Advanced High

Temperature Alloys

Prof. Dr.-Ing.
g Uwe Glatzel
Metals and Alloys
University Bayreuth
SS 2010
University Bayreuth, Advanced High Temperature Alloys

Uwe Glatzel, Metals and Alloys

Lecturer:
Prof Dr
Prof.
Dr.-Ing.
Ing habil
habil. Uwe Glatzel
born Dez. 1960
Physik-Diplom (B.Sc.
(B Sc and M.Sc)
M Sc) in Tbingen
(exchange year in Corvallis, Oregon, USA)
PhD thesis at the Institute for Metals Research, Technical
University Berlin, Prof. Monika Feller-Kniepmeier
post-doc (1 Jahr) at Stanford University
Habilitation TU-Berlin
Gerhard-Hess award of the German Science Foundation
(DFG) for young scientist (400.000 )
1996-2003 full professor for Metals and Alloys, Jena
since April 2003 Bayreuth (Chair for Metals and Alloys)

postal address:
Ludwig-Thoma-Str.
d i h
36bb
D-95447 Bayreuth, Germany

University Bayreuth, Advanced High Temperature Alloys

phone:
h
+49 (0)
( ) 921 - 55-5555
e-mail: [email protected]
2

Uwe Glatzel, Metals and Alloys

Literature

R. Brgel
R
Brgel, Handbuch Hochtemperatur-Werkstofftechnik
Hochtemperatur Werkstofftechnik, Vieweg
R.C. Reed, The Superalloys - Fundamentals and Applications, Cambridge Univ. Press
H. Frost, M. Ashby, Deformation-Mechanism Maps, Pergamon Press
G M
G.
Meetham,
th
M
M. V
Van dder V
Voorde,
d Materials
M t i l ffor Hi
High
h Temperature
T
t
Engineering
E i
i
Applications, Springer
J. Betten, Creep Mechanics, Springer
Askeland: Materialwissenschaften, Spektrum Lehrbuch; 1994
Callister: Materials Science and Engineering - An Introduction, Wiley, New York, 1999
H. Schumann, Metallographie, Deutscher Verlag fr Grundstoffindustrie, Leipzig
F. Vollertsen, S. Vogler, Werkstoffeigenschaften und Mikrostruktur, Hauser Verlag
P. Haasen, Physikalische Metallkunde, Springer-Verlag, Berlin
H -JJ. Bargel
H.
Bargel, G.
G Schulze,
Schulze Werkstoffkunde,
Werkstoffkunde VDI
VDI-Verlag
Verlag, Dsseldorf
P. Sarrazin, A. Galerie, J. Fouletier, Mechanisms of High Temperature Corrosion, Trans
Tech Publications

lecture notes: http://www.metalle.uni-bayreuth.de then "Lehre" then "Vorlesungen",

you
will find the link to this lecture notes 3and three review talks we
will do at the end.
University Bayreuth, Advanced High Temperature Alloys
Uwe Glatzel, Metals and Alloys

What You Should Know:

basic thermodynamics
introduction to diffusion
introduction to dislocations
phase diagrams
theory of elasticity
...
basic materials science courses

University Bayreuth, Advanced High Temperature Alloys

Uwe Glatzel, Metals and Alloys

Contents
11. Introduction
Introduction, Basics
2. Stability of Microstructure
3. Mechanical Properties
a)) Static
b) Cyclic (Fatigue)
4 High Temperature Corrosion
4.
5. High Temperature Alloys
6. Lost Wax Investment Casting
p
g on Time: Lectures on
7. Depending
a) SX Ni-Base Superalloys b) LEK 94 c) Pt-Base Superalloys
University Bayreuth, Advanced High Temperature Alloys

Uwe Glatzel, Metals and Alloys

Introduction
only alloys will be looked at (no ceramics,
ceramics no
polymers).
no coatings (BUT : practically all high
temperature systems are coated!), simply not
enough time
time.

University Bayreuth, Advanced High Temperature Alloys

Uwe Glatzel, Metals and Alloys

Maximum Temperatures for

Applications
li i
off Different
iff
Materials
i l
Group

i
service
i temperature
t
t
maximum
[C]

deformation/damage mechanism

Polymer

up to 300

melting, decomposing (pyrolyze)

Glass

up to 800

viscous flow

Metals

Fe-Basis (coated) up to 1100

Fe-ODS
Fe
ODS up to 1300
Ni-base up to 1200
Pt-base up to 1600
refractory metals in inert
atmosphere
h above
b
1600
MoSi2 up to 1800

Ceramics
p
Composits

SiC up to 1600
((SiC/C)) up
p to 1600

University Bayreuth, Advanced High Temperature Alloys

creep, dislocation climb,

grain boundary sliding

viscous flow, glass transition

temperature grain boundary
temperature,
sliding
complex
p

Uwe Glatzel, Metals and Alloys

usable strength
u

Overview Materials

source:
Plansee AG,
AG
Reutte,
Tirol,
Austria

500

temperature [C]

University Bayreuth, Advanced High Temperature Alloys

1500

2000
Uwe Glatzel, Metals and Alloys

usable strength
u

Taking Density into Account

500

temperature [C]

University Bayreuth, Advanced High Temperature Alloys

1500

2000
Uwe Glatzel, Metals and Alloys

usable strength
u

Oxidation Resistance

500

temperature [C]

University Bayreuth, Advanced High Temperature Alloys

10

1500

2000
Uwe Glatzel, Metals and Alloys

Refractory Metals:
wider
definition
of
refractory
metals

Tm of platinum

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Most common definition of

refractory metals (refractory =
widerspenstig, halsstarrig):
two elements of the 5. and
three elements of the 6. period
with melting points higher
than Pt. Processing in general
by powder metallurgy.

