You are on page 1of 8

3.

0 CRYSTAL IMPERFECTIONS (LATTICE DEFFECTS) & MICROSTTRUCTURE

INTRODUCTION
In real life, crystals depart from the ordered arrangement considered in chapter two. It is
these imperfections that dictate most engineering properties of materials (ductility, strength,
heat treatability, electrical conductivity, semi-conductor properties, creep strength, etc.). The
imperfections are caused by several factors:

1) imperfect packing during crystallization,


2) due to thermal vibrations, an atom may jump out of its equilibrium position,
3) during working processes, especially those involving plastic deformation,
4) the presence of impurity atoms,
5) in the case of ionic crystals, by the need to produce a charge balance. An example is FeO -
since ferrous contains some Fe3+ ions, excess O2- are required than suggested by the formula.
To balance the charges, some Fe2+ sites must be empty.

Some of the defects that may occur are given below.

CRYSTAL DEFECTS

Thermal Disorder
Atoms are continuously vibrating about their equilibrium point. The magnitude of vibrations
increases with rise in temperature resulting in a net increase in inter-atomic distance (i.e., a
departure from equilibrium spacing). Macroscopically, this manifests itself as thermal
expansion.

Point Defects
These are zero dimensional interruptions in the regularity of the crystal lattice ( i.e.,
interruptions of 1 atom magnitude in all directions). The main point defects are:

1) vacancy -- occurs when a lattice point, which should normally be occupied by an atom, is
empty. Also called Schottky defect.
2) interstitial atom (self interstitial or interstitialcy) -- occurs when a lattice point, which
should normally be vacant, is occupied by an atom similar to the rest. Also called Frenkel
defect.
3) substitutional impurity atom -- in this case, an atom of another element occupies a lattice
point normally occupied by an atom.
4) interstitial impurity atom -- similar to case 3 above but the impurity atom occupies an
interstice.

b
c
d

Point defects (a) Substitutional, (b) self interstitial atom (c) Vacancy (d) Interstitial impurity

1
It is found in practice that all materials have an equilibrium number of defects 1 and 2 at any
temperature above absolute zero. This suggests that a lower energy is associated with an
imperfect crystal than with a perfect one. Now, the total change in free energy of a system,
ΔG, depends on both the change in enthalpy, ΔH, and the change in entropy, ΔS i.e., :

ΔDG = ΔH - TΔS

In order to create one vacancy, energy = ED is put into the system to remove an atom from a
lattice site to the surface. This increases the enthalpy of the system. But when an atom is so
removed, the system becomes disordered -- thus increasing the entropy. Both effects increase
with increase in the number of vacancies as shown in figure below. The equilibrium
concentration of vacancies Ce corresponds to the point of minimum free energy and is given
by Boltzmann's equation:
Energy

ne

ΔG

-TΔS

Schematic representation of the variation of free energy wit the number of point defects

n -E
e D
C = = A exp
e N kT

where A = 1, N = number of lattice sites, T = absolute temperature and k = Boltzmann's


constant.

In metals, the value of ED to create a vacancy is much higher than that to move an atom into
an interstice (the packing is close hence the interstices are small) and hence there are many
more vacancies than intestitialcies. In ionic crystals, either may dominate: vacancies in close
packed structures and intestitialcies in low packed structures.

2
Line Defects (Dislocations)
These are one dimensional (i.e., about 1 atomic spacing wide but several atomic spacing
long) interruptions in the regularity of the lattice. The two known types are the edge and
screw dislocations.

Edge dislocation: In this case, an extra 1/2 plane of atoms is fitted in the lattice as shown in
figure below. This may be considered as due to a slip wave moving along the crystal. The
dislocation line AD is the edge of the slipped region i.e., the line separating the slipped from
the un-slipped portion. An edge dislocation is shown in diagrams with the symbol I (for a
positive dislocation i.e., one in which the extra 1/2 plane is above) and I (negative
dislocations). Edge dislocations of the same sign repel while those of opposite signs attract
each other.

