Powder Metallurgy Manufacturing Techniques

 

1. INTRODUCTION

 

Among the various metalworking technologies, powder metallurgy (P/M) is the most diverse manufacturing approach. One attraction of P/M is the ability to fabricate high quality, complex parts to close tolerances in an economical manner. In essence, P/M takes a metal powder with specific attributes of size, shape, and packing, and then converts it into a strong, precise, high performance shape. Key steps include the shaping or compaction of the powder and the subsequent thermal bonding of the particles by sintering. The process effectively uses automated operations with low relative energy consumption, high material utilization, and low capital costs. These characteristics make P/M well aligned with current concerns about productivity, energy, and raw materials. Consequently, the field is experiencing growth and replacing traditional metal-forming operations. Further, powder metallurgy is a flexible manufacturing process capable of delivering a wide range of new materials, microstructures, and properties. That creates several unique niche applications for P/M such as wear resistant composites.

 

The applications of P/M are quite extensive. Consider the use of metal powders in the fabrication of tungsten lamp filaments, dental restorations, oil-less bearings, automotive transmission gears, armour piercing projectiles, electrical contacts, nuclear power fuel elements, orthopaedic implants, business machines, high-temperature filters, aircraft brake pads, rechargeable batteries, and jet engine components. Furthermore, metal powders find uses in such products as paint pigments, porous concretes, printed circuit boards, enriched flour, explosives, welding electrodes, rocket fuels, printing inks, brazing compounds, and catalysts. Worldwide market share for P/M parts are given in the following pie chart. Automotive industry is leading with more than 75% of the share. American cars contain more than 16 kg of P/M parts while European cars have 7 kg and Japan cars have 5 kg P/M parts.

 

Distribution of P/M parts in a car

Typical iron and copper based P/M parts

 

2. POWDER PRODUCTION

 

Almost all materials can be made into powder, but the method selected for fabricating a powder depends on specific material properties. Knowing how a powder is made provides a good basis for estimating and understanding some of its characteristics. The four main categories of fabrication techniques are based on mechanical comminution, electrolytic deposition, chemical reactions, and liquid metal atomisation. In addition to these main approaches, several specialty techniques are used for selected materials. Atomisation processes produce more than 60% of all powders consumed in the industry.

 

Mechanical Comminution

 

Brittle materials such as inter-metallic compounds, ferro-alloys, ferro-chromium, ferro-silicon, etc. are crushed mechanically in ball mills. However, milling is not useful for many ductile metals since they do not easily fracture. Instead, the ductile particles cold-weld together and form larger particles. Milling is currently used for production of metallic flakes from ductile metals like aluminium. In this case a lubricant is used for elimination of adhesion and cold welding.

 

           

 

Electrolytic Deposition

 

By choosing suitable conditions; composition and strength of the electrolyte, temperature, current density, etc., many metals can be deposited in a spongy or powdery state. Extensive further processing; washing, drying, reducing, annealing and crushing may be required. Copper is the main metal to be produced in this way, but chromium and manganese powders are also produced by electrolysis. In these cases, however, a dense and normally brittle deposit is formed and requires to be crushed to powder. Electrolytic iron was at one time produced on a substantial scale but it has been largely superseded by powders made by less costly processes. Electrolytic powders are very pure.

 

Chemical Reactions

 

This has been for long the most widely used method for the production of iron powder. Selected ore is crushed, mixed with carbon, and passed through a continuous furnace where reaction takes place leaving a cake of sponge iron which is then further treated by crushing, separation of non-metallic material, and sieving to produce powder. Since no refining operation is involved, the purity of the powder is dependent on that of the raw materials. The irregular sponge-like particles are soft, and readily compressible, and give compacts of good green strength. Refractory metals are normally made by hydrogen reduction of oxides, and the same process can be used for copper.

