Creep and high temperature

materials
Engineering structure
used in ambient temperature
 Design of engineering component

• Based on mechanical strength

(Tensile, creep, fatigue ………)

• Mechanical strength
ability to carry load
• Load
Steady load (creep)
Unsteady load (fatigue)

• Strength of materials
Basic structural sensitive
Temperature sensitive
Atomic Model of Polycrystalline Material

• Single crystal with different orientations

• Grain boundary has porous structure
50 µ m • Grain boundary –
source of weakness at high temperature
 Tensile Strength of materials
Standard
ASTM E8
UTS

Structural component
used at temperatures
< 0.4 Tm
STRESS
Yield point
-- designed based on
tensile strength Fracture

STRAIN
Plastic deformation
 Plastic Deformation in Crystal

Schematic
Actual
Slip along
Force Force Force
slip plane by
dislocation
glide

Details of slip plane 300 µm

Force Force
Force
 Increase in Stress on Continuation of Plastic
Deformation (Cross Slip)

stress τ

Activation of dislocation
source on increasing
stress on other slip plane
to cross slip the dislocation Obstacle
To continue the deformation
stress τ
 Complex dislocation net work and grain boundary as
obstacles to dislocation movement

Grain
boundary

Dislocation
net work

10 nm
 Precipitates as obstacle to dislocation
movement
Dislocation
Precipitate

Precipitate
dislocation
interaction

10 nm
Concept of Creep Deformation
Holding at a particular stress σ and at relatively
high temperature (> 0.4 Tm)

what happened
to strain with time??
STRESS

Fracture

STRAIN
strain εo
 Deformation under the conditions

Stress Constant (σ )

Time
Tempera - Constant (T)
ture
Time

εo•
Strain Remained constant, increased or decreased ??

Time
Steam turbine used in power plant
Gas turbine used in Jet engines

The deformation may become so large that a component can no longer

perform its function — for example creep of a turbine blade will cause the
blade to contact the casing, resulting in the failure of the blade.
Aero Engine ( ≤ 1500 oC)
 Definition of High-Temperature Alloys

• "High" temperature is broadly defined as 300-1200°C.

• Applications for high-temperature alloys are typically 600-1200°C
range.
• Able to maintain high strengths at high temperatures
• Resistance to embrittlement (thermal stability)
• Good resistance to creep and rupture at high temperatures
• Good corrosion and oxidation resistance at high temperatures
• 3 main classes of High Temperature Materials
– Ni – Base (Nimonics, Hasteloy, Waspaloy)
– Ni-Fe – Base (cheaper than Ni-base Inconel family IN600/718)
– Co – Base (Stellites like KC20WN)
 Service Environment and Property Requirements

Liquid Engines : Temp ~1400 °C, High Temp. Strength and

Good erosion resistance

Thrust Chamber: Temp ~ 2000 °C, High Temperature
Strength, Stability

Cryogenic Engine: Temp ~ –253 °C : Mechanical properties,
Co-efficient of thermal expansion, toughness

High temperature stress rupture properties are

special requirement
 Uses for High-Temperature Alloys
Aerospace Gas Turbine Engines
Land-Based Power Generation Turbines
High-Temperature Fasteners (Super alloy or TZM)
Combustion Engine Exhaust Valves
Space vehicles
Rocket engines
Submarines
Nuclear reactors
Hot Working Tooling and Dies
 What Properties are Important?
• Tensile
• Creep and Stress-Rupture
• Fatigue and Crack Growth
• Toughness
• Oxidation and Corrosion Resistance
• Wear/Erosion
• Physical (expansion, conductivity)
• Machinability

• Other properties may be critical depending on the

application.
 Selection of Materials for High Temperature Applications
(Pure Metals)

• Pure Metals or Dilute Alloys

-Melting point limitation
-Drastic Loss of Strength with increase in Temperature
-Oxidation issues

