Module 2

INTRODUCTION
When the periodic and repeated arrangement of atoms is perfect and extends throughout the entirety of
the material without any interruptions, then the resulting crystal will be known as single crystal. All the
familiar crystalline solids are composed of a collection of many small crystals known as grains. Such
materials are termed polycrystalline. The individual grains are not perfect in the arrangement of atoms in
the crystal lattice. Many interruptions exist within the crystal. They are known as crystal imperfections or
defects. Grain structure and the defects develop during solidification of the liquid material.

SOLIDIFICATION OF CRYSTALLINE MATERIALS

Solidification of pure metals, also known as crystallisation is the transition from liquid state to solid state.
In the liquid state, atoms of any material will be in constant motion due to their high kinetic energy owing
to the high temperature.

Consequently, the atoms do not have any definite arrangement. However, when the temperature of the
molten metal is brought down, it is possible that some atoms, at any given instant, may group together.
These chance aggregates or groups are not permanent. They continually, break up and regroup at other
points. The life of the group is determined by the temperature and the size of the group. The higher the
temperature, the greater the kinetic energy of atoms and hence the shorter the life of the group. When the
temperature of liquid is sufficiently decreased, the atomic movement also decreases. This lengthens the
life of the group and also promotes the formation of more groups within the liquid. Such groups are
known as embryos.

Fig: Solidification process

UNDERCOOLING

As the temperature of the liquid metal drops, a stage is reached where the embryos and the surrounding
liquid co-exist. This temperature is known as the solidification point or freezing point. At this point, both
the liquid and solid states are at the same temperature and hence have the same kinetic energy for the
respective atoms. But there is significant difference in the potential energy. The atoms in the solid are
much closer together resulting in lowering of potential energy. Thus, solidification occurs with release of
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energy. The difference in potential energy between the liquid and solid states is known as latent heat of
fusion (or latent heat of solidification). However, at the freezing point, energy is required to establish a
surface between the solid and the liquid. In pure materials, at freezing point, insufficient energy is
released by the heat of fusion to create a stable boundary surface. Hence some undercooling (super
cooling) is necessary to form a stable solid region.

Homogenous Nucleation

At sufficiently low temperatures, nucleation occurs by the grouping of a few atoms from the liquid.
Nucleation of this type, originated with the support of undercooling is known as homogenous nucleation.
This kind of nucleation occurs uniformly throughout the liquid. The nucleus grows further by adding
more and more atoms to it which leads to a small solid region. Such stable solid regions within the liquid
are known as nuclei. Subsequent to the formation of nuclei, release of heat of fusion takes place and the
temperature will be raised to the freezing point again. But loss of heat to the surroundings lowers the
temperature again making more atoms to freeze. These atoms may attach themselves to already existing
nuclei or form new nuclei of their own. Thus the process of solidification continues apparently at constant
temperature till the entire liquid is transformed into solid.

Heterogeneous Nucleation

Nucleation is also facilitated by the presence of some impurity atoms, an inoculant (grain refiner), an
imperfection or a grain boundary. This type of preferential nucleation is called heterogeneous nucleation.
A much lower level of undercooling is sufficient for this type of nucleation to occur. Even the wall of the
container promotes heterogeneous nucleation. Addition of a grain refiner to molten metal can produce
fine grained grains. The grain refiners solidify earlier and form a large number of small solid particles in
the liquid. Solidification of the liquid is initiated by heterogeneous nucleation around these solid particles.

Dendritic Growth

During the process of solidification, each nucleus grows by attracting atoms from the liquid into the space
lattice. Crystal growth continues in three dimensions, the atoms attaching themselves in certain preferred
directions, usually along the axes of the crystal. This gives rise to the characteristic tree-like structure
which is called a dendrite. Since each nucleus is formed by chance, the crystal axes are pointed at
random, and dendrites growing from them will grow in different directions in each crystal.

From the crystal skeleton arms begin to grow in all directions. From the primary arms, secondary,
tertiary etc. arms begin to sprout, leading to the formation of a rather elongated skeleton. In the case of
metallic dendrites, these branches conform to a rigid geometrical pattern. The dendritic arms continue to
grow and thicken at the same time, until ultimately the space between them will become filled with solid.
Meanwhile the outer arms of one dendrite begin to make contact with those of neighbouring dendrites.

