NPG Phase Transformation

Phase Transformation and
Microstructures
During Annealing, Normalising and Hardening
Nilesh Prakash Gurao

Assistant Professor
Materials Science and Engineering
Indian Institute of Technology Kanpur, Kanpur-208016 India
Knowledge Incubation for TEQIP IIT Kanpur

Phase and Phase Diagram
Phase is a region of space of a thermodynamic system
throughout which all physical properties of a material are
essentially uniform
10/23/2015 NRCM X-ray Workshop 2013 2

Phase transformation and Gibbs Phase Rule
A phase transition is the transformation of a thermodynamic

system from one phase or state of matter to another one by
heat transfer
F+P=C+2
where F is degree of freedom,
P is number of phases,
and C is number of components

Metallurgical phase rule
F+P=C+1

Type of phase transformation
1. Diffusion
2. Diffusionless
Phase transformation include

1. Maintaining the type and number of phases (e.g.,
solidification of a pure metal, allotropic transformation,
recrystallization, grain growth)
2. Alteration of phase composition (e.g., eutectoid reaction)
3. Production of metastable phases (e.g., martensitic
transformation)

Change in composition implies atomic rearrangement, which
requires diffusion.
Phase transformation involves: nucleation and growth.
Nucleation is formation of very small amount or nuclei
Growth involves increase in size of the nuclei at the expense of the

surrounding material.

Important deformation processes
Rolling
Wire drawing
Extrusion

The deformed state
Grain changes their shape and there is surprising large increase in

the total grain boundary area
The new grain boundary area has to be created during deformation

by incorporation of dislocations being continuously generated during
deformation
Appearance of internal structure within the grains
Stored energy = sum of energy of all the dislocations and new

interfaces

During deformation, the orientation of single crystals and of
individual grains of a polycrystalline metal changes relative to the
directions of the applied stresses
These changes are not random and involve rotations which are
directly applied to the crystallography of deformation
These rotations lead to the acquisition of preferred orientation, or

texture
Texture becomes stronger as the deformation proceeds

Microstructural hierarchy

Deformed state
Plastic deformation leads to storage of dislocations
Increase in stored energy ∆G = ∆H − T∆S

Slight increase in entropy F = E − TS
Overall free energy increase

in the deformed state
Deformed state is metastable

Residual stress
(a)
Residual stress is that which remains in a body

that is stationary and at equilibrium with its surroundings
Acts at different length scale
Type I macroscopic
Type II mesoscopic intergranular
Type III microscopic intragranular
P. J. Withers, H. K. D. H. Bhadeshia, Materials Science Technology (2001) 17 355

Annealing
A heat process whereby a metal is heated to a specific temperature

/colour and then allowed to cool slowly. This softens the metal which
means it can be cut and shaped more easily. Mild steel, is heated to a
red heat and allowed to cool slowly.
Anisothermal Isothermal
R. E. Reed-Hill, Physical Metallurgy Principles

Physical processes during annealing
G. E. Dieter, Mechanical Metallurgy,

Recovery
Rearrangement of dislocations: Polygonization
Annihilation of point defects
Improvement in conductivity
Little or no change in hardness
Rate of recovery decreases with time

for isothermal annealing

Stress relieving
Type I Residual stress completely removed
Partial relieving of intergranular stress
Stress relieved workpiece retains high hardness of the deformed

microstructure but is more stable than the deformed microstructure
Final step for a product

Recrystallization
Formation of dislocation free microstructure
Nucleation and growth

−Q
RT
Both follow Arrhenius equation Rate = Ae
Activation energy for nucleation and growth
Recrystallization has overlap of both processes
Quantification using Johnson-Mehl-Avarami Kinetics (JMAK)
Monitor fraction of recrystallized grains or hardness

JMAK
N = VN& dτ π
e
Vt = VN& G& 3t 4
3
4π &
e
dVt = G (t − τ )3VN& dτ eVt
3 dVt = dVt (1 − )
V

