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Module 3

Powder metallurgy: Metal powder- methods of preparation of metal powders – Powder


characteristics: properties of fine power, particle size, size distribution, shape, compressibility,
purity etc.- Mixing – Compaction techniques – hot pressing, powder rolling- pre sintering and
sintering- sintering atmosphere- Finishing operations: heat treatment, surface treatment,
impregnation treatment etc. – examples of articles produced and their applications.

MODULE – III

POWDER METALLURGY
INTRODUCTION

Powder Metallurgy is the process of making objects by the heat treatment of compressed metallic
powders. The process involves preparation of metallic powders and the subsequent welding of these
powders in to solid form of the required shape.
The basic operations involved in manufacture of parts using powder metallurgy are:
1. Preparation grading and blending of powders.
2. Pressing or compacting of powders.
3. Sintering of the compacted powders.

Sintering
Cold Compaction
Metal Powders Blending Secondary &
Finishing
Operation
Hot Compaction

Fig: Basic Steps of Powder Metallurgy

PREPARATION OF METALLIC POWDER

For making powder from metal, it is extracted from its ore or converted in to an oxide. There are many
methods of manufacturing powders.

1. Mechanical Pulverization – this method is applicable to brittle materials like antimony. Brittle
metals and alloys are powdered down to a size of 0.001 mm. many varieties of mechanical
pulverizes are in use; some of these have counter rotating plates or rapidly moving hammers. These
carry out the mechanical disintegration to the maximum fineness possible. Mechanical pulverization
is usually followed by ball milling. Other mechanical methods include Machining and Shotting.
Machining results in coarse particles which may be further milled and is usually used for magnesium
powders. Shotting is the operation of powdering molten metal through a sieve or orifice and cooling

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it by dropping it in to water. Spherical or pearl shaped particles are obtained by this process.
Shotting is usually used for metals like Aluminium, Lead and Zinc.

2. Electrolytic Process - this method is mostly used for the manufacture of copper, iron, tungsten,
tantalum, silver, zinc and even tin powders. This process uses a salt of metal. The conventional
electrolytic process is carried out and copper is deposited as a fine powder to the required degree of
fineness. The powder is scrapped from the electrodes and made to collect in the bottom of the vat
and periodically withdrawn when sufficient quantity is accumulated. The powder is washed and
dried. The electrolytic powder is quite resistant to oxidation.
The deposited material usually exists as a soft spongy dendrite structure. Additional crushing and
milling is necessary.

+ __

Powdered metal

3. Chemical Reduction - this process is commonly employed for some of the metals like tungsten
which have high melting points. For example, pulverized tungsten oxide is heated in a current of
hydrogen; the hydrogen reduces the oxide to metallic tungsten powder. Pure iron is made from iron
oxide or ores of iron such as magnetite or hematite. The powder formed by this process has particles
of a sponge like nature and it is ideal for cold pressing due to its softness and plasticity. The methods
like condensation and precipitation are also using. Carbon reduction method is widely used one.

For iron, the reduction is


heat
Fe3O 4 + 4 CO → 3 Fe + 4 CO 2

For Hydrogen reduction


heat
2 CuO2 + 4 H 2 → 2Cu + 4 H 2 O

4. Atomization- in this process, the molten metal is forced through a small orifice and broken up by
a stream of compressed air. Fine powder may be made by this process but it requires special nozzles
and careful control of temperature and pressure etc. oxidation can be prevented by use of an inert

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gas. If air is used little oxidation occurs, the particles get oxidized and form a thin protective coating
up on the surface thus preventing excessive oxidation from occurring. This process is used for metals
like tin, zinc, lead, aluminum, cadmium etc. which have low melting points. Alloy powders are also
produced by this method.
After powder is made it is washed before grading.
Further treatments- the product received by above process is crushed or grinded to reduce
to powder. Annealing is done to remove work hardening. Spherodising of particles for use in filter
achieved by allowing the powder to fall through heated space. The particles are then segregated into
their sizes ranges by screening.

POWDER PROPERTIES

Properties of metallic powder particles that are fundamentally responsible for behavior of
powder in pressing and sintering operations include particle size, size distribution, shape, surface
condition and the Physical characteristics of the metal itself.