-Melting points of selected HT materials

-Strength of pure metals as a function of Temperature
-Copper alloys (OFHC Cu, Cu-0.8Cr, Cu-Cr-Zr-Ti, Cu-Ag-Zr) for Thrust
Chamber Applications
-Thermal Conductivity
 Effect of high temperature in
combination with stress
• Atoms get mobility (diffusion-controlled process).
• This affects mechanical properties of materials.
• Greater mobility of dislocations (climb).
• Increased amount of vacancies.
• Deformation at grain boundaries.
• Metallurgical changes, i.e., phase transformation,
precipitation, oxidation, recrystallisation.
High temperature materials/alloys
• Improved high temperature strength.
• Good oxidation resistance.
 Defect in Crystal - Vacancy
typically, crystals contain more vacancies at higher temperatures
..vacancies make it easier for atoms to move through the
crystal structure; atoms next to a vacancy can jump into it;
this process is diffusion

purple atoms have moved from original positions by jumping

into adjacent vacancy.
note that atoms and vacancies diffuse in opposite direction
applied stress creates gradient in vacancy concentration;
atoms migrate down gradient causing material to flow
 Vacancy

 −Q 
nv = n. exp 
 RT 

Nv = No. of vacancies pr cm3

n = No. of atoms per cm3
Qv = energy required to produce one mole of vacancies in
cal/mole or j/mole
R = gas constant, T = temperature in K
Grain boundary sliding during creep causes (a) the creation of voids at an inclusion
trapped at the grain boundary, and (b) the creation of a void at a triple point where
three grains are in contact
Creep cavities formed at grain boundaries in an austentic stainless
steel (x 500). (From ASM Handbook, Vol. 7, (1972) ASM
International, Materials Park, OH 44073.)
 Failure Analysis of a Pipe

A titanium pipe used to transport a corrosive material at 400oC is found

to fail after several months. How would you determine the cause for the
failure?

Since a period of time at a high temperature was required before failure

occurred, we might first suspect a creep or stress-corrosion mechanism
for failure. Microscopic examination of the material near the fracture
surface would be advisable. If many tiny, branched cracks leading away
from the surface are noted, stress-corrosion is a strong possibility.
However, if the grains near the fracture surface are elongated, with many
voids between the grains, creep is a more likely culprit.
 Evaluation of Creep Behavior

 Creep test - Measures the resistance of a material to

deformation and failure when subjected to a static load
below the yield strength at an elevated temperature.
 Climb - Movement of a dislocation perpendicular to its slip
plane by the diffusion of atoms to or from the dislocation
line.
 Creep rate - The rate at which a material deforms when a
stress is applied at a high temperature.
 Rupture time - The time required for a specimen to fail by
creep at a particular temperature and stress.
Slip of an edge dislocation
Dislocations can climb (a) when atoms leave the dislocation line to create interstitials
or to fill vacancies or (b) when atoms are attached to the dislocation line by creating
vacancies or eliminating interstitials
• Creep occurs when a metal is subjected to a constant
tensile load at an elevated temperature.
• Undergo a time-dependent increase in length.
• Since materials have its own different melting point, each
will creep when the homologous temperature > 0.5.
• The creep test measure the dimensional changes which
occur when subjected to high temperature.
• The rupture test measures the effect of temperature on
the longtime load bearing characteristics.
• Homologous temperature = Testing temperature/Melting
temperature
 Creep Testing Machine
Load application by lever

Standard: ASTM E 139

Stress variation: < 1 %

Temperature variation:
- up to 1000 oC
± 2 oC

- above 1000 oC
± 3 oC
 Creep curve under constant load/stress

Constant stress
curve

A typical creep curve showing the strain produced as a function

of time for a constant stress and temperature
 Classical creep curve
Creep strength - is the stress at a given
temperature, which produces a steady-state
creep rate

1) Primary creep provides decreasing creep rate. – strain hardening

2) Secondary creep gives the representing constant creep rate. –
compensation of strain hardening by recovery process
3) Tertiary creep yields a rapid creep rate till failure.
Associated with effective reduction of cross sectional area because
of necking and void formation. Metallurgical changes such as coarsening of
precipitates, recrystallisation and diffusional changes happens.

