Intro to Grain Refinement

Through Thermomechanical Treatment

What is Thermomechanical Treatment?

For most commercial products in steel industry, the external shapes are the result of hot-
deformation, such as hot rolling. The mechanical properties are obtained from alloy design and by
heat treatment after rolling. Improvement in mechanical properties is just considered as the alloying
effect on heat treatment process.

In forging process, the materials properties directly quenched after forgings then tempered are
sometimes improved compared with material air-cooled after forging and then quenched and
tempered. In this cases, the hot-deformation itself become necessary as the constituent of the
heat treatment and the metallurgical changes caused by hot-deformation result in additional
beneficial effects on the properties of the steel.

The thermomechanical treatment is a technique designed to improve the mechanical properties of

material by controlling the hot-deformation process which originally were designed the required
external shape of the product. Controlled-rolling, controlled-cooling and direct quenching are typical
examples of thermomechanical treatment. Such processing gives save energy in steel
manufacture by minimizing or even eliminating the heat treatment after hot-deformation, thus
increasing the productivity for high-grade steel. In this process we control the temperature (T),
strain (ε), strain rate (ε∗), flow stress (σ), and time (t) .So we can define that thermomechanical
treatment is a process of changing the microstructure of materials by heat treatment and
mechanical working as combination of the process.
Recovery, Recrystallization and Grain Growth
During recovery, some stored internal strain energy is relieved by virtue of dislocation motion, as a
result of enhanced atomic diffusion at the elevated temperature. There is some reduction in the
number of dislocation (called dislocation annihilation) and dislocation configurations are produced
having low strain energies. In addition, the strength of the material will decrease.

Even after recovery is complete, the grain is still in relatively high strain energy state.
Recrystallization is the reformation of a set grains with relatively high strain energy stored into
anew set of strain free and equiaxed grains (having approximately equal dimension in all direction),
that has low dislocation density and characteristic of precold-work condition. Here the words high
strain energy stored is the main things that force to produce the new grain structure. Thus,
recrystallization of cold work metals may be used to refine the grain structure.

Figure 2.1 the influence of annealing temperature on the tensile strength and ductility
Grain structure during recovery recrystallizaaation and grain growth.

During recrystallization, the mechanical properties that were changed as result of cold working are
stored to their precold-work values, that is the metal becomes softer, weaker, yet more ductile.
Than some heat treatments are designed to allow the recrystallization occurs.

The influence of temperature is demonstrated in figure 2.1, which plot tensile strength and ductility
(at room temperature) of brass alloy as a function of the temperature and for a constant heat
treatment time of one hour. The grain structures found at various stage of process are also
presented schematically.

The recrystallization behavior of a particular metal alloy is sometimes in term of a recrystallization

temperature. Typically it is between one third and one half of the absolute melting temperature of a
metal or alloy and depends on several factors, including amount of prior cold working and the purity
of the alloy. Increasing the percentage of cold work enhances the rate of recrystallization, with the
result that the recrystallization temperature is lowered, this effect is shown in figure 2.2.

After recrystallization complete, the strain free grains will continue to grow if a metal specimen is
left at the elevated temperature, this phenomenon called grain growth. Grain growth does not
need to be preceded by recovery and recrystallization, it may occur in all polycrystalline materials,
metals and ceramics are alike.

As grain increase in size, the total boundary area decreases, yielding an attendant reduction in the
total energy, this is the driving force for grain growth.

Grain growth occurs by migration of grain boundaries. Obviously, not all grains can enlarge, but
large ones grow at the expanse of small ones that shrink. Thus the average grain size increases by
time and at any particular instant there will exist a range of grain size. Boundary motion is just the
short-range diffusion of atom from one side to the boundary of the other. The direction of boundary
movement and atomic motion are opposite to each other, as shown in figure 2.3

Figure 2.3 Schematic representation of grain growth

via atomic diffusion.

The mechanical properties at room temperature at room temperature of a fine grained metal are
usually superior (high strength and toughness) to those of coarse-grained ones. If a grain structure
of a single phase alloy is coarse than that desire, refinement may be accomplished by plastically
deforming the material, then subjecting to a recrystallization heat treatment.

Figure 2.4, the logarithmic of grain diameter versus the logarithmic

of time for grain growth in brass at several temperatures
 Figure 2.5 three stages of the controlled rolling process and the changes in
microstructure accompanying each stages.

