Chapter 9c Creep

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CREEP

Review of plastic deformation and


failure
Creep Mechanisms (and Maps)
Creep Resistant Materials MATERIALS SCIENCE
& A Learner’ s Guide
Creep in Nanomaterials ENGINEERING
AN INTRODUCTORY E-BOOK
Superplasticity Anandh Subramaniam & Kantesh Balani
Materials Science and Engineering (MSE)
Superplascity in Nanomaterials Indian Institute of Technology, Kanpur- 208016

George E Dieter
McGraw-Hill Book Company, London (1988)
Mechanisms / Methods by which a can Material can

Elastic deformation
Chemical /
Creep Physical
Fatigue Electro-chemical
Plastic degradation
Fracture degradation
deformation
Microstructural
Twinning changes
Wear
Slip Twinning
Corrosion Erosion
Phase transformations
Oxidation
Grain growth

Particle coarsening
Though plasticity by slip is the most important mechanism of plastic deformation,
there are other mechanisms as well
:

Plastic Deformation in Crystalline Materials

Slip Twinning Phase Transformation Creep Mechanisms


(Dislocation
motion) Grain boundary sliding
+ Other Mechanisms
Vacancy diffusion
Grain rotation
Dislocation climb
High-temperature behaviour of materials
Designing materials for high temperature applications is one of the most challenging
tasks for a material scientist.
Various thermodynamic and kinetic factors tend to deteriorate the desirable
microstructure. This is because kinetics of underlying processes (like diffusion) are
an exponential function of temperature.
Hence, a small increase in temperature can prove to be ‘ catastrophic’ .
Strength decreases at high temperature and material damage (e.g. void formation)
tends to accumulate.
Phenomena like creep and accelerated oxidation kick-in.
Cycling between high and low temperature will cause thermal fatigue.
Increased vacancy concentration at high temperatures more vacancies are
thermodynamically stabilized (this will further increase the diffusion rate).
Thermal expansion material will expand and in multiphase materials/hybrids
thermal stresses will develop due to differential thermal expansion of the
components.
High diffusion rate → diffusion controlled processes become important.
Phase transformations can occur this not only can give rise to undesirable
microstructure, but lead to generation of internal stresses.
◘ Precipitates may dissolve.
Grain related:
◘ Grain boundary weakening may lead to grain boundary sliding and wedge
cracking. ◘ Grain boundary migration
◘ Recrystallization / grain growth decrease in strength.
Dislocation related these factors will lead to decrease in strength
◘ Climb
◘ New slip systems can become active
◘ Change of slip system
◘ Decrease in dislocation density.
Overaging of precipitates and precipitate coarsening decrease in strength.
The material may creep (time dependent elongation at constant load/stress).
Enhanced oxidation and intergranular penetration of oxygen.
Etc.
Creep
In some sense creep and superplasticity are related phenomena: in creep we can
think of damage accumulation leading to failure of sample; while in superplasticity
extended plastic deformation may be achieved (i.e. damage accumulation leading to
failure is delayed).
Creep is permanent deformation (plastic deformation) of a material under constant
load (or constant stress) as a function of time. (Usually at ‘ high temperatures’ →
Normally,
lead creepsincreased
at RT). plastic deformation takes place with increasing load (or stress)
In ‘ creep’ plastic strain increases at constant load (or stress)
Usually appreciable only at T > 0.4 Tm
Mechanisms of creep in crystalline materials is different from that in amorphous
materials. Amorphous materials can creep by ‘ flow’ .
At temperatures where creep is appreciable various other material processes may
also active (e.g. recrystallization, precipitate coarsening, oxidation etc.- as
considered before).
Creep experiments are done either at constant load or constant stress and can be
classified based on Phenomenology or underlying Mechanism.