1. Particle size and size distribution- particle size is one of the most important characteristics
of any powder. The most important method for measuring is to pass the powder through
screen (sieves) having definite number of meshes. Their size is commonly reported by
screening out the coarse, then the medium and then the fine particles and reporting as below.
66% - 100 to 200 mesh; 17% - 200 to 325 mesh; 17% - 325 mesh.
2. Physical and structural characteristics – the powder, as it is produced is loose and there is
considerable swell. When compacted in the die, it is reduced in volume as most of the voids
are filled up due to interlocking of the grains. The compression ratio(the ratio of the density
of the compact to the apparent density of the powder) varies between 2:1 and 3:1
(Apparent Density – the loading weight of powder may be considered to be the mass of
loosely heaped powder necessary to completely fill a given die cavity. In terms of weight to
volume, this is referred to as the apparent density)
3. Flow Characteristics- Flow ability of powders is most important in cases where moulds
have to be filled quickly. A measure of flow ability may be obtained by determining the
weight of powder which will flow through 0.8mm diameter orifice in one minute. Powders
with good flow may fill the mold uniformly. Particle size distribution, particle shape and the
coefficient of friction of the metal being handled excert considerable influence on flow
characteristics.
4. Surface area – this is the area per unit massof the powder. It indicates the area available for
bonding and also the area on which the adsorbed films or contaminates may be present. The
specific surface area is defined as the total surface area per unit weight. It depends on size,
shape, density and surface conditions of the particle. High specific surface not only results in
high sintering rate but also causes entrapment of air and bridging effects thereby causing the
compact to crack either before or during sintering.
5. Surface condition – oxides may present in powder and they greatly weaken the final product
by cold pressing. Chemical characteristics are depending on the purity, amount of oxides
permitted and the percentage of other elements allowed. Clean surface of particles is essential
for attaining desired mechanical properties.
6. Green Strength - Green strength of a powder is defined as the mechanical strength of a
green compact required to withstand, without damage to sharp edges and fracture

3.3
ADVANTAGES AND DIS ADVANTAGES OF POWDER METALLURGY

Advantages

1. Such parts which have special properties can be produced which otherwise cannot be
produced.
2. Machining operations are eliminated.
3. Scrap losses are reduced and often results in lower unit cost for a given part in comparison to
any other production method.
4. Metals and alloys can be mixed together in any proportion which is difficult and some times
not possible by melting.
5. Metals and non metals can be mixed together in any proportion.
6. There is better control of composition and structure of the component by this process.
7. Articles any desired porosity can be manufactured.
8. Super hard cutting bits, which can never be manufactured by any other methods are made by
powder metallurgy, eg. Sintered carbides, satellites.
9. This process is suitable for mass production because the stroke of the pressing or compacting
consists of a press at a speed of 60 strokes/ minutes.
10. Antifriction alloy strips made by powder metallurgy can be made to adhere on a strong alloy
backing piece.
11. The process is very economical and loss of material is lesser as compared to other processes.
12. Diamond impregnated tools for cutting porcelain, glass and tungsten carbides are made
possible only by powder metallurgy.

Disadvantages

1. Metal powders are very expensive and in some cases difficult to store without deterioration.
2. The equipments used for the operation are high.
3. Presses up to 100 tone capacity are used for even small products.
4. Dies used must be of high accuracy and capable of withstanding high temperature and
pressure.
5. Due to high compacting pressures required to press the powder, the wear on the dies is high.
6. Due to high rate of wear of dies, high costs for dies and presses the method is uneconomical
particularly for small runs.
7. Shapes that may be maid by this method are limited.
8. The physical properties obtained for the products are lower than those for the other.
9. In the low melting powders like tin, zinc and cadmium, sometimes certain thermal difficulties
occur.
10. Many metal powders are explosive at room temperature.
11. During sintering shrinkage occurs. So it is difficult to keep close tolerances.
12. Few metals cannot be compressed since they have the tendency to cold weld to the walls of the
die causing wear on the die.

APPLICATIONS OF POWDER METALLURGY

3.4
1. Porous Products- articles by powder metallurgy can be made with any degree of porosity.
Hence used for oil Impregnated bearings which are self lubricating.
2. Babbitt bearings for automobiles- Powder metallurgy techniques are employed for the
manufacture of Babbitt connecting rod and main bearings for automobile engines. The process
consists of applying a mixture of copper and nickel powders to a steel backing piece and
passing the same in sintering furnace. The copper will form a strong bond with steel backing
piece and nickel will alloy and form composite porous bearing material with the copper.