Edge dislocation

Dislocations are identified by their "Burgers vector", b, which is the magnitude and direction
of the slip resulting from the motion of a dislocation. The Burgers vector can be determined
by doing a "Burgers circuit" around the dislocation as follows:

Illustration of Burger’s vector determination by plotting a Burger’s circuit for an edge


dislocation

i) draw a circuit around the dislocation jumping from atom to atom and count the number of
jumps in each direction, until the circuit closes.
ii) repeat a similar circuit taking a similar number of jumps in each direction around an un-
slipped portion of the crystal. This time the circuit does not close. The magnitude and
direction of the "step" required to close the circuit equals Burgers Vector.

We notice that the Burgers vector of an edge dislocation is perpendicular to the dislocation.
This is the distinguishing characteristic of the edge dislocation.

3
Edge dislocations can glide (i.e., slip in direction of the Burgers Vector) but this takes place
only in preferred planes and directions (called slip planes and slip directions). They may also
climb (i.e., move in a direction perpendicular to the Burgers vector) if the line of atoms
immediately above it are removed. Climb is always slower than glide since it (climb)
involves diffusion of atoms/vacancies.

Screw dislocation results from atoms being displaced in two separate planes perpendicular to
each other. The result is a shearing action. Doing a Burgers circuit as explained above, we
notice that the Burgers vector is parallel to the dislocation. We also notice that the Burgers
circuit traces the path of a right hand screw -- hence the name screw dislocation.

Fig. A mixed dislocation. The screw dislocation at the front face of the crystal
gradually changes to an edge dislocation at the side of the crystal.

Screw dislocations also glide but there is no preferred plane hence their glide is easier than
those of edge dislocations. Further, no climb is possible with the screw dislocation.

Most dislocations are a mixture of edge and screw dislocations and all are zones of stress
(tension on one side and compression on the other) and therefore represent areas of high
energy.

Dislocations can be defined as narrow or wide - the width being that distance over which the
displacement of atoms exceeds b/4. A dislocation in which |b| = one lattice spacing is
termed a unit or perfect dislocation. Dislocations with other widths are imperfect - those with
|b| < a are called partial dislocations while those with |b| > a are termed super dislocations.

The density of dislocations is defined as the total length of dislocations in a unit volume.
This is equivalent to the number of dislocations piecing a unit area and is approximately
8 2
10 /cm . It is found from experiment that when a material is plastically deformed, the density
of dislocations rises. This happens by a multiplication mechanism termed Frank Reed Source.

Planar Defects
These are two dimensional breaks in the regularity of a lattice and include:

4
Grain boundaries: in polycrystalline materials, each crystal is called a grain. An area of
mismatch between two grains, usually approximately 3 atoms thick is the grain boundary
(orientation based boundary). Grain boundaries may also be composition based, i.e., the area
between phases in multiphase systems or result from differences in the size of crystals.

Grain Boundary

Grain boundary atoms are less packed than the rest of the crystal and are therefore high
energy areas. In orientation based boundaries, the energy varies with the angle of orientation
θ as:

E = Eol(A - lnθ)
where Eo and A are constants and l is the length of the boundary. Boundaries associated
with high values of θ are high angle grain boundaries while those with low values of θ are
low angle boundaries.

In an attempt to reduce the grain boundary area, systems try to reduce the grain boundary
area by:

i) grain growth or coarsening (in single phase systems)


ii) spherodization (multiphase systems)
iii) partial coarsening

Surfaces: the atoms on the surface do not have neighbours on one side and hence represent a
break in the lattice continuity. Their higher energy is exemplified by effects like surface
tension and adsorption effect.

Surface atoms

Tilt Boundaries: Also referred to as low angle boundary as the orientation difference between
two neighbouring crystals is less than 10o. It is composed of edge dislocations lying one
above the other along a boundary:-

5
Tilt boundary

Twin interfaces: a crystal is twined if one part is a mirror image of the other. The plane of
symmetry (the twinning plane) represents the discontinuity.

