Transient liquid phase sintering of high density Fe3Al using Fe and Fe2Al5/FeAl2 powders Part 1: Experimentation and results

Abstract

High density Fe₃Al was produced through transient liquid phase sintering, using rapid heating rates of greater than 150 K min^-1 and a mixture of prealloyed and elemental powders. Prealloyed Fe₂Al₅/FeAl₂ (50Fe/50Al, wt-%) powder was added to elemental iron powder in a ratio appropriate for producing an overall Fe₃Al (13·87 wt-%) ratio. The heating rate, sintering time, sintering temperature, green density and powder particle size were controlled during the study. Heating rate, sintering time and powder particle size had the most significant influence upon the sintered density of the compacts. The highest sintered density of 6·12 Mg m^-3 (92% of the theoretical density for Fe3Al) was achieved after 15 minutes of sintering at 1350°C, using a 250 K min^{- 1} heating rate, 1-6 μm Fe powders and 5·66 μm alloy powders.

SEM microscopy suggests that agglomerated Fe₂Al₅/ FeAl₂ particles, which form a liquid during sintering, are responsible for a significant portion of the remaining porosity in high sintered density compacts, creating stable pores, larger than 100 μm diameter, after melting. High density was achieved by minimising the Kirkendall porosity formed during heating by unbalanced diffusion and solubility between the iron and Fe₂Al₅/FeAl₂ components. The lower diffusion rate of aluminium in the prealloyed powder into the iron compared with elemental aluminium in iron, coupled with a fast heating rate, is expected to permit minimal iron-aluminium interdiffusion during heating so that when a liquid forms the aluminium dissolves in the iron to promote solidification at a lower aluminium content. This leads to a further reduction in porosity.     

Comparison of sintering of titanium and titanium hydride powders

Abstract

The cold compaction and vacuum sintering behaviour of a Ti powder and a Ti hydride powder were compared. Master sintering curve models were developed for both powders. Die ejection force, green strength and green porosity were lower for hydride powder than for Ti powder, all probably resulting from reduced cold welding and friction during compaction. For sintering temperatures above ～1000°C, most of the difference in the sintered density of Ti and hydride is explained by assuming equal densification, while taking into account the lower green porosity of compacts made from hydride powder. However, there is evidence that particle fracture during compaction also contributes to increased sintered density for hydride powder. The Ti powder conformed to a master sintering curve model with apparent activation energy of 160 kJ mol^?. The activation energy for Ti hydride also appeared to be about 160 kJ mol^?, but the model did not fit the experimental data well.     

THE POWDER METALLURGY OF RUTHENIUM

Abstract

An investigation of the powder metallurgy of ruthenium is described, from the reduction of ammonium ruthenium chloride to the working of sintered compacts. The powder properties measured were specific surface area, by a simplified BET method, and tap density. The dependence of these properties on the conditions of reduction has been determined. The surface area of powders varies from 1 to 10 m²/g in the temperature-of-reduction range 700-350°C. The tap density is also variable (1–3 g/c.c.) and is generally related to the surface area. The effects of compacting pressure and temperature on sintering are described, the progress of sintering being observed by measurements of the “open” and “closed” porosity present in samples. Compact densities up to 95% of theoretical can be obtained by sintering at 1500°C. The selection of powder properties and compacting pressures to be used in the production, by vacuum sintering at 1500°C, of high-density compacts for working, is governed by the necessity to maintain open porosity during the heating cycle up to at least 1200°C, as considerable gas evolution occurs at this temperature; at the same time it is essential that good densification shall have occurred even at this stage. These conditions can be met by using powder with a surface area of 2–5 m²/g and compacting pressures in the range 0·5–25 tons/in ².

Observations on the hot working of sintered compacts indicate that ease of working is related to the surface area of the powder.     