Uwe Glatzel, Metals and Alloys

Density
Re
R
W
Ta
Ru, Rh, Pd

Tc

Os, Ir

Pt
Au

Hf
Pd

Mo

Ag

Nb

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Uwe Glatzel, Metals and Alloys

Abundance of Elements

to find 1 atom Rh
within a bunch of Siatoms is comparable to
find one individual
person within the word
population
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Uwe Glatzel, Metals and Alloys

Material Choice

temperature
environment
moving/non-moving part
design complexity (how to manufacture)
price constrictions (depending on application
of system). Reduction of 1 kg in weight:
car ~ 0 - 5
plane ~ 100 500
aerospace ~ 100.000 - 500.000

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Uwe Glatzel, Metals and Alloys

Influence of ... on ...

temperature:
phase transitions, volume fractions, ...
diffusion ( recrystallization, dislocation climb, diffusional creep, ... )
thermal fatigue (TF)

mechanical:
creep
fatigue (low cycle, LCF, high cycle fatigue, HCF)

environment:
i
t
oxidation
corrosion

combinations:
thermo
thermo-mechanical
mechanical fatigue (TMF)
stress corrosion cracking, stress oxidation, ...
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Uwe Glatzel, Metals and Alloys

Basics
Thermodynamics Kinetics
Boltzmann-statistics: energy of
movement increases with temperature
p
u kin

u total atom = 2 u kin

U total mol = 3 R T

atom

3
= 2 kB T = 3 kB T
2

0,33 eV, bzw. 32 kJ/mol bei 1000C

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atom

3
kB T
2

& = & 0 e

Q
R T

Arrhenius-plot

Uwe Glatzel, Metals and Alloys

Vacancy Concentration
F = U - TS
T S non-zero vacancy concentration
t ti is
i
in thermodynamic equilibrium
cv = e

Q vac
R T

Qvacnickel = 1,36 eV (energy necessary to create one vacancy)

T[C]

20

300

450

800

1000

1200

1454

T/Tm

0.17

0.33

0.42

0.62

0.74

0.85

1.00

10-23 310-12

10-9

10-6

10-5

710-5

310-4

cv

equilibrium vacancy concentration for nickel

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Uwe Glatzel, Metals and Alloys

Nickel Vacancy Concentration

10-55

10-10

10-15
-4

vacancy con
ncentration [10 ]

vaccancy concentration

100

10-20

Nickel Vacancy Concentration

10-25
0

200

400

600

800

1000 1200 1400 1600

Tm

temperature [C]

1,00

Nickel Vacancy Concentration

0,10
0,01
0

200

400

600

800

1000 1200 1400 1600

temperature [C]

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Tm

Uwe Glatzel, Metals and Alloys

Diffusion
r
v
j = D c

1. Fick's law
[j] = (atoms)
(
) m-22 s-11
[D] = m2 s-1
[c] = (atoms) m-3

vacancy diffusion
diff i or
volume diffusion

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Uwe Glatzel, Metals and Alloys

Coefficient of Diffusion
Qvac
Qmigration
i ti
QSD

energy to create a vacancy

activation energy to migrate a vacancy
activation energy for volume diffusion
QSD = Qvac + Qmigration

D = D0 e
QSD 17 kB Tm

( Q vac + Q migration )
k T

= D0 e

Q SD
k T

QSDnickel 2.5 eV = 244 kJ/mol

(for a perfect crystal; defects will lower the activation energies)

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Uwe Glatzel, Metals and Alloys

Dependence Melting Point and

Enthalpy of Vacancy Creation
element

Tm
[C]

17RTm

Qvac
[eV]

crystal
t l
structure

Pb

327

0 88
0.88

0 57
0.57

fcc

Al

660

1.36

0.68

fcc

Cu

1 085

1.99

1.29

fcc

Ag

1 235

2.21

1.12

fcc

Ni

1 455

2.53

1.78

fcc

Pt

1 768

2 98
2.98

1 32
1.32

fcc

Mo

2 623

4.23

3.00

bcc

3 422

5.40

4.00

bcc

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Uwe Glatzel, Metals and Alloys

QSD versus Tm

400 kJ/mol

0 13 kkJ/(molK)
0.137
/( l )
17 kB NA

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Uwe Glatzel, Metals and Alloys

Coefficient of Diffusion
Steepp slope
p indicates a
high activation energy.
Small
S
ll elements
l
t diffuse
diff
faster.
Diffusion in fcc crystals
slower than in bcc crystals.
y

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Uwe Glatzel, Metals and Alloys

Coefficient of Diffusion with Defects

surface diffusion

Coefficient of diffusion of Th
i W.
in
W

grain boundary diffusion

Overall velocity for diffusion

depending on grain boundary
thickness, grain size and
dislocation density.

volume diffusion
pipe
diffusion

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Uwe Glatzel, Metals and Alloys

Pipe Diffusion
Deff = DSD + adisl. Ddisl.
adisl. area of dislocation core
( 5 b2 00.33 nm2)

volume
ol me diffusion
diff sion
dominant
pipe diffusion
dominant
increasing

dislocation density
Ddisl. pipe
i diffusion
diff i along
l
dislocation core
atom
t
flux
fl ~ Darea
D

decreasing

atoms
2
~ DSD d grain

time grain

dashed line:

identical atom fluxes if:

diffusion in crystal by the velocity of pipe diffusion

University Bayreuth, Advanced High Temperature Alloys

atoms
2

~ D disl. b n
i
time
disl.

25

DSD d grain = D disl. b 2

n
d grain

= D disl. b 2

Uwe Glatzel, Metals and Alloys

Grain Boundary Diffusion

Deff = DSD + / d Dgrain bound.
volume diffusion
dominant
grain boundary diffusion
dominant
fine
grain
coarse
grain

dashed line: diffusion in crystal

y
by
y the velocity
y
of grain boundary diffusion
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with:

effective grain boundary

thickness ( 2 b 0.5 nm)

grain size

Ddisl. pipe diffusion along

dislocation core

Uwe Glatzel, Metals and Alloys

Activation Energies Indicating

Mechanism Changes
~ QSD

Single crystal aluminium, oriented such that <110>{111} slip is activated.