If the material is pure, there shall be no evidence of dendritic growth once the solidification is complete,
since all the atoms are identical. If the material is impure, dissolved impurities will often tend to remain in
the molten portion of the metal, which ultimately solidifies in the spaces between the dendrites. The areas
containing impurity will appear as patches between the dendrite arms.

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 Fig: Dendritic growth

Grains

Various stages in the solidification of a crystalline material are illustrated in the following figure. The
randomly formed nuclei will be having different crystallographic orientations. The nuclei grow into
crystals by the successive addition of atoms from the surrounding liquid. All these neighbouring crystals
(or grains) will be oriented differently due to their independent formation. As these grow, the outer arms
of the neighbouring crystals meet similar extremities of other neighbouring grains. Finally at a certain
stage, further growth outwards becomes impossible, the remaining liquid is used up in thickening the
existing dendrite arms and solidification will be completed. This independent formation of each crystal
leads to the irregular shape of the crystal. These crystals are commonly called grains.

A grain is a portion of the material within which the atomic arrangement is nearly identical. But the
orientation of the atomic arrangement may be different for adjoining grains. The area, along which the
grains meet is known as grain boundary.

Single Crystal & Poly crystals

When a liquid is cooled slowly in equilibrium with the surroundings, the solid that form contains tiny
crystals called grains. The number of grains formed during solidification depends on the number of
nuclei formed. If all nucleation sites except one are suppressed, the liquid solidifies into a single grain.
Single crystals show excellent high temperature properties because of the absence of grain boundaries.
When the liquid is normally cooled under equilibrium condition, there would be abundant nucleation sites
and the liquid solidifies into a large number of small grains. Although these grains look alike, the
crystallographic orientations are different and the orientation changes randomly from one grain to other.
Such a solid is called polycrystalline.

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Grain Size

The rate at which a molten metal is cooled when it reaches the freezing point affects the size of the crystal
which forms. A slow fall in temperature leads to a small degree of undercooling at the onset of
solidification. This promotes the formation of relatively few nuclei, so that the resultant crystal size will
be large. Rapid cooling on the other hand, leads to high degree of supercooling at the onset of
solidification. This results in the formation of a large number of nuclei and hence a large number of
crystals or grains smaller in size will be formed.

As the grain size is having effect on material properties, there are methods to control the nucleation
process and thereby the material properties. Grain size in materials is also controlled by the combination
of controlled deformation and thermal treatments, called thermo mechanical treatments.

Grain Shape

Nature of the container in which the liquid metal cools, will also affect the shape and number of grains.
The following figure shows the nature of the grains formed when solidification takes place in a large
mould (or container).

Fig: Grain growth

When the molten metal first strike the mould, the mould is cold and has a chilling effect. This results in
the formation of a large number of nuclei and consequently large number of fine grains along the surface
of the solidifying metal. As the mould is warmed up, the chilling effect is reduced, so that nuclei
formation is retarded as the solidification progresses. Thus the crystals formed towards the centre of the
mould will be larger in size. In the intermediate portion, the rate and nature of cooling are favourable to
the formation of elongated columnar grains.

Thus, ordinarily, three separate zones can be distinguished in an ingot solidified in a large mould:

 First zone is near to the mould walls where fine grains are observed,
 Followed by a zone of long columnar grains and
 The third zone towards the centre of mould having coarse, equi-axed grains.

If the mould is narrow, or longer, the equi-axed zone may be absent.

Similarly, metallic mould tends to produce a fine grained structure, while sand mould a coarse grained
structure.

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Also thin Sections are subjected to relatively larger rate of cooling, resulting in fine grains. A grain is
called equi-axed when it is having the same dimensions along the three co-ordinate directions.

Orientation of Grains

Usually, the grains formed are having random crystallographic orientations. But there are metallurgical
techniques with which the grains can be made oriented along some specified direction. As an example,
grains of iron oriented along the [100] direction have a higher magnetic permeability than any other
orientation.

Grain Boundary

The grain boundary in a polycrystalline material is a region of disturbed lattice of a few atomic diameters
wide. At some locations along the grain boundary, the atoms are so closer that they cause a region of
compression. In some other areas, the atoms are so far apart and lead to regions of tension. On moving
from one grain to another, the crystallographic orientation changes abruptly. This misalignment between
adjacent grains can be quantified by the angle between the respective crystallographic orientations as
shown in figure. When this misalignment is of the order of a few degrees (upto 10°) it is called as low-
angle grain boundary (tilt boundary). The high-angle grain boundary will have more mismatches in the
orientation.

