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Chapter 7

Recovery, Recrystallization, Grain Growth


7.1 Phenomena and terminology
Plastic deformation strain hardening dislocations
Annealing
decrease in strength, increase in ductility
Recrystallization reconstruction of the grain during annealing of deformed metals.
proceeds by generation and motion of high angle grain boundaries or grain boundaries migration.
Recovery
a rearrangement of dislocation or annihilation of dislocations.
Dynamic recrystallization, dynamic recovery processes occur during deformation
Static recrystallization, static recovery processes occur during annealing treatment after cold forming
Recrystallization

-Primary recrystallization
- also called discontinuous recrystallization
- nucleation and nucleus growth
- the dislocation density in metal is not removed
homogeneously
- grain boundaries migration
- Continuous recrystallization or in-situ recrystallization
- occur to the metal subjected to large cold deformation or
the metal which the grain boundaries migration is
strongly impede, i.e. dispersion of a secondary phase.
- a new microstructure has been formed without the
migration of high angle grain boundaries.
- occurs homogeneously

If the degree of prior cold forming is small


- nucleation cannot occur
- existing grain boundaries migrate locally and remove the
dislocation structure in the swept volumes
(SIBM strain induced grain boundary motion) fig 7.3.
- not all grains are deformed equally
- during SIBM : a less deformed grain grows into the
adjacent grain of higher energy and removes the
deformed microstructure.

If the heat treatment is continued after complete primary


recrystallization, grain size increases, grain growth, occurs in 2
modes
- Continuous or normal grain growth
average grain size continuous increases
- Discontinuous or abnormal grain growth
Also called Secondary recrystallization
only a few grains grow rapidly while the other grains grow
slowly or not at all

Continuous or normal grain growth


- the average grain size ln Dm is shifted to larger values
the maximum and the standard deviation remain
unchanged, fig. 7.6 a.
- called self-similarity
- From a graph of distribution VS ln(D/Dm) the normalized
logarithmic grain size
The distribution does not change during normal grain
growth
The integral of the distribution has a constant value.

Discontinuous grain growth: secondary recrystallization


- the grain size distribution does not remain self-similar
- during secondary recrystallization 2 types of distribution
develop
1. the slowly-growing grains becomes smaller and finally
disappears.
2. the rapidly-growing grains
the few abnormally growing grains significantly changes
the average grain size, ln Dm,a and the max frequency,
fmax increase with increasing annealing time until
completion, fig. 7.6.

Tertiary recrystallization
Normal grain growth usually ceases if the grain size becomes
comparable to the smallest specimen dimension (sheet
thickness)
In some cases (thin sheet) discontinuous growth of a few
grains is observed after continuous growth has come to an end
Called Tertiary recrystallization
- because of its discontinuous appearance
- to distinguish from discontinuous grain growth
owing to different energetic reasons.

7.2 Energetics of recrystallization


If grain boundary of area dA is displaced by distance dx,
the Gibbs free energy change
d G = - p dA dx = - p dV
7.1
dV is the volume swept by the moving grain boundary
p = - dG/dV
7.2
p - is the driving force
- the gained free energy per unit volume (J/m3)
- can be considered as a force acting per unit area
on the grain boundary (N/m2)
- pressure on the grain boundary
The driving force for primary recrytallization is the stored
energy of the dislocation.
The deformed metal - dislocation density ~ 1016 m-2
The recrystallized grains - dislocation density ~ 1010 m-2
The energy of a dislocation/unit length
Ed = ()Gb2
G = shear modulus
7.3
b = Burgers vector
If - a dislocation density
The driving force for primary recrystallization
p = Ed = ()Gb2
For 1016
m-2
G 5.104 MPa
b 2.10-10 m

The driving force for grain growth


Total grain boundaries area is reduced
Assume - the consumed grains have a cubic shape
d - diameter of grain boundary
- grain boundary energy (J/m2)
I The driving force for discontinuous grain growth
(secondary recrystallization)
The driving force on a boundary sweeping such a volume
equals
p = (3d2)/d3
= 3/d
7.5
3 factor - each of the 6 faces of cubic is shared by
2 adjacent grains
If the consumed grains
d = 10-4 m
p 0.03 MPa
1 J/m2
3x104 J/m2