Lytton, Shepard and Dorn, Trans. AIME 212 (1958) 220
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Uwe Glatzel, Metals and Alloys

Diffusion in Ordered Structures

(
(Intermetallic
lli Phases)
h
)
High binding energies high activation
energies low coefficient of diffusion
For example NiAl: very low enthalpy of ordered
B2 structure low enthalpy outweighs entropy
ordered up to melting
t
temperature
t
TmNi = 1454C
TmAl =
660C
TmNiAl = 1638C
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Uwe Glatzel, Metals and Alloys

Second Fick
Fick'ss Law
c
= D c
t

C be
Can
b concluded
l d d directly
di tl from
f
first
fi t Fick's
Fi k' law.
l
Similar in heat transfer systems,
systems electrical
potential, ... .
f1 ( x ) = 1 (x )

x
f 2 ( x ) = 1

0.5

0.8
0.6

x
f 3 ( x ) = 1

0.05

f1(x)

0.4

f2(x)
0.2

solution to these
boundary conditions:

c( x , t ) = c1 (c1 c 0 )
2 Dt

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f3(x)
0.5

1.5

Uwe Glatzel, Metals and Alloys

Thermal Conductivity
The most simple, stationary case: no heat radiation, constant
temperatures in front and back of component.
coefficient of heat (or thermal)
conductivity:
= a cp
a coefficient of temperature conductivity
cp heat capacity
density

compare:
r
r
j = D c
c
= D c
t
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r
r
q& = T
T
= a T
t

Uwe Glatzel, Metals and Alloys

Temperature Distribution with

Thermal
h
l Barrrier
i Coating
i (TBC)
(
)

cooling air

hot air

TBC

bond coat

Wrmedmmschicht

Haftvermittlerschicht

substrate

Grundwerkstoff

In case of transients, the temperature should reach a stable distribution as fast as possible in
order to reduce thermal stresses ( temperature conductrivity as high as possible).
I case off stationary
In
t ti
circumstances,
i
t
heat
h t conductivity
d ti it leads
l d to
t heat
h t flow
fl into
i t the
th solid.
lid
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Uwe Glatzel, Metals and Alloys

Material Parameters at RT
material/property

heat cond.
cond

heat cap.
cap
cp

density

temp. cond.
temp
cond
a

W
m K

J
kg

gK

g
3
cm

6 m 2
10

ferritic steel

45

460

7.8

13.0

austenite steel

15

500

8.0

3.8

Ni-base alloys

11

450

8.2

3.0

Mo

145

240

10.2

59.0

530

4.5

2.9

Al

210

890

2.7

87.0

Al2O3 bei RT
( Al2O3 bei 1000C )

25
( 6)

800

3.9

8.4

Ti alloys (-rich)

source: Brgel

Attention: Heat conductivity strongly depends on alloy composition,

composition see steels and pure
Ni with 91 W/(mK) in comparison to Ni-base alloys with 11 W/(mK)
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Uwe Glatzel, Metals and Alloys

Contents
11. Introduction
Introduction, Basics
2. Stability of Microstructure
3. Mechanical Properties
a) Static
b) Cyclic (Fatigue)
4 High Temperature Corrosion
4.
5. High Temperature Alloys
6. Lost Wax Investment Casting
7. Depending on Time: Lectures on
a) SX Ni-Base Superalloys b) LEK 94 c) Pt-Base Superalloys
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Uwe Glatzel, Metals and Alloys

Microstructure is NOT stable

annealed

deformed

stress-relieved

recrystallized

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Uwe Glatzel, Metals and Alloys

Recrystallization
time dependence of
recrystallization can be
approximated by
Avrami Johnson Mehl
Avrami-Johnson-Mehl
function:

fr = 1 e

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t
t0

Uwe Glatzel, Metals and Alloys

Grain Coarsening
driving force: reduction of grain boundary
gy
energy
T > 0.7 Tm
no pre-deformation
d f
i necessary
se
self-similar
s
sys
system
e
Ostwald ripening d ~ t1/3 (big grains eat up
small
ll grains)
i )
new g
grains have low dislocation densityy
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Uwe Glatzel, Metals and Alloys

Grain Coarsening
monomodal

bimodal (some grain

boundaries are pinned,
e.g. by precipitates)

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Uwe Glatzel, Metals and Alloys

Precipitate Hardening
Requirements:
solid solution at higher
t
temperatures
t
(ability
( bilit to
t
homogenization heat
treatment)
during cooling a two-phase
region
g
should be reached
in general: cooling rate as
g as possible,
p
thereafter
high
annealing (in the two-phase
region) to let grow the
precipitates
i i
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Uwe Glatzel, Metals and Alloys

Thermodynamic Kinetic

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Uwe Glatzel, Metals and Alloys

Example: Al-Cu
Al Cu Alloy
Guinier-Preston
G
i i P t
Zones leading to
-Precipitates
(Al2Cu) have
paved the way
to the success of
Al-alloys

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Uwe Glatzel, Metals and Alloys

Other Examples of
precipitate
i i
hardening:
h d i
Al2Cu in AlCu alloy:

platinum-base superalloy
University Bayreuth, Advanced High Temperature Alloys

nickel-base superalloy
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Uwe Glatzel, Metals and Alloys

Time Dependence of
Precipitation Hardening
nucleation growth,
nucleation,
growth

coarsening

T = const.

dT precipitate size

T distance between precipitates

fT volume fraction of precipitates

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Uwe Glatzel, Metals and Alloys

Coherent - Semicoherent - Incoherent

(mit Orientierungsbezug)

(ohne Orientierungsbezug)

aT aM
a T a M a T a M a

misfit :=
1 (a + a )
aM
aT
a
2
T
M
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Uwe Glatzel, Metals and Alloys

Energy Consideration
Gtotal = Gvol + Gboundary + Gstrain + Gdefect
total change in free enthalpy
strain enthalpy (elastic energy + dislocation line energy)
reduction of enthalpy by precipitation coupled with a defect
enthalpy
py of pphase boundary
y ((scales with surface))
enthalpy of formation of matrix to precipitate (scales with volume)