The major purpose of controlled rolling process is to refine the grain to enhance both strength and
toughness. Controlled rolling process is usually divided into three stages. Figure 2.5 illustrate these
stages, the micro structural changes accompanying deformation in each stages :
1. The deformation at recrystallization temperature range. The austenite grain is refined by
repeated recrystallization. A small austenite grain size obtain by recrystallization at this
state leads to refinement of ferrite grain. In general recrystallized austenite grain size
decrease rapidly with an increase in the amount of rolling reduction and reaches a limiting
value which limit the degree of ferrite grain refinement achieved by austenite
recrystallization.
2. The deformation at the unrecrystallizaed temperature range. The austenite grains are
elongated and deformation structures are introduced within the grains. The deformation in
this stage substantially increases the nucleation rate at austenite grain boundaries and
within austenite grains. This intra granular nucleation of ferrite is one of the most important
aspects of control rolling process. Microallooying elements such as niobium and titanium,
etc, can increase the recrystallization temperature of austenite.
3. The deformation in the intercritical area. The austenite is further work hardened and
deformation of ferrite produces substructures.
Accelerated cooling after hot-rolling is currently being recognized as further advanced
thermomechanical treatment in the hot-rolling process. The cooling process is characterized by
accelerated cooling in austenite to ferrite transformation range just after controlled-rolling. It has
been shown that the accelerated cooling refines the ferrite grains size and thus further improves
both the strength and toughness.

Dynamic Recrystallization
Steels are usually deformed by slip at room temperature, and work-harden by the increase of the
dislocation density. On the other hand at the elevated temperature both slip mechanism and the
creep phenomenon occur when the material is subjected to low strain rate. Creep is really depends
on the temperature (T) and strain rate (ε*). Slip in creep deformation rise from the movement of
dislocation accompanying the dragging of solute atoms.
In the case of deformation at high strain rates –such as hot-rolling of γ-- in the grain boundary
sliding is hardly occur even at elevated temperature, only the slip take place by the movement of
dislocation without dragging effect of solute atoms. However, the recovery occurs for some extent
during work hardening. When the dislocation density is increase at a certain value, the
recrystallization can take place during deformation. Recovery and recrystallization during this time
called ‘dynamic recovery’ and ‘dynamic recrystallization.

When the steady state deformation occurs during initial work-hardening and the true-stress true
strain curve such as in Figure 2.6 is obtained. In the stage of steady state deformation, the work
hardening and the softening due to dynamic recrystallization are balance. Hence the true stress-
true strain curve remained constant.

For dynamic recrystallization. The dislocation density is gradually increase and finally, the
recrystallizationstarts to occur during deformation. The true stress in lowered beyond the peak of
the curve, and reach a steady state condition for a certain level. Here the work hardening and
softening (due to the recrystallization) are balance. The schematic of true strain – true stress is
shown in Figure2.6 (b). In Figure 2.6 (b) the range of strain value up to about 0.7 εp. form of work
hardening region. The strain between 0.7 εp and εs (strain when steady state deformation starts
)forms the partially dynamic recrystallization and the strain rate after εs, show the partial steady
state dynamic recrystallization.
 Figure 2.6 schematic illustrations of two types true strain-true stress curves
accompanying the steady state deformation at elevated temperature

Figure 2.7 shows the change in optical microstructure with strain in Fe with 31% Ni, 0,3 %C
austenitic alloy with was tensile-deformated at 1000OCat strain rate of 1.7 X 10-2/s.
Dynamic recrystallization becomes easier when the initial grain size do of γ is smaller. Therefore,
in the case of fine initial grain size, εp and εs become small vent at deformation under the same Z
(zenner-holomon parameter) condition. However, σp and σs are independent of do , the average

grain size d of dynamically recrystallized grain is only function of Z an it is expressed as

follow:
d = C1 ZC2
Z = ε∗ exp (Q/RT)
Where :
d = the average dynamic recrystallized grain size
Z = zenner-holomon parameter
C = constant
ε∗= strain rate
Q = activation energy for deformation (J/mol)
R = universal gas constant (J/mol)
T = temperature (K)

It should be noted that d is independent to do .

 Figure 2.7 Optical micrograph, showing the formation process of dynamically recrystallized γ in Fe-31% Ni,0.3% C
austenitic alloy deformed at 1000OC. 1.7 X 10-2 /s. (a) ε = 0, (b) ε = 0.08, (c) ε = 0,24, (d) ε = 0.40

TABLE 2.1 Approximate values of C1 and –C2

Material C1 -C2 Q (kj/mol)
Low alloy carbon steel 5 x 10-4 0.30--0.35 200
Niobium steel 2 x 10-6 0.41 330
High alloy steel 10-5 ~10-6 0.35--0.40 330—370
18—8 stainless steel 4 x 10-7 0.40 435