7.4

p = 10 MPa
~ 107 J/m3
~ 2 Cal/cm3

The driving force for primary recrytallization is greater by


orders of magnitude than for the discontinuous grain growth
(or secondary recrystallization)
Therefore, the grain growth proceed very slow or become
faster at higher temperature.
II The driving force for continuous grain growth
Grain boundary always be a curvature. The force acts on
the curved boundary in the direction towards the center of
curvature to become straight line. Grain boundary area
reduces. The driving force on a boundary segment the
pressure on a curved surface. (The driving force for
continuous grain growth)
p = 2 / R
7.6

The driving force for tertiary recrystallization


p = (2 o) / h
o = 02 - 01
For o
h

0.1 J/m2
10-4 m

7.7

p 2x10-3 MPa
2x103 J/m3

Since - surface energy depends on the ambient temperature


o can be made larger, or change sign by selecting an
appropriate annealing atmosphere.
Therefore, tertiary recrystallization depends on the annealing
temperature.

R - radius of curvature (assume ~ grain size)


But the curvature is small the radius of curvature is
substantially larger than the grain size (by factor of 5-10)
Therefore, the driving force continuous grain growth e.q. 7.6
is about 5-10 times smaller than for discontinuous grain
growth e.q. 7.5 (the secondary recrystallization)
III The driving force for tertiary recrystallization is
caused by the orientation dependence of the free surface
energy. The grain will grow at the expense of its neighbor if
its surface energy, o, is smaller than that of its neighbor. Fig.
7.9, thin sheet thickness h, width B, grain size is larger
compared to the thickness. The grain boundaries move
perpendicular to the sheet plane.

7.3 Deformation microstructure


Deformed metals can recrystallize.
Recrystallization can proceeds from a deformed metal.
Deformed metal dislocation motion influenced by solute
atoms, precipitates
- by other dislocations, dissociation of the
dislocation.
The normalized stacking fault energy SF /Gb *SF
controls the dissociation width of the dislocations.
- the smaller *SF the larger is the width
- increasing the width
cross slip or climb become more difficult
- obstacles can not be as easily circumvented
- work hardening increases
- material with low stacking fault energy, the flow stress
can reach the level required to activate mechanical twinning.
Twinning is a major deformation affects microstructure.
At large degrees of deformation
- for fcc deformed microstructure can have twin or
absence of twin depending on
- the magnitude of *SF
- deformation temperature

At low degree of deformations


- dislocation are not homogeneously distributed
- dislocations form cell structure with distribution of cell sizes
- cell walls has high dislocation density
- inside a cell has relatively low dislocation density.
- the character and appearance of a cell structure depends on
- the material
- determined by the normalized stacking fault
energy, *SF
- degree of deformation
- deformation temperature
With increasing temperature, larger *SF
- thickness of the cell wall decreases
- until eventually sharp subgrain boundaries are formed
- cell interior becomes depleted of dislocations
The degree of deformation affects - the cell size
- misorientation between
adjacent cells
with increasing degree of deformation
- the average cell size decreases
- the orientation difference between adjacent cells increases
At large stains, deformation inhomogeneities
- tend to form a globular cell structure
- bands in tensile test
- shear bands in rolling (inclined 35o to rolling plane)
- orientation quite different from the matrix orientation. 5

7.4 Recovery
A cold worked metal contains dense dislocations networks.
The recovery (stage of annealing) is
- concerned with the rearrangement of these dislocations to
reduce lattice energy
- does not involve the migration of high angle grain boundaries
- the rearrangement of dislocation assist by thermal activation
- the dislocation rearrange to form cell walls, fig. 10.15
(Smallman). This process is called Polygonization.
Dislocations all of one sign align themselves into walls to
form small-angle or sub-grain boundaries
- during deformation a region of the lattice is curved
- formation of excess edge
dislocations parallel to the axis
of bending
- during annealing - dislocations form sub-grain boundary
by align themselves into walls.
Polygonization - sub-boundary formation
- dislocation climb change arrangement from
horizontal to a vertical grouping.
- the process involves migration of vacancies to or
form edge dislocations.
- vacancies removes also the strain energy of
dislocation decreases
hardness decreases dislocations density decreases
electrical resistivity decrease because of vacancies decrease