Atomisation

 

In this process molten metal is broken up into small droplets and rapidly frozen before the drops come into contact with each other or with a solid surface. The principal method is to disintegrate a thin stream of liquid metal by subjecting it to the impact of high energy jets of gas or liquid. Air, nitrogen and argon are commonly used gases, and water is the liquid most widely used. By varying the several parameters; design and configu­rations of the jets, pressure and volume of the atomising fluid, thickness of the stream of metal, etc., it is possible to control the particle size distribution over a wide range. The particle shape is determined largely by the rate of solidification and varies from spherical, if a low heat capacity gas is employed, to highly irregular if water is used. In principle, the technique is applicable to all metals that can be melted, and is commercially used for the production of iron, tool steels, alloy steels, copper, brass, bronze and the low-melting-point metals, such as aluminium, tin, lead, zinc, cadmium. The readily oxidising metals, for example chromium-bearing alloys, are being atomised on an increasing scale by means of inert gas, especially argon. Atomisation is particularly useful for the production of alloys in powder form, since the constituent metals are fully alloyed in the molten state. Thus each powder particle has the same chemical composition.

 

gas atomisation  illustration

 

In addition, there are several other atomisation processes that are finding increasing application, an important one being centrifugal atomisation in which droplets of molten metal are discharged from a rotating source. There are basically two types of centrifugal atomisation processes: in one a cup of molten metal is rotated on a vertical axis at a speed sufficient to throw off droplets of molten metal, or a stream of metal is allowed to fall on a rotating disc or cone; in the other, a bar of the metal is rotated at high speed and the free end is progressively melted, e.g. by an electron beam or plasma arc. This latter process is called the Rotating Electrode Process (REP), and the bar may be rotated either on a horizontal or on a vertical axis. A special advantage of these processes is that they can be carried out in a sealed vessel in a controlled atmosphere, even vacuum, and thus produce clean powders of highly reactive metals.

 

Other Processes

 

Thermal decomposition of a chemical compound is used in some cases, a notable one being nickel carbonyl. This Carbonyl Process was originally developed as a means of refining nickel, crude metal being caused selectively to react with carbon monoxide under pressure to form the carbonyl which is gaseous at the reaction temperature and which decomposes on raising the temperature and lowering the pressure. The same process is used for iron, and carbonyl iron powder finds small-scale application where its very high purity is useful. Recently, demand for very fine powders for the injection moulding process has given a considerable impetus to the carbonyl process. Typically the particle size of carbonyl iron powder is 1 - 5 μm, but, as in the case of nickel, it can be tailored to suit particular requirements. Another case of thermal decomposition is platinum powder of which is made from sponge produced by heating salt platinum ammonium chloride. In the Sherritt-Gordon process, nickel powder is made by hydrogen reduction of a solution of a nickel salt under pressure. Chemical precipitation of metal from a solution of a soluble salt is used in other cases, e.g., silver, powder of which is produced by adding a reducing agent to a solution of silver nitrate. This is, of course, the same basic process as is used to produce black and white photographs.

Powder Characteristics

 

The further processing and the final results achieved in the sintered part are influenced by the characteristics of the powder: particle size, size distribution, particle shape, and structure and surface condition. A very important parameter is the apparent density of the powder, i.e., the mass of a given volume of powder without any pressing or settling. The apparent density is a function of particle shape and the degree of porosity of the particles. The choice of powder characteristics is normally based on compromise, since many of the factors are in direct opposition to each other. An increase in the irregularity and porous texture of the powder particle, i.e., decrease in apparent density, increases the reduction in volume that occurs on pressing and thus the degree of cold-welding, which in turn gives greater green strength to the compact. This increase in contacting surfaces also leads to more efficient sintering. Compressibility, density achieved at a specified pressure, is also an important powder property. Low compressibility powders require greater pressure and consequently larger presses and stronger dies. The ease and efficiency of packing the powder in the die depends to a large extent on a wide particle size distribution. So that the voids created between large particles can be progressively filled with those of smaller size.


The purity of the powder is critically important. Impurity levels, which can be tolerated, depend to a large extent on the nature and state of combination of the substances concerned. For example, the presence of combined carbon in iron tends to harden the matrix so that increased pressures are required during compaction. Free carbon, however, is often an advantage, acting as a lubricant during the pressing operation. A thin oxide film coats most metal powder particles, but in general these do not interfere with the process, since they are ruptured during the pressing operation to provide clean and active metal surfaces which are easily cold-welded. Their final reduction under the reducing sintering atmosphere is essential for complete metal bonding and maximum strength.
 