Fabrication and characterisation of bulk Al2O3/Mo nanocomposite by mechanical milling and sintering

Abstract

In this study, fabrication and mechanical properties of alumina based ceramic matrix nanocomposite reinforced with 15 and 26·6 vol.-%Mo particles were investigated. Alumina–molybdenum nanocomposite powders were prepared by ball milling of Al and MoO₃ in an SPEX8000 type ball mill. The powder particles were consolidated by cold uniaxial pressing followed by sintering in vacuum atmosphere at 1300 and 1400°C. The structural evaluation of as milled and sintered samples was studied by X-ray diffraction, differential scanning calorimetry and scanning electron microscopy. Sintered samples were examined by hardness measurements and three-point flexural strength. Results show a significant improvement in flexural strength of Al₂O₃–Mo nanocomposites in comparison to monolithic alumina and increases by Mo content. During sintering, grain growth and α-Al₂O₃ to γ-Al₂O₃ transformation occurred. In addition, an increase in temperature of sintering resulted in higher density and hardness of consolidated nanocomposites.     

New technological approach to fabrication of high density PM parts by cold pressing sintering

Abstract

A new technological approach to the fabrication of high density powder metallurgy (PM) parts via single pressing sintering, allowing cold compaction to be performed without admixed lubricants, has been studied. The influence of in pore gas on the compacts' green density and their sintered properties were evaluated. A mathematical expression relating in pore gas pressure in the compacts to the green density was developed. The expression showed that in order to reduce the negative influence of gases trapped in the pores it is necessary to ensure effective air drainage from the compaction zone. In order to ensure sufficient air evacuation during cold compaction, a new design of porous die was developed. The behaviour of powder mixes with different lubricants during cold compaction in porous die was investigated. All the test conditions were evaluated in terms of green and sintered properties, including the ejection force, green and sintered densities, tensile strength and surface hardness. In the context of the experimental work, compaction in porous die promoted the improved combination of green and sintered properties compared with compaction in conventional dies.     

Synthesis and characterisation of Al2O3/Ni-type composites obtained by spark plasma sintering

This paper presents the influence of sintering on the structure, morphology and compressing strength of alumina/nickel composite compacts obtained by spark plasma sintering (SPS). Al₂O₃/Ni composites were prepared by SPS in argon atmosphere at temperatures in the range of 1000–1200 –C with a holding time of 2, 5 and 10?minutes. The heating rate was 200 C?min^?1. These composites have been characterised by X-ray diffraction, SEM and EDX. The relative density and compressive strength of the as-obtained compacts were determined. The results showed that the alumina particles are uniformly dispersed in a quasi-continuous Ni network, and there was no sign of phase changes during sintering. The maximum strength of the alumina/nickel composite with a content of 75 vol. ? Al₂O₃ and 25 vol. ? Ni was about 240?MPa for the samples sintered at 1200?C for 10?minutes.

Special block from the conference RoPM2017 guest edited by Ionel Chicinas, Technical University, Cluj-Napoca.     

THE PROPERTIES OF POROUS NICKEL PRODUCED BY PRESSING AND SINTERING

Abstract

The effects of compacting pressure and of sintering temperature and time on the properties of porous sintered nickel compacts have been studied, using three carbonyl and two reduced nickel powders. For all five powders, the density of the green compacts and the porosity of the sintered compacts were linearly related to the log compacting pressure. Similar relationships with pressure were observed for strength and electrical conductivity.

Photomicrographs of sections through the sintered compacts made from the reduced nickel powders show that there are pores in two different size ranges, originating from the porosity between the original powder particles and the pores within the particles. It is concluded that sintered compacts from all five powders containing 40–50% porosity have adequate strength and conductivity for use in fuel-cell electrodes.     

EQUATIONS DESCRIBING DIMENSIONAL AND DENSITY VARIATIONS IN SINTERED BODIES: APPLICATION FOR PREDICTING OPTIMUM PRODUCTION PRACTICE

Abstract

A system of equations is established describing how variations in powder characteristics and process parameters are related to the quality of the sintered product.

The basic assumption is that a cylindrical body is to be fabricated by cold pressing and sintering. It is also assumed that the allowable variations in the diameter, the bulk density, and/or the linear density of this sintered body are specified.

