Synthesis and characterization of single-crystalline alpha-MoO3 nanofibers for enhanced Li-ion intercalation applications

High quality, single-crystalline alpha-MoO3 nanofibers are synthesized by rapid hydrothermal method using a polymeric nitrosyl-complex of molybdenum(II) as molybdenum source without employing catalysts, surfactants, or templates. The possible reaction pathway is decomposition and oxidation of the complex to the polymolybdate and then surface condensation on the energetically favorable 001] direction in the initially formed nuclei of solid alpha-MoO3 under hydrothermal conditions. Highly crystalline alpha-MoO3 nanofibers have grown along 001] with lengths up to several micrometres and widths ranging between 280 and 320 nm. The alpha-MoO3 nanofibers exhibit desirable electrochemical properties such as high capacity reversibility as a cathode material of a Li-ion battery.

Combined Cryo and Room-Temperature Ball Milling to Produce Ultrafine Halide Crystallites

The combined milling at cryogenic temperature as well as room temperature (RT) has been carried out to prepare ultrafine NaCl crystallites. The milling has been done in evacuated tungsten carbide vials backfilled with high-purity Ar. The results indicate the effect duration of cryomilling prior to RT milling has a strong effect on the final crystallite size. The deformation aided sintering of NaCl crystallites during RT milling and leads to the formation of bimodal distribution of crystallites. The cuboidal-shaped NaCl crystallite undergoes a roughening transition due to plastic deformation. The experimental results are explained using the temperature-dependent mechanical properties of NaCl single crystals and plastic-deformation-induced roughening.

EXAFS and MAS NMR studies of sodium molybdophosphate and sodium tungstophosphate glasses

he local order around molybdenum and tungsten atoms in various sodium molybdophosphate and sodium tungstophosphate glasses has been investigated using extended X-ray absorption fine structure (EXAFS). Both molybdenum and tungsten atoms are present in six-coordinated environment in these glasses. Magic angle spinning nuclear magnetic resonance (MAS NMR) of P-31 suggests that metaphosphate or neutral [POO3/2] groups are present in these glasses.

Group-VI metal-carbonyl-complexes of (amino)spirocyclic cyclotriphosphosphazenes

The reactions of (amino)spirocyclotriphosphazenes, N3P3(NMe2)4(NHCH2CH2NH) (1) and N3P3(NMe2)4(NHCH2CH2CH2NH) (2) with molybdenum- and tungsten-hexacarbonyls give complexes of the type [M(CO)4(L)] (L = 1 or 2) in which the phosphazenes act as bidentate chelating ligands via one of the phosphazene ring nitrogen atoms and one of the nitrogen atoms of the diaminoalkane moiety.

Processing map for hot working of Ni–16Cr–8Fe alloy (IN 600)

The hot deformation characteristics of IN 600 nickel alloy are studied using hot compression testing in the temperature range 850-1200-degrees-C and strain rate range 0.001-100 s-1. A processing map for hot working is developed on the basis of the data obtained, using the principles of dynamic materials modelling. The map exhibits a single domain with a peak efficiency of power dissipation of 48% occurring at 1200-degrees-C and 0.2 s-1, at which the material undergoes dynamic recrystallisation (DRX). These are the optimum conditions for hot working of IN 600. At strain rates higher than 1 s-1, the material exhibits flow localisation and its microstructure consists of localised bands of fine recrystallised grains. The presence of iron in the Ni-Cr alloy narrows the DRX domain owing to a higher temperature required for carbide dissolution, which is essential for the occurrence of DRX. The efficiency of DRX in Ni-Cr is, however, enhanced by iron addition.