7.4 Recovery
Two dislocations with Burgers vectors b1 and b2 . The
interaction force
F = b2 = [(Gb1b2)/2rd(1-])coscos2

7.11

rd - distance between the dislocations


- angular coordinate, = 0o on the slip plane
- Poisson ratio
On the same slip plane:
-dislocation with the same sign repel (force is positive)
-dislocation with the opposite sign attract (force is negative)
Fig. 7.15
-If antiparallel dislocations on the same slip plane meet, they
recombine and annihilate
-If antiparallel dislocations on the adjacent slip plane
vacancies form dislocation climbs
even if dislocations are several lattice apart, they can
annihilate by climb.
-the equilibrium arrangement of two parallel dislocations is an
arrangement of one above the other, = 90o. e.q. 7.11, F=
0, this arrangement is low-angle symmetrical tilt boundary
(LATB). The energy of each dislocation is substantially
decreases.

If Zd number of dislocations per unit length in this arrangement,


The energy per unit area
LATB = Zd [{Gb2/4(1- })ln(rd/2b) + EC]
7.12
EC - energy of dislocation core
= b/rd
7.13
1/rd = /b = Zd number of dislocations per unit
length in LATB
LATB = (K1 K2 ln )

7.14

K1 = Ec/b - K2 ln 2
K2 = Gb/4 (1-)

7.15
7.16

Screw and mixed dislocations can also form low angle


boundaries. They can form network of many low angle grain
boundaries (sub boundaries). The energy is much smaller than
the energy of the same dislocations distributed randomly in7the
crystal.

From eq. 7.12


Polygonization formed, LATB
Because LATB tend to combine in order to decrease rd
-but this will cause to increase high angle grain boundaries
can be generated
Climb and cross slip
control recovery
depend on the normalized stacking fault energy *SF
are promoted by increasing stacking fault energy
materials with high *SF strong recovery
e.g. fcc (Al) and most of bcc metals, high stacking fault
tend to recovery.
but Ag, Cu (fcc) but have low stacking fault energy show
little tendency to recovery.
Dynamic recovery
- recovery process occur during deformation at elevated temp
- decrease work hardening rate
- dislocations form cell walls or sub grain boundaries (in the
case of strong recovery)
- extent of recovery depends on the type and prior arrangement
of the dislocations
- in deformation inhomogeneities (kink bands in tensile
deformed single crystals) sub grains form during deformation, but
in other area dislocations remain disordered.
Fig. 7.20: recovery does not need incubation time but
recrystallization does.
- the kinetics are different
- but the property changes are similar.

Fig. 7.21.
Al hardness of deformed Al changes due to recovery
(stacking faults energy)
Cu hardness changes due to recrystallization.
After some annealing time recrystallization can occur then
hardness change linearly with the crystallized volume fraction.
In most case
- recovery competes with, but also promote recrystallization
- recovery leads to the formation of nuclei for primary
recrystallzation.
In some materials under special circumstances
- recovery can be strong enough to suppress completely
recrystallization

7.5 Nucleation
In order to generate nucleus for recrystallization, three
criteria have to be met, fig. 7.22.
1. Thermodynamic instability
In order to initiate recrystallization the nucleus to be larger
than a critical size. The critical nucleus radius depends on the
driving force as in eq. 7.17.
The critical nucleus radius
rc = 2/p = 4 / Gb2
7.17
- Because of the low driving force for recrystallization
- The nucleation rate is too small to initiate recrystallization
Assume:
- pre-existent nucleus in deformed microstructure which is a
dislocation cell or sub grain.
- therefore recovery process is needed to activate a
dislocation cell nucleation for recrystallization.

2. Mechanical instability
- inhomogeneous dislocation distribution
- a local imbalance of sub grain sizes developed during the
incubation period by recovery process.

Both cause imbalance driving force cause


nucleus start to grow.
3. Kinetic instability
- The surface of nucleus (or the grain boundary) must be
mobile to make nucleus grow and only high angle
grain boundaries have sufficient mobility. The
generation of a mobile high angle grain boundary
from a deformed microstructure is one of the most
difficult steps of nucleation of recrystallization.
- the proposed mechanisms which are still in discuss:
discontinuous sub grain growth, nucleation at prior
grain boundaries and deformation inhomogeneities.
Considering all 3 criteria
- nucleation is always connected to recovery process which
occur in incubation period of recrystallization
- on the other hand recovery and recrystallization are
competing processes because recovery decreases
the driving force for recrystallization
- In materials with strong recovery high *SF like Al,
discontinuous recrystallization can be delayed or
even suppressed.

7.6 Grain boundary migration


The grain boundary moves under the driving force p (J/m3).
Atom detaches from the shrinking grain and attaches
to the growing grain, thermal activated diffusion jumps.
The free energy of each atom pb3 where b3 is the
atomic volume.
v is the velocity of grain boundary, the displacement
per unit time , eq. 7.18.
All typical recrystallization temperature T > 0.4 Tm the
small driving force for recrystallization
pb3 << kT

7.19

For strongly deformed Cu, at 0.5Tm ~ 400oC


pb3 10-22 J , kT 1/20 ev 10-20 J
pb3/kT 0.01
v = mp

7.20

If:

m mobility
Dm - diffusion coefficient through the grain boundary
Qm - the activation energy for jumps through the grain
boundary
From Nernst-Einstein relation
m

= mo e-Qm/kT

7.21

mo = b2Do/kT

10

The mobility of a grain boundary


- A small concentration of impurities strongly influences grain
boundary mobility since impurities tend to segregate at the
grain boundary and exert a drag force on the boundary upon
its motion high activation energy Qm.
- Depends on the orientation relationship between adjacent
grain.
m = m (<h k l>)
7.22
- rotation angle, <h k l> - rotation axis
example: high mobility of Al - 40o < 1 1 1 >
Zn - 30o < 0 0 0 1>
Fe-3%Si 27o < 1 1 0>
- impurities tend to segregate at high angle grain boundary.
Impurities will drag grain boundary and grain bowing become
less mobile. Coincidence boundaries is highly ordered
structure have highly mobility because of its less prone to
segregation. With an increasing content of solute atoms, grain
boundary migration is reduced.

7.7 Kinetics of primary recrystallization


The deformed metals containing high dislocation density is
thermodynamically unstable at all temperatures.
Recrystallization removes dislocations and can be considered
as a phase transformation without a true equilibrium
temperature. But the kinetics recrystallization are frequently
described in terms of recrystallization temperature in order to
complete in a certain time (around 1 hour).
Recrystallization
- is thermally activated
- depends on Boltzmann factor , exp Q/kT
- small change of temperature cause large changes in time.
- But changes in time cause small change of recrystallization
temperature.
Primary recrytallization
The nucleation rate = (dZN/dt)/(1-x)
The growth rate
v = dR/dt

7.23
7.24

X
t
R
ZN

= VRX/V - recrystallized volume fraction


- annealing time
- the radius of a grain
- the number of observed nuclei per unit volume
- the number of nuclei generate per unit time and per
volume in the uncrystallized volume
Assume: nuclei is sphere and isotropic growth.

11

Fig. 7.35 measured recrystallized volume fraction X as a


function of annealing time, t, for cold deformed aluminium.
X = 1 exp{-(t/tR)q}
7.25
tR - characteristic time for recrystallization
time necessary for recrystallization to go to completion
In order to obtain tR : defined
X(tR) = 1 (1/e) = 0.63
The value of X can be 0.99.
If X close to 100% - deviation from eq. 7.25.
The value of X should be an intermediate one, in order to
obtain sensible tR.
If tR, d, x, q known and v can be calcualted.
If grain is sphere (isotropic growth)
nucleation occurs homogeneously and v remain
constant
3
4
X(t) = 1 - exp [ -(/3) v t ]
7.26
tR

= [(/3) v3]t1/4

2 v tR

= 2(3v/ )1/4

7.27
7.28

The recrystallized grain size depends on temperature.


d = (48vo/ o)1/4 exp (Q - Qv )/4kT
7.32
- an increase of the growth rate lead to a a larger grain size
- an increase of the nucleation rate at constant growth rate
leads to finer grain size.
Influence: -primary recrystallization
- Degree of deformation
Degree of deformation increase
- and v increase
- affect more strongly than v
- the recrystallized grain size
- The smaller the grain size prior to deformation, the smaller
the recrystalized grains.
- Alloying elements
Low concentration of alloying element - and v are
reduced in the same extent.
d depends on ratio v/ , if v/ has a small changes, the
change of d is also small.
If v and vary in the same extent has little effect on
d.