The powder material is characterized by the slope, K, of the curve of green density vs. sintered dem,ity. Values near unity give least variation in sintered diameter. An important parameter of the process is the variation, B_g, of the green density.

Variation of the parameters, B of bulk density, L of linear density, and D of sintered diameter are dependent on two groups of variables. The total variation may be composed of variations in the powder quality and the sintering conditions (group 1) or of variations in the green density (group 2).

Taking a practical example, equations are derived for the variables controlling the production of ground and unground sintered ceramic nuclear fuel pellets.     

Effect of copper infiltration on fracture mode in sintered steels

Abstract

The fracture mode of PM steels depends on features, such as pores, densification, diffusion of any added alloying elements, contact area between particles, microstructural homogeneity, and applied load conditions. Consequently, when a sintered steel is infiltrated, several factors that determine the fracture behaviour are affected. The density is raised (in absolute terms, because the infiltrant is usually of higher density, and in relative terms, because activated sintering is promoted by permanent liquid phase sintering). The liquid phase promotes a rounding of the pores which enhances stress transmission from the necks to the particles. Sintered steel with 0˙6%C was infiltrated with three amounts of copper to study the influences of the amount of infiltration and the resultant final density on the fracture mode. Specimens were first uniaxially pressed to 7˙0 g cm^–3 green density, then sintered and infiltrated simultaneously at 1120°C in a 90N₂–10H₂ atmosphere. The mechanical results and microstructures were analysed to evaluate the fracture behaviour and fracture surfaces. The mechanical behaviour was characterised by hardness, tensile and three point bending tests.     

THE PREPARATION AND SOME PROPERTIES OF CHROMIC OXIDE-CHROMIUM CERMETS MADE BY PARTIAL REDUCTION OF THE OXIDE

Abstract

Compacts of chromic oxide/carbon mixtures have been sintered in vacuum to produce oxide-metal cermets. The effect of carbon addition, type of carbon, purity of oxide, compacting pressure, and sintering temperature on the green and sintered density has been studied, and this has been supplemented by tests of hardness and compressive strength.

Considerable densification can be attained by a small addition of carbon to the powder mixture, and this is accompanied by an increase in compressive strength to 20 tons/in², compared with 3 tons/in² for the pure oxide sintered to the same temperature.     

HIGH-STRENGTH SINTERED IRON-BASE ALLOYS BY USING TRANSITION METAL CARBIDES

Abstract

A simple method of producing alloy steels by mixing, pressing, and sintering iron powder with carbides of transition metals is described. The carbides must have a high carbon content and be soluble in iron. These characteristics are found in the carbides of chromium, tungsten, molybdenum, and vanadium. Tensile strengths of ～800 N/mm² have been achieved in annealed specimens having carbide additions of 1–12 wt.-%, depending on the carbide. The additions produce steels with partly air-hardening properties.

The effects of concentration and particle size of the carbides, sintered density, sintering conditions, and cooling rate on mechanical properties have been determined. The alloys are not very sensitive to the sintering atmosphere. The effect of heat-treatment on the mechanical properties of Fe-Cr₃C₂ alloys is reported. A tensile strength >1300 N/mm² was observed with 4 wt.-% Cr₃C₂. Dilatometric measurements were conducted with different carbide concentrations and heating conditions to study the sintering process. The important process of homogenization was investigated by electron microprobe analysis.     

The properties of tungsten processed by chemically activated sintering

Two tungsten powders have been treated with small concentrations of sintering activators to provide for enhanced low temperature sintering. The experimental study focused on the determination of the processing effects on properties such as sintered density, grain size, hardness, and strength. Variables in the plan included tungsten particle size, type of activator, amount of activator, compaction pressure, and sintering temperature. The sintered density is found to have a dominant effect on strength and hardness. The various processing variables are analyzed in terms of their effects on density. At high sintered densities, grain growth acts to degrade the strength. Additionally, the nature of the sintering activator influences the fracture strength. In this study optimal strength occurred with a 0.7 μm tungsten powder treated with 0.29 wt pct Ni, sintered at 1200 °C for one hour. The resulting density was 18.21 g/cm³, with aR _A hardness of 69 and a transverse rupture strength of 460 MPa.     

