Recrystallization Annealing

Recrystallization annealing is a type of heat treatment process by

which a cold deformed material is heated to a specified temperature
and soaked at that temperature for a specified period of time
usually one hour, to produce comparatively defect free structure at
the expense of deformed matrix followed by cooling. The driving
force for microstructural changes is the reduction in free energy that
is accomplished by the reduction in stored energy. Reduction is
strongly dependant on temperature.

Recrystallization annealing takes place in three steps at increasing

temperature of heating. Stages: Recovery, Recrystallization and
Grain growth. Recrystallization annealing is also called process
annealing or intermittant annealing, subcritical annealing.

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 Recrystallization annealing stages
Recrystallization annealing is given to a cold deformed product
mainly to restore ductility and modify other mechanical
properties like hardness, yield strength, tensile strength,
toughness, ductility and physical properties like electrical
resistivity and magnetic permeability of ferromagnetic material
like iron and steel.

A: pure metal, store energy is minimum

B: slightly impure metal
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C: highly alloyed.
Isochronal annealing
Highly sensitive differential calorimeter is used to find the energy
release rate with respect to temperature and it is measured as
specific heat difference and denoted by ΔP or power difference
plotted as a function of temperature. The difference in power
required to heat two similar specimens (one is as-received, other cold
deformed) at the same rate (oC/s ). Measurement of the difference in
power gives direct evidence of the rate at which the heat is released
in the cold worked specimen.
Isothermal annealing
The free energy release rate is measured in the form of power
difference or heat with respect to annealing time heat by a very
sensitive calorimeter while the specimen is maintained at a constant
temperature.

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 Recovery

• Recovery is restoration of physical properties without

any observable change in microstructure. Recovery is
the annihilation and rearrangement of point
imperfections and dislocations without migration of high
angle boundaries.
A pair of vacancy and an interstitialcy can mutually annihilate
each other. The point imperfection also find an sink in high
angle boundaries and at edge dislocations. Excess vacancies
can disappear at edge dislocations making them to climb up.
On further increase of annealing temperature dislocation
recovery process start. A positive and a negative edge (or
screw) dislocation on the same slip plane can mutually
annihilate each other. This annihilation for edge dislocation is
by glide on same slip plane and on different slip plane by
cross-slip for screw dislocation. 4
In cross slip, slip occurs simultaneously at more than one plane (basal
{0001}+prism {10-10} in the given case of HCP structure ) with a common
slip direction <11-20>. screw dislocation move from one plane to other and
back to same plane as shown in Fig C

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Excess dislocations of same sign left over after this lower their
energy by arranging themselves in low angle boundaries. Edge
dislocations form tilt boundaries (climb), screw dislocations
form twist boundary. The process of low angle boundary
formation is known as polygonization.

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 Grain boundaries
Low angle boundary: Tilt boundary, twist boundary

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The extent of recovery depends on temperature and time of
annealing.
Fraction of recovery= R=(σm-σ)/(σm-σ0), σm =flow stress of
deformed matrix, σ=flow stress of recovered matrix, σ0 =flow stress
of undeformed material.

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 Larger deformation lead to smaller recovery of properties.
Metals with low SFE (Cu, Ni, α-brass, γss) usually show little
recovery. Metals with high SFE (α-iron, Al) show appreciable
recovery in mechanical properties due to greater dislocation climb.
Properties sensitive to point defect concentration may change
significantly like density, resistivity. Cell size increases and cell
boundary sharpens. Sharpness is more for more SFE materials.
Recovery is a thermally activated process.
1/τ=Aexp(-Q/RT), τ=time required to recover a given fraction of
total yield point recovery, Q=activation energy, R=universal gas
constant, T is the absolute temperature, A =constant.

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Fe-Si single crystal 12
Si-Fe single crystal, 8% CR 1000oC 13
TEM micrograph, polygonised Fe, 14
 Bend contours are called
Bragg contours, formed due
to bending of crystal in thin
film and Bragg diffraction
Bend contours and high angle
boundaries 15
 Recrystallization
Recrystallization is the thermally activated microstructural
evolution process in which a new set of comparatively strain
free grains nucleate at the expense of deformed matrix until it
is consumed by the passage of a high angle boundary. The
driving force is the reduction in free energy by the decrease in
dislocation density (remaining after recovery).
Recrystallisation produces a drastic change in mechanical and
other physical properties of the deformed metals to the level
corresponding to those of annealed condition.

Recrystallization takes place over a small temperature range.