3. Oil Pump Gears- gears for automobile oil pumps are extensively manufactured by powder
metallurgy. Iron powder is mixed with graphite, compacted under a pressure of about 40
kg/mm2 and sintered in an electric furnace with an atmosphere of hydro carbon gas. Then
these gears are impregnated with oil and finishing operation is done. Only about 0.02 to 0.1
mm material is removed by machining.

4. Cemented Carbides- these are very important products of powder metallurgy and find wide
application in cutting tools, wire drawing dies and deep drawing dies. This consists of carbides
of titanium, tantalum and molybdenum.

5. Refractory metal composites- these materials being developed for service up to 1300oC,
consists of metals or alloys combined in various ways with ceramic oxides, carbides, nitrides,
borides and silicides.

6. Tungsten wires- wires for filaments in lamp industry are made by pure tungsten powder which
is pressed and sintered to form a bar of tungsten.

7. Diamond impregnated tools- these are made from mixture of iron powder and diamond dust.

8. Electrical contact materials- electrical contact materials are manufactured to produce


components with properties which cannot be obtained by any other known method. One type
of composite contact material combines the low contact resistance, current carrying capacity
and thermal conductivity of metals such as silver or copper. With hardness and compressive
strength of refractory metals such as W, Mo or Ta. These materials are used in applications
such as circuit breakers, relays and resistance welding electrodes. Cu –graphite brushes are also
made.

9. Magnetic materials- magnetic materials fabricated from powders include those of permanent
and soft magnetic characteristics. Alnicos are in permanent magnet category. These alloys are
difficult to cast and not machinable. Pole piece for dc motors or generators and cores for high
frequency inductance.

MIXING (BLENDING) OF POWDERS

Blending is an operation of thorough intermingling of different powders of the same composition or


various grades of the same powders, while mixing refers to the thorough intermingling of powders of

3.5
more than one material. However both terms are frequently employed interchangeably. Blending or
mixing is extremely desirable,
1. in the preparation of alloys from elemental powders.
2. in the production of dispersion strengthened alloys.
3. in the production of porous bearings.
4. in the production of electrical and magnetic materials.
Additives such as binders and lubricants are usually included in both types of process to facilitate
pressing and to achieve the required green strength and controlled porosity in the finished part. Both
these operations not only completely mingle the powder mix but also exert a grinding action on the
powder particles. These operations always precede compaction and can be carried out in the same type
of equipment.
Mixing of powders is most complex process, which relies on the movement of mass of one powder
component in to that of another powder component. This movement depends not only in the powder
material, particle size, particle shape and surface conditions but also on the environmental conditions.
i.e. temperature and atmosphere surrounding the particles.

PRESSING OR COMPACTION OF METAL POWDERS

The main object of pressing or compacting is to effect cold pressure welds between the particles so
that some cohesion is conferred, this is usually measured by the strength of the green compact and is
termed the green strength.
Compacting produces the following effects
1. Reduces voids between powder particles and increases density of compact.
2. Produces adhesion and cold welding of the powder and sufficient green strength.
3. Plastically deforms the powder to allow recrystallisation during subsequent heating.
4. Plastically deforms the powder to increase the contact areas between the powder particles,
increasing green strength and facilitating subsequent sintering.

• Pressing or compacting is carried out by pouring a measured amount of metal powder in to


the die cavity and then compacting the metal powder into coherent mass by means of one
or more plungers (fig 4-1). Compressing from both top and bottom of the (fig 4-2) compact
is better than from compacting from the top only, as pressure distribution and porosity
distribution are more uniform.

-The compacting pressure required depends on the characteristics and shape of the
particles, methods of blending and the lubrication. The pressure required for pressing metal
powders range from 70 MN/m2 for aluminum to 800 Mn/m2 for high density iron parts.

• In compacting powders in steel dies at room temperature, pressures from 7.5 kN/cm2 to
37.5 kN/cm2 are employed. Mechanical presses are employed for 500 kN and hydraulic
presses for higher pressures.
- Extremely hard powders slower and more difficult to press.
- In hot pressing if powder is heated to proper temperature the pressure for complete
densification is only 150 to 300 bars.