Microstructure characteristics in Al-C system after mechanical alloying and high temperature treatment

Abstract

In this work elemental powders of Al and 2 wt-% graphite were mechanically alloyed in a high energy horizontal attritor under purified argon atmosphere for 0·5-2 h. Powder mixes were then cold pressed at 1200 MPa and sintered at 550°C for between 2-32 h under the same protective atmosphere. Structural evolution was characterised by X-ray diffraction, scanning electron microscopy and transmission electron microscopy techniques. Results revealed that mechanical alloying was very effective in pulverising the powder mix, where after 2 h, the mix was fine enough to oxidise rigorously when exposed to open air. In general however, mechanical alloying was found to be inefficient to synthesise Al with C. But after sintering, Al₄C₃ phase nanosized particles were formed in the microstructure. When the duration of sintering was prolonged, the particle population multiplied in number. Hence because of improvement in dispersion strengthening, the room temperature hardness of the material increased gradually.     

Microstructure and mechanical properties of PM Ni56Fe19Al25 alloy

Abstract

Scanning electron microscopy and X-ray diffraction analysis were used to study microstructure and mechanical properties of PM Ni₅₆Fe₁₉Al₂₅ alloy. The results indicate that as sintered specimen is (β+γ) dual phase structure, and its density is 6·54 g cm^?3 (the relative density is 94·0%), tensile strength is 771 MPa and the total strain is 4·3%. As quenched specimen presents a large superelasticity with the maximum recovery strain of 4·5%, and its tensile strength is 850 MPa and the total strain is 9·2%. The fracture modes of Ni₅₆Fe₁₉Al₂₅ alloy is transgranular, intergranular and tough mixed type.     

Processing and characterisation of nano crystalline AlCoCrCuFeTix high-entropy alloy

In this work multi-component equiatomic and non-equiatomic AlCoCrCuFeTi_x hexanary high-entropy alloys (HEA) was synthesised through mechanical alloying. The prepared powder was sintered via spark plasma sintering. Influence of alloying element variation in the multi-component system was studied in terms of phase formation and crystal structure by using Thermo-Calc and X-ray diffraction characterization technique (XRD). Particle morphology and chemical analysis studies were carried out through scanning electron microscopy along with Electron Dispersive X-ray Spectroscopy. The crystal structure and nano crystallinity of the hexanary system were recognised using transmission electron microscope (TEM and Selected Area Electron Diffraction [SAED]) while the formation of a solid solution was also studied and discussed. From the XRD and TEM characterisation of 20?h in, milled powders and sintered samples, it was confirmed that the developed HEA system forms a single solid solution BCC phase. The sintered alloy exhibits 97% relative density and an average hardness of 590?VHN.

Special theme block on high entropy alloys, guest edited by Paula Alvaredo Olmos, Universidad Carlos III de Madrid, Spain, and Sheng Guo, Chalmers University, Gothenburg, Sweden.     

FACTORS AFFECTING THE RADIAL AND AXIAL SHRINKAGE IN SOFT-METAL POWDER COMPACTS

Abstract

The variables affecting the radial: axial (R/A) shrinkage ratio in copper-powder compacts have been investigated. The value of R/A is linearly dependent on compacting pressure, green density, and sintering temperature, and also increases with decrease in the particle size of the powder. The observed variation of R/A is attributed to the differences in density in the green compacts, which result in anisotropic stresses in sintering. Surface-tension forces or residual stresses introduced during compaction cannot alone be regarded as the main driving forces responsible for shrinkage; anisotropic stresses also play an important role in the densification of metal-powder compacts. By proper control of these variables, parts can be produced from the compacts to close dimensional tolerances.     