Phenomenology
Constant load (easier)
Creep can
Creep tests can
be
be carried out
classified Constant stress
at
based on Mechanism
Constant load creep curve
In a typical creep test the load and temperature are kept constant and the elongation
is monitored with time. The strain (typically engineering strain) computed from the
elongation is plotted as function of time. The loads employed are typically below the
elastic limit.
Three stages may be observed in such a plot: (i) decreasing rate with time, (ii)
approximately constant rate, (iii) increasing rate with time. These stages have to be
understood keeping in view underlying mechanisms (& necking in stage-III).
The instantaneous strain seen ( 0) is the elastic strain, which Measured
develops on the application of the load.
as strain rate (note that this
Stages of creep strain rate is not the one imposed as
in UTT, but the one which develops in
Stage-I the material)
I II Creep rate decreases with time.
Effect of work hardening more than recove
Strain ( ) →

A technical term
III Stage-II
Stage of minimum creep rate → ~ constan
Work hardening is balanced by recovery.
The distinguishability of the Stage-III
three stages strongly depends Absent (/delayed very much) in constant
on T and stress tests (shown later).
0 → Initial instantaneous strain
Necking of specimen starts in this stage.
0
t → Specimen failure processes set in.
Constant Stress creep curve
In stage-III (due to necking) the engineering stress is no longer a correct measure of
the state of stress. To keep the stress constant, the instantaneous area has to be
taken into account.
If this is done, then the increasing strain rate part is not observed. Note: if load is
kept constant then in stage-III the stress is actually increasing (for the material it is
stress which matters and not load).

I II
Strain ( ) →

III

t →
Effect of stress on the creep curve (constant load)
On increasing the load at which the experiment is conducted: (i) the instantaneous
strain ( elastic) increases, (ii) for a given time (say t1) the strain is more, (iii) the time to
failure (tf) decreases (i.e. as expected, specimens fail earlier).

Fracture

Strain ( ) →

Increasing stress
With increasing load there
is increased initial elastic
strain
increases


0

t1 t →
Effect of temperature
On increasing the temperature at which the experiment is conducted:
(i) the instantaneous strain ( elastic = 0) increases (slightly),
(ii) for a given time (say t1) the strain is more, (iii) the time to failure (tf) decreases.
The instantaneous strain 0 increases with increasing T because of the slight
decrease in the Young’ s modulus (E) of the material.

Strain ( ) →
E↓ as T↑ Increasing T

As decrease in E
with
increases

temperature is
usually small the
0 increase is
also small

0

0
t1 t →
Creep Mechanisms of crystalline materials
Stress and temperature are the two important variables, which not only affect the
creep rate, but also the mechanism operative. Three kinds of mechanisms are
operative in creep:
1 dislocation related,
2 diffusional,
3 grain boundary sliding.
These and their sub-classes are shown in the next page.
At high temperatures the grain boundary becomes weaker than the grain interior and
two grains can slide past one another due to shear stress. The temperature at which
the grain is as strong as the grain boundary is called the
A combination of these mechanisms could also be responsible for the creep strain.
Depending on the stress and temperature other mechanisms of plastic deformation
or microstructural changes may occur concurrently with creep. These include plastic
deformation by slip and dynamic recrystallization.
Deformation mechanism maps can be drawn with homologous temperature (T/Tm)
and normalized shear stress ( /G) as the axis (other combination of variables may
also be chosen for these plots: T/Tm vs shear strain rate, normalized shear stress vs
shear strain rate, etc.). Typically these maps overlay descriptors, which are based
on phenomenology and mechanism.
Creep Mechanisms

Cross-slip

Dislocation related Climb

Glide

Coble creep

Creep Diffusional Nabarro-Herring creep

Dislocation core diffusion creep

Interface-reaction controlled diffusional flow


Grain boundary sliding

Accompanying mechanisms: creep with dynamic recrystallization


Dislocation related mechanisms
Two roles can be differentiated with respect to of dislocations activity: (i) it is the
primary source of strain, (ii) it plays a secondary role to accommodate local strain
(while the major source of strain is another mechanism (e.g. grain boundary sliding).