.
Figure 2.8 static and dynamic recrystallization

Static Recrystallization
When the hot-deformation is finished at work-hardening stage figure 2.6 (b), the work hardened γ is
softened by the usual static recrystallization by the isothermal holding after deformation.
However, if the strain is too small, the recrystallization cannot occur only the recovery
occur. On the other hand, when the specimen is isothermally held after deformation to the
range of a steady state deformation, in which the dynamic recrystallization has occurred,
the recrystallization and grain growth can occur continuously during holding aafteer hot
deformation. Such a recrystallization called metadynamic recrystallization or post
metadynamic recrystallization, i.e. the dynamically recrystallized structure is further
softened by the metadynamic recrystallization. When specimen is deformed in the range
of (II) figure 2.6 (b), in which the work hardened γ and dynamically recrystallized γ have
coexisted, the static recrystallization occurs in work hardened γ and the metadynamic
recrystallization occurs simultaneously in dynamic recrystallized γ.
In case of rolling by hot strip in which slabs are rolled into several passes, the static restoration
process occur during interval between rolling pass has a great influence on the deformation of
each subsequence pass.

Fractional softening X occurring during isothermal holding right after hot-deformation can be
evaluated by the two step deformation test from the equation bellow :
σ m − σ y2
X =
σ m − σ y2

where σm is the flow stress before unloading,σy2 is the yield stress after reloading after holding the
specimen under various periods of time an σy1 is the initial yield stress.
The statically average recrystallized grain size is expressed as below :
d rex =C3ε−0.5 do Z0.06
where :
d rex = The statically average recrystallized grain size
Z = zenner-holomon parameter
C = constant
ε= strain

Nucleation Sites Density for Recrystallization of New Grains.

To obtain finer grains we need as many as possible nucleation site for recrystallization of new
grains. There are three kind of nucleation site will be produced along the mechanical working, they
are :
1. The increasse in the grain surface area by elongated grains
2. T the formation of ledges on the austenite grain boundaries which multiply the number of
nucleation sites on the grain boundary.
3. the formation of additional nucleation sites inside the austenite grains such as annealing
twins, deformation bands, etc.
By increasing the nucleation site, means we increase the nucleation rate and obviously we will
obtain the finer grain.

Figure 2.9 The change of grain, (a) before rolling (b) after rolling

Figure 2.10, Schematic drawing showing α nucleation at ledge on deformed γ grain boundaries

(a) a ledge of grain boundary, (b) α nucleation at the ledge

Effect of Microalloying Elements on Grain Refinement Process
The effect of alloying element on the restoration process during or after hot deformation is very
important. Microaddition of Niobium and titanium causes a remarkable retardation effect on
recrystallization due to suppression of grain boundary migration. The suppression of grain
boundary migration due to microalloying is cause by either :
1. The solute dragging effect due to segregation of microalloying elements to the boundary
2. Pinning effect due to precipitate of carbonitride of alloying elements at grain boundaries.
As examples, molybdenum to the γ grain boundaries, resulting the suppression of grain boundary
migration. Niobium and Titanium are precipitated as fine Carbonitride particles and this precipitates
suppress the grain boundary migration by the pinning effect.In Niobium carbonitide precipitation,
which can stops static recrystallization during hot rolling Niobuim micro alloyed steel. Such
precipitation is accelerated by deformation, hence the thermomechanical history of the steel must
be followed to be able to determined the on set of precipitation. Such precipitation will so slow
down recrystallization that it can be considered to have stopped within practical rolling time. Figure
2.12 illustrate the interaction of Nb(C,N) precipitation and static recrystallization under isothermal
conditions. The three different prior deformation show how sensitive the interaction is to the
processing condition.
Figure 2.12, interaction of strain induced precipitation and static recrystallization under isothermal holding condition
(a) ε =0.022,ε∗=16.8/s,TDEFOR =980Oc,(b) ε =0.20, ε∗=17.4/s,TDEFOR =962OC (c) ε =0.17, ε∗ =18.1/s, TDEFOR = 940OC

conclusion
Above we have discussed about recovery, recrystallization, grain growth, dynamic and static
recrystallization hot deformation of austenite, nucleation site, and strain induced precipitation.
Grain refinement is about them.
And it mention above that all of them are function of temperature (T), strain (ε), strain rate (ε∗),
flow stress (σ), and also time (t). Consequently the modeling is needed to predict the stage of
grain refinement process in order to control the process well, to obtain a finer grain to strengthen
and toughen the materials.

References
1. Imao Tamura, Kyoto University; Hiroshi Sakine, Nippon steel Corporation; Tomo Tanaka,
Kawasaki Steel Corporation; Nipon Kokan Corporation : Thermomechanical Processing of
High-Strength Low-Alloy Steel. Butterworth &Co.(Publishers) Ltd. 1988
2. Callister, Jr. William D: Materials Sience and Engineering. John Willey &Sons, Inc. 1997