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Recrystallization
nucleation and growth of
strain free grains
Grain growth
What drives these reactions?
Grain growth:
Boundary curvature
Most of the energy expanded during cold working is dissipiated
as heat, but a small fraction of it remains in the metal as stored
energy, ES.
Recovery Recrystallization
CW Annealed CW Annealed
E E
Es Es
CW Annealed CW Annealed
E E
Es
Es
STORED ENERGY
A A
C
B B B B
b
b
b
Grain Size. The amount of stored energy increases as the grain size
decreases. Consider a large grain that is deformed a given amount.
Now imagine this same volume to be divided into many small
grains and then deformed the same amount. In this second case the
deformation would result in many more grain-boundary-dislocation
interactions. Since the grain boundaries are effective in blocking
dislocations, the smaller grain size promotes dislocation interaction
and multiplication.
Second phase particles. Depends on the size, distribution,
volume fraction and nature of the second phase. For few
undeformable particles of large size, there would be increased
dislocation density only around particles, thus non uniform
distribution of deformation.
For the uniform distribution of fine particles, because of
dislocation particle interaction, stored energy should be higher.
However the distribution of deformation should be uniform as
well, since particles are not only acting as barriers to
dislocations but also as sources.
Uniform deformation
structure in an
aluminum alloy with
fine Al4CuMg5Si4
dispersoids.
Comparison of driving forces:
Time
Isochronal Annealing: Two specimens (one cold worked and one
annealed) are heated in separate identical furnaces and power
necessary to maintain the same rate of rise of temperature in each
specimen is measured. Power needed for deformed specimen will
be less because it will release its stored energy of cold work. So
power difference P is proportional to the released stored energy.
Stage I (recovery),
II (recrystallization),
the III (grain growth)
recrystallized
Energy released
grains first
appear at the
onset of the
large power I II III
peak
Temperature
The fraction of the stored energy released during recovery is small for type A
and large for type C. Type A curves are usually obtained for pure metals and
type B or C for impure metals.
The fraction released stored energy due to recovery has been found to vary
from 0.03 for high-purity metals to as high as 0.7 for some alloys. It is apparent
that impurity atoms inhibit the nucleation of recrystallized grains and thereby
allow a larger fraction of the stored energy to be released by recovery processes
prior to the onset of recrystallization.
PROPERTY CHANGES
Hardness. There is usually only a small change in hardness
during recovery, about one-fifth of the total change. Since
hardness (and strength) are decreased with decreasing dislocation
densities, Figure indicates only a small drop in dislocation density
during recovery but a large drop during recrystallization. We
expect the latter result because the new recrystallized grains are
essentially strain free.
Resistivity. The electrical resistivity of a metal is a measure of the
resistance offered by the metal lattice to the flow of electrons
produced by an electric field. Defects in the lattice may act as
scattering sites for the moving electrons and thereby increase
resistivity. Point defects such as vacancies and interstitial atoms
are more effective at scattering than dislocations, so that changes
in resistivity reflect changes in vacancy and interstitial
concentrations. The drop in resistivity during recovery means that
a significant decrease in point-defect concentration must occur
during recovery.
Density. The density of a cold-worked metal is decreased due to
the generation of vacancies. Edge dislocations also make a small
contribution to the lower density because of the dilation of the
lattice about this type of dislocation. The recovery mechanisms
must involve a decrease in vacancy concentration and probably
some decrease in edge dislocation density.
Cell Size. The cell size grows only slightly in the first portion of
the recovery stage but shows a definite increase just prior to
recrystallization.
RECOVERY MECHANISMS
This is probably
accomplished by
movement of
interface
dislocations
involving climb
so that diffusion
is required
Subgrain Coalescence
HVEM bright field images of the same area after in situ annealing
at 700 °C for 5 min (a) and 30 min (b) in a deformed (55%)
Zr–2Hf alloy. Subgrain A, B and C form a larger subgrain D
Polygonization: After the single crystal has been bent, an
excess of positive edge dislocations is generated. Annealing
causes these edge dislocations to line up over one another in
small-angle tilt boundaries. It should be clear that in order for the
dislocations to become lined up they must undergo both glide and
climb. Polygonization is not as well defined in polycrystalline
materials because of the complexity of the deformation. However,
we may say that, in general, (a) polygonization requires an excess
of edge dislocations, (b) it is only produced at higher recovery
temperatures because dislocation climb is involved, and (c) it
produces subgrains that are roughly 10 times larger than those
produced via dislocation tangle condensation.
KINETICS OF RECOVERY
Zn single crystals were strained in pure shear by some amount γ1.
This increased the yield stress from to to tmax.
Recovery causes the yield stress to decay from tmax back toward to ,
and the rate is a function of time and temperature
t (t,T ) = ?
Let P be some physical property that changes during the
recovery stage (e.g., resistivity, yield stress etc.). We may write
P = P0 + Pd
P0 is the value of the physical property in the annealed state prior
to deformation, base value, and Pd is the increment in the
physical property due to the defects produced by deformation.