 

3. PRODUCTION OF P/M PARTS

 

The general sequence of operations involved in the P/M process is shown schematically in the flow chart. The component powders are mixed, together with lubricant, until a homogeneous mix is obtained. The mix is then loaded into a die and compacted under pressure, after which the compact is sintered. An exception is the process for making filter elements from spherical bronze powder where no pressure is used; the powder being simply placed in a suitably shaped mould in which it is sintered. There are various powder compaction methods such as; uniaxial pressing, rolling, extrusion, injection moulding, isostatic pressing, etc. Selection of the method is dependent to part geometry and number of production.

 

Mixing

 

The metal powder is mixed with lubricant and optional alloying elements to form a homoge­nous blend. 0.5 - 1.5% lubricant is normally added in the mix, and metallic stearate and waxes are commonly used lubricants. The main function of the lubricant is to reduce friction between the powder mass and the surfaces of the tool, die walls, core rods etc., along which the powder must slide during compaction. This assists the achievement of uniform density from top to bottom of the compact. Of equal importance is the fact that the reduction of friction also makes it easier to eject the compact. As an alternative to pre-alloyed powders, alloying elements can be added to the mix as powders. The high compressibility of a pure iron powder is thus maintained and the solution-hardening effect of the alloying elements is avoided. The most commonly used alloying element is carbon, which is added as graphite powder.

 

        

Pressing

 

The most common way of compacting is axial pressing in a steel or carbide die under pressures of 300 - 800 MPa. It is possible to press parts with complicated shape in a single operation and with high production rate, up to 25 part/minute. The part achieves sufficient strength to be ejected from the tool die and can be handled before sintering by interlocking and cold-welding between the particles. Highly compressible iron powder can achieve a density of 7.3 g/cm3 (or 93%) of the theoretical density at a compacting pressure of 800 MPa.

 

 

Pressing Steps

 

By utilising Warm Compaction, which means that a powder mix with special lubricant and the tool set are heated to 130°C and 150°C respectively, density can be increased by up to 0.2 g/cm3, compared to conventional cold compaction. Warm compacted components have a strength high enough to allow some machining operations before sintering, which drastically decreases tool wear.                 

 

Sintering

 

Sintering is a heat treatment wherein the pressed parts gain strength. The most common sintering temperature range for iron-based alloys is 1100 - 1150°C. In some cases, higher sintering temperatures up to 1250°C are employed. The time at temperature varies between 10 and 60 minutes, depending on the application. The most common type of furnaces is the mesh belt furnace. Components are placed on a tray, or directly on the mesh belt, which transports them through the furnace. Mesh belt furnaces are limited to a temperature of maximum 1150°C. For higher temperatures, walking beam or pusher-type furnaces are common. The sintering cost increases significantly if sintering temperatures higher than 1150°C are used. An atmosphere, which prevents oxidation, is necessary in the sintering furnace. Dissociated ammonia, endothermic or nitrogen-based atmospheres are commonly used. It is of great importance also to have a controlled carbon potential, in order to ensure consistent mechanical properties and tolerances on the sintered components.

 

      

 

A sintering operation consists of de-waxing, sintering and cooling steps. In the de-waxing zone of the furnace, the lubricant is burned off. During the sintering, several reactions take place. Initially, the furnace atmosphere reduces oxides on the surface of the particles, and an initial bond between particles in contact is formed. The main mechani­sms of sintering are surface and volume diffusion. By diffusion, a coherent body of metal is formed, and the admixed alloying elements are distributed into the iron. Driven by the force to minimise free energy, stated by the laws of thermodynamics, rounding of pores takes place and small pores disappear in favour of larger. In the cooling zone of the sintering furnace, the parts are cooled under protective atmosphere in order to not oxidise in contact with air. The cooling speed, especially in the range 850 - 500°C, also affects the mechanical properties, due to phase transformations in the material. During the sintering, a moderate dimensional change takes place. Most materials shrink but some alloying elements, such as copper, cause growth. In design of the press tool, the dimensions must be compensated for the dimensional change.

