Compaction
Compaction
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     Methods for compacting of powder materials can be divided to two basic groups:
 1. Compaction with the aid of static or dynamic compacting pressure at room or elevated
    temperature – compacting by single-action or multi-action static compacting pressure in a die
                                           A
    with an upper and bottom punch for high-volume manufacturing of parts of various types:
    forging, isostatic pressing, extrusion pressing, rolling, hot pressing e.g. for draw tools from
    cemented carbides.
 2. Pressureless compaction – free pouring (e.g. a manufacture of filters), jolting, vibration
    compacting e.g. for fuel elements for nuclear technology and the ceramic casting method.
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     In Table 6.1, basic differences in behaviour of powder particles during their pressure forming and
pressureless forming are shown.
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      Table 6.1 Basic differences in behaviour of powder particles during pressure compacting and
                                        pressureless compaction.
                                                  compacting pressure.
  A shape of pores depends on the particle A shape of pores depends on the pressing
  morphology                                      method and the applied pressure
                                                  Most of the pores are open, closed pores are
  Pores are open (interconnected) – open porosity
                                                  existing already, too.
Cold forming involves all methods by which compacts can be made which have a demanded
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geometrical shape with such dimensions, so that after sintering they have final dimensions and such a
consistency (green strength), that it is possible to handle them (e.g. to take-off from a pressing tool, to
place into a sintering furnace etc.). The necessary “green” strength can be achieved by compacting, i.e.
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reducing porosity and increasing particular interparticle adhesion. Pressing is used most frequently for
this purpose.
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         When pouring powder, particles become arranged by acting of gravitational forces. Poured
powders include bridges and cavities which can be reduced by jolting and vibrations.
         By using slurry, a tighter arrangement can be reached due to reduction of interparticle friction.
After drying-up of “cast” shape compacts, they can be handled freely. When pressing in tools, which
is prevailing in the industrial scale, a shape body is subjected to a complicated mechanical loading.
The applied compacting pressure leads to the compaction of powder. However, the pressure
                                            A
distribution in a compact is not uniform, which is given by the fact that a part of the incoming energy
is consumed to overcome the friction between particles and mould walls and among particles
themselves.
compact with an increasing pressure (Fig. 6.1): 1. Arrangement of particles occurs, formed clusters
(bridges) are removed and cavities are filled. 2. A contact between particles increases as a result of the
plastic deformation and a particle surface is levelled. An oxidation layer is torn and a formation of the
agglomerate occurs by mechanical interlocking of particles. Particles are strengthened. 3. Further on,
when pressure increases, an increase of a contact surface between particles and further strengthening
of particles occur, adhesion between particles increases and particles, which have run out of their
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plasticity, disintegrate.
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          According to the quality of the powder, which can consist of particles of different sizes or
various chemical composition, these processes can run simultaneously and they occur more or less
depending on the powder properties. A density and porosity change influences other measurable
values which can be used for a description of properties of compacts, in particular for formable
materials. For example, this is hardness which depends on a degree of strengthening, a powder size, a
degree of oxidation etc., or electrical conductivity which increases with decreasing porosity at first,
but an increasing hardness slows down this rise.
          During die pressing the conditions are strongly affected by friction on the die walls, which
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causes uneven distribution of material density in a compact. During single-action pressing, the highest
compacting pressure is on edges of a pressing tool, the lowest on the bottom edge of a compact.
During double-action pressing, i.e. when using a movable upper and bottom punch, compacts of a
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double height can be pressed. The pressure distribution is better than during the single-action pressing,
but it is also influenced by friction on the pressing mould walls.
          Inhomogeneous pressure distribution in the vertical and horizontal direction causes a
disintegration of a compact to horizontal layers of a “plate” shape while pushed-off from the die.
According to some authors, during pressing parabolic areas are formed in a compact, which do not
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contain a tangential component of stress. On these areas, there is no shear motion of particles, and not
even occurrence of cold welded joints.
