Characteristic of interconnected porosity in ferrous PM compacts

Abstract

The purpose of this work was to quantitatively describe the interconnected porosity in iron compacts, both in macro- and microscale. Size and volume fraction of micro-, meso- and macropores were examined in the compacts with density within 5˙6–6˙4 g cm^?3, made in laboratory conditions of two iron powders: NC100˙24 and ASC100˙29 manufactured by Höganäs Company. The interconnected porosity was determined using the method based on measuring the sorption isotherms of CO₂ and benzene at T=25°C in static conditions in a high vacuum gravimetric appliance equipped with McBain–Bakr weighers.

Volume distributions of individual size classes of micro- and mesopores in the compacts made of both iron powders with fixed density were compared.

Relationships between density and the interconnected micro- and macroporosity of the examined compacts were determined.     

FRICTION COEFFICIENTS BETWEEN IRON POWDER COMPACTS AND DIE WALL DURING EJECTION USING VARIOUS ADMIXED ZINC STEARATE LUBRICANTS

Abstract

Laboratory compaction and ejection studies have been made using a reduced iron powder mixed with a number of zinc stearates having median particle sizes between 4 and 22μm. Comparable experiments were carried out on a fully instrumented production press, which was operated at compacting pressures between 300 and 500 MN/m² to produce compacts with true densities ranging from 5·90 to 6·70 g/cm³. Determination of ejection forces by the two methods enabled calculations of the coefficients of friction between compact and die wall to be made for mixtures containing 0·5–2·0 wt.% zinc stearate. These showed that the behaviour during compaction and ejection was comparable on both laboratory and production scales and gave very similar results. An interpretation of the results is given and values of coefficients of friction are presented which show that these are dependent on the type of zinc stearate used.     

Lean Cr iron powders for obtaining high performance PM steel grades

Abstract

Ecological and economic demands are driving PM markets to incorporate less expensive, yet effective, alloying elements in iron based powders. To investigate their potential for this purpose recently developed sinter-hardening iron powders containing Cr and smaller amounts of Mo and Ni were industrially sintered at 1120 and at 1240°C under laboratory conditions. One set of samples, containing 0·8% graphite additions, was cooled so to obtain sinter-hardened steels. A second set of samples, containing 0·3% graphite, was cooled under normal conditions and subjected to a secondary carburising treatment. The microstructures and mechanical properties developed were compared.     

SINTERING OF ZIRCONIUM BORIDE WITH ACTIVATING ADDITIONS

Abstract

Since the hot pressing of ZrB₂ compacts has a number of limitations, the possibility of pressureless sintering by the addition of small amounts of various metals to provide a liquid phase has been investigated. Changes in microstructure and porosity of the compacts have been studied. Additions of up t0 3% of iron, nickel, cobalt, or high-melting-point metals enable satisfactory sintering at 2000°C in argon or in vacuum to be achieved in < 60 min. The effect is associated with an appreciable contraction of the ZrB₂ lattice.     

Effect of plasma nitrocarburising on fatigue resistance of low alloy Cr–Mo sintered steel

Abstract

A nitrocarburising treatment was carried out on a low alloyed Cr–Mo sintered steel (1·5%Cr, 0·2%Mo) to evaluate its influence on the bending fatigue resistance of the material. Fatigue performance was compared with that obtained by a conventional through hardening and a plasma carburising. Two different green densitise (7·1 and 7·4 g cm^?3) and two different sintering temperatures (1120 and 1250°C) were adopted during preparing the as sintered steels. Fatigue strength after nitrocarburising on 1120°C sintered steels considerably increases. It is comparable with that obtained by through hardening and slightly better than that obtained by plasma carburising. On samples sintered at 1250°C the fatigue resistance of the nitrocarburissed is worse than expected, because the microstructure is softer and less homogeneous.     

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.     