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Uwe Glatzel, Metals and Alloys

Heterogeneous Nucleation

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Uwe Glatzel, Metals and Alloys

TEM-Micrograph of TiC Precipitates at

Di l
Dislocations
i
in
i an Austenitic
A
i i Steel
S l

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Uwe Glatzel, Metals and Alloys

Ostwald-Ripening
Ostwald
Ripening of Precipitates
d3 - d03 ~ Dt

here for T/Tm 0.74

'' particle
ti l size
i in
i IN 738 LC att
T = 920C.
particle coarsening constant of
(50 nm)3/h

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Uwe Glatzel, Metals and Alloys

Contents
11. Introduction
Introduction, Basics
2. Stability of Microstructure
3. Mechanical Properties
a) Static
b) Cyclic (Fatigue)
4 High Temperature Corrosion
4.
5. High Temperature Alloys
6. Lost Wax Investment Casting
7. Depending on Time: Lectures on
a) SX Ni-Base Superalloys b) LEK 94 c) Pt-Base Superalloys
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Uwe Glatzel, Metals and Alloys

Room Temperature (RT) versus

Hi h Temperature
High
T
(HT) Deformation
D f
i
most alloy properties at room temperature are time and
rate independent (elastic constants, tension stress, ... ),
tension stress experiment.
p
(deformation)
(
) will be time
For T > 0.4 Tm the pproperties
and rate dependent, creep experiment.
deformation hardening

fine grain hardening

solid solution
strengthening

precipitate
hardening

cold deformation (RT)

strong

medium

medium to strong

medium to strong

creep (HT)

temporary hardening,
reduced creep rupture
strength, may lead to
recrystallization

reduced strength with

fine grain material
coarse grain, ideally
single crystal

medium

medium to strong

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Uwe Glatzel, Metals and Alloys

Change in Materials Properties

with Temperature

Material properties of steel and

Ni alloys at elevated
Ni-alloys
temperatures. Comparison
b t
between
short-term
h tt
andd longl
term parameters.

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Uwe Glatzel, Metals and Alloys

Tension Creep Experiment

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Uwe Glatzel, Metals and Alloys

Elastic (E-)Modulus and

Poisson's
i
Ratio
i

shear modulus G

E
G=
2 (1 + )

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Uwe Glatzel, Metals and Alloys

Anisotropy and Temperature Dependence of

El i Constants
Elastic
C
in
i Ni-base
Ni b
Superalloys
S
ll

D. Siebrger, H. Knake, U. Glatzel, Mat. Sci. Eng. A298 (2001)

Orientation dependence of
Youngs modulus E of matrix
phase Distance from the center to
phase.
the surface indicates the
magnitude of the Youngs modulus
i this
in
thi direction.
di ti
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Uwe Glatzel, Metals and Alloys

High Temperature Deformation

dislocation glide (Peierls stress, in fcc and hcp very small and for T >
0.15 Tm negligible)
cross slip
li off screw dislocations
di l ti
andd dislocation
di l ti interactions
i t
ti
(for
(f a low
l
stacking fault energy larger dislocation spacing thermal
activation necessary,
necessary T > 0.2
0 2 Tm, influence on deformation rate)
climb of edge dislocations to overcome obstacles:
diffusion at complete
p
dislocation line
T > 0.4 Tm

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Uwe Glatzel, Metals and Alloys

Dislocation Climb
climb of edge dislocations to
annihilate each other.
arrangement in low energy
configurations (sub-grain
boundaries), climbing around
b
l (leaving
(l i the
h glide
lid
abstacles
plane)
movement of screw
dislocations with
ith kink
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Uwe Glatzel, Metals and Alloys

University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys

Internal Back Stress

Dislocations
il
i
climb
li b allows
ll
annihilation
ihil i off dislocations
di l
i
and to establish a constant dislocation density,
resulting in an internal back stress of:

int . = G b
Gb 1

dislocation =
2 r

and

1
=
r

G shear modulus, constant 0.3 - 1, b magnitude of Burgers vector

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Uwe Glatzel, Metals and Alloys

Creep Experiment
behavior of pure metals:

primary
University Bayreuth, Advanced High Temperature Alloys

secondary
58

tertiary:
Uwe Glatzel, Metals and Alloys

Creep Experimental Setup

up to 1400C

Constant
temperature
aandd stress
st ess oor
load

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Uwe Glatzel, Metals and Alloys

Creep Experimental Setup for

Electrical Conductivityy Material
up to Melting Temperature

Pyrometer from left, optical strain

measurement from right,
g , both contact-free.
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Uwe Glatzel, Metals and Alloys

Interrupted creep tests

single crystal (SX) nickel base superalloy (habilitation thesis Glatzel)
7

[001] orientation,
orientation 1123K,
1123K 650MPa

straiin rate [1/s]

sstrain [%]

8x10-6

4
3
2
1
0

6x10-6

[001] orientation, 1123K, 650MPa

4x10-6
2x10-6
0

10

20

30

40

50

60

70

10

20

30

40

50

60

70

time [h]

time [h]

strain rate [1/s]]

10-5

1123K,, 650 MPa

logarithm of strain rate versus strain

(most valuable information for
materials
i l scientist)
i i )

10-6

10-7
0

University Bayreuth, Advanced High

Alloys
strainTemperature
[%]

61

Uwe Glatzel, Metals and Alloys

Different Creep Stages

primary creep: strain rate d/dt decreases
material hardens
secondary creep stage: strain rate constant
hardening and softening are in equilibrium
dislocation multiplication and annihilation in
equilibrium disl. density = const.
tertiary creep: necking (creep pores) develop
local stress and strain rate increases
drastically
drastically.
University Bayreuth, Advanced High Temperature Alloys