          Consider a cylindrical compact of a diameter D and height l, where its element dl is analysed
(Fig. 6.2). The pressure in the upper part of the element p and the pressure passing through an element
pb differs by a normal (perpendicular) force acting against friction. Force equilibrium along the
compression axis can be expressed mathematically as:
                                             A
                                        F = 0 = A·(pb - p) + ·Fn
                                       where Ff = µ·Fn; A = D2/4
The normal force can be expressed with the aid of an applied press and a constant of proportionality z,
which changes with a compact density:
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                                             Fn = ·z·p·D·dl
The friction force Ff can be calculated directly from the normal force and the friction coefficient µ as:
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                                            Ff = ·µ·z·p·D·dl
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D
Fig. 6.2 Relation of the applied compacting pressure to its distribution in the compact volume.
         Combining the above mentioned relations, the difference in pressures dp of the upper and
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decreases with an increasing distance from the punch in the depth under the punch.
        The double-action pressing has a profile of the simultaneous compacting pressure profile both
from the upper and from the bottom punch. For this type of compression the obtained relation px is
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valid, however, the distance x expresses the distance to the nearest punch. The result is a more
homogenous pressure distribution in the compact. In such a case the pressure distribution depends on
the compact height to diameter ratio, which should be as low as possible. The single-action
compression is usually limited to a simple geometry of a compact.
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6.1.2 Activation effect of pressing
        When shapes and sizes of particles and their contact areas are changing during pressing, lattice
and structure imperfections occur (e.g. dislocations the number of which is proportional to the
increasing compacting pressure and pressing speed). These increase the activity structure of powder,
which has been formed during its manufacture, and thus also free energy of the dispersive substance
and during the follow-up sintering lead to an increase of compaction intensity. Phenomena
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contributing to the sintering process activation are influenced by pressing conditions. These are in
particular as follows:
     a change in a particle specific area by further disintegration;
     an enlargement of a particle contacting area as a result of a failure of surface oxidation layers;
     an increase of the number of lattice imperfections.
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        These phenomena belong among the main ones, which have a crucial influence on a sintering
process and thus on the final product properties.
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        Properties of compacts depend on the pressing process to a great extent. In Fig. 6.3, basic
principles of the most widely used processes of die pressing are shown. The double-action pressing is
preferred, as it ensures more favourable density distribution and complex density of a compact.
Further, it enables to eject a compact off a die faster.
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 Fig. 6.3 Methods of die pressing: a) single-action pressing; b) double-action pressing; c) floating die
                                              pressing [1].
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         During this pressing method the powder poured into a die occupies a height H (loose powder
height) and at the upper and bottom punch acting simultaneously it is compressed to a height h. In Fig.
6.4, the particular cycles of the pressing process are shown – 1. Filling a die with powder; 2. Pressing
of the powder; 3. Ejection and take-off of a compact.
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                      Fig. 6.4 Particular cycles of the process of die pressing [2].
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6.2.1.1 Powder behaviour during pressing
         Powder behaviour when compressed can be evaluated from various points of view. To
determine dimensions of pressing tools, a ratio of a loose powder height H to a compact height h is
important. In order not to extend a pressing path, the height H has to be as short as possible, which
assumes an adequate powder apparent density. The H:h ratio should not exceed a value of 3.
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         A degree of compaction at pressing is usually characterized by relative density which is
defined as a ratio of a density of a porous compact to an adequate compact material density. The
relation of relative density to compacting pressure for selected metal powders is given in Fig. 6. 5.
         In principle, high density of compacts is required. It ensures a satisfactory strength and
manipulability of a compact and its low shrinkage during the subsequent sintering, so that demanded
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dimensions of a product can be achieved more easily. However, the enhancement of density of a
compact is limited by economical and constructional factors. The density enhancement requires higher
compacting pressures, resulting in faster wear of pressing tools and an increase of dimensions of
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pressing machines. Therefore in a case of an unsatisfactory density, other enhancement methods are to
be used, e.g. coining. This means a re-pressing of a compact in order to achieve accurate dimensions
and to improve properties, while enhancing the relative density substantially at the same time.