Cross-sli
p
This kind of creep is observed at relatively low temperatures. Herein screw
dislocations cross-slip and give rise to plastic strain as a
function of time.
Dislocation climb
Edge dislocations piled up against an obstacle can climb to another slip plane and
cause plastic deformation. In response to stress this gives rise to strain as a
function of time. It is to be noted that at low temperatures these dislocations (being
pinned) are sessile and become glissile only at high temperatures.
Rate controlling step is the diffusion of vacancies.
Diffusional creep Nabarro-Herring creep → high T → lattice diffusion

Coble creep → low T → Due to GB diffusion

In response to the applied stress vacancies preferentially move


from surfaces/interfaces (GB) of specimen transverse to the
stress axis to surfaces/interfaces parallel to the stress axis→
thus causing elongation.
Diffusion of vacancies in one direction can be thought of as
flow of matter in the opposite direction.
This process like dislocation creep (involving climb) is
controlled by the diffusion of vacancies (but diffusional creep
does not require dislocations to operate).
The diffusion could occur predominantly via the lattice (at high
temperatures) or via grain boundaries (at low temperatures).
The former is known as Nabarro-Herring creep, while the later is
known as Coble creep.
Diffusion through edge dislocation cores (pipe diffusion) could
play an important role in creep.
Grain boundary sliding

At low temperatures the grain boundaries are ‘ than the crystal interior
and impede the motion of dislocations.
Being a higher energy region, the grain boundaries before the crystal interior.
Above the temperature, due to shear stress at the ‘ local scale’ , grain
boundaries slide past one another to cause plastic deformation.
The relative motion of grain boundaries can lead to wedge cracks at triple lines
(junction of three grains). If these wedge cracks are not healed by diffusion (or slip),
microstructural damage will accumulate and will lead to failure of the specimen.

Wedge crack due to


grain boundary
sliding
Phenomenological descriptions of creep

One of the important descriptions of creep is using the power-law formula. The shear
strain rate is a power function of the shear stress. Clearly this formula is not based
on a mechanism operative, but a fit of data.

Power-law behaviour can arise from:


Only glide at low temperatures (~0.3TM). Here the exponent n ~ 3.
Glide + climb (referred to as climb controlled creep) occurs at higher temperatures.
Above ~0.6TM climb is lattice-diffusion controlled. At low temperatures than this
pipe diffusion may play an important role in creep.
At high stresses (> 10 3G) the power law breaks down. At high stresses the
mechanism changes from climb controlled (creep) to glide controlled (slip).
Deformation Mechanism Maps

Time and temperature are coupled when it comes to processes like diffusion.
At large values of stresses and at low T, the time ‘ available’ is less (as material
‘ immediately’ begins to deform plastically) and creep mechanisms do not have time
(/activation) to operate.
Usually contours of constant strain rate are superimposed on these diagrams (not shown
here). Stress or strain rate can be used as axes (variable). In components (e.g. truss in a
structure, pressure vessel, etc.) stress is ‘ prescribed’ , while in processing (e.g.
extrusion, forging, etc.), strain rate is ‘ prescribed’ .
At high stresses
plastic flow will take
place

Dynamic recrystallization
gives rise to
‘ strain-free’ grains.

At high temperature and


low stress Diffusional
creep dominates
Creep Resistant Materials

The is a growing need for materials to operate at high temperatures (and in some
applications for long times). For example, higher operating temperatures gives
better efficiency for a heat engine. Hence, there is a need to design materials which
can withstand high temperatures.
It is to be noted that material should also be good in other properties for high
temperature applications (like it should possess good oxidation resistance). Factors
like cost, ease of fabrication, density, etc. play an important role in determining the
final choice of a material.
Some of the material design strategies, which work at low temperature are not
useful at high temperatures (e.g. work hardening, precipitation hardening with
precipitates which coarsen, grain size reduction, etc.).
Some strategies which work are: (i) having grain boundaries aligned along the
primary loading axis, (ii) produce single crystal components (like turbine blades), (iii)
use precipitates with low interfacial energy for strengthen (which will not coarsen
easily), (iv) use dispersoids for strengthening.