 

Infiltration

 

The interconnected porosity is filled with an alloy having a melting point lower than the sintering temperature of the metal of which the component is made, e.g., copper-based alloys infiltrate ferrous parts, usually during the sintering phase. Infiltration makes the components impermeable and there is some increase in mechanical properties, but at expense of dimensional accuracy. Infiltration simplifies some heat treatments. For instance, it is easier to obtain a defined case depth without interconnected porosity.

           

Oil Impregnation

 

Sintered parts achieve greater protection against corrosion by being impregnated by oil or other non-metallic material. Self-lubricating bearings are manufactured by impregnating porous sintered bearings with lubricants and these bearings can only be produced by powder metallurgy.

 

Sizing and Coining

 

Sizing and coining are additional press operations after sintering. The main objective is to improve the dimensional accuracy, but the surface finish is also normally improved. Quite moderate pressures are normally required for sizing, since only a slight plastic deformation is necessary. Coining has a double purpose. Not only is dimensional accuracy improved, but the use of higher pressures also increases the density of the part. Normally, a press tool specific to the task of sizing or coining is used.

 

          

Double Pressing

 

A second pressing operation serves to decrease porosity for applications where density is crucial to achieve the required mechanical or magnetic properties. By pre-sintering the pressed part at temperatures of 700-800°C, the admixed lubricant is burned off and re-crystallisation takes place. Once the work hardening and internal stresses are removed, the material reacquires its ductility and therefore its capacity for further densification. After re-pressing, the parts are sintered for the second time.

 

 

 Steam Treatment

 

Applicable only to ferrous parts. By heating the parts to a temperature of 550°C and exposing them to water vapour, a thin layer of Fe3O4 is formed both on the outer surface and along the interconnected porosity. Steam treatment induces considerable corrosion resistance, increased hardness, increased resistance to compressive strength, and improved wear resistance.

 

       

 

Machining

 

Although a major attraction of producing sintered components is the ability to produce complex shapes and close tolerances, limitations do exist. Therefore, machining operations such as milling, drilling (e.g., holes perpendicular to the pressing direction), threading and machining can be used to achieve features not possible to obtain by pressing in rigid dies. Sintered metals are generally less easy to machine than wrought alloy of similar composition, so cutting speed and cutting tools should therefore be adjusted for optimum results. To increase tool life, machinability-enhancing additives such as MnS can be admixed with the powder. After sintering, they remain evenly distributed in the structure and mechanical properties are only marginally affected.

 

De-burring

 

This operation removes burrs resulting from the compacting operation or machining step. The most common method is tumbling, and sometimes a liquid medium with an abrasive powder is employed.

 

Joining

 

Larger parts and very complex shapes can be obtained by joining. Several techniques exist for joining, such as diffusion bonding, sinter brazing and laser welding.

 

                  

 

Heat treatment

 

Phase transformation depends on the composition and homogeneity of the alloy, not on its porosity, so all heat treatments applicable to the cast and wrought alloys are applicable for sintered materials as well. Hardening operations with quenching and tempering substantially increase strength, and improve wear-resistance; but at the expense of ductility. Surface hardening by carburising and carbonitriding is extensively used on sintered parts.

 

Surface plating

 

When needed, corrosion protection can be obtained by plating. However, low-density parts must be impregnated before plating, to prevent electrolyte from entering the pores and causing subsequent corrosion.

4.  PROPERTIES OF P/M PARTS

 

The properties of sintered materials are depending on a range of factors and can be optimised to fit special requirements. Chemical composition and density of the component are important factors to consider when the material is to be specified for a certain application.

 

Chemical composition and mechanical properties are commonly used factors to specify the properties of a sintered machine part. Some examples are given below:

 


      Chemical composition
      Fe

      Fe-Cu
      Fe-Cu-C
      Fe-Cu-Ni-Mo-C
      Fe-P

      Fe-P-C

        Mechanical properties

Hardness

Density

Ultimate tensile strength, yield strength

Transverse rupture strength

Young’s modulus


 

The mechanical properties of P/M materials are degraded by the presence of pores. The tensile strength and hardness are linearly correlated to the porosity, while there is a non-linear correlation between porosity and elongation, and impact strength. The mechanical properties are given either as compulsory values or as typical values. For comparison of sintered materials to cast and wrought materials, the yield strengths of various materials are showed in the following graph.