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 Laws of recrystallization
1. Recrystallization temperature is defined as the temperature at
which a given metal with a certain amount of cold deformation
will completely recrystallize in a specific time, usually 1 hr
(practically 95%).
Recrystallization temperature is also arbitarily defined as the
temperature at which 50 % of the cold worked matrix recrystallizes in
1 hour.
It is a function of prior strain, purity, initial grain size, temperature of
deformation, and texture.
Prior strain: a minimum deformation is necessary to cause
recrystallization and recrystallization temperature decreases with
strain.
Purity: recrystallization occurs at measurable rate at temperature
above 0.3 to 0.6 Tm, Tm =m. p. The solute atoms drastically lower
the boundary migration rate. The recrystallisation temperature 17
increases markedly in the presence of impurities.
 Al

Grain size: lower initial grain size decreases recrystallisation

temperature.
Deformation temperature: Recrystallization temperature decreases
with decreasing temperature of deformation.
Heating rate: Recrystallization temperature decreases with rapid rate
of heating due to reduced recovery.
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3. Increasing the annealing time decreases the temperature required
for recrystallization.
Approximate relation
1/T=Klog10 (1/τ)+C
1/τ=Aexp(-Qr/RT)

4. Greater the degree of deformation and lower the annealing

temperature, the smaller the final grain size. The rate of
recrystallization increases with increased amount of deformation,
decreased deformation temperature and with increased annealing
temperature.

5. The larger the initial grain size, the greater amount of cold work
required to achieve an equivalent recrystallization temperature
and time. Recrystallization temperature decreases with decreasing19
grain size.
6. The new grains don’t grow into deformed grain of identical
or slightly deviating orientation or into grains close to a twin
orientation. The migration rate is more for more difference in
orientation between the two grains separated by boundary.
Certain specific orientations give rise to high migration rates.
The favorable orientations for FCC crystal are rotation of one
of the crystal by 38o and 22o about a <111> axis common to
both crystal. For BCC crystal a rotation of 30o about a <110>
axis. These orientations generally corresponds to those which
give rise to the highest density of coincidence sites on the
boundary. Fast growth of certain orientations results in
development of preferred orientations after
recrystallization, known as recrystallization texture. All
orientation may nucleate, but crystals, which have the highest
growth rates corresponds to special orientations, out grow the
rest of them giving rise to texture.
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7. Continued heating after the completion of recrystallization
causes the grain size to increase.

9. For a given percentage of deformation, the recrystallization

temperature is raised with slower heating rate, because
recovery usually occurs during heating.

10. As the grain boundaries of the matrix play a role in the

nucleation of strain free crystals, finer initial grain size lowers
recrystallization temperature.

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 Nucleation of recrystallized grains
Recrystallization takes place by heterogeneous nucleation of
strain free crystal at or near preexisting original grain
boundaries, second phase particle boundary which are present
prior to deformation or those induced by deformation such as
transition bands and shear bands.
There are three mechanisms by which nucleation takes place
(1)Subgrain coalescence via the evaporation of edge
dislocations constituting the subboundaries between them.
(Under low strain). The enlarged subgrains so formed, much
larger than their neighbors, could act as nucleus. The
subboundary dislocations link continuously with dislocations
in a neighboring high angle grain boundary; the disappearance
of subboundary involve a perceptible rearrangement of the
dislocations (by climb and glide) in the grain boundary. Grain
boundaries act as sink rather than dislocation sources. 22
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(2)Strain induced boundary migration (SIBM): Under high
strain and low stacking fault energy, a subgrain within a
deformed grain grows into its adjacent grain, forming a bulge
which has the same orientation as the original grain but is
predominantly free of dislocations.

(3) Nucleation from recovery twins. (For alloys where

annealing twins form at early stage of subgrain growth, brass,
Cu, stainless steel, low SFE materials). Most of the
recrystallized orientations donot exist in the deformed
microstructure, which becomes modified by multiple twinning
on specific twinning variants after nucleation.

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 Kinetics
Recrystallized nucleus may be defined as a crystallite of low
internal energy growing into deformed material from which it is
separated by a high angle boundary. The basic characteristics of
the kinetics of primary recrystallisation process are as follows
1. An initial incubation period is necessary
2. It is followed by slow rate of change at the initial stage,
accelerated rate of change at the intermediate stage and finally
slow rate of change at the final stage.
The general form of the equation
f(t)=1-exp(-ktn), k=kinetic parameter related to constant growth
rate, nucleation rate and a shape factor. n is the JMAK exponent.
n= between 1 and 2 for one dimensional nucleation (for wire
products)
=between 2 and 3 for two dimensional nucleation ( in thin sheet)
=between 3 and 4 for three dimensional nucleation (in lump) 25
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 Grain growth
Further annealing after completion of primary recrystallisation
leads to an increase in grain size. This process, called grain
growth, is entirely controlled by grain boundaries and is
carried out by migration of high angle grain boundaries into a
fully recrystallized matrix.