Assume that Pd is proportional to the volume concentration of
defects, Cd , produced by deformation,
P = P0 + const Cd
Cd ( P − P0 )
Time rate of change of the physical property
d ( P − P0 ) dCd
= const (1)
dt dt
d ( P − P0 )
= − K ( P − P0 )n e−Q / kT
dt
d ( P − P0 ) − Q / kT
= − Ae dt
( P − P0 ) n
Let n=1
d ( P − P0 )
( P − P0 )
− Q / kT
= − Ae dt
P − P0
and residual recovery, 1− R =
PCW − P0
Then,
( P − P0 )
ln = − Ae − Q / kT t
( PCW − P0 )
ln(1 − R) = − Ae − Q / kT t
1 − Q / kT
ln = Ae t
1− R
1 Q
ln ln = ln A − + ln t
1− R kT
Then is it possible to obtain information concerning the mechanisms of recovery
from analysis of the kinetics of recovery?
From a plot of lnt versus 1/T at a constant value of P, we determine a value of Q
from the slope.
1 Q
ln ln = ln A − + ln t
1− R kT
constant
Q
Rearrange, ln t = const +
kT
lnt Q/k
1/T
If n>1, then
d ( P − P0 )
( P − P0 )n
− Q / kT
= − Ae dt
1 1− n − Q / kT
( P − P1− )
n( P − P0 ) 0
11− n −cons . = − Ae
A t
− Q / kT
− 1 = − e t
1 − n ( PCW − P0 )1−n ( PCW − P0 )1−n
Applying the initial condition that, t = 0, P=PCW
( P − P0 )1−n A (1 − n ) −Q / kT
1− n
− 1 = − 1− n
e t
( PCW − P0 ) ( PCW − P0 )
(1 − R )
1−n
Then, = 1 − Be−Q / kT t
The above example, data on Zn gave a linear relation between lnt and 1/T ,
indicating that only one activation energy and, hence, only one defect
annihilation process was involved.
Q was found to be approximately the same as the activation energy for self-
diffusion, implying that vacancy migration is involved in this recovery process.
It therefore indicates a dislocation climb controlled recovery process.
Subgrain
Growth
Nucleation of grains results from the sudden growth of a high-
mobility boundary. These boundaries are either:
1. An original high-angle boundary.
2. (a) A high-angle subgrain boundary formed by a subgrain
enlargement mechanism.
(b) An existing high-angle subgrain boundary modified by
unknown atomic rearrangements.
Mechanisms 1 and 2(a) are more common in lightly deformed
metals and mechanism 2(b) is more common in highly deformed
metals.
The "nucleation" event appears to be a growth phenomenon so that
variables affecting growth will also affect "nucleation" in a similar
way. Even though the new grains do not spontaneously nucleate in
the sense of the classical nucleation picture, we may still treat the
recrystallization transformation as being composed of nucleation
and growth stages.
Subgrain Growth
The growing subgrain, as its boundary acquires more dislocations,
will become progressively more misoriented with respect to its
neighbours. Eventually they undergo a transition to a conventional
high angle boundary.
Subgrain Coalescence
Similar to previous
model based on the
hypothesis of
coalescence of
neighbouring
subgrains.
Strain Induced Boundary Migration (SIBM)
Nucleation at high mobility grain boundaries usually is preceeded
by grain boundary bulging. A critical bulge size has to be exceeded
for a bulge to be a nucleus..
Usually the driving forces on both sides of a grain
boundary are assumed to be equal, but actually an
imbalance can be present due to a dislocation
density or subgrain size distribution difference
across the grain boundary.
For the method to operate, the dislocation
distribution must be inhomogeneous on a
sufficiently large scale, i.e., a particulary large
subgrain neighbouring to a grain boundary may
cause that grain boundary to bulge across the
entire width of the subgrain.
Strain induced grain boundary migration can occur after a relatively
small or moderate amounts of cold work. Differring from
recrystallization in that no new crystals are formed. Rather the
boundaries between pairs of grains move so as to increase the size
of one grain while the other to decrease.
No new crystals are formed, instead, a boundary between two
grains move at the expense of the more deformed one. Hence,
the "nucleation" event is essentially a growth phenomenon.
Assume that the mobile boundary is pinned at two points as it bulges out. Let the
volume change in going from position I to II be dV and the overall free-energy
change per volume be ΔG. The surface free energy of the boundary is taken as γ,
and the stored energy per volume in the cold-worked grain is Es. For the
boundary moving from position I to II a free-energy balance gives,
dA
G dV = − E s dV + g dA G = − Es + g
dV
Released
stored energy
is used to
create a larger
surface area.