62

Uwe Glatzel, Metals and Alloys

Modelling of Primary and

Secondary
d
Creep Stage

velocity
l i

density

& = b v

University Bayreuth, Advanced High Temperature Alloys

63

Uwe Glatzel, Metals and Alloys

Problem with Low Creep Rates

Life time of stationary gas turbines > 20 years.
years Assuming a
maximum deformation of 3%, this leads to an assumed
steady
d state strain
i rate (neglecting
( l i primary
i
andd tertiary
i
creep) of about &steady state = 510-11 s-1. Reliable data in labs
can only be obtained down to 110-9 s-1 (1 m change with
l0 = 25 mm after 10 h one creep experiment with 3.5%
strain per year!).
Therefore
Th
f
within
ithi university
i
it llabs
b we are ttwo andd more
orders of magnitude too fast than real life in a stationary
gas turbine!
University Bayreuth, Advanced High Temperature Alloys

64

Uwe Glatzel, Metals and Alloys

Engineering Creep Curves

raw data creep curves:

time to failure:

time - strain

isochrone time to failure:

University Bayreuth, Advanced High Temperature Alloys

isochrone strain

65

Uwe Glatzel, Metals and Alloys

Natural Creep Law

& steady state = b v
external

Gb

v~

1
external

& ~
G b

3
external
2

University Bayreuth, Advanced High Temperature Alloys

natural creep law

66

Uwe Glatzel, Metals and Alloys

Norton Creep Law (Empirical)

& = A

n
external

Q creep
R T

with the Norton creep exponent "n" and

Qcreep Qself diffusion

power law
l break
b k
down (plb)

stress dependence
of the stationary
creep rate of the
austenitic steel 800
H at 900C and
1000C:

T = const.
dislocation
climb
diffusional creep
University Bayreuth, Advanced High Temperature Alloys

67

Uwe Glatzel, Metals and Alloys

Diffusional Creep
Nabarro-Hering creep (pure volume diffusion)
& NH = 2

D self

diffusion
2

k T

Coble creep (grain boundary diff.)

& C = 2

D grain

h grain size,

boundary
3

k T

thickness of grain boundary

University Bayreuth, Advanced High Temperature Alloys

68

Uwe Glatzel, Metals and Alloys

Combined NH and Coble Creep:

& diffusion
diff i creep

Dself diffusion D grain boundary D eff

~
= & NH + & C = 2

+
2
2
3
k T
h
h
kT h
D eff = Dself diffusion +

D grain boundary
h

real geometry (non-cuboidal grains)

University Bayreuth, Advanced High Temperature Alloys

69

Uwe Glatzel, Metals and Alloys

Temperature Dependence of
Stationary
i
Creep Rate

= 28 MPA = const.

fcc alloys:
n

Qc

3, 5
& s = A SF
e R T
E

Austenitischer Stahl 800H

University Bayreuth, Advanced High Temperature Alloys

70

Uwe Glatzel, Metals and Alloys

Activation Energy for Creep

slope = 1

University Bayreuth, Advanced High Temperature Alloys

71

Uwe Glatzel, Metals and Alloys

Constant Load Constant Stress

n

F (1 + )
F

n
= & 0 0n (1 + )n
& = & 0 = & 0 = & 0
A
A0
failure

in case the gauge length

deforms uniform with
constant volume
This method is applicable to
determine the stress exponent "n"
only,
y, if the secondaryy creepp state
lasts to at least 10%

ln & = ln & 0 + n ln 0 + n ln (1+) = const. + n ln (1+)

University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys

Ashby Deformation
Mechanism Maps

n=3

University Bayreuth, Advanced High Temperature Alloys

73

Uwe Glatzel, Metals and Alloys

Ashby Deformation
Mechanism Maps
Versetzungsklettern !
dislocation climb !

University Bayreuth, Advanced High Temperature Alloys

74

Uwe Glatzel, Metals and Alloys

Deformation Mechanisms:
Elastic Deformation: Spontaneous and reversible deformation. In the elastic region: = E (rule of
thumb: e, max 10-3, but definitely << 1%). Plastic or non-reversible deformation achieves way higher
strains. Coble-creepp (g
(grain boundary
y diffusion)) is in theory
y possible
p
even at 0 K.
Dislocation Glide: without significant time dependent recovery (climb). Is dominant in the complete
temperature regime from 0 K up to the melting point Tm at moderate and higher stress levels. At low
temperatures (< 0.4T
0 4 Tm) dislocation glide has the lower boundary in the range of the elastic stress limit
(typically 10-3E).
Dislocation Climb: At higher temperatures (> 0.4Tm) and lower stress levels dislocation climb plays the
major role => time dependent constant strain rate (d/dt)ss ~ n, with a Norton stress exponent in-between 3
und 8.
Diffusional Creep: In
In-between
between 0 K und 0.8T
0.8 Tm and very low stress levels: Coble
Coble-creep
creep (grain boundary
diffusion). Below 0.4Tm not measurable. For geological times a time dependent deformation can be
determined. Transition to Nabarro-Herring creep (volume diffusion) is dependent on grain size and grain
boundary thickness
thickness. The transition temperature from coble to Nabarro-Herring
Nabarro Herring creep can be explained by
the different activation energies of volume and grain boundary diffusion.
University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys

Creep of Alloys
i = G b + solid solution

a) interaction dislocation
and impurity (low temp.)
b) stationary dislocation
pinned by impurities
(C
(Cottrell
ll clouds)
l d)
c) pulled off Cortrell clouds
(Ld bands)
(Lders
b d)
d) gliding dislocation trails
i
impurities
iti behind
b hi d (viscous
( i
glide)
lid )

e) impurities faster than dislocation (very high temp., no hardening)

f) annihilation due to dislocation climb
University Bayreuth, Advanced High Temperature Alloys

76

Uwe Glatzel, Metals and Alloys

Precipitation Hardening
i = G b + solid solution + precipitate
threshold stress concept (with n 3 - 4 and Qcreep = Qself diffusion):
n

