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PRODUCTION OF IRON AND STEEL POWDERS

At present there are two basically different production methods which together account for
more than 90% of the world production of iron and steel powders, viz. The Höganäs spongeiron process and the water-atomizing process. The former process is based on reduction of
iron ore, yielding a highly porous sponge-iron which subsequently is comminuted to powder.
The latter process is based on atomization of a stream of liquid iron (or steel) by means of a
jet of pressurized water.
In the manufacturing of sintered parts, iron powders are always used admixed with a small
amount of lubricant in powder form in order to minimize the friction in the compacting tool. In
many cases, they are also blended with alloying elements in powder form, like graphite,
copper, nickel, molybdenum and others (in order to achieve increased strength properties).
The Höganäs Sponge Iron Process
The Höganäs sponge iron process, is essentially a chemical process in which finely divided
iron ore is being reduced with coke breeze yielding a spongy mass of solid metallic iron,
which can readily be comminuted to iron powder. The iron ore used at Höganäs is a
magnetite (powder Fe3O4) obtained from selected sources. This magnetite, which by nature
contains only very small amounts of gang and has extremely low contents of sulfur and
phosphorus, is being dressed and concentrated while still at the mining location and then
delivered to Höganäs in a highly pure state.
The Höganäs Water-Atomizing Process

This raw material (1) is melted down in an electric arc furnace of 50 tons capacity (2) where.The raw material for this process is a carefully selected iron scrap and sponge iron from the process described in the preceding paragraph. if desired. The melt is teemed slag-free through a bottom hole into a ladle (3) where it is refined with an oxygen lance (4). alloying elements can be added. The ladle is then transferred to the atomizing station (5). and the liquid iron (or steel) is teemed slag-free through a bottom hole in the ladle into a specially designed .

others unite in small irregularly shaped agglomerates while freezing. the atomized powder particles are not only superficially oxidized but also very hard because. . swept along by the water jet. • Yield fully homogeneously alloyed sintered parts. Routines for homogenizing. like e.g. due to the extremely high cooling rates residing in the atomizing process. and eventually transported in special containers (11) to the works at Höganäs for further processing. The dry powder is magnetically separated from slag particles (8). Air. the liquid iron (or steel) flows in a well controlled stream (B) through the center of a ring-shaped nozzle (D) where it is hit by jets of highly pressurized water (C). metallic alloying elements are commonly introduced by either of the following two methods: Method 1: Water atomization of the liquid iron alloy. and letting the actual alloying process take place during sintering of the parts compacted from the powder mix. The powder is. copper. Both methods have their advantages and disadvantages: Homogeneously alloyed powders: Advantages: • Alloying elements do not segregate when the powder is handled . Some of these droplets freeze immediately to small spheres. quality checking. where they are settling as a mud. carbon and other suitable alloying elements. soft-annealed.tundish (A). From there. they have solidified in the martensitic state – despite their low carbon content. While carbon is normally admixed to the iron powder in the form of graphite. screened (9) and homogenized (10). have to be introduced. This powder mud is dewatered (6) and dried (7). The solidified droplets and the atomizing water are collected in a huge container. nickel. The stream of liquid iron (or steel) explodes into fine droplets (E). packaging and storing are the same as for sponge iron powders. cause superficial oxidation of the small droplets. resulting in a homogeneously alloyed powder. In the state as leaving the atomizing plant. therefore. Alloying Methods In order to achieve hardenable sintered ferrous materials. and water vapor arising in the atomizing process. and its surface oxides and residual carbon are reduced in belt furnaces. Method 2: Mechanically blending plain iron powder with the respective alloying elements in powder form. and molybdenum.