dA 1 1 2g
Where, = + For spherical boundaries; G = − Es +
dV r1 r2 r
r
In order to have growth, the value of ΔG
must be negative, so that Es must be larger
than 2γ/r. Since the boundary is pinned at a a
distance of 2a , the radius of curvature will progress
t0 t1 t2 t3
100
Sigmoidal kinetics
% Product
50 y = 1 − exp( −ktn )
Incubation
period
t 50 log (time)
0
5
impingment
R
Growth rate R = G (t − t )
G=dR/dt
t t
4 3 4 3
= R = G ( t − t )
3
Volume of a spherical nucleus; Vnuclei
3 3
Number of nuclei formed in volume V in time interval dt is
n = N dt V
number nuclei formed/unit time
N=
untransformed volume
The total volume transformed until time t = n*dt
ndt
Vtransformed = (vol. per nuclei )*(# of nuclei /dt)
0
t
Vtransformed = G (t − t ) * N Vdt
4
3
3 3
0
It is more convenient to work with the fraction of the volume
transformed,
t
Vtransformed
X transformed = = 43 G 3 (t − t ) 3 * N dt
V 0
X transformed = G 3 N t 4
3
Experimental
X transformed = G N t 4
3
3 sigmoidal curve
Xtransformed
time
dVr = 43 G 3 (t − t ) 3 * N Vu dt
V = Vr + Vu
dVr = G (t − t ) * N (V − Vr )dt
4
3
3 3
V − Vr
dX r = G (t − t ) * N dt = 43 G (t − t ) * N (1 − X r )dt
4 3 3 3 3
3
V
Xr t
dX r
0 1 − X r 0 3
= − t dt
4 3 3
G ( t ) * N
assume t=0
− ln(1 − X r ) = G 3t 4 N
3
Johnson-Mehl
Eq’n X r = 1 − exp( − 3 G 3 N t 4 )
3 4
Johnson-Mehl eq. X real = 1 − exp − G Nt
3
applicable to any heterogeneous phase transformation
subject to the four restrictions :
random nucleation, constant Ń, constant G, and small t.
3 4
X real = 1 − exp − G Nt
3
Avrami considered the case where the nucleation rate decayed
exponentially with time. In this case the above analysis with
X r = 1 − e− kt
n
Q
k = k0 exp −
RT
Growth rate G is a usually constant but the nucleation rate
Ń is not in solid state phase transformations, particulary at
the early stages, probably because of the experimental
difficulties in the determination of small nuclei.
EXPERIMENTAL DETERMINATION OF G AND Ń
− Qn / RT
N = N 0e
Activation energy for Ń and G is roughly the same except at
low strains.
OVERALL EFFECT ON RECRYSTALLIZATION
Strain
Grain size
Impurity
Xr
CONTROL OF
RECRYSTALLIZATION TEMPERATURE
AND GRAIN SIZE
From a practical point of view we are interested in
controlling the recrystallization temperature and the
recrystallized grain size. To estimate how these are
affected by the parameters which we may control,
Johnson-Mehl equation will be used
3 4
X real = 1 − exp − G Nt
3
RECRYSTALLIZATION TEMPERATURE
Ln t0.95=K + Q/RT
Trecry 0.4Tm
RECRYSTALLIZED GRAIN SIZE
R=G(t-t) G*t
t R/G
3 4
X real = 1 − exp − G N ( R G )
3
14
G
d = 2 R = const
N
Small recrystallized grain size is promoted by a high nucleation
rate and a slow growth rate; that is, the grains nucleate at a high
density and grow very little.
The predominant factors that affect Ń and G are:
(1) amount of prior strain,
(2) temperature of anneal,
(3) prior grain size, and
(4) purity.
Prior Strain
Trecry is decreased by
high strains since high
strains increase both Ń
and G.
d is decreased by fine
grains.
The smaller grains cause
inhomogeneous
deformation, which
increases Ń faster than G.
Impurities
Addition of impurities increases the amount of stored energy at a
given strain, so that one might expect the growth and nucleation
rates to increase. However, impurities are extremely effective at
decreasing the interface mobility and this latter effect is dominant.
So, impurities decrease the growth and possibly the nucleation rate.
Strain , Es ;G ,t also N
Impurity , Es but due to drag ; G , effect on N ?
Grain size , Es ;G and complex strain pattern ; N
Temperature ; G, N both arrhenius dependence with similar Q
Nucleation
site
Finely dispersed particles are detrimental for nucleation, because
usually they homogenize slip. Moreover they hinder dislocation motion
(recovery) and grain boundary migration, lowering the nucleation and
growth rates. Hence recrystallization is always retarded.
Over the years there was some debate on the relative merits of
these mechanisms; but there are many evidences now that shows
that both can take place.
The cube texture,
{001}<100>, is often
obtained as the
recrystallization
texture in fcc metals.
Low = B( ) n
= B ( Sinh )
n
High = B exp( b )
B = A exp(-Q/RT)
CREEP → Low → power law → tested under constant
load (or ) → independent (measured) parameter is
strain rate → recovery dominated
HOT WORKING → High → exponential law → tested at
constant strain rate → independent (measured)
parameter is stress → recrystallization dominated
= B ( )
n
where
= − i
is the applied true stress and i the true internal stress.
i is modified by dynamic recovery and recrystallization
2 , T2
1 , T1
1 2 ; T1 T2
Dynamic recrystallization
is observed as the
dominant mechanism in
austenitic alloys and
appears as a single peak or
oscillations in the flow
curve.
A .
T1 or 1
T1< T2
. > .
B .
T or
1 2
2 2 A .
T 1 or 1
T1< T2 B T2
.
or
. . 2
1> 2
strain strain