MODULE 2
Crystallization
Temperature
Freezing point
Time
Crystallization
Temperature
Undercooling
Time
Crystallization
Liquid state Crystalline state
Crystallization
⦿ During solidification of liquid crystalline
materials, atoms become highly organized to
form crystals.
⦿ The kinetic energy of atoms in liquid state is
dissipated as heat energy on solidification.
Crystallization
Crystallization
Crystallization / Solidification process –
⦿ Nucleation – refers to the initial stage of
formation of crystalline phase from an
undercooled liquid.
⦿ Crystal growth – increase in the size of
nuclei particles to form dendrites, and finally
resulting in the formation of grains separated
by grain boundaries.
Crystallization / Solidification process –
TEMPERATURE
Nuclei
Dendrites
Nucleation
Nucleation
TEMPERATURE
Molten metal
Nucleation
Solidified metal
Nucleation
TEMPERATURE
impurities
Molten metal
Types of nucleation –
Homogeneous nucleation Heterogeneous nucleation
Nuclei forms at container
Nuclei forms uniformly surfaces, insoluble impurities,
throughout the liquid phase. grain boundaries,
dislocations, grain refiners.
A low level of undercooling is
Nucleation is originated with
required to initiate this type of
the support of undercooling.
nucleation.
Crystallization / Solidification process –
Crystallization / Solidification process –
Dendrites
Crystallization / Solidification process –
⦿ Grain is a portion of the solidified crystal within
which the atomic arrangement is identical.
⦿ The area along which two adjacent grains meet
and provides a mismatch in its orientation is
called grain boundary.
Grain boundary
Grain
Effect of grain size and grain boundary on the
strength of the material –
Effect of grain size and grain boundary on the
strength of the material –
Effect of grain size and grain boundary on the
strength of the material –
If the angle is
greater than 10º,
it falls under high
angle grain
boundaries.
Effect of grain size and grain boundary on the
strength of the material –
⦿ As the grain size decreases, the number of
grain boundaries will be high.
⦿ Finer the grains, more will be the strength of
the material.
⦿ Finer grains are promoted by the formation
of large number of nuclei after undercooling.
Effect of grain size and grain boundary on the strength
of the material –
The amount of nuclei formation (or size of grains) can
be controlled by the following methods.
⦿ Rate of undercooling – Rapid rate of cooling leads to
the formation of large number nuclei or fine grains.
⦿ Shape of container – Narrow containers promote fine
grains whereas wide containers promote coarse
grains.
⦿ Metal inserts and grain refiners – External metallic
inserts or chills and grain refiners act as nuclei
formation sites and promote formation of fine grains.
Effect of grain size and grain boundary on the strength
of the material –
⦿ Shape of container – Narrow containers promote fine
grains whereas wide containers promote coarse
grains.
1 – Fine grains
2 – Coarse grains
3 – Columnar grains
3 1 2
Hall-Petch equation
⦿ Mathematical relationship between the yield
strength of the metal and its grain size.
⦿ As the grain size (diameter of grain) decreases,
the yield strength increases.
Imperfections in crystals
Defects
Volume
Point defects Line defects Surface defects
defects
Edge
Vacancy defect Grain boundaries
dislocation
Interstitial Screw
Tilt boundaries
defect dislocation
Substitutional Twin boundaries
impurity
Interstitial
impurity
Frenkel defect
Schottky defect
Vacancy defect
⦿ Vacancies are empty spaces created in the
lattice when atoms are missing from its
regular positions.
Lattice site
Void / interstitial site
Interstitial defect
⦿ A self interstitial atom is an extra atom that
has moved into an interstitial void in the
crystal structure.
Impurity atom
⦿ It is an atom of a different type than the
parent atoms, which has entered into the
lattice of parent crystal structure.
Substitutional impurity atom Interstitial impurity atom
⦿ Frenkel defect occurs when an ion leaves its
original lattice position and occupies an
interstitial position.
⦿ Schottky defect occurs when a pair of cation
and anion leaves their lattice points and
creates vacancies.
Line defects or dislocations
⦿ Lines along which whole rows of atoms in a
crystal are arranged differently.
⦿ The direction and magnitude of such
distortion is expressed in terms of a Burgers
vector (b).
⦿ Two types – edge dislocation and screw
dislocation.
Edge dislocation
Burgers vector or direction of distortion is
perpendicular to the dislocation line (𝑏 ⊥ AB).
Edge dislocation
Edge dislocation
Burgers vector or direction of distortion is
perpendicular to the dislocation line (𝑏 ⊥ AB).
Screw dislocation
Burgers vector or direction of distortion is parallel
to the dislocation line (𝑏 ∥ PS).
Frank-Read Source of Dislocation
⦿ Mechanism explaining the generation of
multiple dislocations in slip planes in crystals
under deformation.
A B
A B
A m n B
Frank-Read Source of Dislocation
⦿ Mechanism explaining the generation of
multiple dislocations in slip planes in crystals
under deformation.
