Lecture 5: Structural Transformation Driven by Strain Energy

MATE 507, Spring 2014, Prof.
Steve May
Lecture 5: Structural transformation driven by strain energy
Goals: 1) How is energy stored in cold work

2) How to measure this stored energy
3) Basics of Recovery
4) Basics of Recrystallization
1
MATE 507, Spring 2014, Prof. Steve May
Structural transformation driven by strain energy
Recovery: Reduction of dislocation/defect concentrations, also rearrangement of dislocation

structure
Recrystallization: Formation and growth of new strain-free grains, requires motion of high
angle grain boundaries (next lecture)
Morphology of epitaxial films: Strain induced changes from 2D to 3D (islands) morphology in

thin films (next lecture)
2
Plastic deformation
Cold work (strain hardening) – plastic deformation to increase strength
rolling wire drawing
3
Plastic deformation
Cold work (strain hardening) – plastic deformation of a metal to increase strength
% CW = (A0 – AD)/A0
4
Callister, Materials Science and Engineering: An Introduction
Energy of plastic deformation
EW = EQ + ES
HS ~ ES
5
Energy of plastic deformation: Measurement techniques
Single step method: Measure temperature change (EQ) during

deformation (EW)
EW = EQ + ES
Obtained from Measured with

stress-strain curve thermocouple
(tension
measurement)
6
R. O. Williams, Acta. Met. 12, 745 (1964)
Single step method: Measure temperature change (EQ) during

deformation (EW)
Results from copper single crystals
7
Two step method: Isothermal annealing
Anneal deformed sample in

calorimeter.
Measure temperature difference

between sample and jacket of
calorimeter as a function of time.
Sample gets hotter than jacket as it

releases stored energy.
This method also gives information

about kinetics of defect removal.
8
Martin, Doherty and Cantor,
Two step method: Isothermal annealing
Anneal deformed sample in

calorimeter.
Measure temperature difference

between sample and jacket of
calorimeter as a function of time.
Sample gets hotter than jacket as it

releases stored energy.
This method also gives information

about kinetics of defect removal. Main problem with technique: how much energy
is released before the start of the anneal?
9
Martin, Doherty and Cantor,
Two step method: Anisothermal annealing
Differential thermal analysis
T
Deformed and reference sample in same
chamber, heat chamber.
Deformed Reference
Measure temperature of both samples,
sample sample difference will correspond with stored
energy
TD TR
10
White and Koyama, Rev. Sci. Instrum. (1963)
Differential power analysis
Heat both deformed and reference

sample at same rate (°C/min).
Deformed Reference
Measure power need to maintain
sample sample heating rate. Difference in power will
correspond to stored energy.
T(PD) T (PR)
11
12
Nanocalorimetry: Measurement of very small samples is now possible
13
Two step method: Solution/reaction calorimetry
Dissolve both deformed and reference

sample in liquid metal or react samples
with another material.
Difference in heat effects will be due to

stored energy in deformed material.
14
Kravitz and Leach, J. Sci. Instrum. 1965
Where is the energy stored?
Two main mechanisms:

1. Lattice strain/deformation
2. Introduction of defects/dislocations
Point defects
Planar defects
Dislocations
15
Stored energy of dislocations
Energy of dislocation per length: Edis = (mb2/4pK) ln(r/r0) + core energy
~ (mb2/10)
Energy per volume: Edis = r(mb2/4pK) ln(r/r0)
16
Variables affecting stored energy
1. Mechanism of deformation
- Tension, compression, torsion, rolling, wire drawing
Each method imparts a different amount of strain energy per amount
of work done.
75Au-25Ag
Also, reduced deformation temperature leads to increased stored energy

17
Bever et al, Prog. Mat. Sci. 1973
2. Material composition
In general, stored energy increases with increasing bond strength (melting temperature)
18
3. Solute effects
Ag-Au
Ni-Cu deformed at 4 K
19
4. Grain boundary – more stored energy in materials with fine grain

boundaries
5. Precipitates – addition of second phase precipitates increases the
amount of stored energy
20
This stored strain energy can be used to drive structural transformations:
Recovery: Reduction of dislocation/defect concentrations, also rearrangement of dislocation

structure, occurs throughout sample
Recrystallization: Formation and growth of new strain-free grains, requires motion of high
angle grain boundaries, occurs via nucleation and growth
21
P. G. Shewmon, Transformations in Metals, 1969
Recovery
Annealing to reduce or redistribute the concentration of point defects

and dislocations.
22
Recovery

and dislocations.
EA point defects < EA dislocations < EA planar defects
Main effect of recovery is reduction of

point defects and dislocations
23
Recovery

and dislocations.
Simple model: dx/dt = -ax, where x is the macroscopic property related

to defect/dislocation concentration. a ~ A exp (-E/kT) is the probability
of eliminating a given defect/dislocation per unit time.
24
Recovery

and dislocations.
However most recovery kinetics don’t follow this form:

1. There are many different types of imperfections that are affected
during recovery.
2. The driving force is reduced with time.
Recovery is complicated and nearly impossible to quantify due to the many variables.
25
Recovery
Different metals deformed at 78K.