         Regarding to pressing and sintering, contending demands are often posed on powders. For
good sintering, fine powders with a large specific surface are demanded. However, these materials
have the high loose powder height H and thus the pressing process is made more difficult. A similar
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situation is for mechanically “activated” powders which are often strengthened as much that their
deformation is not possible at room temperature. Then, these compacts exhibit low relative density
after pressing. To enhance the density, such powders must be processed in a different way.
In principle, the very pressing can be performed in two ways:
  Pressing by a stable compacting pressure – performed on hydraulic presses which have to be
   set to a required maximum compacting pressure. Compacts may show certain differences in
   height as a result of different properties of the initial powder material. Pressing force calculation:
D
                                                 F = S·p
 where F – pressing force (N), S – total compressed area (m2), p - compacting pressure (N.m-2).
  Pressing to a constant height – performed on mechanical presses with a constantly set stroke of
   a punch. Differences in the initial powder quality result in density changes of obtained compacts.
   Determination of the loose powder height:
                                               HV = HS·q
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 where Hv – loose powder height (mm), Hs – height of a compressed part (mm), q – filling coefficient
 (q = k/s); k – density of a compact (kg.m-3), s –apparent density of powder material (kg.m-3).
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Fig. 6.5 Relation of the relative density to the compacting pressure for selected metal powders: 1 – Al,
     2 – electrolytic Cu, 3 – sponge Fe, 4 – electrolytic Fe, 5 – carbonyl Fe, 6 – H2-reduced W [3].
        A proper design and specifications of pressing tools ensure their long-time service life and
proper functioning. For a low-volume manufacture, pressing tools of tool steels are usually used, for a
high-volume manufacture - cemented carbides. When designing a pressing tool dimension, one has to
consider shrinkage, or swelling, of a compact as a result of sintering and
“relaxation” (elastic
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recovery) after ejection of a compact from the die. Pressures applied during pressing are limited by a
tool shape and a type of material. Moreover, a pressing tool design is influenced by the pressure
intensity, a movement, a shape complexity and a demanded surface finishing. Compressed powder
shapes are usually complicated and consisting of several levels or thicknesses in a pressing direction,
therefore the successful pressing of complicated shapes demands an independent control of tool
movements – Fig. 6.7.
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Fig. 6.7 Ways of crack origination during pressing as a result of an improperly designed pressing tool:
a) different dilatations of two bottom punches; b) ejection of a compact in a sharp corner of a die [1].
                                             A
        When forming parts with an unequal height, it is necessary to use several different punches
which are connected. Their movement is controlled, so that particles can only move along the
direction of the pressing. Separation of as-compressed sections from the rest of the compact by shear
must be avoided. This leads to an origination of cracks which do not reach up to the surface and
cannot be eliminated during sintering (Fig. 6.8).
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Fig. 6.8 Typical errors during the pressing: a) crack origination during the pressing as a result of
improper filling (1 – the crack does not reach to the surface, 2 – the area of failure is smooth); b) crack
origination during the ejection (3 – the crack protruding and visible, 4 – the fracture area is rough) [3].
6.2.1.3 Presses
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  Hydraulic presses – above a pressing force of 1000 kN; the pressing force is well-controllable.
   However, the pressing speed is low and they allow 10 – 15 strokes per minute (Fig. 6.9b).
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       a)                                                    b)
             Fig. 6.9 Hydraulic (a) and mechanical (b) press made by DORST company.
Fig. 6.10 Schematic depiction of the hot pressing equipment: a) indirect heating through a heating tube
 or a heating spiral; b) direct heating by passing current through punches; c) direct heating of a die; d)
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        Temperatures above 800 °C are achieved by direct heating of a tool or a compact. In order to
avoid powder oxidation, the pressing equipment is placed into a casing with a protective atmosphere
inside. The hot pressing technology is used for difficult to press powders and difficult to sinter
powders - e.g. dispersion-hardened powders, cermets etc. Another application is a manufacture of
compacts of cemented carbides with low porosity.
        A low productivity and high wear of pressing dies resulted in seeking possibilities for
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achieving demanded effects. For cemented carbides, isostatic additional compacting at high
temperatures is applied.
6.2.2 Extrusion
         This is a procedure of metal powder compaction or semi-products, manufactured by pre-
pressing, or possibly by pre-sintering, in a continuous strand. The process can be carried out at a
normal or elevated temperature (sintering temperature). In the case of extrusion pressing at room
temperature, a mixture of powder and a plastificator is pressed through a nozzle into rods or tubular
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forms. A plastificator is an additive, usually an organic substance (e.g. wax, methylcellulose, synthetic
resin, etc.), which is added to metal powders in order to form a plastic pasty material suitable for
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forming. A principle scheme of the direct and undirect way of extrusion is shown in Fig. 6.11.
         The extrusion technology is used for all materials which can be processed using powder
metallurgy procedures. These are cemented carbides, high-temperature materials with high hardness
and especially technical ceramics. A pressing mixture contains 20 – 30 % of a plastificator which has
to be removed prior to the actual sintering. The compacting pressure is performed using e.g. a piston
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or a screw. Fine powders require higher pressures than for coarse powders extrusion, because more
joints occur, which are fractured and welded repeatedly during the process. A schematic depiction of a
powder material extrusion machine is shown in Fig. 6.12.
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              Fig. 6.11 Extrusion methods: a) undirect extrusion; b) direct extrusion [5].
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             Fig. 6.12 Schematic depiction of the powder material extrusion machine [6].
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Fig. 6.13 Powder rolling arrangement: a) horizontal arrangement with a screw powder feed, b) vertical
              powder feed (bimetal), c) vertical powder feed (trimetal preparation) [7].
                                           A
        Processes occurring during powder rolling are shown in Fig. 6.14. In a region 1, there is a non-
compacted loose powder material. When passing into the second zone, characterized by an angle ,
the compacting process induced by friction between contra-rotating rolls and powder particles starts to
be performed. The applied forces reach the maximum values in the narrowest point between the rolls.
In contrast to rolling of compact materials, the acting pressure increases slowly at first.
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  Fig. 6.14 Powder in the rolling gap: region 1 – non-compacted powder, region 2 – zone of powder
                                            compaction [3].
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         Only at the end of the compaction zone the pressure increases as much that the running-out
strip has a satisfactory strength. A relation between a thickness ho and h1 can be expressed as follows:
                                         ho 2 R 1- cos α
                                            =            +1
                                         h1      h1
If neglecting a difference in a speed of powder inlet and strip running-out, a relation applies for the
powder density in the zone 1 (o – bulk density) and the rolled strip density 1:
011
                                        ρ1 2 R 1- cos α
                                           =            +1
                                        ρ0      h1
The value h1 represents the strip thickness, which must not be exceeded at the demanded density ratio
1 /o. It can only be varied by a change of a radius of rolls. The bulk density o is given by powder
properties. The same applies for the angle of repose  , moreover, it can be changed within a narrow
limits by roughing the rolls.
         When planning a technical arrangement of powder rolling, there is often a tendency to
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implement subsequent sintering of a green strip, further cold forming, annealing with a possible
further cold rolling into one technological line. However, owing to various speeds of individual
operations, it is sometimes more effective to perform these operations separately.
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         For powder materials which can be processed by casting and rolling into strips, rolling is
preferred because thin strips can be made with only low number of passes through the rolling stand.