d obtained from eq. 7.28 is only roughly estimated but it


gives right order-of-magnitude even though deformation and
annealing conditions also can affect the value of d.
v = vo exp(-Qv/kT)
= o exp(Q/kT)
Qv and Q activation energies
vo and o independent of temperature

7.29
7.30

12

7.8 The recrystallized diagram, fig 7.39


The recrystallized diagram represents the dependencies
between recrystallized grain size, degree of deformation and
annealing temperature.
Use; - useful for industrial applications
- show the grain size after constant annealing time
- grain size increases with increasing degree of
deformation and increasing annealing temperature.
- recrystallization begins above certain temperature.
At low temp.
- recrystallzation has not yet occurred or has not gone to
completion at chosen annealing time. In this case it is
impossible to define a recrystallized grain size.
At high temp with chosen annealing time.
- grain size obtain from
primary recrystallization complete and then
grain growth starts
large grain size high annealing temp.
(because of grain growth)
- but from recrystallization diagram, increasing
recrystallization temperature grain size increases.
Therefore, grain size increase during grain growth process.
- In fact heating up time also affect recrystallization
process, because slow heating rate cause recovery which
decrease the number of recrystallization nuclei.
Annealing has to be terminate immediately after
complete recrystallization.

7.9 Recrystallizaion in homogeneous alloys


The alloying elements have
- little influence on nucleation rate
- strong influence on grain boundary migration, fig 7.40
Solute atoms segregate at grain boundaries. During grain
boundary motion, solute atoms have to move along with grain
boundary via diffusion and exert a back driving force, pR
(considered as drag force) on grain boundary which depends on
the boundary migration rate, v, and concentration of solute, c.
v = m (p pR(c,v))
7.33
If grain boundary is loaded with solute atoms
-At low velocity; the back force increase with increasing velocity.
-At high velocity; the grain boundary can detach from solute
cloud and move freely.
-At intermediate velocity; may be discontinuous transition from
loaded to free state of the boundary.
The grain boundary velocity and the
13to
driving force are not proportional
each other

When the grain boundary contacts with a particle, particle


surface replaces part of the grain boundary and the respective
grain boundary is reduced.
When the grain boundary detaches from the particle, the part
of grain boundary has to be regenerated.
The respective retarding force (Zener force) or the back
driving force on grain boundary
pR
Rp
f

f/Rp
7.10 Recrystallization in multiphase alloys
The presence of second phases has a substantially influence
on recrystallization.
- coarse particles speed up the recrystallization process
- fine dispersion of particles strongly hindered
recrystallization
Particles influence on the deformation structure, nucleation
and grain boundary migration.
During deformation:
The hard particles dislocations cannot cut but have to go
around
Nucleation and grain boundary migration
The large particles help the nucleation by particle-stimulated
nucleation (PSN). Finely dispersed particles are less influence
for nucleation but they hinder dislocation motion (recovery) and
grain boundary migration (due to a back driving force on grain
boundary).

-(3/2) f/Rp

- the radius of the particles


- the volume fraction of the particles
- the grain boundary energy
- the degree of dispersion

Only the effective driving force peff = p + pR is available for


grain boundary migration, pR is negative. peff may be small.
In heterogeneous alloys with a high degree of dispersion
- the back driving force can become large
recrystallization is retarded.
- benefit for commercial application, the particles stabilize
grain size after primary recrystallization. Because Zener force is
large, grain growth become small or even suppressed
For example:
f = 1%
rP = 1000 A
= 0.6 J/m2

Zener force 0.1 MPa


The same order of magnitude or
larger than the driving force for grain
growth.

