. The retention of the initial phases after SPS was confirmed by phase analysis using X-ray diffraction and Raman spectroscopy. Energy dispersive spectrum analysis showed that Ag was distributed uniformly in the CNT/HA matrix. The breakage of CNTs into spheroid particles at higher temperatures (1700 degrees C) is attributed to the Rayleigh instability criterion. Mechanical properties (hardness and elastic modulus) of the samples were evaluated using nanoindentation testing. Ag reinforcement resulted in the enhancement of hardness (by similar to 15%) and elastic modulus (similar to 5%) of HA samples, whereas Ag reinforcement in CNT, Ag addition does not have much effect on hardness (0.3 GPa) and elastic modulus (5 GPa). The antibacterial tests performed using Escherichia coli and Staphylococcus epidermidis showed significant decrease (by similar to 65-86%) in the number of adhered bacteria in HA/CNT composites reinforced with 5% Ag nanoparticles. Thus, Ag-reinforced HA/CNT can serve as potential antibacterial biocomposites.