STUDIES ON THE ACTIVATION-SINTERING OF IRON POWDER

Abstract

A study of the sintering behaviour of iron compacts containing additions of tin up to 1 wt.-% has been made. A tensile strength of 234 MN/m² (34 x 10³ lbf/in²) has been achieved with an optimum tin addition of 0·5 wt.-%, sintering being carried out for 10 min at 1100°C (1373 K) in a reactive halide atmosphere. Combination of the two ‘activating’ techniques (addition of tin and sintering in a reactive atmosphere) permits current properties to be attained at considerably lower sintering temperatures or sintered densities, and is much more effective than when they are applied individually. A tensile strength of 165·3 MN/m² (24 x 10³lbf/in²), achieved by sintering at 1200°C (1473 K) for 10 min with an addition of 0·5 wt.-% tin can be obtained by reactive-sintering the same composition at 900°C (1173 K) for 10 min. Alternatively, the density of the part can be reduced from 6·7 to 6·2 g/cm³ with no loss of strength or elongation. Tin in excess of 0·5 wt.-% causes deterioration in properties under the sintering conditions studied and a reason for this is cited. The improvements in properties are lost also if admixed lubricant is used in the compactionprocess.     

THE PRODUCTION OF GRAIN-ORIENTED 50 : 50 NICKEL–IRON MAGNETIC STRIP BY COLD ROLLING FROM SINTERED COMPACTS

Abstract

50 : 50 nickel–iron strip was cold rolled from sintered compacts to thicknesses of 0·0015 and 0·004 in., with final reductions of 92–99%. After annealing at 1050°–1200° C., the cube texture developed, thus giving a material with a rectangular hysteresis loop when magnetized in either the rolling or the transverse direction.

The alloys with the best magnetic properties contained 48–50% nickel. In this range of composition the remanence ratio and coercivity varied from 0·91 to 0·94 and 0·11 to 0·19 respectively, depending upon the processing schedule used.

With the recommended processing schedule, values for the remanence ratio and coercivity of 0·92–0·94 and 0·11–0·13 respectively were obtained.

Unlike the texture of strip rolled from a conventionally cast ingot, the development of cube texture in strip rolled from a sintered compact is not critically dependent on the temperature of the final anneal.     

PM processing of elemental and prealloyed 6061 aluminium alloy with and without common lubricants and sintering aids

Abstract

A comparison has been made between compaction, sintering, microstructural and mechanical properties of the 6061 aluminium alloy prepared via premixed elemental (EL) and prealloyed (PA) powders (as received and degassed) with and without additions of sintering aids and various solid and/or liquid lubricants. Both EL and PA powders were cold pressed at different pressures, ranging from 250 to 770 MPa, and sintered under vacuum in the range 580–640^°C for 30–120 min. and then under pure nitrogen atmosphere for comparison. Vacuum degassing of the PA powder provided better compressibility and thus higher green densities than those for the as received PA or the premixed EL powder compacts pressed at compaction pressures ≥340 MPa. Near full sintered densities of , ～98%TD were obtained for both EL and PA 6061 Al alloys. Degassed PA Al with 0·6 wt-% paraffin wax (PW) or with only 0·12 wt-%Pb addition as sintering aid and no lubricant, and premixed EL with only 0·12 wt-%Pb addition and no lubricant gave the best optimum properties. It became apparent that additions of some solid lubricants such as lithium stearate (LS) and acrawax to both the premixed EL and PA powders provided reasonable green densities, but had deleterious effect on sintered densities and microstructures, particularly under vacuum sintering. Heating data curves during the sintering cycle, revealed formation of both transient and persistent liquid phases for the EL and mainly supersolidus liquid phase sintering (SLPS) mechanism for the PA. Tensile properties of the degassed, vacuum or nitrogen sintered PA Al alloy in T6 condition were higher than those of the equivalent alloy prepared by EL mixing with the former giving a tensile strength of 330 MPa and 6–8% elongation to failure, which are similar to those of the commercial (wrought) 6061 Al alloys.     