Multiple energy release peaks
indicates many different types of
imperfections are present.
26
Recovery
Attempts to quantify recovery aimed at isolating single defect. For

example vacancies.
Electrical resistivity is strongly dependent on vacancies. Measure

resistivity during recovery to learn about vacancy elimination rates.
27
Recovery
Attempts to quantify recovery aimed at isolating single defect. For

example vacancies.
Electrical resistivity is strongly dependent on vacancies. Measure

resistivity during recovery to learn about vacancy elimination rates.
Recovery kinetics in copper
28
Cotterill and Mould, Recrystallization and Grain Growth in Metals, 1976
Recovery
In deformed samples: vacancies, dislocations, grain boundaries, etc all

contribute to changes in resistivity.
Recrystallization
Copper deformed at 78°C
Recovery
29
Recovery
How are defect/dislocation densities reduced?
Vacancies:
30
Recovery
Dislocations:
31
Recovery
Change in dislocation
Dislocations: separation with time
dx/dt = -2bfm
32
J. C. M. Li, Recrystallization, grain growth and texture 1966
Recovery
Example: ion implantation (Si) in poly-Si using nanocalorimetry
33
Recovery
Example: ion implantation (Si) in poly-Si using nanocalorimetry
Example illustrates how complex recovery can be.
34
Recrystallization (compared to recovery)
Formation and growth of new strain-free grains, requires motion of high

angle grain boundaries, occurs via nucleation and growth, ~0.3TM
35
Recrystallization
Microscopic view of recrystallization
Deformed sample Nucleation of strain free grains Growth of strain free grains
36
Recrystallization
Microscopic view of recrystallization
37
Recrystallization (compared to recovery)
Formation and growth of new strain-free grains, requires motion of high

angle grain boundaries, occurs via nucleation and growth, ~0.3TM
Recovery kinetics in iron
N G
Recovery begins immediately Recrystallization
38
Recrystallization
Kinetics of recrystallization follow Avrami equation: f = 1 – exp(-ktn)
N G
39
Recrystallization
Qualitative rules of recrystallization:
1. Recrystallization temperature decreases as the amount of strain (stored

energy) increases.
copper
40
Recrystallization

energy) increases.
2. At higher temperatures, recrystallization process occurs faster.
41
Recrystallization

energy) increases.
2. At higher temperatures, recrystallization process occurs faster.
3. For a given amount of stored energy, the recrystallization temperature
decreases with: reduced cold working temperature, faster rate of heating to
anneal temperature, smaller initial grain size
42
Recrystallization
Nucleation of recrystallization: Application of classic nucleation theory
43
Recrystallization
Classic nucleation applied to recrystallization
Copper: g for a high angle grain boundary: 535 erg/cm2 = 3.3 x 1014 eV/cm2
ES = 3 cal/mol x 2.6x1019 eV/cal x 1 mol/63.5 g x 8.94 g/cm3 =

1.1 x 1019 eV/cm3
Es = 7.3 x 1018 eV/cm3
44
Recrystallization
Classic nucleation applied to recrystallization
Copper: g for a high angle grain boundary: 535 erg/cm2 = 3.3 x 1014 eV/cm2
ES = 3 cal/mol x 2.6x1019 eV/cal x 1 mol/63.5 g x 8.94 g/cm3 =

1.1 x 1019 eV/cm3
Es = 7.3 x 1018 eV/cm3
r* = 2g/ES
Does the classic model of nucleation describe recrystallization?