• In order to change or correct the composition of a fully alloyed powder. Due to inter-diffusion between the diffusion bonded alloying particles and the iron particles. Disadvantages: • Yield less homogeneously alloyed sintered parts. the fine particles of the added alloying elements are safely bonded to the surfaces of the coarser iron powder particles. The Distaloy™ process can be described as follows: Alloying elements used in the Distaloy™ process are mainly copper. .Disadvantages: • Have low compressibility. A large variety of standard and tailor-made powder mixes produced according to these processes are offered under the trade-names Distaloy™ and Starmix. because their particles are solution-hardened. • No additional mixing operation is required as the powder has to be admixed with a lubricant anyway. • The composition of a powder mix can very easily be changed or corrected by re-mixing it with additional amounts of either iron powder or alloying elements. The process starts with weighing-in a production lot of 30 tons of iron powder and alloying powders in exactly controlled proportions. a new melt (usually 50 tons at time) will have to be atomized. During this heat-treatment. Distaloy and Starmix In order to eliminate the segregation problem with powder mixes. Special precautions are taken to prevent segregation of the mix when discharged from the mixer. Powder mixes. Höganäs AB has developed two special processes for the production of segregation-proof iron powder mixes. • Alloying elements tend to segregate when the powder mix is transported and handled. The so produced powder mix is heat-treated in a continuous furnace under a reducing atmosphere at a temperature somewhat below the melting point of the lowest melting alloying element. nickel and molybdenum (but not graphite!) in the form of very finely grained powders. because the admixed alloying elements (except carbon) diffuse very slowly in solid iron. if ever so little. Advantages: • Have higher compressibility. This lot is mixed in a double-cone mixer.

Geometrical properties ⇒ particle size distribution ⇒ external particle shape ⇒ internal particle structure (particle porosity) 3. • powders of irregular particle shape have better green strength after compacting than . and lubricants would burn-off. Graphite and lubricants have to be excluded from the Distaloy™ process because. • coarser powders and powders of regular particle shape flow better than fine powders and powders of irregular particle shape.used in the production of sintered parts can be characterized by three categories of properties: 1. The fact that the iron powder particles are locally pre-alloyed has practically no negative effect on the compressibility of the mix. General aspects Iron and steel powders . For instance: microstructure and microhardness are depending on chemical composition. to a certain extend. The so treated powder mix contains the alloying additives as finely and evenly dispersed as possible . graphite would carbonize the iron particles and spoil the compressibility of the powder mix. Metallurgical properties ⇒ chemical composition and impurities ⇒ microstructure ⇒ microhardness 2. Some of them are interrelated with each other. during heat-treatment of the powder mix. green strength and spring-back All these powder properties are inherited from and specific to the process by which the powder was produced. increasing particle porosity and decreasing particle size. The Starmix process uses special types of organic binders to glue graphite and lubricants to the iron powder particles during the mixing procedure. locally pre-alloyed. Mechanical properties ⇒ flow rate ⇒ bulk density ⇒ compressibility.as well as other metal powders .the latter become. • compressibility decreases with increasing microhardness.

Metallurgical properties are determined by chemical analysis and metallographic procedures. Non-metallic impurities may have an adverse effect upon compressibility and upon the life of compacting tools. Finer powders are suspended in water and analyzed by means of laser diffraction methods External particle shapeis analyzed by means of scanning electron microscopy Internal particle structure is analyzed by means of metallographic techniques Flow rate or rather its reciprocal value. particle shape and particle porosity.powders of regular particle shape. and dividing the weight of powder contained in the cup by the cup volume (25 cm3). Green density is the compact density of a small cylindrical powder compact (Ø 25 mm) pressed with a standardized pressure (either 4. Compact density is the weight of a powder compact divided by its bulk volume. Apparent density is influenced by type and amount of lubricant admixed to the powder. The compressibility of the powder . determine the powder’s specific surface which is the driving force of the sintering process Particle size distribution is determined by sieve analysis if particle sizes are above 45 μm (minimum screen aperture). The chemical composition of a ferrous powder has a great influence upon the final strength properties of the sintered parts. Compact density is influenced by type and amount of lubricant admixed to the powder. Flow rate is influenced by type and amount of lubricant admixed to the powder. The apparent density of the powder decides about the required filling depth of the compacting tool. leveling-off the surplus powder on top of the cup. particle size distribution. The flow rate decides about how fast a compacting tool can be filled with powder. Compressibility is the name of a curve obtained by plotting the compact densities of a series of small cylindrical powder compacts (Ø 25 mm). is the time in seconds which an amount of 50 g dry powder needs to pass the aperture of a standardized funnel. over the applied pressures. Geometrical properties viz. Bulk density (Apparent density) is determined by filling the powder through a standardized funnel into a small cup. and thus is a limiting factor in the compacting cycle of the powder press.2 tons/cm2 or 600 N/mm2).