Fig: Low angle and high angle grain boundaries

Effects on Dislocation and Creep

A high-angle grain boundary represents an area of lattice disorder between neighbouring grains. This can
be viewed as a group of immobile dislocations which forms a step or grain boundary ledge. As the angle
of mismatch increases, density of the ledge increases and the ledges are good sources of dislocation.
While a low angle boundary can be considered as a regular array of dislocations. Other moving
dislocations tend to pile-up at grain boundaries. These pileups introduce stress concentration ahead of the
slip planes and generate new dislocations in adjacent grains. As more slip planes are in operation near the
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grain boundaries, hardness will be higher near the boundary than at the centre. When the grain size is
reduced, the behavior near the boundary will also be felt at the centre of grain and the grains will have
uniform hardness. Simply, a fine grained material imposes more barriers to dislocation mobility (due to
the greater grain boundary area) and leads to higher strength and hardness. Effect of strain hardening will
also be greater in a fine grained material than a coarse one. Grain boundary sliding is a phenomenon
observed at temperatures above 0.5 Tm (Tm is the melting point in degree Kelvin). This becomes
prominent with increasing temperature and deformation occurs by sliding along the grain boundaries.
This phenomenon leads to creep in a crystalline material.

HALL - PETCH EQUATION

The Hall-Petch equation gives a general relationship between the yield stress and grain size of a material.

k
σ O=σ i+
√D
where σ O is the yield strength (the stress needed to cause plastic deformation),

D is the average diameter of grains,

σ i and k are constants for the material.

The equation is not valid for both very large and extremely fine grain materials. But it is applicable to
boundaries between different phases (like ferrite-cementite in pearlite) and twin boundaries. The Hall
Petch equation is valid for grains as small as about 50nm.

Problem:

The yield strength of mild steel with an average grain size of 0.05mm is 138 MPa. The yield strength of
the same steel with a grain size of 0.007 mm is 276 MPa. What will be the grain size of the same steel
with a yield stress of 207 MPa. Assume the Hall-Petch equation is valid and that the changes in yield
stress are due to changes in grain size.

Solution:

k
σ O=σ i+
√D
For a grain size of 0.05mm, the yield strength is 138 MPa; using Hall-Petch equation,

k
138=σ i + (1)
√0.05
For a grain size of 0.007mm, the yield strength is 276 MPa; using Hall-Petch equation,

k
276=σ i + (2)
√ 0.007
Solving eqn (1) and (2) we get,

k =18.4 MPa √ mm and σ i=55.5 MPa

Now for an yield stress of 207MPa,

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 k
σ O=σ i+
√D
18.4
⇒ 207=55.5+
√D
⇒ D=¿ 0.015 mm

CRYSTAL IMPERFECTIONS
In ideal crystals the atomic arrangement is perfectly regular and continuous throughout. But real crystals
are never perfect, lattice distortion and various imperfections, irregularity or defects are generally present
in them.

Many physical and mechanical properties are affected by the imperfection in the crystal.

The study of imperfections has two purposes:

1) A better understanding of how they affect metal properties.

2) Minimizing or eliminating these defects.

CRYSTAL DEFECTS / IMPERFECTIONS

POINT DEFECTS LINE DEFECTS SURFACE DEFECTS VOLUME DEFECTS

Vacancy defect Edge dislocation Grain boundary Cracks
Interstitial defect Screw dislocation Tilt boundary Stalking faults
Impurity defect Twist boundary
Electronic defects Twin boundary

Point defects

Point defect is one which is completely local in its effect. Introduction of a point defect into a crystal
increases its internal energy as compared to that of the perfect crystal. Some of the point defects are:

Vacancy defect:

Vacancies are simply empty atom sites. Vacancy defect is the defect caused due to the absence of atoms
or ions in some lattice points. Industrial process of annealing, homogenization, precipitation, surface
hardening, oxidation and creep, all involves the transport of atoms through the lattice with the help of
vacancies. Vacancies may occur due to the imperfect packing during original crystallization. It may also
occur due to thermal vibrations at elevated temperatures. The atoms surrounding a vacancy tend to be
closer together, thereby distorting the lattice planes.

