Heat Treatment of Ferrous and Non-Ferrous Metals and Alloys

Course No MME 321

Lecture 8
Recovery, Recrystallization and Grain Growth

Dr. SASIKUMAR, Asst Prof., MME

Department of Materials & Metallurgical Engineering (MME)

MAULANA AZAD NATIONAL INSTITUTE OF TECHNOLOGY
Bhopal, M.P., India
COLD WORK
 cold work is a Plastic deformation in the temperature range (0.3 –
0.5) Tm .

 Cold work is one of the method to increase the strength of metals

and alloys.

 During cold work the point defect density (vacancies, self

interstitials…) and dislocation density increase. This leads to an
increase in the internal energy of the material.

 Typical cold working techniques are rolling, forging, extrusion etc.

 Point defects and dislocations have strain energy associated with them.
(1 -15) % of the energy expended in plastic deformation typically is
stored in the form of strain energy (in these defects)
The amount of energy stored depends on the material, temperature,
strain rate and type of deformation, grain size, etc.
The cold worked material is in a microstructurally metastable state.
Depending on the severity of the cold work the dislocation density can
increase 4-6 orders of magnitude or more. The material becomes
stronger, but less ductile.

↑ point defect density

Cold work Annealed material Stronger material
Cold
 work

↑ dislocation density  dislocation ~ (106  109 )  dislocation ~ (1012  1014 )
 Heating the material (typically below 0.5 Tm) is and holding for sufficient
time is a heat treatment process called annealing. Recrystallization
Annealing
 Depending on the temperature of annealing processes like Recovery (at
lower temperatures) or Recrystallization (at higher temperatures) may take
place. During these processes the material tends to go from a
microstructurally metastable state to a lower energy state (towards a
stable state).
 this is not a phase transformation but a microstructural transformation.
 Further ‘annealing’ of the recrystallized material can lead to grain growth.
Low T
Recovery

Cold work Anneal

High T Recrystallization
RECOVERY
 Recovery takes place at low temperatures of annealing (after cold work).
 “Apparently there no change in microstructure” (i.e. if seen in an optical
microscope, the microstructure looks similar before and after recovery).
 Two processes which occur during recovery are:
 Reduction in point defect density (+ their reconfiguration),
 Annihilation of dislocations and their arrangement into low energy
configurations.
 Note: not all point defects and dislocaitons participate in the above
processes.
 It was noted that excess point defects are created during cold work. During
recovery these are absorbed by processes which include (there are other
processes which also may be active):
► at surface or grain boundaries
► or by dislocation climb process.
RECOVERY
 During recovery, random dislocations (statistically stored dislocations) of
opposite sign come together and annihilate each other. However, the
overall reduction in the dislocation density by this process is small.

 Dislocations of same sign arrange into low energy configurations.

► Edge dislocations ‘rearrange’ to form Tilt boundaries
► Screw dislocations ‘rearrange’ to form Twist boundaries.

 The formation of low angle tilt and twist boundaries is termed as

POLYGONIZATION (figure in next page).

 Hence, the overall reduction in dislocation density is small during recovery.

POLYGONIZATION

 During recovery polygonization takes

place.
 In this process, dislocations of the
same sign arrange themselves in a
low energy configuration.
 This leads to the formation of sub-
grain boundaries or low-angle grain
boundaries.
RECRYSTALLIZATION
 During recrystallization, ‘strain free grains’ replace the ‘cold worked grains’.
 For recrystallization we can define a temperature: TRecrystallization (or Trx). Unlike
the usual definitions we encounter in materials science, the definition of Trx
is a little ‘convoluted’ (it involves a percentage and time!).
 TRecrystallization is the temperature at which 50 % of the material recrystallizes in
1 hour.
 The recrystallization tempearture typically is in the range of 0.3-0.5 of the
melting point. Trecrystallization  (0.3 – 0.5) Tm
 Two processes contribute to the formation of strain free grains:
(i) “Nucleation” and growth of new strain free grains and (ii) migration of the
grain boundaries to a region of high dislocation density. Process (ii) does not
involve the nucleation of new grains and during the migration of grain
boundaries to a region of higher dislocation density, dislocation density
reduces (grain boundaries accommodate the excess dislocations).
Region of higher
dislocation density Region of lower
dislocation density
Direction of grain
boundary migration
 The driving force for recrystallization is the free energy difference between the deformed and
undeformed material.
G (recrystallization) = G (deformed material) – G (undeformed material)
 Increased deformation (cold work) leads to a decrease in recrystallization temperature (Trx).
 If the initial grain size is smaller then the recrystallization temperature is lower.
 Higher amount of cold work + low initial grain size leads to finer recrystallized grains.
 The Trecrystallization is a strong function of the purity of the material.
 For very pure materials Trecrystallization is about 0.3 Tm
[Trecrystallization (99.999% pure Al) ~ 75oC ]
 For impure materials Trecrystallization ~ (0.5 – 0.6) Tm
[Trecrystallization (commercial purity) ~ 275oC].
 Impurity atoms tend to segregate to the grain boundary and retard their motion → Solute drag
(can be used to retain strength of materials at high temperatures).
 Second phase particles can also be used to pin down the grain boundary and impede its migration.
ROLE OF SECOND PHASE PARTICLES
ZENER PINNING
 ZENER PINNING