Green strength increases with increasing compact density and is influenced by type and amount of lubricant admixed to the powder.decides about how high a compacting pressure is needed to achieve a desired compact density. If the green strength of compacts is high enough. The more complex and delicate the shape of a compact. the powder particles are bonded together by diffusion and other atomic transport mechanisms.g. Sufficient green strength is required to prevent compacts from cracking during ejection from the compacting tool and prevent them from getting damaged during handling and transport between press and sintering furnace. Spring-back increases with increasing compacting pressure and is influenced by type and amount of lubricant admixed to the powder. they may even be machined prior to sintering (e. . and the resulting somewhat porous body acquires a certain mechanical strength. • composition of the powder mix. The spring-back value is important for calculating the exact dimensions of the compacting tool in relation to the required dimensions of the compact. the higher its green strength should be. Green strength is the bending strength of a green (i. • geometrical structure of the powder particles.e. • density of the powder compact. Sintering Sintering is the process by which metal powder compacts (or loose metal powders) are transformed into coherent solids at temperatures below their melting point. undercuts. Spring-back is the elastic expansion of a cylindrical powder compact (Ø 25 mm) after ejection from the compacting die. Its value is expressed as the difference between the OD of the compact and the ID of the (empty) die divided by the ID of the die. During sintering. • composition of the protective atmosphere in the sintering furnace. The sintering process is governed by the following parameters: • temperature and time. compacted but not sintered) rectangular test bar. traverse slots and holes). and by the elasticity coefficient of the die material in which the powder is compacted.

1150°C). Again. At given sintering conditions. Density of the powder compact. Particles of commercial iron powders (spongy or compact types) for structural parts are usually ≤ 150 μm Composition of the powder mix. iron. copper in iron powder mixes). In iron powder metallurgy. common sintering conditions are: 15 . and the more efficient are bonding and alloying processes during sintering. nickel and molybdenum) are sintered. If the powder mix contains a component that forms a liquid phase at sintering temperature (e. The greater the density of a powder compact. This constitutes a dilemma: From the view point of production efficiency.60 min at 1120 – 1150°C. alloying processes are slow (except between iron and carbon). in terms of mechanical strength). these processes are enhanced by the disturbances in the particles’ crystal . Geometrical structure of the powder particles. The higher the sintering temperature. shorter sintering times would be preferable. sinter faster than powders consisting of coarse compact particles. we have a dilemma: Fine powders are usually more difficult to compact than coarse powders. bonding between particles as well as alloying processes are accelerated. Furthermore.Temperature and time.g. and a complete homogenization of the metallic alloying elements is not achievable. Chapter 3). and compacts made from fine powder shrink more during sintering than compacts made from coarse powder.g. the larger is the total contact area between powder particles. powders consisting of fine particles or particles of high internal porosity (large specific surface).g. but the correspondingly higher sintering temperatures are less economical because of higher maintenance costs for the sintering furnace. the shorter is the sintering time required to achieve a desired degree of bonding between the powder particles in a powder compact (specified e. At common sintering temperatures (1120 . The components of powder mixes are selected and proportioned with a view to achieving desired physical properties and controlling dimensional changes during sintering (ref. alloying between the components takes place simultaneously with the bonding process. When mixes of two or more different metal powders (e.

lattice caused by plastic deformation during compaction Composition of the protective atmosphere in the sintering furnace. • neutral type: cryogenic nitrogen (N2). cracked ammonia (75% H2. 0-0.1 Solid state sintering of homogeneous material Judging by the changing shape of the interspace between sintering particles. . the total pore volume shrinks. On the one hand. This illustrates the problem of choosing the right atmosphere for each particular type of sinter goods. on the other hand. the bulk volume of the sintering particles shrinks – in the early stage.2. and 2) a late stage with pore-rounding and pore shrinkage. the sintering process passes through two different stages: 1) an early stage with local bonding (neck formation) between adjacent particles. In both stages. if desirable with minor additions of H2 (to take care of residual oxides) or of methane or propane (to restore carbon losses). the following sintering atmospheres are common : • reducing-decarbonizing type: hydrogen (H2). N2). it is to prevent decarbonization of carbon-containing material and. the center distance between adjacent particles decreases. bal.2% CO2.5% CH4. • reducing-carbonizing type: endogas (32% H2. In iron powder metallurgy.2 Basic Mechanisms of Sintering 6. 23% CO. prevent carbonization of carbon-free material. 0-0. vice versa. 6. in the late stage. 25% N2). the atmosphere is to protect the sinter goods from oxidation and reduce possibly present residual oxides. The protective atmosphere has to fulfill several functions during sintering which in some respects are contradictory.

• evaporation/condensation of atoms on surfaces. alloying takes place at locations where necks are formed between particles of different metallic identity. five different transport mechanisms are possible: • volume diffusion (migration of vacancies). a delaying or no effect at all on the growth rate of the neck. the growth rate of the neck now depends not only on the diffusion rates in the two pure metals but also on the different diffusion rates in the various alloy phases being formed in and on either side of the neck. • surface diffusion. • viscous or plastic flow (caused by surface tension or internal stresses). 6. On the other hand. 6. The outcome of this interaction varies with the chemical identity of the two metals: it may have an accelerating. These two processes interact with one another: On the one hand.2.3 Sintering in presence of a transient liquid phase . the neck width controls the rate of alloy formation.2. • grain-boundary diffusion.The driving force behind these sintering phenomena is minimization of the free surface energy (ΔGsurface< 0) of the particle agglomerate In the absence of a liquid phase.2 Solid state sintering of heterogeneous material When a mixture of particles of two different metals is being sintered.

and the bulk volume of the compact shrinks. in the example above. If.Consider a compact made from a mixture of particles of two different metals. if the initial proportion of the liquid phase is smaller than its solubility in the solid phase. The micrograph at Fig. while the framework of solid particles increases in volume corresponding to the amount of dissolved liquid phase. See schematic illustration at Fig. Consequently. 6. These examples explain why additions of copper to iron powder mixes result in less shrinkage .13 shows beginning disintegration of pearlitic iron particles under the influence of liquid copper. It can be seen that the liquid copper not only infiltrates the gaps between the iron powder particles but also penetrates their grain boundaries. the arising liquid phase is first being pulled by capillary forces into the narrow gaps between the particles of the solid component. the liquid copper penetrates the interfaces between ferrite and cementite lamellae.11. 6. Then. the initially rigid framework of solid particles collapses locally. the liquid phase eventually disappears. The bulk volume of the compact swells because the melting particles leave behind large pores. the pure iron particles are substituted with carbonized iron particles having a pearlitic microstructure. If one component of the mixture melts at sintering temperature. creating the largest possible contact area between liquid and solid phase. This leads eventually to a partial disintegration of the pearlitic particles. alloying takes place and.