High melting point → E.g. Ceramics


Creep Dispersion hardening → ThO2 dispersed Ni (~0.9 Tm)
resistance Solid solution strengthening
Single crystal / aligned (oriented) grains
Creep Resistant Materials, cotd..

Commonly used materials → Fe, Ni (including superalloys), Co base alloys.


Precipitation hardening involving ‘ usual precipitates*’ is not a good method as
precipitates coarsen (smaller particles dissolve and larger particles grow
interparticle separation ↑ thus lowering the strength)
Ni-base superalloys have Ni3(Ti,Al) precipitates, which form a low energy interface
with the matrix. This reduces the driving force for coarsening. (Note: other
phenomena like rafting may lead to the deterioration of the properties of such
materials).
Cold work cannot be used for increasing creep resistance, as recrystallization can
occur which will produced strain free crystals.
Fine grain size is not desirable for creep resistance (this is contrary to what is usually practiced for
increasing the low temperature strength)→ grain boundary sliding can cause creep
elongation/cavitation. Hence, the following two strategies can be used:
► Use single crystals

► Aligned/oriented polycrystals → as all the grain boundaries are aligned along the
primary tensile axis, they experience no shear stress and creep is negated.
Creep in Nanomaterials
Due to fine grain size nanostructured materials (grain size in the nanoscale regime)
are expected to: (i) show creep at relatively lower temperatures, (ii) display higher
creep rates for a give temperature, (iii) experience predominance of mechanisms like
grain boundary diffusion and grain boundary sliding. We now see what is actually
seen in experiments.
In nanocrystalline Pd (~40 nm) and Cu (~20 nm), there seemed to be no increase in
creep rate as compared to micron grain sized materials (in some temperature
regimes ). This is in direct contradiction
with the expectation that nanocrystalline materials will experience a higher creep rate.
Studies on Cu (10-25 nm GS), Pd (35-55 nm GS) (TEM showed porocity in sample)
[1]
creep in the low T regime (0.24-0.33 Tm) → low creep rate, low grain growth
creep in the medium T regime (0.33-0.48 Tm) → creep rate decreasing even after
long testing time, grain growth (25 nm → 100s of nm)
Cu creep rates of nc sample was
comparable to micron GS sample
Pd nc sample exhibited lower creep
rates

[1] P.G. Sanders, M. Rittner, E. Kiedaisch, J.R. Weertman, H.Kung, Y.C. Lu, Nanostruct. Mater. 9 (1997) 433.
[2] D.L. Wang, Q.P. Kong, J.P. Shui, Scr. Metall. Mater. 31 (1994) 47.
In some cases the creep rate increased with a decrease in grain size in the
nanoscale regime of grain sizes (e.g. in Ni-P nanocrystalline material the creep rate
of ~30 nm grain sized material was higher than that of 250 nm material [2]).
In cases where high creep rate expected for nanocrystalline materials (e.g. Pd, Cu)
was not observed, the reason attributed are:
(i) presence of low angle grain boundaries and twin boundaries (which are not
prone to sliding and have low diffusivity for vacancies),
(ii) reduced dislocation activity in nanocrystalline samples.
Creep of nc-Ni at RT (GS: 6, 20, 40 nm) [1]:
Smaller grain size (6nm) showed faster creep rate.
Behaviour consistent with Grain boundary sliding controlled by grain boundary
diffusion mechanism.
At high stresses and larger GS (20, 40 nm), dislocation creep was observed.