For design purpose, Minimum creep rate – 0.0001% per hour or 1%/10000 hours
Cold work Anneal Recovery Recrystallization

Grain growth

Low angle grain boundaries

Effect of stress on creep curves at
constant Temperature
 Structural changes

1) Deformation by slip
More slip systems operate at high temperature
2) Sub grain formation
3) Grain Boundary sliding
Produced by shear process and promoted by increasing
temperature/or decreasing strain rate.
Results in grain boundary folding or grain boundary migration.
 Mechanism of creep
Dislocation glide
 Involves dislocation moving along slip planes and overcoming
barriers by thermal activation.
 Occurs at high stress.
Dislocation creep
 Involves dislocation movement to overcome barriers by diffusion of
vacancies or interstitials.
Diffusion creep
 Involves the flow of vacancies and interstitials through a crystal
under the influence of applied stress. - Occurs at high temperature
and relatively low stress
Grain boundary sliding
 Involves the sliding of grains past each other.
 Creep deformation mechanism
Stress constant Under creep condition
Stress: constant
Temperature: constant
STRESS

> 0.4 Tm
Tensile curve
Yield point

STRAIN Glide
plane Obstacle

NOW stress is not sufficient

strain

Creep curve for the dislocation to bypass

the obstacle by initiating glide
in another slip plane as in
tensile test since stress is
constant and is not sufficient
 Creep Deformation Mechanisms
High Temperature ( > 0.4 Tm)
Dislocation can climb with the help of diffusion

Vacancy
Dislocation

Vacancy
 Dislocation creep mechanism
τ
Diffusion of atoms
Climb
unlock dislocations
from obstacles to obstacle
Glide plane Glide plane
glide them for plastic
deformation
τ
Glide Climb

Glide Climb

Climb
obstacle τ
Plastic deformation by diffusion of atom itself
under stress
Stress

Stress

Applied stress creates a gradients in vacancy concentration so

that atoms migrate down the gradient causing plastic deformation
by diffusion itself
 Diffusion creep mechanisms
Diffusion Creep
Biased movement of atom under stress
Flow of vacancies from grain boundaries
Atom experiencing tensile stresses to region of
compressive stresses.
Simultaneously there is a flow of atoms in the
vacancy

reverse direction – elongation of grain

vacancy
Atom
σ Atoms move σ σ
under stress
through Atoms move σ
matrix along the
vacancy grain
vacancy
boundary

Atom
Atom

Nabarro-Herring Creep Coble Creep

Creep Deformation Mechanism Map

Typical uses of deformation

mechanism map

 Location of testing domains

(Creep, tensile tests)

 Rate controlling mechanism

(Strengthening methods)
 Mechanisms of Creep
• High rates of diffusion permit reshaping of
crystals to relieve stress
• Diffusion significant at both grain boundaries
and in the bulk
• High energy and weak bonds allow
dislocations to “climb” around structures that
pin them at lower temperature
 Creep and stress rupture
Parameters Creep Stress rupture
load Low high
Creep rate Minimum High
Test period 2000-10000 h 1000 h
Total strain 0.5% 50%
 Creep in a filament bulb

• Sagging due to creep deformation

• The adjacent turns of the coil touch one another, causing
an electrical short and local overheating, which quickly
leads to failure of the filament
 Some practical examples
• In steam turbine power plants, steam pipes
carry superheated vapour under high
temperature 565.5°C and high pressure often
at 24.131 MPa or greater.
• In a jet engine temperatures may reach to
~1000°C, which may initiate creep
deformation in a weak zone.

For these reasons, it is crucial for public and operational safety to

understand creep deformation behavior of engineering materials.
 Threshold for Creep

The Critical Temperature for Creep is 40% of

the Melting Temperature.

If T > 0.40 TM  Creep Is Likely

 Example
Will Lead Creep at Room Temperature?

TM = 327 °C = 600 °K
TROOM = 23 °C = 296 °K

100 x 296 / 600 =49.3 %  Will Creep

 Creep in Ice
How cold does your freezer need to be to avoid
creep in the ice cubes?

0C = 273 K

0.4 * 273 = 109.2K = -163.8 C!