Processing map for hot working of powder

The constitutive flow behavior of a metal matrix composite (MMC) with 2124 aluminum containing 20 vol pct silicon carbide particulates under hot-working conditions in the temperature range of 300 °C to 550 °C and strain-rate range of 0.001 to 1 s-1 has been studied using hot compression testing. Processing maps depicting the variation of the efficiency of power dissipation given by [2m/(m + 1)] (wherem is the strain-rate sensitivity of flow stress) with temperature and strain rate have been established for the MMC as well as for the matrix material. The maps have been interpreted on the basis of the Dynamic Materials Model (DMM). [3] The MMC exhibited a domain of superplasticity in the temperature range of 450 °C to 550 °C and at strain rates less than 0.1 s-1. At 500 °C and 1 s-1 strain rate, the MMC undergoes dynamic recrystallization (DRX), resulting in a reconstitution of microstructure. In comparison with the map for the matrix material, the DRX domain occurred at a strain rate higher by three orders of magnitude. At temperatures lower than 400 °C, the MMC exhibited dynamic recovery, while at 550 °C and 1 s-1, cracking occurred at the prior particle boundaries (representing surfaces of the initial powder particles). The optimum temperature and strain-rate combination for billet conditioning of the MMC is 500 °C and 1 s-1, while secondary metalworking may be done in the super- plasticity domain. The MMC undergoes microstructural instability at temperatures lower than 400 °C and strain rates higher than 0.1 s-1.

Effect of laser processing parameters on the structure of ductile iron

Laser processing of structure sensitive hypereutectic ductile iron, a cast alloy employed for dynamically loaded automative components, was experimentally investigated over a wide range of process parameters: from power (0.5-2.5 kW) and scan rate (7.5-25 mm s(-1)) leading to solid state transformation, all the way through to melting followed by rapid quenching. Superfine dendritic (at 10(5) degrees C s(-1)) or feathery (at 10(4) degrees C s(-1)) ledeburite of 0.2-0.25 mu m lamellar space, gamma-austenite and carbide in the laser melted and martensite in the transformed zone or heat-affected zone were observed, depending on the process parameters. Depth of geometric profiles of laser transformed or melt zone structures, parameters such as dendrile arm spacing, volume fraction of carbide and surface hardness bear a direct relationship with the energy intensity P/UDb2, (10-100 J mm(-3)). There is a minimum energy intensity threshold for solid state transformation hardening (0.2 J mm(-3)) and similarly for the initiation of superficial melting (9 J mm(-3)) and full melting (15 J mm(-3)) in the case of ductile iron. Simulation, modeling and thermal analysis of laser processing as a three-dimensional quasi-steady moving heat source problem by a finite difference method, considering temperature dependent energy absorptivity of the material to laser radiation, thermal and physical properties (kappa, rho, c(p)) and freezing under non-equilibrium conditions employing Scheil's equation to compute the proportion of the solid enabled determination of the thermal history of the laser treated zone. This includes assessment of the peak temperature attained at the surface, temperature gradients, the freezing time and rates as well as the geometric profile of the melted, transformed or heat-affected zone. Computed geometric profiles or depth are in close agreement with the experimental data, validating the numerical scheme.

The role of strain rate response in plane strain abrasion of metals

Titanium flats were scribed by silicon carbide wedges over ranges of temperatures and applied strains and with lubrication. The response of the material to scribing was noted by recording the coefficient of friction, the surface morphology of track and the subsurface deformation. Additional data were obtained from (1) uniaxial compression of titanium, (2) scribing of oxygen-free high conductivity copper and (3) scribing of aluminium under dry and lubricated conditions to analyse and explain the observed variation in response of titanium to scribing with strain, temperature and lubrication.

Reduction of electric are furnace slags in stainless steelmaking - Part 1 Observations

Simultaneous reduction of iron and chromium oxides from synthetic electric are furnace stainless steelmaking slag in a graphite crucible has been studied. Above the melting point of iron the reduction of iron oxide leads to a carbon saturated Fe-C melt, but below the melting point of iron initially solid iron or iron carbide forms on the crucible surface. Only when a certain number of Fe-C droplets are formed does the reduction of chromium oxide start to form an Fe-Cr-C alloy. The reaction proceeds with pronounced foaming which depends on the basicity, temperature, and iron oxide content of the slag. IS/1352a (C) 1998 The Institute of Materials.

Microwave preparation of oxide bronzes

Several vanadium, tungsten, and molybdenum oxide bronzes have been prepared using microwave irradiation. Metal oxides and alkali metal iodides were used as starting materials, Intermittent grinding and inert atmosphere were found to be necessary for the synthesis of most of the bronzes, The reaction temperatures are remarkably lower than those employed for conventional synthetic techniques and the microwave assisted reactions proceed at extremely fast rates. The microwave synthesized bronzes consist of particles having long, rectangular rod-like morphology. (C) 1999 Academic Press.