As the activator continues to diffuse deeper into the particles of the base metal. As can be seen from the binary phase diagram shown at Fig.2.or produce growth during sintering of structural parts. Here. where the crystal structure of iron changes from ferrite to austenite. • Tensile strength and elongation adopt noticeable values first at sintering temperatures above 650 and 750°C respectively. See Fig. in the manufacturing of so called heavy metals. the liquid phase (eutectic) disappears again. The added metal or metal compound is called the activator.% again. sintering proceeds faster in ferrite than in austenite. The sintering of iron powder can be activated through small additions (e.5 wt.6 and 0.4 Activated sintering A special kind of sintering with a transient liquid phase is often referred to as activated sintering. Just above 910°C.6 wt.%. the values of tensile strength and elongation suddenly . 6. Consequently. its concentration at the surface drops below 2. During sintering at 1120°C. and the particles melt superficially. the coefficient of selfdiffusion (volume diffusion) for iron is approx. Here. 300 times greater in ferrite than in austenite. they increase almost exponentially until reaching an intermediate maximum at approx. From there-on. During sintering. Activated sintering is utilized e. 3 wt.14.g. forms a low-melting eutectic together with the base metal.%) of finely ground ferro-phosphorous (Fe3 P). the phosphorous concentration at the surface of the iron powder particles temporarily exceeds 2. As will be seen in the next paragraph. and why additions of carbon (graphite) to iron-copper powder mixes compensate the growth-producing effect of copper 6.15. atoms from the activator diffuse into the particles of the base metal until the latter begin to melt superficially. This superficial melting enhances the formation of necks between adjacent particles of the base metal.g. 6. But as the phosphorous diffuses deeper into the iron particles.6 wt. Fe and Fe3P form a eutectic at 1050°C. although having a melting point above sintering temperature. at equal temperature. a second benefit of phosphorous becomes effective: Surface regions of the iron particles with phosphorous concentrations between 2. a base powder is admixed with a small amount of a metal or metal compound which. and the liquid phase disappears. 900°C. an addition of only a few percent of nickel powder to tungsten powder produces a transient tungsten-rich eutectic at 1495°C which substantially accelerates the sintering process.% have changed from austenite to ferrite. Then.

and those which are heated up to higher temperatures have already acquired a certain level of strength before they change from ferrite to austenite. densities up to 7. but more slowly than below 910°C.650 N/mm2). elongation and impact strength exponentially. All test bars begin to sinter already during the heating-up period. This density range can be extended . In order to utilize the advantage of a transient liquid phase during sintering and to achieve higher strength properties. The carbonization of the iron caused by the graphite additions boosts the mechanical strength of the sintered parts. SINTERED IRON-BASED MATERIALS There are several ways to achieve desired strength properties with iron-based sintered materials.4 The sintering atmosphere The main purpose of sintering atmospheres is to protect the powder compacts from oxidation during sintering and to reduce residual surface oxides in order to improve the metallic contact between adjacent powder particles.2 g/cm3 are achievable. A further purpose of sintering atmospheres is to protect carbon-containing compacts from decarbonization.3). 6.2. Graphite additions to iron-copper powder mixes counteract the dimensional growth caused by the copper (see § 6. while still in the ferrite state. With maximum pressing loads tolerable under mass production conditions (600 .7. Copper additions to iron powder can produce undesirable dimensional growth during sintering.drop a little and then increase again.1 . because tensile strength and fatigue strength increase in approximate linear proportion. many commercial iron powder mixes contain copper. with sintered density. The most important parameters of influence are: • Density • Sintering conditions • Alloying elements • Heat-treating conditions Density is of prime importance with respect to the physical properties of sintered structural parts.

In iron powder metallurgy. can be achieved by means of hot-forging pre-pressed (and pre-sintered) compacts [9. See Fig.8 g/cm3. and (3) whether sensitive alloying elements oxidize or not.2). 9.2].7. Still higher densities. Sintering conditions decide (1) how fast and efficient powder particles in the compact weld together and pores get rounded.1150°C.1].6 g/cm3 can only be achieved by pre-sintering and re-pressing the compacts before final sintering (chapter 7.4 g/cm3 when utilizing a warm-pressing technique developed by HÖGANÄS AB [9.2b.7 . Alloying elements also influence the dimensional change of structural parts during sintering. 9. give rise to the formation of various microstructures and increase the materials resistance to deformation. § 7. Sintering temperatures of 1250 -1350°C accelerate the homogenization of alloying elements and allow the use of beneficial but oxygen-sensitive alloying elements like chromium and manganese.7. Time at temperature is usually no longer than 20 to 30 minutes. Meshbelt furnaces cannot withstand temperatures above 1150°C.up to 7. . sintering is most commonly carried out in continuous mesh-belt furnaces operating at 1120 to max. chromium alloys can now be sintered at 1120° C. See Fig.5 .3 . With modern materials and furnaces. Alloying elements dissolved in the base metal. since longer sintering times yield only marginally improved properties which do not justify the increased sintering costs.7. up to 7.2a. (2) how fast homogenization of alloying elements takes place. Alloying elements are indispensable with respect to the hardenability of conventional as well as sintered steels. Densities up to 7.