A m n B
P Q
Frank-Read Source of Dislocation
⦿ Mechanism explaining the generation of
multiple dislocations in slip planes in crystals
under deformation.
P Q
P Q
Climb
⦿ Occurs when a complete row of dislocation
atoms of an edge dislocation moves out of its
slip plane to another parallel slip plane just
above or below it.
Climb
⦿ Occurs when a complete row of dislocation
atoms of an edge dislocation moves out of its
slip plane to another parallel slip plane just
above or below it.
Cross slip
⦿ Process by which a screw dislocation moves
from one slip plane to another slip plane.
Jogs and Kinks
Process by which a screw dislocation moves from
one slip plane to another slip plane.
Q
W Z
B
P
C b2
b1
D
A
X Y
S
Jogs and Kinks
Process by which a screw dislocation moves from
one slip plane to another slip plane.
Q
P
b1
W
Z
b2
X Y
R
S
Jogs and Kinks
Process by which a screw dislocation moves from
one slip plane to another slip plane.
Q
W
b1 Z
b2
X Y
R
S
Jogs and Kinks
⦿ Sharp break is called a jog (JJ').
W
J
Z
J’ b2
X
Y
b1 R
S
Jogs and Kinks
Process by which a screw dislocation moves from
one slip plane to another slip plane.
P
b3
W
Z
b4
X Y
R
S
Jogs and Kinks
⦿ When the Burgers vector of the intersecting
dislocations are parallel to each other, kinks are
formed on both the dislocation lines.
Q
P
b3
W
Z
b4
X Y
R
S
Forest of dislocation
⦿ Dislocations moving one behind another along
an active slip plane.
Dislocation density
⦿ Number of dislocation lines that move across a
unit cross sectional area.
Surface Defects
⦿ Grain boundaries
⦿ Tilt boundaries
⦿ Twin boundaries
Forest of dislocation
⦿ Dislocations moving one behind another along
an active slip plane.
Dislocation density
⦿ Number of dislocation lines that move across a
unit cross sectional area.
Surface Defects
⦿ Grain boundaries
⦿ Tilt boundaries
⦿ Twin boundaries
Forest of dislocation
⦿ Dislocations moving one behind another along
an active slip plane.
Dislocation density
⦿ Number of dislocation lines that move across a
unit cross sectional area.
Surface Defects
⦿ Grain boundaries
⦿ Tilt boundaries
⦿ Twin boundaries
Preparation of Specimen
Metallography – study of metals by
microscopic examination.
Metallographic examination reveals the
structure of the grains, grain boundaries,
presence of micro-phases and defects.
Preparation of Specimen
• Selecting and cutting the specimen
• Rough grinding
• Fine grinding
• Polishing
• Etching
Preparation of Specimen – Cutting the specimen
By abrasive cutting or saw.
Specimens of sizes 10-15 mm in diameter
and mounted using thermoplastic resin.
Preparation of Specimen – Grinding
Rough grinding by rubbing the specimen on a
file, grinding wheel, motor driven emery belt.
Fine grinding carried out by emery papers of
progressively smaller grit sizes.
Preparation of Specimen – Grinding
Rough grinding by rubbing the specimen on a
file, grinding wheel, motor driven emery belt.
Fine grinding carried out by emery papers of
progressively smaller grit sizes.
Preparation of Specimen – Polishing
By a rotating polishing cloth pad impregnated
with a polishing powder.
Preparation of Specimen – Etching
Etchant is used to dissolve the amorphous
layer to observe the microstructural features.
Picral, Nital, Keller’s reagent, Marble’s reagent.
Determination of Crystallographic Structure
X-Ray Diffraction
Scanning Electron Microscope
Transmission Electron Microscope
X-Ray Diffraction (XRD)
X-Ray Diffraction (XRD)
If the path length difference between 1-P-1ʹ and
2-Q-2ʹ (SQ + QT) is equal to n times the
wavelengths, diffraction occurs.
nλ = 2d sin θ Bragg’s law
X-Ray Diffraction
θ – Bragg angle
2θ – Diffraction angle
X-Ray Diffraction (XRD)
The interplanar distance d for planes having
Miller indices h, k, l is given by
a
d=
h2 +𝑘 2 +𝑙 2
Scanning Electron Microscope (SEM)
Transmission Electron Microscope (TEM)
SEM TEM
• Based on scattered electrons. • Based on transmitted electrons.
• Focuses on the sample’s surface and • Provides details on internal
its composition. composition.
• Bulk specimen – should be • Thin foil specimen – need not be
conducting. conducting.
• Electron beam gets reflected without • Electron beam passes through the
passing through the specimen. specimen and gets diffracted
• Image obtained by reflected rays on • Image obtained by diffracted rays on
CRT monitor. fluorescent screen.
• Magnification up to 10-50000x. • Magnification upto 1000000x.
Can resolve as close as 20 nm. Resolution is much higher than SEM.
• Provides a 3-D image. • Provides a 2-D picture.
• Used for imaging of dislocations, grain
• Used for surfaces, powders, polished
boundaries, tiny precipitates and
and etched microstructures, IC chips.
defects.
