Effect of boron on vacuum carburising depth of iron powder metallurgy compacts

Abstract

The work was aimed at determining the effect of boron on vacuum carburising of iron compacts with density over 7·2 g cm^–3. An attempt was made to determine the effectiveness of boron on carbon diffusion rate into the material of compacts with no additional effect of interconnected porosity. Vacuum carburising of compacts made of iron powder with an addition of boron was carried out at 1050°C in a laboratory vacuum furnace.

The effect of boron content within 0·005 to 0·02% on the vacuum carburising depth was analysed. It was found that the boron addition up to 0·01% increased the carburising depth by ～0% in comparison with the compacts of pure iron.     

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.     

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.     

Mechanical properties of green compacts. II. Effect of powder relative bulk density on the strength of compacts with different forming temperature conditions

Mechanisms of strength for green compacts made from powders of iron, nickel and its alloys, copper, tin, and zinc are analyzed. The strength of green compacts prepared from metal powders of medium fineness with a relative bulk density (RBD) from 0.119 to 0.568 by two-way compaction in rigid dies with homologous temperatures from 0.15 to 0.59 (pressure from 200 to 800 MPa, powder deformation rate 10^?2–10^?3 m/sec) is studied. Compact strength is determined by diametric compression of cylindrical compacts. The dependence of strength on compact porosity is studied by the Bal’shin equation. The possibility is demonstrated of using this relationship in order to describe hot compaction and formally describe cold compaction of powders with RBD up to 0.40. The effect of homologous temperature and powder RBD on compact strength is determined. The homologous temperature for transition from warm to hot compaction and the effect of compact density (degree of deformation) on this temperature is studied. It is shown that linear approximation is possible for the dependence of compact strength on powder RBD according to the equation σ _f.c = 87–217?RBD.     

INFLUENCE OF TIN POWDER CHARACTERISTICS ON THE SINTERING OF IRON-TIN-COPPER POWDER COMPACTS

Abstract

In view of increasing industrial interest in the use of tin additions as an aid to the sintering of iron-based powder compacts, an examination has been made of the influence of the characteristics of the tin powder on sintering performance.

The effect of additions of narrow size-range fractions of atomized tin powder on the dimensional changes and tensile properties obtained on sintering Fe-Sn-Cu compacts made with –100 mesh (–152 μm) or – 300 mesh (– 53 μm) sponge iron and – 300 mesh (– 53 μm) atomized copper powders has been determined. The compacts contained tin and copper in the ratio 2:3. The narrow size fractions were separated from – 300 mesh tin powder by air elutriation. It was found that the use of coarse tin powder reduced the tensile strength of – 300 mesh iron-based Fe–1% Sn–1 ½% Cu compacts, but had no influence when this mixture was based on –100 mesh iron powder, or when the mixture composition was Fe–2% Sn–3% Cu. The effects have been examined in relation to the sintering mechanism by scanning electron microscopy and by X-ray microanalysis.     

INFLUENCE OF IRON POWDER TYPE ON THE PROPERTIES OF SINTERED IRON AT VARIOUS DENSITY LEVELS

Abstract

The properties of various commercial and experimental iron powder types and of compacts made from them in the density range 6·8–7·87 kg/dm³ by single-pressing, double-pressing, and hot-forging techniques have been determined. It was shown that the ductility in all cases was more adversely affected than the tensile strength by the presence of porosity. However, it was also shown that at any particular density level or with a given processing schedule the mechanical properties varied widely, depending on the iron powder used. On the basis of the mechanical-property results, the powder types to be preferred at different density levels are indicated.     

Reactive sintering in Fe-Co system

Abstract

Low porosity powder metallurgy compacts have been manufactured from treated elemental iron and cobalt powders sintered at 1150°C under an H_2(g) atmosphere. Their microstructures consist of an interconnected mixed oxide network which encapsulates both the iron and cobalt phases. The production technique employed is an innovative process termed reacto-thermitic sintering (RTS), which leads to near full density and near net shape parts utilising conventional uniaxial compaction and mesh belt furnace practices. The RTS technique relies on microscale exothermic reaction between small quantities of added elemental Al and oxides present on the surface of the bulk powder, together with the bulk powder itself. This results in the production of a transient liquid phase which freezes rapidly and consolidates the compact without slumping. In order to generate an interconnected mixed oxide network, experiments were designed such that the Al powder reacts with the cobalt and the surface of the iron powder which is artificially doped with Fe and Cr oxides.

Differential thermal analysis (DTA) and energy balance calculations revealed that the Al and the oxide coating reaction does not proceed directly. Instead the main contribution to the exothermic process is the reaction between Al and Co/Fe. The system does not exhibit true RTS behaviour and the interconnected network of mixed Al, Cr, and Fe oxides is created by subsequent reaction of Co-Al and Fe-Al intermetallics with the artificial Fe-Cr oxide coating on the Fe. The microstructure obtained exhibits negligible porosity with the metallic particles on the whole fully encapsulated by the oxide.     