3.6
- Hot pressing requires die material having high strength. Since even sturdy dies
(made of graphite) usually sustain only one operation, therefore, hot pressing is
limited to the manufacture of articles of costly metals.

ISOSTATIC PRESSING

Isostatic Powder Compacting is a mass conserving, shaping process. Fine metal particles powdered
are placed into a flexible mold and then high gas or fluid pressure is added to the mold. The piece
produced is then sintered, which increases the strength of the part, in a furnace to bond the metal particles.
This manufacturing process produces very little scrap metal and can be made into different shapes. The
tolerances that this process can do are very precise, ranging from +/- 0.008 inches for axial dimensions
and +/- 0.020 inches for radial dimensions. This is the most efficient type of powder compacting.(The
following subcategories are also from this reference.) This operation is generally applicable on small
production quantities, as it is more costly to run due to its slow operating speed and the need for
expendable tooling.

Process Characteristics

• Compacts powdered metal withing a flexible mold by uniformly applied, high fluid/gas pressure
• Parts are sintered to increase strength through metallurgical bonding
• Produces very little scrap material
• Can use alloy combinations and filler
• Can produce complex workpiece geometries

Fig: Isostatic Powder Compaction

Hot Isostatic Pressing (HIP)

3.7
In this operation, the part is compressed and sintered simultaneously by applying heat ranging
from 900°F (480°C) to 2250°F (1230°C). Argon gas is the most common gas used in HIP because it is an
inert gas, thus preventing chemical reactions during the operation.

Cold (room-temperature) Isostatic Pressing (CIP)


This typically uses fluid as a means of applying pressure to the mold. After removal the part still
needs to be sintered.

POWDER ROLLING OR ROLL COMPACTING


In Powder rolling, the rolls are set directly above each other so that the strip emerges horizontally
or they are set side byside so that the strip emerges vertically downward. The powder is fed to the roll gap
in a two high rolling mill, and is compacted in to a continues strip at speeds of up to 0.5m/s . the rolling
process can be carried out at room temperature or at elevated temperature.
Sheet metal for electrical and electronic components and for coins can be made by this process.
Production of poros material suitable for fuel cell and alkaline batteries.

Loose
powder
Roll

Compacted powder

Hopper

Fig: Powder rolling or roll compacting

Advantages

1. it is possible to produce uniformly dense component of any required length, relatively large in
breadth and very thin.
2. The large pressing equipment employed in conventional die compation is not required there to
produce large products.
3. High productivity

SINTERING

3.8
It is the process of heating of pressed compact to below the melting temperature of any constituent
of the compact, or at least below the melting temperature of all principal constituents of the compact. Such
heating facilitates the bonding action between the individual powder particles and increases the strength of
compact. Heating is carried out in a controlled, inert or reducing atmosphere, or in vacuum to prevent
oxidation.
- Prior to sintering the compact is brittle and hence its strength known as green
strength is low. The nature and strength of the bond between the particles and hence
sintered product depend on mechanism of diffusion plastic flow, evaporation of
volatile materials in the compact, recrystallisation, grain growth and pure shrinkage.
- During sintering the bonding takes place in any of the following three ways
1. Melting of minor constituent
2. Diffusion
3. Mechanical bonding.
- Aluminum and its alloys can be sintered at temperatures from 350 to 500 oC for
periods up to 24 hrs.
- Copper and copper alloys can be sintered at temperatures ranging from 700 oC to
temperatures that may melt one of the constituent metals.
- Compacts of iron powders sintered at temperatures from 1000 oC to 1200 oC for
approximately half an hour.

• During sintering, ordinarily, the density of the compact is increased and shrinkage results.
Shrinkage fills the holes with in the compact.
• Sintering may be carried out in batches or continuously in batch type and continues
furnaces respectively it can be gas fired oil fired or electrically fired.