can have beneficial effects on sintered steels (chapter 6. that the scatter of these dimensional changes is kept within the closest possible limits.In principle.4). With alloy compositions yielding hardness levels above 150 . phosphorous (”blue brittleness”). Alloy compositions of sintered steels for structural parts have to be carefully selected not only with respect to desired strength but also with respect to dimensional stability during sintering.g. However. alloying elements have the same effect on sintered steels as on conventional steels. as e. Mn. it is important that dimensional changes of the structural parts during sintering are as small as possible and. even more important. § 6. On the other hand.2. like e.4).180 HV. are too easily oxidized in commercial sintering atmospheres (chapter 6. and V.g. Asymmetric cooling during quenching of a sintered . elements undesirable in conventional steels. § 6. must be especially well controlled to ensure the highest possible degree of dimensional stability of the component in the hardening and tempering procedure. not all alloying elements common in conventional steels can be utilized in sintered steels because some of them. Heat-treating conditions. when applied to sintered steel components.

3 illustrate the influence of small variations in compact density. sintering conditions and powder composition on the dimensional changes of powder compacts during sintering.Carbon .Carbon • Iron .Carbon • Iron . It can be seen from these examples that intelligently chosen types and amounts of alloying elements can make dimensional changes of sintered compacts less sensitive to varying processing parameters.Carbon • Iron .Nickel .Copper • Iron . Two examples shown at Fig. Dimensional stability of the sintered parts depends on the accuracy with which the above mentioned parameters can be controlled.component. may lead to distortions so severe that the part must either be rejected or subjected to expensive remachining which would wipe out the cost advantage of P/M technology over conventional production methods. Microstructures and Properties In the majority of cases.Copper . 9. 9.2 Alloying Systems. sintered iron and steel components are today made of materials based on one or the other of the following alloying systems: • Plain Iron • Iron . especially when of complex shape.Phosphorus .Copper .

nickel. While carbon diffuses very rapidly in the basic iron powder and soon reaches equilibrium during sintering. ductility and soft-magnetic properties are improving. these materials will always exhibit a certain degree of heterogeneity. and molybdenum diffuse much slower and would reach equilibrium only after extremely long sintering times (chapter 6. these materials are mechanical mixtures of plain iron powder with the respective elements and some lubricant in powder form.Copper . mechanical powder mixtures tend to segregate when transported and handled. Such mixtures can be compacted much more easily than fully pre-alloyed powders. With decreasing grain size. other alloying elements like copper. However. Grain size is a parameter which has an important influence upon the physical properties of plain iron. Microstructures of sintered alloyed steels. Fig.9). produced from powder mixes. but with increasing grain size. produced under commercially acceptable sintering conditions.Molybdenum – Carbon Normally. strength generally increases. 6. Finely dispersed pores have a greater negative effect on soft-magnetic properties than coarser pores Plain Iron . are typically much more heterogeneous than those of conventionally alloyed steels. Therefore are many of these materials today available in the form of partially pre-alloyed non-segregable pressready powder mixes known under the trade-names Distaloy™ and Starmix (chapter 3). Hence.• Iron .Nickel .

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these microstructures are practically identical with those of corresponding conventional plain carbon steels. However.Copper. Iron . this is achieved by adding graphite powder to the iron powder before compacting and sintering.Copper .Carbon .2. successful sintering of carbon containing materials requires a very carefully controlled nondecarbonizing sintering atmosphere Apart from the presence of pores.2 Iron . 9.3 Iron .9.Carbon A very efficient way to boost tensile strength and hardness of sintered iron is to alloy it with carbon.2. carbon dissolves very rapidly in the iron powder structure during sintering. Being an interstitial alloying element. Most conveniently.