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 Fig: Vacancy defect Fig: Schottky defect

Schottky defect is a type of vacancy defect where an atom or an ion is removed from a normal lattice site
and replaced in an average position on the surface of the crystal.

Interstitial defect:

It is the defect caused when an atom occupies a definite position in the lattice that is not normally
occupied in the perfect crystal. The interstitial atom may be either a normal atom of the crystal or a
foreign atom. Interstitial defect occurs in crystal whose atomic packing factor is low. The atoms
surrounding an interstitial defect tend to push the surrounding atoms farther apart, thereby distorting the
lattice planes.

Fig: Interstitial defect Fig: Frankel defect

Frankel defect is a type of interstitial defect where an atom or an ion is removed from a normal lattice site
and replaced in an interstitial site.

Impurity defect:

Impurities may be small particles embedded in the structure, or foreign atoms in the lattice. Impurity
atoms are introduced into the crystal structure as substitutional or interstitial atoms. Impurities may distort
the lattice. Impurity defects occur in metallic, covalent and ionic solids. It plays a very important role in
many solid state processes such as diffusion, phase transformation and electrical and thermal
conductivity.

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 Fig: Substitutional impurity Fig: Interstitial impurity

Electronic defects:

Electronic defects are the result of errors in charge distribution in solids. A vacancy or an interstitial
impurity may produce the excess or the deficit of positive or negative charges, by an excess of metal ions.

Line defects

The most important line defect is the dislocation. A dislocation may be defined as a disturbed region
between two substantially perfect parts of a crystal. The dislocation is responsible for the phenomenon of
slip, by which most metals deform plastically.
Dislocation occurs due to:
a) Growth accidents
b) Thermal stresses
c) External stresses
d) Phase transformations etc.

Fig: a dislocation

The two basic types of dislocations are:

(i) Edge dislocation
(ii) Screw dislocation

Edge dislocation:
An edge dislocation lies perpendicular to its burger’s vector. An edge dislocation moves in the direction
of the Burger's vector.

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 Fig: Perfect crystal Fig: Crystal with edge dislocation

The following figure shows how edge dislocation (D) gets glided along the slip plane under the action of
shear stress (S) and how the slip is caused by the movement of an edge dislocation.

Fig: Edge dislocation mechanism

Edge dislocation is useful in explaining slip in plastic flow during mechanical working.

Screw dislocation:
A screw dislocation lies parallel to its Burger's vector. A screw dislocation moves in a direction
perpendicular to the Burger's vector.

Fig: Screw dislocation

Speed of movement of a screw dislocation is less than that of an edge dislocation. The following figure
shows the mechanism of movement of screw dislocation.

Fig: Screw dislocation mechanism

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Screw dislocation is useful in explaining crystal growth as well as slip in plastic deformation.

Sources of Dislocation
A very large number of dislocations are necessary in a crystal to facilitate plastic deformation. These
dislocations are originated through different sources. One of the principal sources is those which appear
as a natural consequence of crystal formation and growth.

Fig: Frank Reed source of dislocation

Even in nearly perfect crystals there is an equilibrium concentration of imperfections including

dislocations. Though it provides the basic supply, it is only a minor source of supply of dislocations
actually needed for plastic deformation. Dislocation multiplication can also arise from condensation of
vacancies, by the cross slip mechanism or by creation of new dislocations from high angle grain
boundaries. Another source of dislocation is found in the process of deformation itself. Experimental
observations revealed that during plastic deformation, the dislocation density in the crystals increased by
two to six orders of magnitude depending upon the amount of deformation undergone by the crystal. This
indicates that there must be a mechanism of generating dislocations in a cold worked metal. One such
scheme by which dislocation could be generated from existing dislocation is known as Frank - Read
source.