Fig 4.4

Table: Sintering Temperature and time for various metals

Material Temperature Time (min)


(oC)
Copper, Brass, bronze 760-900 10-45
Iron & Iron graphite 1000 - 1150 8-45
Nickel 1000 - 1150 30 – 45
Stainless steels 1100 - 1290 30 – 60
Alnico alloys ( for permanent magnets) 1200 - 1300 120 – 150
Ferrites 1200 - 1500 10 – 600
Tungsten carbide 1430 - 1500 20-30
Molebdenum 2050 120
Tungsten 2350 480
Tantalum 2400 480

The principle variables in sintering are temperature, time and the furnace atmosphere. Sintering
temperatures are generally within 70 to 90 % of the metal or alloy. Sintering temperature range from a

3.9
minimum of 10 minutes for iron and copper alloys to as much as 8 hours for tungsten and tantalum, table
given above describing the same. Continuous sintering furnaces used today have three chambers:
1. A burn off chamber for volatilizing the lubricants in the green compact, in order to improve
bond strength and prevent cracking.
2. A high temperature chamber for sintering.
3. A cooling chamber.

Sintering Mechanism
Sintering mechanism depends on the composition of metal particles as well as on the processing
parameters. As temperature increases, two adjacent particles begin to form a bond by “diffusion
mechanism” (solid state bonding). As a result strength, density, ductility, and thermal and electrical
conductivities of the compact increases. At the same time, however, the compact shrinks; hence,
allowances should be made for shrinkage as is done in casting.
Another mechanism is vapor- phase transport. Because the material heated to very close to its
melting temperature, metal atoms will release to the vapor phase from the particles. At convergent
geometries (the interface of two particles), the melting temperature is locally higher and the vapor phase
resolidifies. Thus the interface grows and strengthens, while each particle shrinks as a whole.
If two adjacent particles are of different metals, alloying can takes place at the interface of two
particles. One of the particles may have low melting temperature than the other; in that case one particle
may melt and because of the surface tension surround the particles that have not melted. “Liquid – phase
sintering”. An example is cobalt in tungsten carbide tools and dies. Stronger and denser parts ca be
obtained in this way. In this the concentration of the heavier components may be higher at the bottom
than at the top of the part because of the effects of gravity. In order to obtain a more uniform distribution,
experiments are being conducted in space shuttles under conditions of microgravity.
Another method, which is still at an experimental stage, is spark sintering. In this process, loose
metal powders are placed in a graphite mold, heated by an electric current, subjected to a high – energy
discharge and compacted, all in one step. The rapid discharge strips contaminants from the surface of the
particles and thus encourages good bonding during compaction at elevated temperatures.

PRE SINTERING
If a part made by p/m needs some machining (say drilling), it will be rather very difficult if the
material is very hard and strong. This machining operation can be made very easier by pre sintering
operation, which is done before sintering operation. The compact is heated to a temperature well below
the final sintering temperature. The compact will gain enough strength to be handled and machined
without any difficulty. After this, the part undergoes the final sintering operation.
Pre sintering is necessary when holes are to be drilled in hard machine parts. Pre sintering in
addition removes lubricants and binders added to the powders during the blending operation. Pre sintering
can be eliminated if no machining of the final product is desired.

SINTERING ATMOSPHERE
To obtain optimum properties, proper control of furnace atmosphere is important for successful
sintering. An oxygen free atmosphere is essential, to control the carburization and de carburization of iron
and iron based compacts and to prevent oxidation of powders. A vacuum is generally used for sintering
refractory metal alloys and stainless steel. The gases most commonly used for sintering a variety of other
metals are hydrogen, dissociated or burned ammonia, partially combusted hydro carbon Gases and
nitrogen.

3.10
There is a change in composition of the atmosphere before its introduction, which affects the properties of
the work being sintered. This is mainly due to,
1. The reaction of the constituents of the atmosphere amongst each other at the sintering temperature
2. The reactions of the atmosphere with material to be sintered
3. The reactions of the atmosphere with the furnace refractories.

Functions of Sintering Atmosphere

i). It must prevent oxidation on the metal surface at the sintering temperature otherwise it would inhibit or
interface with the sintering process.
ii). It must avoid carburizing and de carburizing reactions and nitriding conditions in certain metals.
iii). It must have the tendency to reduce surface films such as oxides on powder particles, if they are
present and remove or replace absorbed gases.
iv). It must not contaminate the metal powder compact at the sintering temperature.