There are two types of grain growth: normal or continuous

grain growth and abnormal, exagerated or discontinuous grain
growth also called secondary recrystallisation.

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 Normal grain growth
Normal grain growth is associated with the growth of major
grains. The grain size distribution, however remains more or
less same during normal grain growth. Reduction in interfacial
energy per unit volume forms the driving force for grain
growth. This driving force is an order of magnitude smaller
than that for recrystallisation.
For a spherical grain, grain boundary energy per unit volume=
4πR2σ/(4/3πR3)=3σ/R, where σ=surface energy/unit area and R
is the radius of curvature.
For a curved boundary, the radius of curvature is positive in
one side and negative on the other.
The free energy difference per unit volume
IΔgI=cσ(1/R1-1/R2), where R1=-R2=R, c=constant.
=2cσ/R, boundary moves from convex side to concave side.29
For a stable grain structure the grains tend to appear as regular
hexagon. The sides of the grain will be flat and every set of three
grain boundaries would meet at a triple junction point at a
dihedral angle of 120˚. The grains that have less than six sides
will necessarily have some of the boundaries curved concave
inward to give 120˚ intersections whereas those having more
than six sides will have some of their boundaries curved concave
outward. The former grains (<six sided) will trend to shrink or
vanish and latter tend to grow.

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 Grain growth kinetics
D=C1tn, Do =initial grain size, small and neglected, D=average
grain diameter.
For simplified growth model
dD/dt∞IΔgI=c2IΔgI=c3σ/D, D=2R,
Integrating within boundaries gives
Dt2-Do2=2C3σt~Kt, K=ko exp(-Q/RT)
or, Log((Dt2-Do2)/t)=-Q/(2.3RT)+logKo

If Do is neglected
Dt∞t1/2, however time exponent, n, is often less than 0.5 specially
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at low temperature of annealing.
 Pinning by second-phase particle
Presence of particle at boundary reduces gb area, when boundary
moves away from particle, gb increases so particle exert pinning
force.

The critical stage in pinning occurs at small grain sizes, when the
volume fraction of the precipitate particles is high or the average
particles size is small.
Pinning action is similar during recrystallisation or grain growth.
Both solute drag effect and particle pinning effect are applicable to
both recrysytallisation and grain growth. However, solute drag effect
is less effective than particle pinning by second phase particles. 32
 Abnormal grain growth or secondary recrystallization
When the annealing of an initially deformed material is
continued for long time (even) after the complete formation of a
(primary) recrystallized structure, a few grains starts growing
preferentially and very rapidly until they impinge upon one
another. A radical change in grain size distribution is termed as
discontinuous or abnormal grain growth or secondary
recrystallisation. The requirement for secondary
recrystallisation is the strong impediment of normal grain
growth, with exception of a few grain that act as nuclei for
secondary recrystallisation.

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1. Introduction of less stable particles capable of inhibiting
normal grain growth and heated above grain coarsening
temperature i.e. a temp above which particles dissolve and
grain growth takes place rapidly.

2. While the average grain diameter D after primary

recrystallisation has reached a limiting value which is twice
the thickness of the sheet. Abnormal grain growth is not
feasible.

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3. Presence of strong single orientation in a fine grained
recrystallised structure favors SR on further annealing at high
temperature. The grain boundary within highly textured
volume have a lower misorientation and therefore a much
lower energy and lower mobility than those within a normal
grain structure.

4. Abnormal grain growth may result either from an

abnormally high mobility or from a higher driving force than
that of normal grain growth.

5. Abnormal grain growth occurs above grain coarsening

temperature where thermal energy is sufficient for particle
become unstable. Grain coarsening temperature is the
temperature at which particles can grow to or exceed the
original radius(i.e. limiting size) 35
Growth kinetics can be described by Avrami relationship.
f(t)=1-exp (-ktn), t=time
The driving force is the large reduction in total interfacial energy of the grain boundary.
Application of SR
Single crystal wire to avoid intergranular fracture. Mo, W wire used for filament in
electron microscopy. Coarse grained structure is highly desired in production of soft
magnet. Fe-Si, Fe-Mn alloys are used in transformer core. Coercive force decreases
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with increasing grain size.