14

7.11 Normal grain growth


After completion primary recrystallization, the grains are
stain-free. In equilibrium state, all grain have 6 corners. All
boundaries are straight, fig. 7.48.
In single phase metal:
- contact angle = 120o because surface tension of most
grain boundaries is similar.
In multiphase alloys:
- contact angle can be different from 120o because of
different surface tension at interface boundaries. In /
brass at triple junction of one and two is 95o .
2D
If a grain has a number of edges different from 6 for instant
5-sided grain, fig 7.48.
1. To attain equilibrium at least one grain boundary is
curved. There is a force acting on the curve boundary toward
the center of curvature to minimize grain boundary area.
2. The angle must be different from 120o equilibrium
3. To establish equilibrium; the other grain boundaries have
to readjust by migration.
4. again cause grain boundary curvature and repeat 3.
Therefore, a stable equilibrium can never be reestablished.
The grain with 6 sides straight line
The grain with more than 6 sides has concave curvature
large grain and become larger
The grain with less than 6 sides has convex curvature
small grain and become smaller and disappear

3D
The contact angle at 4 grains meet is around 109o. Therefore,
in 3 D granular structure is never possible to establish
interfacial equilibrium.
The average grain size during isothermal annealing can be
predicted
D Ktn
n = 0.5 - for high purity metals and for annealing
temperature close to Tm
n = 0.2 0.3 - for commercially pure metals fig. 7.51.

15

Grain growth in thin sheet


The grain growth will slow down if average grain size reach
the size of the smallest specimen dimension.
If the grain boundary touches a free surface, a triple junction
between the grain boundary and 2 external crystal surface is
generated.
The formation of a (thermal) groove along grain boundary,
fig. 7.52. If the grain boundary migrate, this groove has to be
dragged along or left behind.
The retarding force independent of the depth of the groove
pGR = - 2GB / h s
h specimen thickness s
GB - grain boundary energy

- surface energy

This retarding force reduces the growth rate of grains in


contact with the surface and grain growth cease at the grain
size ~ 2 times of the sheet thickness.

Material contains precipitates


- the continuous grain growth is limited by Zener drag.
Zener force, pZ = - 3 f/dp
f - volume fraction of particle
dp diameter of particle
- a maximum grain size depends on the dispersion of the
second phase.
- the grain growth terminates if the driving force and retarding
force are equal
2 / = 3 f/dp
- constant relating radius of curvature of grain boundaries
and grain size.
The terminal grain size
dmax = (2/3) 1. dp/ f

7.42

dp increases with annealing temperature

16

7.12 Discontinuous grain growth (Secondary


recrystallization)
Discontinuous grain growth most of the grains remain
stable except for the growth of a few grains.
Occurs in 2 phase materials during annealing close to
solvus temperature.
- during annealing precipitates locally dissolve and initiate
grain growth while the remaining grains remain stabilized by
the precipitates.
- the locally growing grain become very big. They can
overcome Zener pinning (drag) and consume near by small
grain pinned by Zener drag.
The critical grain size for a grain to grow discontinuously into
a matrix with precipitate
d > avg d/ (1 - avg d/dmax)

7.43

avg d - average grain size of the pinned grain structure


dmax - maximum grain size according to eq.7.42
Discontinuous grain growth occurs during annealing
above critical temperature. There are small amount of high
angle grain boundaries comparing to the low angle grain
boundaries. HAGB - high mobility can grow and finally
consume the low mobility grain boundaries.

7.13 Dynamic recrystallization


Dynamic recrystallization
- occur during plastic deformation at elevated temperature
T > 0.5Tm
- evidence in flow curve, fig. 7.54, with a single peak or
oscillation of the flow curve
- is associated with a sudden loss of strength, fig. 7.55.
- can occur during creep recognized by a sudden
increase of creep rate, fig. 7.56.
- the critical values of stress and strain at which dynamic
recrystallization is initiated depend on material and
deformation.
- many concentrated alloys and dispersion strengthened
materials do not recrystallization dynamically, fig. 7.57.
- the flow stress to set-off dynamic recrystallization
decreases with increasing deformation temperature, fig. 7.58.
and decreasing strain rate, fig. 7.59.
Dynamic recrystallization
- is important for hot forming
- keeps the flow stress level low requires low deformation
forces.
- increase ductility, fig. 7.60
- dynamic recrystallized grain size is directly related to flow
stress.
- the flow stress increases, the grain size decrease, fig. 7.61.
- the recrystallized grain size can be adjusted by select
deformation condition
- the recrystallized grain size does not depend on the initial
grain size, but strongly affected by the deformation schedule.

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