Figure 1:(a) The particles located within a distance of the grain boundary plane
can interact with the boundary.
(b) The forces at the junction between the boundary and the particle. Think of the
particle as a sphere which is intersecting a planar surface. The perimeter defining
the intersection is 2ϖr.cos (θ)
 ZENER PINNING
 Recrystallisation and grain growth involve the movement of grain boundaries. The motion will be
inhibited by second phase particles. The drag on the boundary due to an array of insoluble, incoherent
spherical particles is because the grain boundary area decreases when a boundary intersects the
particle. Therefore, to move away from the particle requires the creation of new surface. The net drag
force on a boundary of energy per unit area due to a particle of radius is given by (Fig. 1), Since r.
sin(θ) = force per unit length
 Force = γ. sin(θ) . 2ϖr.cos (θ)
 Fmax = γϖr at θ = 450
 Suppose now that there is a random array of particles, volume fraction, f with N particles per unit
volume. Note that N = f / (4/3 ϖr3)
 Only those particles within a distance ± can intersect a plane. The number of particles intersected by
a plane of area 1 m2 will therefore be n= 2rN = 3f/2ϖr2
 The drag pressure is then often expressed as P= Fmax. n = 3γf/2r
 This may be a significant pressure if the particles are fine. Anisotropic particles may have a larger
effect if they present a greater surface area for interaction with the boundary.
 A grain of radius r has a volume 4/3ϖr3 and surface area 4ϖr2 . The grain boundary energy
associated with this grain is 4ϖr2 γ where is the boundary energy per unit area and we have taken
into account that the grain boundary is shared between two grains. If follows that:
 Energy per unit volume = 3γ/2r = 3γ/D, where D is the grain diameter.
 It is this which drives the growth of grains with an equivalent pressure of about 0.1 MPa for typical
values of γ =0.3 J/m2 and D= 10 μm. This is not very large so the grains can readily be pinned by
particles (Zener drag).
 ZENER PINNING
 In order to move past the particle some new boundary
must be created, and this is energetically
unfavourable. While the region of boundary near the
particle is pinned, the rest of the boundary continues
trying to move forward under its own driving force.
 This results in the boundary becoming bowed
between those points where it is anchored to the
particles.
total force acting on the particle-boundary interface is
The maximum restraining force occurs when θ = 45° and so Fmax = πrγ .

Given the assumption that all particles apply the maximum pinning force, Fmax, the total
pinning pressure exerted by the particle distribution per unit area of the boundary is

This is referred to as the Zener pinning pressure.

It follows that large pinning pressures are produced by:

•Increasing the volume fraction of particles
•Reducing the particle size
Knowing the concept of recrystallization we are in a position to define hot and cold work

Hot Work and Cold Work  Hot Work  Plastic deformation above TRecrystallization
 Cold Work  Plastic deformation below TRecrystallization
Often the range is further subdivided into Hot, Cold and Warm working as in the figure
Hot Work

0.9  When a metal is hot worked, the conditions of deformation are

Tm such that the sample is soft and ductile. The effects of strain
0.8
hardening are negated by dynamic and static processes (which keep
Tm
0.7 the sample ductile).
Tm  The lower limit of temperature for hot working is taken as 0.6 T m.
0.6
Tm
Warm 0.5
Tm
working 0.4 Recrystallization temperature (~ 0.4 Tm)
Tm
0.3
Tm
0.2
 The effects of strain hardening is not negated. Recovery mechanisms
Cold Work

Tm
0.1 involve mainly motion of point defects.
Tm  Upper limit  0.3 Tm.
Grain growth
Grain growth
 The growth of larger grains at the expense of smaller ones, leading to the increase in the average
grain size is termed as grain growth. (Obviously all the grains cannot grow!).
 This is also called ‘grain coarsening’.
 A related term to this is ‘Ostwald ripening’. Similar processes is observed in the case of
precipitation, wherein larger precipitates grow at the expense of smaller ones, leading to an overall
increase in the size of the precipitates (called precipitate coarsening).
 For grain growth to occur, both the global and the local criteria must be satisfied.
 The global criterion is easy to understand. Grain growth is Globally driven by reduction in grain
boundary energy (per unit volume).
 The local condition is explained in the next page. If we make ‘hexagonal grains’ as in the figure
below, the system will not coarsen.
 Grain growth will lead to a further drop in the strength of the material (i.e. after recrystallization has led to a
considerable drop). The strength of a material depends on the grain size via the Hall-Petch relation
(wherein larger grains imply a lower strength).

A conceptual model of hexagonal

grains, which will not coarsen, as the
local criterion will not be satisfied.
 Locally grain growth is driven by bond maximization (coordination number
maximization). This can be visualized as in the schematics as below. The smaller grains
have a larger curvature. Let us assume that a small grain G1 is in contact with a larger
grain G2. Due to higher curvature an atom at the grain boundary (from G1 side) is
bonded to less number of atoms (3 in the schematic), while a similar atom on the G2
side is bonded to more number of atoms (4 in the schematic). The system can lower its
energy by the jump of an atom from G1 to G2. Such jumps lead to the shift (migration)
in the GB towards the smaller grain (G1 in the current example). This leads to a
shrinkage of the smaller grain (at the benefit of the larger grain).

JUMP
Bonded to
4 atoms

Bonded to Direction of grain

3 atoms boundary migration

G1 G2
 Due to cold work changes occur to almost all physical and mechanical properties.
 The cold worked material is stronger (harder), but is brittle (as noted before).
 The electrical resistance of the material increases due to primarily the increase in point
defect density. (This is mostly reversed during recovery).
 Changes can also be noted in the X-Ray diffraction pattern.
► Laue patterns of single crystals show pronounced asterism → due to lattice curvatures.
► Debye-Scherrer photographs show line broadening → Residual stresses + deformations.

↑ Strength ↑ Hardness
Cold work
↑ Electrical resistance
↓ Ductility

Internal stress
Electical conductivity

Tensile strength

Ductility
Cold work Recovery Recrystallization Grain growth
STRUCTURAL CHANGES
MICROSTRUCTURAL CHANGES