However, a disadvantage is a higher price of the initial powder material and low rolling speeds,
therefore this process is always considered for individual respective cases.
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         The powder rolling technology is often the only possible way of processing for a manufacture
of porous strips or strips of special materials or those difficult to form. For example, this is the
manufacture of strips with special magnetic or electrical properties made of Al-Ni-Co or Cu-Ti alloys.
Further, this method is applied for the manufacture of coated strips for friction and sliding materials
(Fig. 6.13a) and bimetallic (Fig. 6.13b) or trimetallic strips (Fig. 6.13c).
        Isostatic pressing enables to reach higher densities of pressed materials (Fig. 6.15), to
manufacture components of larger dimensions and to process powders difficult to compress - e.g. a
manufacture of molybdenum rods.
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method – Fig. 6.16).
         When pressing smaller parts, substantially higher pressing outputs can be achieved in a device
called as a “system with a bolt closure with a dry sheath” (“dry bag” method – Fig. 6. 17). Powder is
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filled into a flexible tube an upper and bottom opening of which is connected to a pressing chamber.
Then the openings are closed and pressure is transferred through a liquid which encloses a flexible
sheath. After finishing the pressing and evacuating the chamber, the flexible sheath is moved to the
pressure housing walls and thus the compact is freed to be taken-out.
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Fig. 6.16 Principle diagram of the cold isostatic pressing – the ASEA system (isostatic press made by
                                      KOBE STEEL, LTD) [8].
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  Fig. 6.17 Principle diagram of the cold isostatic pressing – the dry bag method with a bolt closure
                          (isostatic press made by KOBE STEEL, LTD) [9].
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         The isostatic pressing is used mainly for compacts of larger dimensions and rotating shapes
from materials difficult to form. Products of SiN, ceramics and graphite, cemented carbides (rolls,
dies), molybdenum, tungsten, etc. can be obtained this way. Molybdenum and tungsten powders are
processed by this technology to consumable electrodes for arc remelting, which have a weight of 1 – 2
tons. A principle diagram of individual process steps of the dry bag cold isostatic pressing is depicted
in Fig. 6.18.
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                                              A
      Fig. 6.18 Principle diagram of individual process steps of the dry bag cold isostatic pressing [9].
separating a working area (high temperature application) from the steel pressure vessel a temperature
of which must not exceed c. 150 °C, so that tensile properties of the steel housing cannot drop (Fig.
6.19).
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          Argon is used as a medium for pressure transfer, while working with pressures up to 200 MPa.
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Non-porous sintered materials can be hot isostatic pressed without any further actions. Porous
compacts and powders have to be placed into a sheath of plate (commonly steel or titanium) or glass
and they are evacuated.
        Hot isostatic pressing makes use of a combination of elevated temperature and isostatic
pressing by gas. A principle diagram is depicted in Fig. 6. 20. Powder is placed into a flexible sheath
and vacuum degassed. The sheath is closed hermetically and inserted into the working area of a press.
Pressure is transferred through an inert gas or an auxiliary medium. While heating the container,
pressure is increasing. The sheath can be removed by machining (simple shapes) or acid leaching
(complex shapes) – Fig. 6.21.
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        The HIP technology is used e.g. for high-speed steels, Ti-alloys and superalloys. Its advantage
is a possibility of processing large sintered parts with very low (residual) porosity. For example, in
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cemented carbides the content of pores after pressing and sintering is 1 – 2 %. The powder compaction
to close-to-finished (near-net) dimensions allows reaching a high material utilization.
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                                            A
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                     Fig. 6.20 Particular steps during the hot isostatic pressing [7].
which a homogenous structure without pores and shrinkage holes can be obtained (Fig. 6. 22). An
advantage of this process, i.e. a combination of casting and HIP, is reaching higher static and
particularly dynamic strength, better ductility, better machinability with higher quality of a work-piece
surface, higher corrosion resistance as well as longer operating life of parts.