1 − Vt e Vt
dVt = dVt e ln(1 − Y ) = Y=
1 − Vt / V V V
Y = 1 − exp( − Kt n ) K = πN& G& 3 / 3 and n = 4

ln( − ln[1 − Y (t )]) = ln K + n ln t
JMAK for an aluminium

alloy
Heatherly and Hutchinson, Recrystallization and Related Phenomenon

Deformed and annealed Al-Zn-Mg-Cu alloy
Materials 2014, 7(1), 244-264; doi:10.3390/ma7010244

Annealing of steel
Full annealing
Process Annealing
Stress-Relief annealing
Spherodise annealing
Isothermal annealing
Bright Hub Engineering online resource

1. Full Annealing - The process involves heating the steel to 30 to 50 degrees
Centigrade above the critical temperature of steel and maintaining the
temperature for a specified period of time, then allowing the material to
slowly cool down inside the furnace itself without any forced means of
cooling. Hot Worked sheets, forgings, and castings made from medium and
high carbon steels need full annealing.
2. Process Annealing - This process is mainly suited for low carbon steel. The
material is heated up to a temperature just below the lower critical temperature
of steel. Cold worked steel normally tends to posses increased hardness and
decrease ductility making it difficult to work. Process annealing tends to improve
these characteristics. This is mainly carried out on cold rolled steel like wire
drawn steel, etc.

3. Stress Relief Annealing - Large castings or welded structures tend to possess
internal stresses caused mainly during their manufacture and uneven cooling.
This internal stress cause brittleness at isolated locations in the castings or
structures, which can lead to sudden breakage or failure of the material. This
process involves heating the casting or structure to about 650 Degree
centigrade. The temperature is maintained constantly for a few hours and
allowed to cool down slowly.
4. Spherodise Annealing - This is a process for high carbon and alloy steel in order
to improve their machinability. The process tends to improve the internal
structure of the steel. This can be done by two methods
a. The material is heated just below the lower critical temperature about 700
Degree centigrade and the temperature is maintained for about 8 hours and
allowed to cool down slowly.
b. Heating and cooling the material alternatively between temperatures just
above and below the lower critical temperature.

5. Isothermal Annealing – This is a process where is steel is heated above the
upper critical temperature. This causes the structure of the steel to be converted
rapidly into austenite structure. The steel is then cooled to a temperature below
the lower critical temperature about 600 to 700 Degree Centigrade. This cooling is
done using a forced cooling means. The temperature is then maintained constant
for a specified amount of time in order to produce a homogenous structure in the
material. This is mainly applicable for low carbon and alloy steels to improve their
machinability.
6. Inter and sub critical Annealing – heating steels to below the full annealing
temperature (typically 723-910°C) according to composition. A prolonged soak is
followed by cooling to ambient temperature. At a temperature for steels of
typically 650-720°C, allowing a prolonged soak before cooling to ambient
temperature.

7. Homogenization Annealing – applied to both ferrous and non-ferrous materials
and is a prolonged high-temperature soak intended to break down segregation in
the material’s structure.
8. Solution Annealing – applied commonly to austenitic stainless steels, typically at

1010-1150°C. With unstabilised grades, the treatment must be followed by fast
cooling or quenching. It is applied as a softening process during manufacture or to
optimise corrosion resistance (e.g. after welding).

Normalizing
Normalizing is an austenitizing heating cycle followed by cooling in still

or slightly agitated air
The workpiece is heated to a temperature about 55 °C (100 °F) above

the upper critical line of the iron-iron carbide phase diagram
o above Ac3 for hypoeutectoid steels
o above Acm for hypereutectoid steels.
To be properly classed as a normalizing treatment, the heating portion

of the process must produce a homogeneous austenitic prior to cooling.
Normalizing is also frequently thought of in terms of microstructure

The areas of the microstructure that contain about 0.8% C are
pearlitic (lamellae of ferrite and iron carbide). The areas that are low in
carbon are ferritic (body-centered cubic, or bcc, crystal structure).
In hypereutectoid steels, proeutectoid iron carbide first forms along

austenite grain boundaries. This transformation continues until the
carbon level in the austenite reaches approximately 0.8%, at which
time a eutectoid reaction begins as indicated by the formation of
pearlite
Air-hardening steels are excluded from the class of normalized

steels because they do not exhibit the normal pearlitic microstructure
that characterizes normalized steels.