Studies on indentation fracture toughness on ceramic and ceramic composite using acoustic emission technique

This paper is aimed at investigating the acoustic emission activities during indentation toughness tests on an alumina based wear resistant ceramic and 25 wt% silicon carbide whisker (SIC,) reinforced alumina composite. It has been shown that the emitted acoustic emission signals characterize the crack growth during loading. and unloading cycles in an indentation test. The acoustic emission results indicate that in the case of the composite the amount of crack growth during unloading is higher than that of loading, while the reverse is true in case of the wear resistant ceramics. Acoustic emission activity observed in wear resistant ceramic is less than that in the case of composite. An attempt has been made to correlate the acoustic emission signals with crack growth during indentation test.

Characterization of electrochemically deposited Cu-Ni black coatings

Electrochemically deposited Cu-Ni black coatings on molybdenum substrate from ethylenediaminetetraacetic acid (EDTA) bath solution are shown to exhibit good optical properties (alpha = 0.94, epsilon = 0.09). The deposit is characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Cu is present in metallic and +2 oxidation states in the as-prepared Cu-Ni black coating, whereas Ni2+ as well as Ni3+ species are observed in the same coating. Cu and Ni are observed in their metallic state after 10 and 20 min sputtering. X-ray initiated Auger electron spectroscopy (XAES) of Cu and Ni also agrees well with XPS investigations. (C) 2002 Elsevier Science Ltd. All rights reserved.

In situ synthesis of Al2O3-ZrO2-SiCW ceramic matrix composites by carbothermal reduction of natural silicates

In situ formations of Al2O3 + ZrO2 + SiCW ternary composite powders have been obtained by carbothermal reduction of a mixture of Sillimanite. Kaolin and Zircon using two different carbon sources. Products formed were mixtures of alumina and zirconia along with silicon carbide in the form of whiskers. The effects of composition of the reactants, the role of fineness of the starting precursors and the nature of the carbon Source on the final product powder obtained are presented. XRD and SEM analyses indicate complete reaction of the precursors to yield Al2O3 + ZrO2 + SiCW as product powders, with the SiC having whisker morphology. It is also seen that zirconia could be stabilised to some extent in the tetragonal form without any stabilising agent by tailoring the starting materials and their composition. (C) 2002 Published by Elsevier Science B.V.

Low-pressure MOCVD of Al2O3 films using aluminium acetylacetonate as precursor: nucleation and growth

A study of the deposition of aluminium oxide films by low-pressure metalorganic chemical vapour deposition from the complex aluminium acetylacetonate, in the absence of an oxidant gas, has been carried out. Depositions on to Si(100), stainless steel, and TiN-coated cemented carbide are found to be smooth, shiny, and blackish. SIMS, XPS and TEM analyses reveal that films deposited at temperatures as low as 600 degreesC contain small crystallites Of kappa-Al2O3, embedded in an amorphous matrix rich in graphitic carbon. Optical and scanning electron microscopy reveal a surface morphology made up of spherulites that suggests that film growth might involve a melting process. A nucleation and growth mechanism, involving the congruent melting clusters of precursor molecules on the hot substrate surface, is therefore invoked to explain these observations. An effort has been made experimentally to verify this proposed mechanism. (C) 2002 Elsevier Science B.V. All rights reserved.

MOCVD of aluminium oxide films using aluminiurn beta-diketonates as precursors

Deposition of Al2O3 coatings by CVD is of importance because they are often used as abrading material in cemented carbide cutting tools. The conventionally used CVD process for Al2O3 involves the corrosive reactant AlCl3. In this paper, we report on the thermal characterisation of the metalorganic precursors namely aluminium tristetramethyl-heptanedionate [Al(thd)(3)] and aluminium tris-acetylacetonate [Al(acac)(3)] and their application to the CVD of Al2O3 films. Crystalline Al2O3 films were deposited by MOCVD at low temperatures by the pyrolysis of Al(thd)(3) and Al(acac)(3). The films were deposited on a TiN-coated tungsten carbide (TiN/WC) and Si(100) substrates in the temperature range 500-1100degreesC. The as-deposited films were characterised by x-ray diffraction, optical microscopy, scanning and transmission electron microscopy, Auger electron spectroscopy. The observed crystallinity of films grown at low temperatures, their microstructure, and composition may be interpreted in terms of a growth process that involves the melting of the metalorganic precursor on the hot growth surface.