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a) b)
Fig. 6.21 Encasing of powder material (a) and the finished product after annealing and machining (b)
                                                [11].
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                             Fig. 6.22 Additional compaction of castings.
                                                         .B
         This technology combines powder metallurgy advantages with die forging processes. This
way quite complicated shapes with high density (up to 99.5 %) and product accuracy can be produced
(Fig. 6. 23). In general, either forging of a non-sintered compact (i.e. powder forging) or of a sintered
compact, mostly in a hot protective atmosphere, can be performed. Technological operations of
forging:
  a) preparation of a powder mixture – mixing of powder metal with pressing additives (lubricants,
     graphite, etc.);
  b) pressing of preforms;
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  c) heating in order to remove lubricant under a protective atmosphere;
  d) sintering (in the case of a sintered compact forging);
  e) forging;
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  f) finishing operations (heat treatment, smoothing etc.).
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 conventional pressing of metal powders. Usual systems cylinder – piston can be used, whereas an
 impulse is imposed on a punch either through a pressure wave or a shock wave of a steel cylinder set
 to motion by detonation of an appropriate explosive charge.
        This dynamic and high-energy process of forming enables enhancement of mechanical
properties of powder products.
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                 a)
                                                       .B      b)
                                          A
  Fig. 6.24 Principle diagram of the explosive compaction of powder materials (a) and the industrial
                           equipment for the explosive compaction (b) [13].
6.25.
D
             Fig. 6.25 Particular phases of the metal injection moulding technology [14].
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    (binder plastificatioon), injecting the melt into a mould under pressure of 15 – 30 MPa and cooling
    the mould down to solidify the powder and binder mixture (Fig. 6. 26). The compact is called a
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    “green body”.
                                                          .B
                                            A
  Fig. 6.26 Schematic depiction of the injection press and its main components: 1 – feed hopper, 2 –
  granulate, 3 – reciprocal screw, 4 – heating, 5 – a stationary half of a mould, 6 – a moving half of a
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                                   mould, 7 – melt, 8 – compact [15].
d) Binder removal – this is a key process, critical for product properties, therefore it requires very
                mm
   careful control. In this phase, “extraction” of the binder out of the compact occurs, after which a
   porous structure is formed, the so-called “brown body”. Time needed for the binder removal
   depends on the used method, a maximum thickness of a compact wall and a bonding system and
   can last up to several days. Basic methods of the binder removal involve the following: 1) thermal
   decomposition – heating a compact, so that the polymer binder can melt, decompose and ultimately
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Fig. 6.27 Change in colour of the compact after the particular processes: a) the compact after injecting,
            b) the compact after the binder removal, c) the sintered finished product [16].
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        MIM technology products are used mainly in applications for high-volume manufacturing,
where it leads to as much as 70 % production cost reduction. For example, these are applications for
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military industry (triggers, hammers, cartridge ejectors), in electronics for a manufacture of
complicated and precision parts for telecommunication, printers, copying machines, video recorders,
cameras, etc., in health service for scissors, parts of medical and dental instruments, in automotive
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industry for safety elements for airbag systems, fuel injection, turbochargers, etc. (see – Fig. 6. 28).
                                                           .B
                                             A
                          Fig. 6.28 Examples of MIM technology applications.
applied. Slurry is the more stable, the finer the powder is and the higher the viscosity of the liquid
carrier is (metal powder to liquid ratio 3:2). As metal powders are often coarser than ceramic ones and
viscosity cannot be increased with regard to casting, stabilizers play a decisive role for the slurry
preparation (e.g. sodium and ammonium salts of alginic acid). The stabilizers allow the slurry to be
processed prior to separation of the solid state suspension from the liquid and settling onto the bottom
of the mould. On the contrary, liquid separation from the suspended phase is necessary in a mould a
front side of which has to be permeated by a continuous capillary system which takes the liquid carrier
away.
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                                            A
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