Hardening
Increase in hardness or strength on heat treatment
Precipitation hardening
Grain size hardening
Hardening due to phase transformation
Martensitic hardening

Hardening
Martensitic transformation is a hardening mechanism specific for steel. The
steel must be heated to a temperature where the iron phase changes from ferrite
into austenite, i.e. changes crystal structure from bcc to fcc.
In austenitic form, steel can dissolve a lot more carbon. Once the carbon has
been dissolved, the material is then quenched. It is important to quench with a
high cooling rate so that the carbon does not have time to form precipitates of
carbides. When the temperature is low enough, the steel tries to return to the low
temperature crystal structure BCC.

This change is very quick since it does not rely on diffusion and is called a
martensitic transformation. Because of the extreme supersaturation of solid
solution carbon, the crystal lattice becomes bct (body centred tetragonal )
instead.
This phase is called martensite, and is extremely hard due to a combined

effect of the distorted crystal structure and the extreme solid solution
strengthening, both mechanisms of which resist slip dislocation.
Tempering operation is followed to obtain optimum hardness and sufficient

toughness

10/23/2015
Thank you
NRCM X-ray Workshop 2013
31

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Phase Transformation and

Nilesh Prakash Gurao

Knowledge Incubation for TEQIP IIT Kanpur

10/23/2015 NRCM X-ray Workshop 2013 2

A phase transition is the transformation of a thermodynamic

10/23/2015 NRCM X-ray Workshop 2013 3

10/23/2015 NRCM X-ray Workshop 2013 4

Phase transformation include

10/23/2015 NRCM X-ray Workshop 2013 5

Phase transformation involves: nucleation and growth.

Nucleation is formation of very small amount or nuclei

Growth involves increase in size of the nuclei at the expense of the

10/23/2015 NRCM X-ray Workshop 2013 6

Knowledge Incubation for TEQIP IIT Kanpur

Grain changes their shape and there is surprising large increase in

The new grain boundary area has to be created during deformation

Appearance of internal structure within the grains

Stored energy = sum of energy of all the dislocations and new

Knowledge Incubation for TEQIP IIT Kanpur

These rotations lead to the acquisition of preferred orientation, or

Texture becomes stronger as the deformation proceeds

Knowledge Incubation for TEQIP IIT Kanpur

Knowledge Incubation for TEQIP IIT Kanpur

Increase in stored energy ∆G = ∆H − T∆S

Overall free energy increase

Deformed state is metastable

10/23/2015 NRCM X-ray Workshop 2013 11

Residual stress is that which remains in a body

Acts at different length scale

Type II mesoscopic intergranular

Type III microscopic intragranular

P. J. Withers, H. K. D. H. Bhadeshia, Materials Science Technology (2001) 17 355

Knowledge Incubation for TEQIP IIT Kanpur

A heat process whereby a metal is heated to a specific temperature

R. E. Reed-Hill, Physical Metallurgy Principles

Knowledge Incubation for TEQIP IIT Kanpur

G. E. Dieter, Mechanical Metallurgy,

Knowledge Incubation for TEQIP IIT Kanpur

Rearrangement of dislocations: Polygonization

Annihilation of point defects

Little or no change in hardness

Rate of recovery decreases with time

10/23/2015 NRCM X-ray Workshop 2013 15

Type I Residual stress completely removed

Partial relieving of intergranular stress

Stress relieved workpiece retains high hardness of the deformed

Final step for a product

Knowledge Incubation for TEQIP IIT Kanpur

Formation of dislocation free microstructure

Nucleation and growth

Activation energy for nucleation and growth

Recrystallization has overlap of both processes

Quantification using Johnson-Mehl-Avarami Kinetics (JMAK)

Monitor fraction of recrystallized grains or hardness

Knowledge Incubation for TEQIP IIT Kanpur

Knowledge Incubation for TEQIP IIT Kanpur

Y = 1 − exp( − Kt n ) K = πN& G& 3 / 3 and n = 4

JMAK for an aluminium

Heatherly and Hutchinson, Recrystallization and Related Phenomenon