Transmission electron microscopy sample preparation technique for sintered alloys

Powder metallurgy alloys are typically inhomogeneous with a significant amount of porosity. This complicates conventional transmission electron microscopy sample preparation. However, the use of focused ion beam milling allows site specific transmission electron microscopy samples to be prepared in a short amount of time. This paper presents a method that can be used to produce transmission electron microscopy samples from an Al-Cu-Mg PM alloy. (C) 2003 IoM Communications Ltd. Published by Maney for the Institute of Materials, Minerals and Mining.

Age hardening of a sintered Al-Cu-Mg-Si-(Sn) alloy

The age hardening response of a sintered Al-3.8 wt% Cu-1.0 wt% Mg-0.70 wt% Si alloy with and without 0.1 wt% Sn was investigated. The sequence of precipitation was characterised using transmission electron microscopy. The ageing response of the sintered Al-Cu-Mg-Si-(Sn) alloy is similar to that of cognate wrought 2xxx series alloys. Peak hardness was associated with a fine, uniform dispersion of lath shaped precipitates, believed to be either the betaor Q phase, oriented along < 010 >. directions and theta' plates lying on {001}(alpha). planes. Natural ageing also resulted in comparable behaviour to that observed in wrought alloys. Porosity in the powder metallurgy alloys did not significantly affect the kinetics of precipitation during artificial ageing. Trace levels of tin, used to aid sintering, slightly reduced the hardening response of the alloy. However, this was compensated for by significant improvements in density and hardness. (c) 2005 Elsevier B.V. All rights reserved.

The effect of the atmosphere and the role of pore filling on the sintering of aluminium

Alloys of Al-3.8Cu-1Mg-0.7Si, Al-4Cu-0.6Si-0.1Mg, Al-4Cu-1.2Mg and Al-1.9Mg-1.9Si were made using air atomised powder and conventional press-and-sinter powder metallurgy techniques. These were sintered under nitrogen with a controlled water content which varied from 3 to 630 ppm (a dew point of -69 to -25 degrees C), nitrogen-5%hydrogen, argon and argon-5% hydrogen, all at atmospheric pressure, or a vacuum of

Fatigue crack propagation in a sintered 2xxx series aluminium alloy

Many potential applications for sintered aluminium are limited by the poor fatigue properties of the material. In order to increase understanding of the fatigue mechanisms in sintered aluminium, fatigue tests were carried out on a sintered 2xxx series aluminium alloy, AMB-2712. The alloy has a fatigue endurance strength of approximately 145 MPa (R = 0.1). Three regions were identified on the fatigue fracture surfaces. Region I contains the initiation site and transgranular crack propagation. When the size of the cyclic plastic zone ahead of the crack becomes comparable to the grain size, microstructural damage at the crack tip results in a transition to intergranular propagation. Region 2 mainly contains intergranularly fractured material, whilst the final fracture area makes up Region 3, in the form of dimple coalescence and intergranular failure. Transgranular fractographic features observed on fatigued specimens include fissure-type striations, cross-hatched grains, furrowed grains and grains containing step-like features. (c) 2006 Elsevier B.V. All rights reserved.

On the role of tin in the nitridation of aluminium powder

The role of tin in the mechanism by which aluminium nitride grows on aluminium powder is explored. In the absence of tin, the aluminium powder nitrides rapidly, with growth occurring both into and out from the surface of the particles. In contrast, nitridation occurs more slowly in the presence of tin, which is incorporated in the growing nitride. When the tin is depleted, rapid nitridation occurs. The initial tin concentration determines the point at which the growth rate changes. (c) 2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

On the sintering of uncompacted, pre-alloyed Al powder alloys

The effect of the addition of elemental Mg, Sri and Pb on the sintering of impressed prealloyed 2124 and 6061 powder has been investigated. Despite being sintered at a temperature that resulted in similar to20 vol.% liquid phase, high density was possible only upon the addition of similar to1% elemental Mg as well as trace amounts of Sri or Pb. Additions of Mg facilitated oxide disruption, while Sri and Pb segregated to the liquid phase, where they reduced the liquid's surface tension, thus improving sintering. (C) 2002 Elsevier Science B.V. All rights reserved.

On the role of magnesium and nitrogen in the infiltration of aluminium by aluminium for rapid prototyping applications

Selective laser sintering has been used to fabricate an aluminium alloy powder preform which is subsequently debound and infiltrated with a second aluminium alloy. This represents a new rapid manufacturing system for aluminium that can be used to fabricate large, intricate parts. The base powder is an alloy such as AA6061. The infiltrant is a binary or higher-order eutectic based on either Al-Cu or At-Si. To ensure that infiltration occurs without loss of dimensional precision, it is important that a rigid skeleton forms prior to infiltration. This can be achieved by the partial transformation of the aluminium to aluminium nitride. In order for this to occur throughout the component, magnesium powder must be added to the alumina support powder which surrounds the part in the furnace. The magnesium scavenges the oxygen and thereby creates a microclimate in which aluminium nitride can form. The replacement of the ionocovalent Al2O3 with the covalent AlN on the surface of the aluminium powders also facilitates wetting and thus spontaneous and complete infiltration. (C) 2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Comparison of texture of yogurt made from conventionally treated milk and UHT milk fortified with low-heat skim milk powder

The textures of yogurt made from ultra-high temperature (UHT) treated and conventionally treated milks at high total solids were investigated. The yogurt premixes, fortified with low-heat skim milk powder to 16%, 18%, and 20% total solids, were UHT processed at 143 degreesC for 6 s and heated at 85 degreesC for 30 min using the conventional method. The onset of gelation was delayed in the UHT-processed milk compared with conventionally heated milk. During fermentation, the viscosity of yogurt made, from UHT-treated milk at 20% total solids was close to that of yogurt made from conventionally treated milk with 16% total solids. However, after storage for greater than or equal to1 d, the yogurt made from UHT-treated milk had lower viscosity and gel strength than the yogurt made from conventionally treated milk. The solids level had no influence on yogurt culture growth.