[1] N. Wang, Z. Wang, K.T. Aust, U. Erb, Mater. Sci. Eng., A 237 (1997) 150.
Superplasticity
Superplasticity

The phenomenon of extensive plastic deformation without necking is termed as


structural superplasticity. Superplastic deformation in tension can be >300% (up to
even 2000%).
Typically superplastic deformation occurs when:
(i) T > 0.5Tm
(ii) grain size is < 10 m
(iii) grains are equiaxed (which usually remain so after deformation)
(iv) grain boundaries are glissile (with a large fraction of high angle grain
boundaries).
Presence of a second phase (of similar strength to the matrix- reduces cavitation
during deformation), which can inhibit grain growth at elevated temperatures helps
(e.g. Al-33%Cu, Zn-22% Al)).
Many superplastic alloys have compositions are close to eutectic or eutectoid points.
Superplastic flow is diffusion controlled (can be grain boundary or lattice diffusion
controlled).
A plot of stress versus strain rate is often sigmoidal and shows three regions:
i. Region-I- low stress, low strain rate regime ( <10 5 /s) m (0.2,0.33)
Sensitive to the purity of the sample. Lower ductility and grain boundary diffusion.
ii. Region-II- intermediate stress & strain rate regime [ (10– 5, 10– 2)]
m (0.4,0.67)
Extended region covering several orders of magnitude in strain rate. Region of
maximum ductility. Strain rate insensitive to grain size and insensitive to purity.
.
Mechanism predominantly grain boundary sliding accommodated by dislocation
activity (Activation energy (Q) corresponding to grain boundary diffusion (Qgb)).
iii. Region-III- high stress & strain rate regime ( > 10 2 /s) m > 0.33
Creep rates sensitive to grain size.
Mechanism intragranular dislocation process (interacting with grain boundaries).
Superplasticity in Nanomaterials

In most cases the superplasticity has not fulfilled the initial ‘ expectations’ .
In many cases superplasticity is only observed in nanocrystalline samples, where it is
already observed in their microcrystalline counterparts.
Superplasticity was observed in nanocrystalline Ni (20 nm grain size) at 0.36Tm (more
than 450 C lower than that for the bulk material) [1].
Nanocrystalline Ni3Al (grain size 50 nm) also became superplastic about 450 C
below its microcrystalline counterparts.
Ni3Al had a ductility of 350% at 650 C (strain rate of 10– 3 /s).
1420-Al alloy showed superplasticity at a high strain rate of 10– 1 /s. High amount
work hardening and higher flow stress for superplastic deformation as compared to
micron grain sized material is observed in these cases.
Superplasticity was observed in ~40 nm grain size Zn-Al alloy at 373 K, tested at a
strain rate of 10– 4 /s [2]. Microcrystalline samples showed no superplasticity!

[1] S. X. McFadden, R. S. Mishra, R. Z. Valiev, A. P. Zhilyaev and A. K. Mukherjee, Nature 398 (1999) 684.
[2] R.S. Mishra, R.Z. Valiev, A.K. Mukherjee, Nanostruct. Mater. 9 (1997) 4732.
Superplasticity at low temperature (or equivalently Superplasticity at high strain
rates (> 10– 2 /s) at a given temperature in the superplastic regime) is caused by:
increased diffusion, grain boundary sliding and dislocation activity.
Grain growth is a serious issue during superplasticity experiments. In the case of nc-
Ni it was seen that the grain size could increase to micron sizes, from the starting
grain size of the order of 20 nm. In other materials the grain growth could be less.
Grain growth is expected to be less is two phase mixtures (2nd phase as a
precipitate preferred) and intermetallic compounds. In two phase mixtures the 2nd
phase has a pinning effect on the grain boundaries; while in intermetallics (like
Ni3Al) order (with respect to the sublattices) has to be maintained during grain
growth, which restrains the process.
In cases where grain boundary sliding is the predominant mechanism for
superplasticity (e.g. in some Mg alloys), it is seen that
give lower elongation as compared to equilibrium grain boundaries (due
to the long range stress fields associated with non-equilibrium grain boundaries,
which is expected to hamper grain boundary sliding).
In Ni3Al the high flow stresses and extensive strain hardening during superplastic
deformation has been attributed to depletion of dislocations and high stresses
required for the nucleation of new ones [1].

[1] R.S. Mishra, R.Z. Valiev, S.X. McFadden, A.K. Mukherjee, Mater. Sci. Eng., A 252 (1998) 174.

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