Qc

0
& ss = A
e R T
E
temperature

coherent and semicoherent phase

boundaries

in-coherent phase
boundaries

cutting

0 K up to Ts

yes

no

bypass by Orowan

0 K up to Ts

yes

yes

> 0.4T
0 4 Ts

yes

no

mechanism

climb
li b over obstacles
b
l

University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys

Hardening Mechanisms as
Function of Precipitate Size
dT0 initial precipitate size
1 and 2 arbitrary external stress levels
= cutting

passing by: & ~ d T

& ~
climbing:
li bi

1
d T2

Cutting is relevant only for coherent

precipitates

Dependence of stationary creep rate on

initial p
precipitate
p
size for two different
external stress levels
University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys

Pinning of Dislocations by
Carbides
bid in
i Austenitic
i i Steell

T = 1000C,
1000C = 25 MPa,
MP carbides
bid off th
the ttype TiC undd M23C6
University Bayreuth, Advanced High Temperature Alloys

79

Uwe Glatzel, Metals and Alloys

Very High Volume Fractions

Volume fractions of 70% are only achievable with non-spherical
non spherical precipitates.
precipitates
Spacing between precipitates is getting smaller Orowan stress
Orowan
G
Gb/L
b/L necessary. For small strains precipitates are not cut by
O
dislocations. With G = 90 GPa, b = 0.25 nm, L 75 nm => Orowan 300 MPa

nickel base superalloys

ODS alloys:
ll
G b f vol.
Orowan
d part.
University Bayreuth, Advanced High Temperature Alloys

80

Uwe Glatzel, Metals and Alloys

Dispersion Hardening
(oxide dispersion strengthened alloys (ODS-alloys))

yield

precipitate strengthened

stress
dispersion strengthened

temperature

back-side p
pinningg of dislocation byy
ODS-particle (Rssler + Arzt)
University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys

Summary:
Hardening
d i Mechanisms
h i
Internal back stress in steady state regime:

i = G b

Orowan stress in case of precipitates or particles:

Orowan Gb/L

Solid solution strengthening:

solid solution const.

In case of coherent precipitates:

a
coherency
E
a

University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys

Creep Damage
creation of a creep pore in polycrystalline material due to disloction glide:

a) cracks at grain boundaries

University Bayreuth, Advanced High Temperature Alloys

b) cavities (micropores) at grain boundaries

83

Uwe Glatzel, Metals and Alloys

Creep Damage
fracture

nucleation, not detectable with OM

micropore, difficult to detect
micro cracks

pear necklace like chain of

micropores (easy detectable)

University Bayreuth, Advanced High Temperature Alloys

84

Uwe Glatzel, Metals and Alloys

Extrapolation of Time-to-Fracture Data

(L
(Larson-Miller
Mill plot,
l Larson-Miller
L
Mill parameter))
M k
Monkmann-Grant
G t relation
l ti with
ith constant
t t K andd exponentt m 1:
1

K
tf = m
& ss

& ss = B e

or:

ln(t f ) = K m ln(& ss )

or:

1
ln((& ss ) = B1 B2
T

Q creep
R T

1
1
ln(t f ) = K m B1 m B2 = C + P
T
T
with material dependent constants C and P
University Bayreuth, Advanced High Temperature Alloys

85

Uwe Glatzel, Metals and Alloys

Larson Miller Plot

Larson-Miller-Plot
stationary
t ti
gas turbine,
t bi about
b t 20 years off service
i ~ 130.000
130 000 h

Comparison of CMSX-6,
LEK 94 andd CMSX-4,
CMSX 4
patent Wllmer, Glatzel,
Mack, Wortmann
University Bayreuth, Advanced High Temperature Alloys

P = T[20 + ln(tf)]10-3 (T in K, tf in h)
86

Uwe Glatzel, Metals and Alloys

Comparison LEK 94 with

CMSX-4 and
d CMSX-6
CMSX-6 [Wortmann 88] 8.0 g/cm3
CMSX-4 [Erickson 94]
8.7 g/cm3
CMSX-4 [Frasier 90]
8.7 g/cm3
3
LEK-2
8.5 g
g/cm
3
LEK-4
8.2 g/cm
LEK-5
8.2 g/cm3
LEK-3
8.1 g/cm3
LEK-66
LEK
88.3
3 g/cm3
3
LEK-1C
8.4 g/cm
3
LEK-1B
8.3 g/cm
3
LEK-1A
8.2 g/cm

500

stress [M
MPa]

24 K

230
T = 10 K

29 K

120
10 K

25

26

27

28

29

30

31

32

Not corrected
regarding density!

Larsen Miller parameter

Larsen-Miller-parameter
-3
P = T (20+log tB) 10
University Bayreuth, Advanced High Temperature Alloys

87

Uwe Glatzel, Metals and Alloys

Contents
11. Introduction
Introduction, Basics
2. Stability of Microstructure
3. Mechanical Properties
a) Static
b) Cyclic (Fatigue)
4 High Temperature Corrosion
4.
5. High Temperature Alloys
6. Lost Wax Investment Casting
7. Depending on Time: Lectures on
a) SX Ni-Base Superalloys b) LEK 94 c) Pt-Base Superalloys
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88

Uwe Glatzel, Metals and Alloys

Time Dependent Variation of Stress

and/or
d/ Temperature
T
and/or
d/ ...

Whler di
Whl
diagram for
f T < 0.4T
0 4 Tm. Z time
ti fatigue
f ti
limit,
li it D endurance
d
fatigue limit
a) type I metal (bcc)

b) type II metal (fcc) endurance limit at 2107

University Bayreuth, Advanced High Temperature Alloys

89

Uwe Glatzel, Metals and Alloys

Change in Whler Diagram with

Temperature and
d Holding
ldi Time
i

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90

Uwe Glatzel, Metals and Alloys

Thermal Fatigue

Thermal breathing of turbine blade:

a)

heating phase: edges reach high temperatures faster than interior

b) cooling phase: edges cool faster than interior

c)

repeated thermal cycles lead to thermal fatigue cracks at edges

University Bayreuth, Advanced High Temperature Alloys

91

Uwe Glatzel, Metals and Alloys

Thermal Strains and Stresses :

thermal = thermal T, or: thermal = E thermal
thermal = E thermal T

University Bayreuth, Advanced High Temperature Alloys

92

Uwe Glatzel, Metals and Alloys

Lower E-Modulus
E Modulus is Helpful:

orientation of single crystals in <100> direction reduces thermal stresses

University Bayreuth, Advanced High Temperature Alloys

93

Uwe Glatzel, Metals and Alloys

TMF and many other Time

Dependent Test Techniques

Can not be covered in this lecture!