Some Mechanical Properties of Powder-Forged Iron/Alloy Mixtures

Abstract

An investigation was made of the feasibility of producing alloy forgings (nominal composition Fe–0·5C–0·6% Mn), from a powder prepared by mixing the alloying additions with iron powder. The carbon was added as microcrystalline graphite and the manganese as elemental powder and as ferro-manganese powder. Additions of copper and ammonium chloride powders were also made for the purpose of assisting the manganese to alloy with the iron. The copper addition improved the tensile strength but lowered the ductility. The ammonium chloride had little effect except for an apparent lowering of hardness. It was found that useful mechanical properties could be obtained in forgings made from mixtures of the alloying ingredients.     

Metallic iron whisker formation and growth during iron oxide reduction: basicity effect

Abstract

The effect of basicity on the metallic iron whisker growth during wüstite reduction was studied in the present investigation. Compacts of pure and CaO/SiO₂ doped wüstite were synthesised. The annealed compacts were isothermally reduced in thermogravimetric apparatus with CO gas at 800–1100°C. The course of reduction was followed by measuring the weight loss as a function of time. X-ray diffraction (XRD), scanning electron microscope (SEM), optical microscope and porosity measurements were used to characterise the annealed and reduced samples. The influence of temperature and basicity (CaO/SiO₂) on the reduction behaviour and the morphology of the annealed samples were investigated. The reduction rate increased with temperature but decreased by increasing basicity value. Metallic iron whisker shape structure was detected in the pure wüstite samples after reduction at high temperatures while in basic wüstite samples, whiskers were formed at the surface of the compacts. From the activation energy values, the reduction of pure wüstite is most likely controlled by a combined effect of gaseous diffusion and interfacial chemical reaction mechanisms. The reduction of basic wüstite compacts with 0·2 and 0·5 basicity ratios are most likely controlled by chemical reaction mechanism while for 0·8 basicity ratio, the reduction rate is most likely controlled by solid state reaction mechanism.     

Microstructural development during liquid phase sintering of Fe and Fe–Mo alloys containing elemental boron additions

Abstract

The sintering behaviour of Fe and Fe–Mo prealloyed powder compacts containing from 0·5 to 3·5 wt-%Mo and fixed boron additions has been studied with special emphasis on the microstructural development, the formation of the liquid phase and the liquid phase sintering mechanisms involved during the densification process. The basic phenomena involving the formation of a liquid phase and the temperature at which the liquid is generated is strongly influenced by the Mo/B ratio in the initial powder mixture. The effect produced by Mo and its concentration, both, on the final microstructure and on the behaviour of boron prior to, during and after the formation of the liquid phase, was studied under both the optical and the scanning electron microscope. For this purpose interrupted sintering experiments followed by water quenching from specific temperatures and times within the sintering cycle have been carried out. The study shows that the formation of a liquid phase is preceded by noticeable enhancement of solid state sintering at intermediate temperatures. This is accompanied by boron diffusion into the metallic particles, generating inter- and intragranular precipitates in amounts dependent on the Mo concentration. At a later stage boron is found to be preferentially located at the boundaries as the formation of a continuous Fe/Mo/B liquid phase with excellent wetting characteristics proceeds thus producing densification by pore filling and shape accommodation. Final densities up to 7·82 g cm^?3 were obtained for these alloys.     

On phosphorus as additive in iron based soft PM magnets

Abstract

The effect of a phosphorus addition to iron powder for production of soft magnetic materials is investigated. The phase diagrams calculated by ThermoCalc¹ and experiments show the beneficial effect of the phosphorus addition especially when sintering in a carburising atmosphere. The carbon uptake is greatly reduced and is explained by the presence of ferrite in the material during sintering. The phosphorus addition also reduces the magnetic aging both in samples sintered in a carbon containing atmosphere but also in a hydrogen atmosphere. No magnetic aging from precipitation of iron phosphide is seen.     