Consider a segment of dislocation AB as shown in figure (a) of a dislocation lying in a slip plane (assume
the plane of the paper). A and B are points beyond which the dislocation does not lie on this slip plane.
This dislocation cannot grow beyond the end points A and B, due to various reasons. If a shear stress τ
acts on this slip plane, the dislocation bulges out and produces slip as shown in figure (b). For a given
stress, the dislocation line will assume a certain radius of curvature and the loop continues to expand
under increasing stresses. When the loop reaches a stage as in figure (d), the segments m and n will meet,
annihilate each other to form a large loop and a new dislocation segment PQ is formed as in figure (e).
Once the original loop moves into this stage, the loop can continue to expand and the segment PQ is in a
position to repeat the process. A Frank - Read source can operate continuously and produce an infinite
number of loops, provided the loops move out and disappear at the surface of crystal. However, if the

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loops are piled up against an obstacle such as grain boundary, back stresses may begin to build up at the
source and the source gradually dies out.

Surface defects (Planar or interfacial)

Grain boundaries:

A grain boundary is formed when two growing grain surfaces meet. A grain boundary is either:
 a perfect plane of grain contact
 or a layer of atoms crystallographically distinct from either grain
 or a transition region
It is a three dimensional surface. In grain boundaries the atomic packing is imperfect. At the grain
boundary between two adjacent grains there is a transition zone which is not aligned with either grain.
Grain boundaries in commercial metals are often wider, because impurities commonly concentrate at the
grain boundaries during solidification.

Fig: Grain boundary Fig: Tilt boundaries

Tilt boundaries:

It may be regarded as an array of edge dislocations. Tilt boundary is a type of low angle boundary (θ <
10°).

Twist boundaries:

It may be regarded as a set of screw dislocations. Twist boundary is also a type of low angle boundary.

Twin boundaries:

A Twin boundary separates two parts of crystal having the same orientation. They look like mirror image
of each other.

Volume defects

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Volume defects occur when there is only a small dissimilarity between the stalking sequences. The
stacking fault is a difference in the packing sequence of the layers of atoms. For example, instead of a
regular sequence ABCABC there may be a change as ABCACAB due to the stacking fault.

X RAY DIFFRACTION METHODS

It is the most useful tool for studying crystal structure. X ray diffraction methods give the details about:

a) Grain size or crystal size

b) Orientation of the crystals
c) Cold worked, distorted and internally stressed crystals
d) Recrystallization
e) Preferred orientation etc.

Bragg’s law

X rays are electromagnetic radiations that have high energies and short wavelengths. When a beam of x
rays impinges on a solid material, a portion of this beam will be scattered in all directions by electrons
associated with each atom or ion that lies within the beam’s path.

Fig: Bragg’s law

 Consider two parallel planes of atoms A-A` and B-B` which have the same miller indices and are
separated by inter planar spacing dhkl.
 Now assume that a parallel, monochromatic and coherent beam of X rays of wavelength λ is
incident on these two planes at an angle θ.
 The two rays (1 and 2) are scattered by atoms P and Q.
 Constructive interference of the scattered rays 1` and 2` occurs if the path difference between 1-P-
1` and 2-Q-2` (ie., SQ+ QT ) is an integral multiple of λ.
That is, condition for diffraction is:
nλ=SQ+ QT
nλ=d hkl sin θ+d hkl sin θ

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 nλ=2 d hkl sinθ
 This equation is known as Bragg’s law where n is the order of reflection.
 Bragg’s law is a necessary but not sufficient condition for the diffraction by real crystals. It
specifies when diffraction will occur for unit cell having atoms positioned only at corners of the
cell.

X ray Diffraction

Laue’s method Rotating crystal method Powder method

Laue’s back reflection method

Fig: Laue’s back reflection method

This method is used to determine the lattice structure of a metal by X ray diffraction. It is applicable to
single crystals or poly crystalline masses. When a narrow beam of monochromatic x rays is incident on
the specimen of a metal, diffraction takes place. The resultant image is recorded on a photographic film as
a series of spots. The pattern thus created helps to interpret the crystal structure of the metal.

S No STATE OF METAL BACK REFLECTION PHOTOGRAPH

1 Coarse grains > 0.04mm Few clear spots
2 Fine grains 0.004mm Large number of spots in ring
3 Very fine grains 0.0004mm Continuous rings, double resolved
The spots are more irregular in outline and shape.
4 Cold worked
Cold work causes spots to arc and widen radially.
5 Distorted crystal