Twin Boundary

Stacking faults
Another type of crystalline defect which exhibits surface dimensions is the stacking fault.
This imperfection consists f a disruption of the orderly sequence of stacking of close-packed
planes n close=packed crystal structures, such as FCC and HCP. Two representations of the
stacking fault in FCC structures are illustrated in the figure below. An intrinsic fault, one in
which part of a layer (plane) of atoms is missing from the natural stacking sequence of the
lattice. This is shown in part (a). An extrinsic fault consists of an extra partial layer between
planes as illustrated in (b)

6
Schematic representation of stacking faults

Stacking fault may be produced by two different mechanisms. First, if the growth of the
crystalline structure during solidification is disturbed and a new layer starts incorrectly, it
may be incorporated into the structure due to rapid freezing. Such a sequential imperfection
is termed a growth fault. A second mechanism involves the dissociations of a dislocation
into two partial dislocations, producing a configuration known as an extended dislocation.
The stacking in the region between the two partial dislocations is disrupted (A-B is converted
to A-C) and this condition is termed a deformation fault.

MICROSTRUCTURES

Introduction:
A microstructure refers to the structure and arrangement of several grains and is
characterized for each material by the grain size, shape, and orientation. The size of grains
may vary from less than microscopic to several centimeters. Microstructures have a direct
bearing on material properties hence their importance.

Preparation of Microsections
Before a microstructure can be observed under the microscope, it has to be prepared. The
stages in the preparation are: sectioning, mounting, identification, grinding, polishing,
cleaning and etching. Care is needed in all stages to ensure that no changes in microstructure
are produced by the preparation process. In particular, all processes generating heat and/or
pressure are to be avoided or controlled.

Sectioning: a portion which is representative of the material is selected and sectioned off. If
methods likely to cause recrystallization, tempering, etc., (e.g., gas cutting, sawing or
grinding) are used, the cut is made far enough. Usually, the final sectioning is done using
abrasive wheels (bonded Al2O3 or SiC) under running water.

7
Mounting and identification: small or irregular sections are mounted in resin for ease of
handling (also called plastic embedding). The mounted specimens are then engraved for
identification.

Grinding: the purpose is to remove the deformed material and render the surface reflective
and plane. Usually, coarse grinding is done using abrasive mounted on paper or cloth and
attached to a rotating wheel. Running water is continuously passed over the wheel for cooling
and for removing loose particles. Fine grinding, again under running water, follows on
successively finer grains of silicon carbide paper. To avoid directional effects, the specimen
is rotated by 90° after every stage. To wash off particles from the coarser grades of paper,
the specimen is held under running water after every stage.

Polishing (Mechanical): this is done, to produce a mirror finish on the specimen, using a
special cloth attached to a rotating wheel. Abrasive, in the form of powder or paste (diamond
dust, Al2O3, chromic oxide, etc.) is used on the moist cloth and the specimen is rotated
opposite to the rotation of the wheel to avoid directional effects.

Polishing may also be done electrolytically (anodic polishing) or chemically. After


polishing, the specimen is dried rapidly by rinsing in alcohol (which will dissolve any water
including those in the pores/scratches) then blowing with hot air.

Etching is done to impact different appearances to different constituents of the microsection.


It involves selective chemical corroding to produce shades of varying decrees. The specimen
is immersed in the etching solution for a given time (important) and then washed in running
water, rinsed in alcohol, and dried in hot air. For cast iron and steel, the usual etching agents
are nital (2% solution of nitric acid in alcohol) and solution of picric acid in alcohol.

The method of preparation described here involves manual processes. Later developments
are available in which most of the processes are automated.

The Metallurgical Microscope


Prepared microsections are observed in the metallurgical microscope whose distinguishing
characteristic is that it employs the principle of reflected light. In using the microscopes,
start from the lowest magnification and progress to the highest.

For long life of the microscope, the optical system must be kept free of dust and the lenses
should not be touched.

Macro-examination and Sulphur Printing


Macro-examination refers to examination with naked eye or under low power of the
microscope. It is useful in failure analysis (determining type of failure e.g., fatigue);
determination of manufacturing defects (slags, blow holes, lack of fusion, non-uniform
segregation, etc.); physical defects (laminations, pipes).

Sulphur printing reveals the presence of sulphur (an impurity) in steels. Sulphur reacts with
acid to evolve hydrogen which affects bromide (photographic) paper. The photographic
paper is soaked in dilute H2SO4 and placed on the selected surface. If the steel contains
sulphur, hydrogen will be evolved and the photographic paper will be affected.