The atmosphere which prevails in the various types of sintering furnaces are fall in to three groups:
1. Reducing atmosphere
2. Neutral atmosphere
3. Oxidizing atmosphere
The most widely used sintering atmospheres are reducing although inert atmosphere also finds some
applications. Reducing atmosphere may be devided in to three classes.
a). Dry hydrogen or dissociated NH3
b). Exothermic atmosphere having low or medium carbon potential
c). Endo thermic atmosphere enriched with hydrogen gas to produce a carbonizing atmosphere.
The choice of reducing atmosphere is made depending upon the articles to be sintered, the initial and
operating cost of the atmosphere generator.
Vacuum sintering is costly and therefore employed on a small scale in very special cases where it
is essential or research work.

SECONDARY OPERATIONS / FINISHING OPERATIONS

The sintered products are processes further to obtain better properties as follows.

Infiltration / Impregnation - porosity of the sintered products can be improved by process of infiltration,
in which pores are filled with low melting point metal by capillary action. In this a slug of lower melting
point metal is placed against the sintered part and then the assembly is heated to a temperature sufficiently
to melt the slug. The molten metal infiltrates the pores, by capillary action, to produce a relatively pore
free part having good density and strength. Eg. Copper is used as infiltrant to strengthen the iron and steel.
The advantages are that the hardness and tensile strength are improved and the pores are filled.
The inherent porosity of p/m components can be utilized by impregnating them with fluid. A
typical application is to impregnate the sintered part with oil, usually by immersing them in heated oil.
Bearings and bushings that are internally lubricated with up to 30% oil by volume are made by this
method. Such components have a continuous supply of lubricant, by capillary action during their service
lives. Universal joins are made by grease impregnated powder metallurgy techniques and no longer
require grease fittings.

3.11
The pores may be close by impregnation with oil, plastic, high melting point waxes or metal
Oil impregnation- is accomplished on sintered ferrous part and non ferrous bearing materials, which work
without supplementary lubrication.
Plastic impregnation- is the process of closing the voids with polyester or epoxy resins. PTFE may be
used as impregnate to improve the bearing properties of p/m parts.

Surface Treatment – It is to give bright smooth surface finish and in some cases to remove sharp corners
and control dimensions.
Phospahte coating- it consists of immersing the ferrous parts in an aqueous solution of phosphoric acid
with various metal phosphates, which completely penetrates any part with interconnected porosity. Since
treated surfaces are usually boiled before being put in to service. It is essential to remove the entire
processing solutions from the pores. The applied coating not only improves the wear properties of ferrous
parts but reduces the coefficient of friction and therefore the risk of galling and seizure (sticking on the
surface).
Steam Treatment- It consists of heating the p/m parts to about 450 to 570 oC and subjecting them to
superheated steam under a pressure of about 50 lbs/sq.inch for 30 minutes. The steam reacts with iron to
give an adherent layer of black magnetic oxide, Fe3O4 on all exposed surfaces whether they are internal or
external including inter connected porosity. The surface finish obtained is very good and increases the
hardness, wear and corrosion resistance, compressive strength, elastic modulus. It is a usual practice to
immerse the parts after this treatment in oil to further enhance the corrosion and wear resistance.
Sizing and coining- Accuracy and mechanical properties of sintered products are improved by cold
working. Sizing produces better dimensional accuracy with significantly increases the density and at the
same time also improves the mechanical properties, surface finish and dimensional accuracy.

Machining- sometimes sintered parts are finished by conventional machining when high degree of
accuracy is required.

Heat Treatment – A sintered part produced from a powdered heat treatable alloy or produced from a
mixture of metals that responds to heat treatment, can be heat treated to improve various properties.
Carburizing – This treatment is accomplished at conventional temperature in a controlled furnace
atmosphere of high carbon potential. The furnace atmosphere usually employed is the endothermic type
with dew point of 125oF. This atmosphere is enriched with a given amount of natural gas at the furnace to
provide nascent carbon for the carburization of p/m parts dependent up on the surface area of the load
being treated and the temperature employed. The parts after this treatment may then be quenched and
tempered to obtain high surface hardness. Pack carburizing and gas carburizing techniques are
examples.
Carbonitriding – Basically similar to carburizing. It consists of heating the sintered steel parts in a
mixture of endothermic gas with propane and ammonia. Since it is carried out at a lower temperature,
extra care must be taken to prevent the formation of carbide networks. It is used to produce higher
hardness and hardenability of case.

3.12
3.13

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