The Effect of Cooling Rate on the Strength of Sintered Fe—Cu Compacts

Abstract

The effect of cooling rate from the sintering temperature upon the tensile strength of compacts from a mixture of iron and copper powder was investigated. The compacts were pressed at 450 and 390 MPa and sintered in hydrogen at 1120°C for 40 min. The copper content of the compacts varied from 0 to 12%. For alloys with Cu content >4% the tensile strength was found to be strongly dependent upon the cooling rate in the temperature range between 850 and 600°C, with rapidly cooled specimens being considerably stronger. In specimens with 8%Cu the tensile strength increased from 206 to 343 MPa when the cooling rate was increased from 10 to 200 degC min^?1. In specimens with 2%Cu cooling rates above and below 600 degC min^?1 appear to influence the tensile strength. Possible explanations for the observed effects of cooling rate upon tensile strength in sintered Fe–Cu alloys are discussed.     

Microstructural modelling of electrical conductivity and mechanical properties of sintered ferrous materials

Abstract

The role of microstructure on mechanical properties of sintered ferrous materials was studied using a method based on electrical conductivity measurement. The method was accompanied by quantitative fractography to evaluate the dewaxing and sintering process in iron compacts. The effects of manufacturing parameters, such as compacting pressure in the range of 150–800 MPa, sintering temperature from 400 to 1300°C, sintering time up to 8 h, and lubrication mode were investigated. Several mathematical models were checked to obtain the best one for prediction of electrical conductivity changes as a function of manufacturing parameters. The mechanical properties of the sintered compacts were also evaluated to establish a relationship between conductivity, total porosity, pore morphology, and mechanical behaviour. The results show that the electrical conductivity/resistivity of sintered materials is closely related to its microstructure, so that measuring these properties can replace destructive test methods for prediction of mechanical strength of sintered materials with homogeneous matrix microstructure. The application of the method is shown for sintered Fe, Fe–0·8%C, and Fe–1·5%Mo–0·7%C compacts.     

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.     

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.     

Contributors

Abstract

The chemistry of a high performance cast superalloy, ZhS6–K (Ni–10Cr–5Co–5W–5Al–3·5Mo–3Ti–0·2C–0·02B), was modified by slight reductions in carbon, titanium, and aluminium content and minor additions of niobium and hafnium. Two variants of the modified alloy chemistry with different boron contents (0·02 and 0·08 wt–%) were prepared by vacuum induction melting, argon atomization, and consolidation by hot isostatic pressing at three temperatures. It was observed that, unlike carbon, an increase in boron content did not promote the formation of continuous precipitates at the prior powder particle boundaries. Increased boron content narrowed down the consolidation temperature range and changed the morphology of γ′ particles from cuboidal to dendritic. Precipitation of an eutectic γ + γ′ structure and formation of continuous boride films at the grain boundaries severely degraded the mechanical properties of the high boron PM superalloy that was consolidated at a temperature marginally above the γ′ solvus. An optimum consolidation schedule was determined for the high boron alloy, which after a suitable heat treatment produced significant property improvement in stress rupture and tensile properties. PM/0416     

THE IMPORTANCE OF ATMOSPHERE CONTROL IN HARD-METAL PRODUCTION

Abstract

The furnace atmospheres used in the manufacture of hard-metal from the pressed compact to the sintered component are discussed.

The very fine size (0·5–8·0 μm) of the powder particles makes the compacts particularly prone to react with furnace atmospheres. All these reactions affect the carbon content of the alloys, which must be controlled within extremely close limits to ensure good quality.

The removal of pressing lubricant, presintering, and final sintering all involve heating the components to temperatures at which reactions with the furnace atmosphere can occur. Both hydrogen and vacuum furnaces are used and care is required to maintain a quality of atmosphere that will not lead to a deleterious change in carbon content.     

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.