University Bayreuth, Advanced High Temperature Alloys

94

Uwe Glatzel, Metals and Alloys

Contents
11. Introduction
Introduction, Basics
2. Stability of Microstructure
3. Mechanical Properties
a) Static
b) Cyclic (Fatigue)
4 High Temperature Corrosion
4.
5. High Temperature Alloys
6. Lost Wax Investment Casting
7. Depending on Time: Lectures on
a) SX Ni-Base Superalloys b) LEK 94 c) Pt-Base Superalloys
University Bayreuth, Advanced High Temperature Alloys

95

Uwe Glatzel, Metals and Alloys

High Temperature Corrosion

oxidation: external and internal, passivation

carburization (internal carbides)
nitration: internal, seldom nitrite passivation
sulfurization: external (sometimes
passivation),
p
ss v o ), se
seldom
do internal
e

Worldwide 1 ton iron per minute corrodes to rust (low

temperature aqueous corrosion).
corrosion)
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Uwe Glatzel, Metals and Alloys

Ellingham Richardson Diagram

Ellingham-Richardson-Diagram
right hand and lower axes
O2 partial pressure at T = 0.
As an example pO2 of
10-15 Pa = 10-20 bar = 10-17 mbar
is shown as a dashed line.
only the oxides below this line
are thermodynamic stable.

University Bayreuth, Advanced High Temperature Alloys

97

Uwe Glatzel, Metals and Alloys

Time Dependent Oxidation

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98

Uwe Glatzel, Metals and Alloys

Oxidation Mechanisms
logarithmic (not shown) low temperature oxidation
which eventually comes to a stop or no measurable increase
in oxide scale thickness (e.g. Al, Cr, Mg).
g (m/A)
(
)2 ~ t. Diffusion through
g
pparabolic mass change
oxidation layer (either oxygen or metal). Most favorable
oxidation behavior.
linear mass change: oxide layer with cracks continuous
contact with metal (e.g. Ta, Nb).
mass loss: volatile oxides catastrophic oxidation (e.g. V,
Mo W,
Mo,
W Cr,
Cr Pt).
Pt) You can see it inside a broken light bulb.
bulb
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Uwe Glatzel, Metals and Alloys

Pilling-Bedworth
Pilling
Bedworth Ratio
PB = (volume of oxide of one metal atom)/(volume of metal atom)
Oxide

TiO

MgO

Al2O3

MgO2

Ti2O3

ZrO2

Ti3O5

NiO

FeO

TiO2

CoO

PB

0.70

0.81

1.28

1.34

1.50

1.56

1.65

1.65

1.70

1.73

1.86

Oxide

Cr2O3

FeCr2O4

Fe3O4

Fe2O3

SiO2

Ta2O5

Nb2O5

PB

2.05

2.10

2.11

2.15

2.15

2.50

2.68

3.40

ideal is 1.1 to 1.3

Of course thermal expansion coefficients also play a major role for the stability of oxide scales.
University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys

Alloying Effects:
different elements have
different oxygen affinity
concentration changes
diffusion rates are different
oxide layer
y contains other
metals

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101

Uwe Glatzel, Metals and Alloys

Example Ni
Ni-Cr-Al
Cr Al
Ni Cr 10 Al 5
oxide layer
y and
internal
oxidation occurs

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102

Uwe Glatzel, Metals and Alloys

[MB1]noch

andere Eigenschaften reinschreiben?

Observations for the

Superalloy Rene N5

Diploma thesis Bensch, 2009

and submitted paper
layer number

layer

composition

properties

cover oxide layer

NiO, CoO

thick and porous monophase layer

interlayer of oxides

NiAl2O4 , NiTa2O6, Cr2O3

thick and porous layer consisting of two fractions

third oxide layer

Al2O3

dense and thin monophase layer

-free layer

see Tab. 1

Al-content of 2.2 wt. %

reduced layer

composition in-between
in between layer number 4 and 6

reduced Al content,
content
morphology change

two-phase centre region

nominal composition of Ren N5 (Tab. 1)

regular / structure, see Fig. 6 f)

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Uwe Glatzel, Metals and Alloys

Contents
11. Introduction
Introduction, Basics
2. Stability of Microstructure
3. Mechanical Properties
a) Static
b) Cyclic (Fatigue)
4 High Temperature Corrosion
4.
5. High Temperature Alloys
6. Lost Wax Investment Casting
7. Depending on Time: Lectures on
a) SX Ni-Base Superalloys b) LEK 94 c) Pt-Base Superalloys
University Bayreuth, Advanced High Temperature Alloys

104

Uwe Glatzel, Metals and Alloys

High Temperature Alloys

T > 500C, Application in:
energy generation
engines (cars, trains, airplanes, ships, ... )
chemical industry
metallurgy
mechanical engineering

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Uwe Glatzel, Metals and Alloys

Overview Metals
strucstruc
ture

Ttrans.Tm
[C]

[g/cm3]

max O-solubility
max.
O solubility
[at.%]

Ti

hdp
krz
k

882
1855

4.5
4.5

31.9
8

krz

1910

6.1

17

Cr

krz

1863

7.2

0.0053

Mo

krz

2623

10.2

0.03

+ very high creep strength

+ lowth, high thermal conductivity, good thermal fatigue strength
very brittle at RT
catastrophic
p oxidation; Tm((MoO5) = 795C
no long lasting coating available

krz

3422

19.3

+ highest melting point of metals (only C with even higher Tm)

+ very high creep strength
+ low th, high thermal conductivity, good thermal fatigue strength
very brittle at RT
catastrophic oxidation > 1000C durch hohe WO3-Abdampfrate
no long lasting coating available
106 very high density
Uwe Glatzel, Metals and Alloys

ele
m.