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Rotating crystal method

Fig: Rotating crystal method

 A single crystal is mounted on a rotating spindle such that one of its crystallographic axes
coincides the axis of rotation.
 Now a monochromatic beam of X ray is incident on the crystal perpendicular to the axis of
rotation.
 The crystal positioned at the centre of a cylindrical holder. A photographic film is attached at the
inner circular surface of the cylinder.
 Diffraction takes place from those planes which satisfy Bragg’s law for a particular angle of
rotation. The planes parallel to the axis of rotation diffract incident rays in a horizontal plane.
 If a crystal is positioned such that its c- axis coincides with the axis of rotation, all the planes with
miller indices of the type (hk0) will produce the centre line.
 Planes having the miller indices of the type (hk 1∧hk 1) will produce the layer lines above and
below the centre line respectively and so on.
 The vertical spacing between the layer lines depends on the distance between the lattice points
along the c-axis. Hence the distance c can be measured from the photographic film.
 Similarly a and b can be determined by mounting the crystal along a-axis and b-axis respectively.
Thus dimensions of the unit cell can be easily determined.

Powder method (Debye-Scherrer method)

 It is the most widely used diffraction method to determine the structure of cryatalline solids.
 The sample used is in the form of a fine powder containing a large number of tiny crystallites with
random orientation.
 The experimental setup is shown in the figure.

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 Fig: Front view of Debye Sherrer camera

 It consists of a cylindrical camera called Debye Sherrer camera whose length is small as compared
to the diameter.
 The finely powdered sample is filled in a thin capillary tube and mounted at the centre of the
camera. The capillary tube should be of a diffracting material.
 A collimated beam of monochromatic X-rays is produced by passing the X-rays through a filter
and a collimator.
 The collimated beam enters the camera through the collimator and strikes the powdered sample.
 Since the specimen contains a large number of small crystallites, with ramdom orientation, almost
all the possible θ and d values are available.
 Diffraction takes place for those values of θ and d which satisfy the Bragg’s law (2d sinθ = nλ).
 The diffracted rays corresponding to fixed values of θ and d lie on the surface of a cone with its
apex at the sample and the semi vertical angle equal to 2θ.
 Different cones are observed for different sets of θ and d for a particular value of n, and also for
different combinations of θ and n for a particular value of d.
 The transmitted X-rays move out of the camera through an exit hole located diametrically
opposite to the entrance hole.
 A photographic film is attached to the inner side of the curved surface of the camera.
 Each cone of the reflected beam leaves two impressions on the film in the form of arcs on either
side of the exit hole with their centres coinciding with their holes.

Fig: Flattened photographic film after developing and indexing of diffraction lines.

 Similarly cones produced by back reflected X-rays produce arcs on either side of the entrance
hole.
 The photographic film is exposed for a long time, removed from the camera and developed.
 The arcs produced by the reflected rays appear dark on the developed film.
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  The angle θ corresponding to a particular pair of arcs is related to the distance S between the arcs
as:
S
4 θ(radians)=
R
S
4 θ(degree)=57.296
R
Where R = radius of the camera.
 We know that the condition for diffraction is 2d sinθ = nλ. Knowing all possible values of θ and
λ
considering only first order reflections, we have d= .
2 sin θ
 These d values are used to determine the space lattice of the crystal structure.

METALLOGRAPHY
Metallography is the study of metals and their behaviour, with considering their microstructure and
macrostructure.
Microstructure is the characteristic appearance and physical arrangement of a metal as observed with a
microscope.
Macrostructure is the characteristic appearance and physical arrangement of a metal as observed with the
naked eye or with a low power magnification.
Microstructure and Macrostructure of a metal or an alloy are closely interrelated with each other and
knowledge of both is essential for full understanding of any metal.

METALLURGICAL MICROSCOPE
A metallurgical microscope helps determining:
 Grain size and shape.
 Size, shape and distribution of various phases and inclusion.
 Mechanical and thermal treatments of the alloys.
A metallurgical microscope works on the principle of examination by light reflected from the specimen
surface.
A typical metallurgical microscope is shown in the figure.