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.     

OBSERVATIONS ON THE SINTERING OF COMPACTSFROM A MIXTURE OF IRON AND COPPER POWDERS

Abstract

Three grades of iron powder-an atomized steel powder, a sponge iron powder reduced from magnetite with carbon, and a powder reduced from mill scale with hydrogen were mixed with 3% of copper powder and pressed into compacts. The diametral dimensional changes of the compacts during sintering below and above the melting point of copper were measured, their microstructures examined, and both related to the characteristics of the powders, particularly their specific surface. During sintering below the melting point of copper, compacts of all three powders shrank. Micrographic examination showed that the copper is transported by solid-state diffusion along the surfacesand grain boundaries of the iron powder particles. During sintering above the melting point of copper, compacts of the atomized and the MH-100 sponge iron powders grew while those of the hydrogen reduced mill-scale powder shrank. This phenomenon is related to the different mode of penetration of liquid copper in the compacts from the three powders, observed in the microstructures of the compacts.     

THE COMPACTING OF GRAPHITE AND GRAPHITE/URANIUM/THORIUM MIXTURES

Abstract

Fine artificial graphite powders can be cold compacted to give bodies of high density (～ 88% of theoretical), low permeability (B₀ ～10^–14 cm²), and reasonable strength. Such powders, after vacuum annealing, will not compact.

Die-compacted powder has strongly anisotropic properties owing to a high degree of preferred orientation within the compact; this effect is less marked in hydrostatically compacted powder. Minor dimensional changes occur when compacts are annealed in the range 600-1000°C.

The preparation of fuels by incorporation of fissile and fertile materials into graphite powder and cold compacting is described.     

Transient liquid phase sintering of high density Fe3Al using Fe and Fe2Al5–FeAl2 powders Part 2 – Densification mechanism analysis

Abstract

The use of Fe₂Al₅–FeAl₂ prealloyed powders and heating rates >150 K min^?1 overcomes the formation of density restricting Kirkendall porosity in the Fe–Al system. X-ray diffraction, electron probe micro analysis and differential thermal analysis suggest that the absence of a persistent liquid, experienced when liquid phase sintering with elemental powders, is overcome. Homogenisation is greater during heating at a rate of 20 K min^?1 than for 150, 250 or 400 K min^?1 and homogenous Fe₃Al forms across the compact at temperatures below the melting point of the liquid forming constituent, indicating that a liquid will not form under such processing conditions. The maximum density achieved under the processing conditions in the present study is 92% of theoretical density. The presence of large pores shortly after liquid formation suggests that the remaining porosity is largely due to powder agglomeration during mixing.     

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.     

Effect of atomisation medium on sintering properties of austenitic stainless steel by eliminating influence of particle shape and particle size

Abstract

Gas and water atomised 316L stainless steel powders with similar powder morphology and particle size were injection moulded and sintered. The results show that compacts prepared from the gas atomised powder exhibit higher density and tensile strength, whereas those prepared from the water atomised powder exhibit higher elongation, finer grain size and superior corrosion resistance. Chemical analysis shows that the water atomised powder has a higher Si and O content, and microstructural analysis of the sintered compacts reveals that SiO₂ particles disperse as a second phase in the compacts prepared from the atomised powder, which accounts for the property behaviour. Due to the presence of SiO₂, the porosity increases, whereas the pore coarsening and grain growth are inhibited. Besides, SiO₂ particles can also improve the passivation effect of stainless steel, and hence increase the corrosion resistance.     

Effect of residual pressure on vacuum sintering of Ti–Ni alloys

Abstract

In earlier work the authors examined the sintering of Ti–Ni alloys by means of dilatometry of mixed elemental powders. Some notable differences were observed when heat treatments were carried out using a vacuum tube furnace rather than the dilatometer: higher sintered density was achieved due to a combination of lower heating rate and lower residual pressure, and swelling during liquid phase sintering was greatly reduced. This observation is consistent with the idea that gas pressure within closed pores causes swelling during liquid phase sintering and retardation of shrinkage in solid state sintering. In addition to the results of measurements of density and open and closed porosity as a function of Ni content and sintering temperature, macrographs and optical micrographs of the sintered compacts are presented, and the effects of heating rate and compaction pressure are described.     

Effect of particle composition on consolidation of hot briquetted iron

Abstract

The influence of the carbon concentration of directly reduced iron (DRI) powders on the compressibility and fracture strength of hot briquetted iron (HBI) has been studied. Industrially produced DRI, pure iron powder and Fe–C alloy powders (synthetic DRI) were used in the study. It was found that the mechanism of compaction could be attributed to pure yielding. The pressure required to attain a given density increased proportionally with the carbon content. The morphology and phases present in DRI powder had a significant influence on the compressibility. The fracture strength of the compacts increased with increasing carbon content of the DRI powder. These observations are discussed with reference to the current understanding of the mechanisms of compaction and fracture of compacted particulate materials.     