Phase equilibria in the ZnO-rich area of the Fe-Zn-O system in air

The phase equilibria in the Fe-Zn-O system in the range 900-1580degreesC in air have been experimentally studied using equilibration and quenching techniques. The compositions of the phases at equilibrium were determined using electron probe X-ray microanalysis (EPMA). The ferrous and ferric bulk iron concentrations were measured with a wet chemical analysis using the ammonium metavanadate technique. X-ray powder diffraction analysis (XRD) was used to characterise the phases. Iron oxide dissolved in zincite was found to be present principally in the ferric form. The XRD analysis and the composition measurements both indicate that zincite is the only phase stable in the ZnO-rich area in the range of conditions investigated. The solubility of the iron oxide in zincite rapidly increases at temperatures above 1200degreesC; the morphology of the zincite crystals also sharply changes between 1200 and 1300degreesC from rounded to plate-like crystals. The plate-like zincite forms a refractory network-the type of microstructure beneficial to the Imperial Smelting Process (ISP) sinter performance. The software program FactSage with a thermodynamically optimised database was used to predict phase equilibria in the Fe-Zn-O system.

Measurement of glass-rubber transition temperature of skim milk powder by static mechanical test

Stickiness behavior of skim milk powder was investigated based on the mechanical property of the material during the glass-rubber transition. A thermally controlled device was developed for the static mechanical test. This device was attached to a texture analyzer, and skim milk powder, which was used as a model sample, was tested for its glass-rubber transition temperature (Tg-r) using static compression technique (creep test). Changes in compression probe distance as a function of temperature were recorded. Tg-r was determined, in the region where changes in the probe distance were observed, by using linear regression technique. The effect of sample quantity, compression force, and heating rate on the determination of Tg-r was investigated. All these parameters significantly influenced the Tg-r determination (p < 0.05). The Tg-r of skim milk powder measured by this novel technique was found closely correlated to its glass transition temperature (T-g) measured by DSC.

Quil A-lipid powder formulations releasing ISCOMs and related colloidal stuctures upon hydration

The aim of the present study was to prepare solid Quil A-cholesterol-phospholid formulations (as powder mixtures or compressed to pellets) by physical mixing or by freeze-drying of aqueous dispersions of these components in ratios that allow spontaneous formation of ISCOMs and other colloidal stuctures upon hydration. The effect of addition of excess cholesterol to the lipid mixtures on the release of a model antigen (PE-FITC-OVA) from the pellets was also investigated. Physical properties were evaluated by X-ray powder diffractometry (XPRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and polarized light microscopy (PLM). Characterization of aqueous colloidal dispersions was performed by negative staining transmission electron microscopy (TEM). Physically mixed powders (with or without PE-FITC-OVA) and pellets prepared from the same powders did not spontaneously form ISCOM matrices and related colloidal structures such as worm-like micelles, ring-like micelles, lipidic/layered structures and lamellae (hexagonal array of ring-like micelles) upon hydration as expected from the pseudo-temary diagram for aqueous mixtures of Quil A, cholesterol and phospholipid. In contrast, spontaneous formation of the expected colloids was demonstrated for the freeze-dried lipid mixtures. Pellets prepared by compression of freeze-dried powders released PE-FITC-OVA slower than those prepared from physically mixed powders. TEM investigations revealed that the antigen was released in the form of colloidal particles (ISCOMs) from pellets prepared by compression of freeze-dried powders. The addition of excess cholesterol slowed down the release of antigen. The findings obtained in this study are important for the formulation of solid Quil A-containing lipid articles as controlled particulate adjuvant containing antigen delivery systems. (c) 2004 Elsevier B.V. All rights reserved.

A novel method for the production of aluminium nitride

A method has been developed to produce thick (> 400 mu m) AlN surface layers oil aluminium plates at 540 degrees C, under nitrogen at atmospheric pressure. A critical element of the process is the use of Mg powder placed in close proximity to the Al plate surface. The Mg reduces/disrupts the natural, protective oxide film on the Al surface. The nitride layers form through two distinct modes, one growing outward from the Al plate surface and the other growing into the Al. (c) 2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Precipitation induced densification in a sintered Al-Zn-Mg-Cu alloy

It is demonstrated that slow cooling to 200 degrees C from a high sintering temperature (620 degrees C) reduces porosity in an Al-8Zn-2.5Mg-1Cu powder compact when compared to isothermal sintering at the higher temperature for a longer time. The reduction in porosity is attributed to shrinkage associated with removal of solute from the aluminium solid solution and heterogeneous precipitation of the eta phase (MgZn2), particularly onto pore surfaces. (c) 2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.