 Creep Fracture – rupture life

Cavity nucleation at
Cavity grain boundary particle

σ
Slip bands

Crack
50 µm
• Cavity nucleates at particles on grain boundary due to
grain boundary sliding
• Under stress nucleated cavity grow by diffusion of atoms
from cavity surface to grain boundary
 CREEP CAVITY GROWTH – IMPURITY EFFECT

Creep cavity growth model

Stress Creep cavities
Grain boundary
diffusion
Surface Surface
diffusion diffusion

Grain boundaries
atom

Cavity growth involves

• Cavity surface diffusion (DCS)
• Grain boundary diffusion (DGB)

• Segregation of S, O, As, Sb etc.on cavity surface ↑ both DCS and DGB

• Segregation of B segregation on cavity surface ↓ both DCS and DGB
600 h 900 h

1200 h 1500 h

1800 h The progress of creep cavitation in 347BCe steel,

creep tested at 78 MPa and 1023 K, showing the
nucleation of r-type creep cavities and their growth.

The lines shown were inscribed on the specimen surface

by focused ion beam to study grain boundary sliding
 Fracture mode

Strength of GB = grain at the equicohesive temperature

(ECT).

Below ECT small grain sized material is stronger due to high density of grain boundaries to
improve strength.
Above ECT large grain sized material is stronger due to less tendency for grain boundary
sliding.

Note: Single crystal structure is therefore appreciable for high temperature applications,
i.e., nickel base alloy single crystal turbine blade.
 Fracture mode
Transgranular fracture Intergranular fracture
Slip planes are weaker than
Grain boundaries are weaker
grain boundaries
than slip planes.

Note: at T just below Trecrys, ductility drops due to grain boundary sliding – leads to
intergranular failure.
Intergranular fracture
 How Do We Deal With Creep ?

• Reduce the effect of grain boundaries

Use Single Crystals

• Promote a mechanism to Inhibit Slip

• Change Materials
• Change Operating Conditions
 Design to Resist Creep
• Select high melting point material to increase elastic constant
and to decrease self diffusion
• Increase grain size (Single crystal) to avoid creep cavitation
• Directional solidification to suppress creep cavitation
• Restriction of grain boundary sliding by precipitation on the grain
boundary or making the grain boundary corrugated.
• Precipitation hardening to obstruct dislocation glide
• Composite reinforcement to restrict mass flux /dislocation
movement
• Internal cooling to reduce temperature
• Thermal barrier coating to reduce temperature
• Metals with low stacking fault energy has good creep resistance
(resistance to cross slip)
 Summary
• Strength of materials
Structure, temperature and defect sensitive

• Creep
Plastic deformation under constant load and temperature

• Two creep deformation mechanisms

Dislocation creep ( dislocation climb + glide)
Diffusion creep
Nabarro-Herring creep (matrix diffusion)
Coble creep (grain boundary diffusion)

• Creep fracture
Nucleation, growth and coalescence of creep cavities
(Rupture life, tr)
 High temperature alloys
• High temperature alloys are complex in their microstructures to obtain the
required properties at service temperatures.
• High melting point alloys normally has high creep resistance.
– NI (1453C), Co (1495C), Fe (1539C)

• Metals with high stacking fault energy is easy for slip and prone to creep.
• Fine precipitates having high thermal stability are necessary for high creep
resistance (prevent grain growth).
– Ex: (1) Nickel base alloy containing fine precipitates of intermetallic
compounds Ni3Al, Ni3Ti or Ni3(Al,Ti),
– (2) Creep resistance steels containing fine carbides VC, TiC, NbC, Mo2C or
Cr23C6.
 Superalloy
• A superalloy is a metallic alloy which can be used at
high temperatures, often in excess of 0.7 of the
absolute melting temperature.
• Creep and oxidation resistance are the prime design
criteria.
• Superalloys can be based on nickel, nickel-iron or
cobalt based
– Nickel based alloys have highest strength at elevaed
temperatues, followed by Ni-Fe and Co based alloys
– All alloys have FCC structure (aids forgeability)
 Superalloys
• Combination of high strength, good fatigue and creep
properties, good corrosion resistance – Metallurgical stability
• Used in hot portion of jet engines such as blades, vanes,
combustion chambers, etc..
• Strengthening
– Precipitation hardening - Ni3(Ti, Al), Co3(Al,Ti)
– Solid solution hardening (Fe, Cr, Co, Mo, W, Ti, Al etc)
– Carbide hardening
– γ’ - - Ni3(Ti, Al) – FCC ordered phase – low mismatch – high coherency
between γ matrix and γ’ precipitates (spherical particles) – low
coarsening rate- long term stability
– Degree of ordering increases with temperature
Microstructure of super alloy
 Superalloys
γ’’-Ni3Nb found in iron-nickel based alloys
Cr and Al – Good oxidation resistance Al2o3, Cr203
Larger Al and Ti – lowers the melting point of super alloys
Large number of alloying elements – Forms TCP phases – needle like structure –
embrittlement