Compaction and sintering behaviour of A356–fly ash composites: a preliminary investigation

Abstract

In the present study, A356–fly ash metal matrix composites were developed through powder metallurgy route. The composites were mixed by using the ball milling technique, shaped through uniaxial and cold isostatic compaction, and then sintered at 520°C. Scanning electron microscopy and X-ray diffraction were used for microstructure and phase characterisation. The density and microhardness of the composites were evaluated as a function of fly ash content, compaction pressure, sintering time and age hardening time. Uniaxial cold compaction of the composites increased their green density and cold isostatic compaction of the compacts led to a further increase in the density. At a constant compaction pressure, the density decreased with increasing fly ash content, resulting in light weight composites. The microhardness of the composites increased with the addition of 10 wt-% fly ash while it decreased with the addition of 20 and 30 wt-% fly ash. Sintering at 520°C increased the density of the composites and the grain size of the α-Al phase of the matrix. The matrix alloy and the composite containing 10 wt-% fly ash showed some response to age hardening at 160°C. However, no response to age hardening was observed at 200°C.     

Effect of compacting pressure on microstructure and mechanical properties of carbide cutting tools

Abstract

The effects of compaction pressure on properties of carbide cutting tools containing 80·5 wt-%WC, 5 wt-%TiC, 5 wt-%TaC–NbC and 9·5 wt-%Co were studied. These tools were formed by powder metallurgy with different compacting pressures ranging from 77 to 231 MPa (5–15 tons in^?2) and sintered in a vacuum furnace at a constant sintering temperature (1450°C) and at a constant heating and cooling rate of 5°C min^?1. Green and bulk densities, shrinkage and hardness of the produced compacts were measured. Tool cutting performance has been assessed based on machining a medium alloyed steel workpiece under different cutting conditions and measuring the tool flank wear and the workpiece surface roughness. The microstructure of the compacts was metallographically examined using scanning electron microscopy. The results have revealed that both densities and hardness figures increase with increasing compaction pressures, while shrinkage decreases. Cutting performance has not demonstrated a substantial improvement of the tool's performance and life due to the increasing compacting pressure of these tools.     

Effect of distribution of B4C on the mechanical behaviour of Al-6061/B4C composite

In this work, the effect of mixing parameters on the distribution of B₄C in 6061-Al alloy and its correlation with mechanical behaviour was studied. 6061-Al alloy powder was mixed with 10 mass-% B₄C powder in a ball mill and powder rotator mixer by varying mixing time from 1 to 5?h. Mixing was performed in both wet and dry conditions in a ball mill while only dry condition was used in the powder rotator mixer. The green compacts were sintered at 630°C. The quadrat method was used to quantify the distribution of B₄C particles in the microstructures of sintered Al/B₄C composite. The results showed that the distribution was improved with mixing time but the density, hardness and compression strength of Al/B₄C composites were reduced with time during ball milling. On the other hand, the distribution of reinforcement, density, hardness and compressive strength of Al/B₄C composites was improved with mixing time in the powder rotator mixer.     

Swelling during sintering of titanium alloys based on titanium hydride powder

Abstract

Compacts were prepared by pressing titanium and titanium hydride powders mixed with nickel powder and sintering under vacuum. Severe swelling was observed only for compacts based on TiH₂ powder. Pressure changes in the vacuum furnace, dilatometry results and mass loss data all indicate that dehydrogenation of TiH₂ powder compacts occurs at lower temperature than any significant sintering. Swelling appears to have been caused by a contaminant in the TiH₂ powder rather than hydrogen. The onset of severe swelling during heating was associated with the formation of liquid phase as the solidus was crossed. However, some swelling appears to take place under solid state sintering conditions. Various results indicate that the mechanism of swelling is high gas pressure within closed pores. Large pores appear to form by breakage of ligaments between small pores followed by opening of the pore. It appears that the use of (uncontaminated) TiH₂ powder in place of Ti powder would allow the benefit of lower green porosity to be retained during sintering to achieve low sintered porosity.