University Bayreuth, Advanced High Temperature Alloys

advantages/disadvantages
+ low density
+ high melting point
+ abundant
b d t available
il bl
+ low th. (~ 10-5 K-1)
now alloy known with adequate strength for temperatures > 600C
high oxygen and nitrogen solubility > 700C, increased brittleness
linear oxidation > 800C
low thermal conductivity
ignition hazard
catastrophic oxidation; Tm(V2O5) = 658C
very brittle at RT; conventionally not processable

Overview Metals
structure

Ttrans.
Tm
[C]

[g/cm3]

max. Osolubility
[at.%]

krz
kfz
krz

912
1395
1538

7.9
7.7
7.4

0.0008
0.0098
0.029

+ veryy ggood corrosion resistance by

y alloying
y g with Cr or ((Cr + Al))
+ -structure can be stabilized down to RT (by Ni)
+ very good processable and weldable
+ low cost (~ 1 /kg)
strength at high temperatures (> 700C) limited

Co

hdp
kfz

422
1495

8.8
8.7

0
0.048

+ very good corrosion resistance by alloying with Cr or (Cr + Al)

+ Co-alloys castable in air good weldability
only moderate hardening available
Ni-additions necessary to stabilize fcc structure, reduces strength

Nii

kf
kfz

14
1455

89
8.9

00
0.05

+ broad
b d possibilities
ibili i for
f alloying,
ll i
high
hi h strengthh increase
i
possible
ibl
+ very good corrosion resistance by alloying with Cr or (Cr + Al)
+ processable
relatively low melting point
th.
g , low thermal conductivityy
th high,

Pt

kfz

1772

21.5

+ high corrosion and oxidation resistance

+ high melting point
very high density
very expensive (~ 33 /g)

elem.

Fe

University Bayreuth, Advanced High Temperature Alloys

advantages/disadvantages

107

Uwe Glatzel, Metals and Alloys

Evolution of materials
used in aero-engines
The earlier approach of technology
technolog transfer from military
militar to civil
ci il is
tending to switch direction.

www.azom.com
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Uwe Glatzel, Metals and Alloys

10 000 h Life Time

10.000

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109

Uwe Glatzel, Metals and Alloys

Example of Intermetallic
Phases (Ni-Al-System)

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Uwe Glatzel, Metals and Alloys

Ni-Al
Ni
Al Intermetallic Phases
phase

structure

Ttrans.
Tm
[C]

[g/cm3]

Ni3Al

L12

1383

7.5

+ anomalous temperature dependence of strength

+ same structure base
b
than
h Ni matrix
i (fcc)
(f )
+ stable for larger Al variations > 1 wt.% Al
+ ductile as single crystal
high density
brittle
b ittl as polycrystal
l
t l (can
(
be
b hindered
hi d d by
b boron
b
doping
d i (grain
( i
boundary strengthener)
Al-content not sufficient to build stable Al2O3-layer reduced high
temperature oxidation resistance

NiAl

L10

1638

5.85

+ very good oxidation resistance, since 30 wt.% Al

+ high melting point
+ low density
p to melting
g point
p
+ ordered structure up
+ high thermal conductivity
+ low coefficient of thermal expansion
extremely brittle at temperatures below 500C (von Mises criterion
not fulfilled))
low strength at high temperatures

advantages/disdavantages

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Uwe Glatzel, Metals and Alloys

NiAl, B2 Ordered
Intermetallic Phase
At a first sight very interesting (see
g ) but despite
p many
y efforts and many
y
advantages)
100 Mio. US$ research money spent, up today
no bulk usage of NiAl has been achieved.
achieved
BUT: aluminum coatings leading to NiAl
layers is heavily used.

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Uwe Glatzel, Metals and Alloys

Contents
11. Introduction
Introduction, Basics
2. Stability of Microstructure
3. Mechanical Properties
a) Static
b) Cyclic (Fatigue)
4 High Temperature Corrosion
4.
5. High Temperature Alloys
6. Lost Wax Investment Casting
7. Depending on Time: Lectures on
a) SX Ni-Base Superalloys b) LEK 94 c) Pt-Base Superalloys
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113

Uwe Glatzel, Metals and Alloys

MTS-Factory
MTS
Factory in Bayreuth

ground-breakingg ceremony:
g
y 20.02.2008,, topping-out
pp g
ceremony:
y 06.06.2008
start of production:
~ 12/2008
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114

Uwe Glatzel, Metals and Alloys

MTS-Factory
MTS
Factory, June 2008

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115

Uwe Glatzel, Metals and Alloys

MTS-Factory
MTS
Factory, June 2008

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116

Uwe Glatzel, Metals and Alloys

MTS-Factory
MTS
Factory, June 2008

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117

Uwe Glatzel, Metals and Alloys

Processing of a Turbine
Blade
l d

FPI
X-Ray
y

F i
Feinguss,
Wachsausschmelzverfahren,
W h
h l
f h
lost
l wax investment
i
casting,
i ...
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118

Uwe Glatzel, Metals and Alloys

Archaeological Evidence
(Bibracte) ~ 50 B.C.
ceramic mould filled with wax

cloth clip
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119

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Singly Crystal Castin in Bayreuth

at the
h Chair
h i for
f Metals
l And
d Alloys
ll

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Contents
11. Introduction
Introduction, Basics
2. Stability of Microstructure
3. Mechanical Properties
a) Static
b) Cyclic (Fatigue)
4 High Temperature Corrosion
4.
5. High Temperature Alloys
6. Lost Wax Investment Casting
7. Depending on Time: Lectures on
a) SX Ni-Base Superalloys b) LEK 94 c) Pt-Base Superalloys
University Bayreuth, Advanced High Temperature Alloys

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Uwe Glatzel, Metals and Alloys