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 Fig5.1: Metallurgical microscope
Construction
The main parts of a metallurgical microscope include:
 Body tube
 Eye piece
 Objective
 Draw tube
 Plane glass reflector
 Coarse adjustment knob
 Fine adjustment knob
 Light source etc.
The eye piece is carried by the draw tube. Now the draw tube carrying the eyepiece slides over the
body tube with the help of a rack and pinion mechanism. It is done by adjusting the coarse and fine
adjustment knobs. Sliding of draw tube within the body tube varies the distance between the eyepiece and
the objective and thus helps focussing the object. Fine adjustment is done for final focussing of the object.
The objective resolves the image and eyepiece magnifies it.
Eyepieces are made in a variety of powers such as X5, X8, X10 etc. The source of light is inside
the microscope tube itself. Light is diffused with the help of a diffusing disc. The width of the light beam
is controlled by the iris diaphragm. The incident light strikes the plane glass reflector kept at 45° and is
partially reflected down onto the specimen. The rays of light get returned by reflection from the
(polished) specimen, pass through the objective and glass reflector to form the final image which can be
seen through the eyepiece.
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 A photographic camera may be mounted above the eyepiece in order to record permanently the
metallographic structure of the alloy. The maximum magnification obtained with the optical microscope
is about 2000X.

SPECIMEN PREPARATION
Specimen preparation is necessary to study its microstructure, because the metallurgical microscope
makes use of the principle of reflection of light from the specimen to obtain the final image of the metal
structure.
Satisfactory metallographic results can be obtained only, when the specimen has been carefully prepared.
A properly prepared metal specimen:
 is flat
 does not contain scratches
 is nicely polished and
 is suitably etched
Procedure
Selection of specimen:
The specimen should be selected from that area which can be taken as representative of the whole
mass.
Cutting of the specimen:
After selecting a particular area in the whole mass, the specimen may be removed with the help of
a saw, a trepanning tool, an abrasive wheel, etc.
Mounting the specimen:
If the specimen is too small to be held in hand for further processing, it should be mounted in
thermoplastic resin or some other low melting point alloy.

Fig: Mounting of the specimen

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Obtaining flat specimen surface:
It is first necessary to obtain a reasonably flat surface on the specimen. This is done by using a
fairly coarse file or machining or grinding, by using a motor driven emery belt.
Intermediate and fine grinding:
Intermediate and fine grinding is carried out using emery papers of progressively finer grade. Four
grades of abrasives used are: 220 grit, 320 grit, 400 grit and 600 grit (from coarse to fine).
The specimen is first ground on 220 grit paper, so that scratches are produced roughly at right angle to
those initially existing on the specimen and produced through preliminary grinding or coarse filing
operation. Having removed the primary grinding marks, the specimen is washed free of No. 220 grit.
Grinding is then continued on the No. 320 paper, again turning the specimen through 90° and polishing
until the previous scratch marks are removed. The process is repeated with the No. 400 and No. 600
papers. The surface of the abrasive paper shall be lubricated with water to carry away the particles cut
from the surface.

Fig: Intermediate and fine grinding

Rough polishing:
A very small quantity of diamond powder (size - 6 microns) carried in a paste that is oil-soluble is
placed on the nylon cloth covered surface of a rotating polishing wheel.

Fig: Rough polishing

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The lubricant used during the polishing operation is a specially prepared oil. The specimen is pressed
against the cloth of the rotating wheel with considerable pressure and is moved around the wheel in the
direction opposite to rotation of the wheel to ensure a more uniform polishing action.

Fine polishing:
The polishing compound used is alumina power (with a particle size of 0.05 microns) placed on a
cloth covered rotating wheel. Distilled water is used as a lubricant. Fine polishing removes fine scratches
and very thin distorted layer remaining from the rough polishing stage.

Fig: Fine polishing

Etching:
Even after fine polishing, the granular structure in a specimen usually cannot be seen under the
microscope; because grain boundaries in a metal have a thickness of the order of a few atom diameters. In
order to make the grain boundaries visible, after fine polishing the metal specimens are usually etched.
Before Etching, the polished specimen is thoroughly washed in running water. Then, the etching is done
either by immersing the polished surface (of the specimen) in the Etching Reagent or by rubbing the
polished surface gently with a cotton swab wetted with the Etching Reagent. After etching, the specimen
is again washed thoroughly and dried. Now, the specimen can be studied under the microscope.
TYPE OF ETCHANT USES
For etching steels, grey cast iron & black heart malleable
Nital
iron.
Acid ammonium persulphate For etching stainless steels
Ammonia hydrogen peroxide For etching copper, brasses and bronzes
Dilute hydrofluoric acid For etching aluminium and its alloys
Keller’s reagent For etching duralumin type alloys
Mixed nitric & acetic acids For etching nickel and monel metal

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