EVALUATION OF IRON POWDERS FOR SINTERED STRUCTURAL COMPONENTS

Abstract

A new method for evaluation of iron powders is suggested. Ultimate tensile strength is chosen as a base parameter, and the relations between this property and compacting pressure and raw material cost, respectively, are shown. For this purpose it has been necessary to deduce two supplementary parameters, Relative Pressure Response (P_r) and Relative Raw Material Requirement (M_r), which are functions of compacting pressure and ultimate tensile strength, and of compacting pressure and density, respectively.

It is shown that the importance of compressibility of iron powders is overrated in current opinion and, consequently, that it is misleading to judge the overall merits of an iron powder according to its compressibility.

Raw material costs of sintered steels are lower, if sponge-iron powders are used instead of atomized powders, even if the price of all iron powders were equal. This tendency is more strongly emphasized at low densities, where the sponge-iron powder with the lowest apparent density value is preferable. The differences are beginning to lessen and disappear gradually at densities approaching or exceeding 7·0–7·2 g/cm³ (for single-pressed and single-sintered materials).

Alloy composition has a stronger influence on raw-material costs than the choice of iron-powder grades. Close and reliable control of carbon contents and avoidance of oxidation of manganese is essential for lowering of costs in the PM structural-component manufacturing industry.     

Characterisation and sintering studies of mechanically milled nano tungsten powder

Abstract

Elemental tungsten powder was mechanically milled by planetary mill for 100 h. Particles were thinned down to nanometre scale. The shape of the milled powders was flat cylindrical with average diameter and length 12˙5 and 46˙5 nm respectively. The corresponding crystallite size obtained by X-ray diffraction (XRD) was 26˙96 nm. The results obtained by XRD and small angle X-ray scattering were well supported by transmission electron microscopy and high resolution transmission electron microscopy results. The maximum shrinkage of the compact has been observed at ～1500 K, which has been used as a guideline for sintering experiments. The powders sintered at 1773 K have resulted in 96% relative density.     

On suitability of novel fluidised bed technique for separation of metallic powders during commercial powder metallurgical processing

Abstract

Experiments have been performed to test the efficiency with which a novel fluidised bed technique could separate different metallic powders in terms of size and density. The overall aim was to assess the potential of this technique for the commercial separation of defective powder fractions from mechanically alloyed (MA), iron based powders. Separation in terms of size was readily achieved, with the largest powder particles sinking to the bottom of the fluidised bed. In a simulated commercial process, density separation of defective Fe₃Al powder could not be demonstrated as any differences in density were overshadowed by size and morphology differences. However, from a batch of iron based powder (ρ=8·02 g cm^?3), seeded with six other metallic powders, aluminium powder (ρ=2·70 g cm^?3) segregated strongly to the top of the bed from where samples containing 93 vol.-%Al were taken. The process is thought to be sensitive to differences in density of a factor of 1.1–3.     

Effect of compaction density on foamability of Al–TiH2 powder compacts

Abstract

Al-TiH₂ powder mixtures have been cold compacted into precursors for foaming using single action, uniaxial pressing. After heat treatment, at 800°C for 5 min, foaming was only observed for precursors with a theoretical density above 94%. This density limit corresponds to the transition from interconnected to closed porosity, confirming that isolating porosity and enveloping the foaming agent in the matrix are vital to successful foaming. Although the variation in foam density for similar samples was small, the cell structures were different indicating that a low variation in foam density is not necessarily a good indication of achieving reproducible foam structures. The orientation of the sample had little effect on the foaming response for compacts with a length to diameter ratio below 1:2. For longer samples the foaming response was not uniform along the length of the sample indicating that in complex pressings the variation in local pressure must be understood in order to avoid regions being compacted below the critical density for foaming.     

Sintered copper–graphite powder compacts forindustrial applications

Abstract

Studies were made on copper/graphite based powders and sintered compacts for industrial applications. The dependence of particle shape on friction in the powder mass, compression ratio, and electrical receptivity of powder metallurgy components was studied using near spherical precipitated copper powders and angular or flakelike powders generated by mechanical comminution. Results reveal that powders with particles that are nearly spherical in shape have lower friction, lower compression ratios, and higher electrical resistivities in sintered compacts than powders with acicular or flakelike particles. Also, the effects produced by the small additions of lead and zinc (up to 2·5 wt-%) on the electrical resistivity and hardness of sintered copper–graphite compacts are also presented, and the influence of variation of briguetting pressure is discussed.