Metallic carbides (MC, M23C6, M6C, M7C3) from in both grain boundary and well
as within grains

- grain boundary carbides prevents grain boundary sliding and permits

stress relaxation
- carbides in the grain increases strength
-can tie up with other elements that would otherwise promote
instability during service
- Proper heat treatment to be carried out to prevent Continuous
network of carbides – easy fracture path
Material Distribution in a jet Engine
Material Distribution in a GE Engine
A turbine blade experiences

Mechanical forces
Creep
Fatigue
Thermo-mechanical fatigue

High Temperature Environment

Oxidation
Hot corrosion
 Effect of Alloying elements in Superalloys

Improper alloy control can result in undesirable phases such as σ, µ and Laves phases
(AB2). (plate like/needle like morphology)
 Manufacturing

Wrought form
Cast form
P/M

Large grained cast alloys – turbine blade applications

Small grained forged alloys – Turbine disc applications

Cast alloys – more alloy segregations and coarse grain size – better
creep and stress rupture properties
Wrought alloys – uniform with fine grain size – superior tensile
and fatigue properties
Manufacturing methods of Superalloys
 Ingot metallurgy route

Triple melting – VIM + ESR + VAR

VIM
Desired alloy configuration,
reduce dissolved gases,
eliminate slag/dross
coarse and non-uniform grains, shrinkage, alloy seggregation
ESR
Remove oxygen containing inclusions
VAR
reduce compositional segregation during ESR

Homogenization treatment and Hot working

Processing of Superalloys – Ingot Metallurgy route
Investment Casting Process for turbine blades
Processing of Superalloys – P/M route
Cast superalloys – Turbine blade
Creep/Stress rupture properties

980 deg C
Directional solidification
Single Crystal Turbine Blade
How to achieve it?
Single crystal initiation
Single crystal solidification
Microstructure of Ni based Superalloy
Applications

Cast turbine airfoils and other high-integrity

investment-cast gas turbine components

Machined flat disk for aircraft gas turbine

IN-718 in ISRO

Deep drawn IN718 shells

for Ni-H2 cell case
 superplasticity

S U P E R P L A S T I C I T Y
 Superplasticity
 Superplasticity is the ability to withstand very large
deformation in tension without necking.
 Give elongation > 1000%.
 Materials with high strain rate sensitivity (m) at high
temperature (T>0.5Tm) superplasticity
 Materials characteristics: fine grain size (<10 μm) with
the presence of second phase of similar strength to the
matrix to inhibit grain growth and to avoid extensive
internal cavity formation.
 Grain boundary should be high angle and mobile to
promote grain boundary sliding and to avoid the
formation of local stress concentration respectively.
Two-Sheet SPF/DB Aircraft Door
Superplastically formed parts
Pressure vessels
 references
• Constitutive behavior of superplastic materials, International Journal of Non-Linear Mechanics
Volume 37, Issue 3, April 2002, Pages 461–484
• F.C. Campbell, Manufacturing Technology for Aerospace Structural materials
• George E Dieter, Mechanical Metallurgy
• Donald R Askeland, Essentials of Materials science and Engineering
• ASM, Heat Resistant Materials
• Matthew J. Donachie, Stephen J. Donachie, Superllaoys, A technical guide
 Classes of High-Temperature Alloys

Base Class
Super 12% Cr Martensitic Stainless
Steels
Fe
20-23% Cr Austenitic Valve Steels
Fe-Ni
Age-Hardenable Superalloys

Ni Age-Hardenable, Low-Expansion
Superalloys

Co Solid solution strengthened alloys