45
Recrystallization
Nucleation of recrystallization is therefore different from precipitation:
Experimental observations:
1) Nuclei form in regions with the largest amount of stored energy.
The stored energy is the driving force so this makes sense.
46
Cahn, Physical Metallurgy, 1996.
Recrystallization
2) Orientation of nuclei are often correlated with the local orientation
where they form.
Suggests that nuclei are not entirely new entities but rather
grow out of a pre-existing region.
47
Recrystallization
2) Orientation of nuclei are often correlated with the local orientation
where they form.
3) Nuclei exhibit high-angle boundaries with the surrounding grains.
From a nucleation viewpoint this is surprising.
48
Recrystallization
Nuclei exhibit high-angle boundaries with the surrounding grains
A high angle boundary has a larger g than a low angle boundary.
So why are high angle boundaries necessary?

49
Recrystallization
High angle boundaries allow for greater interfacial mobility
v = M DG
M = Abn/kT exp(-DGA/kT)
A – accommodation factor (0 – 1)
At incoherent high angle grain

boundaries, A is much bigger than at
coherent low-angle boundaries
50
Recrystallization
Nucleation of recrystallization: Subgrain nucleation
Crucial that the new grain has high-angle boundary with adjacent grains.
51
Martin, Doherty and Cantor
Recrystallization
Nucleation of recrystallization: Strain-induced boundary migration
Nuclei start at existing grain boundaries and grow into adjacent

grains. No new grain formed.
Boundary before recrystallization
52
Beck and Sperry, J. Appl. Phys, 21, 150 (1950)
Recrystallization
Nucleation of recrystallization: Subgrain coalescence

High angle
boundary
Low angle
boundary
53
Cotterill and Mould, Recrystallization and Grain Growth in Metals, 1969; Cahn, Physical Metallurgy, 1996.
Recrystallization
Growth
v = M DE –> DE difference in stored energy between two grains
M = Abn/kT exp(-DGA/kT)
Interface
a b
DGA
54
Recrystallization
Growth
Factors that inhibit grain growth:

1. Solute atoms
2. Second phase precipitates (Zener drag)
55

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MATE 507, Spring 2014, Prof.

Lecture 5: Structural transformation driven by strain energy

Goals: 1) How is energy stored in cold work

Structural transformation driven by strain energy

Recovery: Reduction of dislocation/defect concentrations, also rearrangement of dislocation

Morphology of epitaxial films: Strain induced changes from 2D to 3D (islands) morphology in

Cold work (strain hardening) – plastic deformation to increase strength

rolling wire drawing

Cold work (strain hardening) – plastic deformation of a metal to increase strength

Energy of plastic deformation

Energy of plastic deformation: Measurement techniques

Single step method: Measure temperature change (EQ) during

Obtained from Measured with

Energy of plastic deformation: Measurement techniques

Single step method: Measure temperature change (EQ) during

Results from copper single crystals

Energy of plastic deformation: Measurement techniques

Two step method: Isothermal annealing

Anneal deformed sample in

Measure temperature difference

Sample gets hotter than jacket as it

This method also gives information

Energy of plastic deformation: Measurement techniques

Two step method: Isothermal annealing

Anneal deformed sample in

Measure temperature difference

Sample gets hotter than jacket as it

This method also gives information

Energy of plastic deformation: Measurement techniques

Two step method: Anisothermal annealing

Differential thermal analysis

Energy of plastic deformation: Measurement techniques

Two step method: Anisothermal annealing

Differential power analysis

Heat both deformed and reference

Energy of plastic deformation: Measurement techniques

Two step method: Anisothermal annealing

Nanocalorimetry: Measurement of very small samples is now possible

Energy of plastic deformation: Measurement techniques

Two step method: Solution/reaction calorimetry

Dissolve both deformed and reference

Difference in heat effects will be due to

Where is the energy stored?

Two main mechanisms:

Stored energy of dislocations

Energy of dislocation per length: Edis = (mb2/4pK) ln(r/r0) + core energy

Energy per volume: Edis = r(mb2/4pK) ln(r/r0)

Variables affecting stored energy

Also, reduced deformation temperature leads to increased stored energy

Variables affecting stored energy

Variables affecting stored energy

Variables affecting stored energy

4. Grain boundary – more stored energy in materials with fine grain

This stored strain energy can be used to drive structural transformations:

Recovery: Reduction of dislocation/defect concentrations, also rearrangement of dislocation

Annealing to reduce or redistribute the concentration of point defects

Annealing to reduce or redistribute the concentration of point defects

EA point defects < EA dislocations < EA planar defects

Main effect of recovery is reduction of

Annealing to reduce or redistribute the concentration of point defects

Simple model: dx/dt = -ax, where x is the macroscopic property related

Annealing to reduce or redistribute the concentration of point defects

However most recovery kinetics don’t follow this form: