Dipl Massl S

Investigation of Deformation Structures
Resulting from Semi-Brittle Fracture in

Recrystallized Tungsten and High
Nb-Containing Two-Phase TiAl
Diploma Thesis
submitted by
Stefan Massl
Department of Material Physics
Montanuniversitat Leoben
March, 2005
Acknowledgements
I would like to express my gratitude to my tutor Doz. Reinhard Pippan for the interestig dis-
cussions and his optimism and motivation when experiments turned out to be more complicated
than expected.
Thanks to Dr. Werner Prantl for his comprehensive introduction to the TEM and helping me
every time I had problems with the microscope.
I would like to thank DI Michael Bischof for ion-thinning of the TEM-samples and DI Harald
Chladil who was a great help whenever I had questions related to TiAl.
Thanks to Dr. Herbert Weinhandl for his support concerning computer problems and L
A
T
E
X.
I would like to thank Dr. Christian Motz for assisting me when I had diculties with the FIB.
Thanks to DI Martin Hafok for helping me with the EBSD system.
Last but not least I want to mention the good working atmosphere at the department which
always supported and motivated me.
Leoben, March 2005
A
Contents
Kurzfassung 1
1 Abstract 2
2 Introduction 3
3 Theoretical Background 4
3.1 Brittle Fracture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
3.1.1 Characteristics of Brittle Fracture . . . . . . . . . . . . . . . . . . . . . . 4
3.1.2 The Grith Concept . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
3.2 Ductile Fracture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
3.2.1 Characteristics of Ductile Fracture . . . . . . . . . . . . . . . . . . . . . . 6
3.3 Ductile versus Brittle Behavior . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
3.3.1 General Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
3.3.2 R-Curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3.4 Dislocations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3.4.1 Geometry and Coordinate Systems of Dislocations . . . . . . . . . . . . . 7
3.4.2 The Dislocation Core . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.4.3 Movement of Dislocations . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
3.4.4 Intersection of Dislocations . . . . . . . . . . . . . . . . . . . . . . . . . . 10
3.4.5 Forces on Dislocations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.5 Dislocation Emission from Cracks . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.5.1 Elastic Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.5.2 The Dislocation Free Zone Concept . . . . . . . . . . . . . . . . . . . . . . 18
3.6 Deformation Twinning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
3.7 Transmission Electron Microscope Analyses . . . . . . . . . . . . . . . . . . . . . 21
3.7.1 Origin of Kikuchi Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
3.8 Remark to the Mechanical Tests: Fatigue Crack Growth under Cyclic Compression 23
4 Materials 25
4.1 High Nb-Containing Globular Titanium Aluminide . . . . . . . . . . . . . . . . . 25
4.1.1 Fabrication of Globular Titanium Aluminide . . . . . . . . . . . . . . . . 25
4.1.2 Phase Diagram and Microstructure . . . . . . . . . . . . . . . . . . . . . . 25
4.1.3 Alloy Elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4.1.4 Lattice Structures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.1.5 Fracture Properties and Deformation Structures . . . . . . . . . . . . . . 29
4.2 Recrystallized Tungsten . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4.2.1 Fabrication of the Investigated Tungsten . . . . . . . . . . . . . . . . . . . 31
4.2.2 Microstructure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
B
CONTENTS
4.2.3 Lattice Structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
4.2.4 Fracture Properties and Deformation Structures . . . . . . . . . . . . . . 32
5 Experimental Method 34
5.1 Denomination of the Specimen . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
5.2 Crack Propagation Investigations . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
5.2.1 Specimens . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
5.2.2 Producing the Fatigue Pre-Crack . . . . . . . . . . . . . . . . . . . . . . . 35
5.2.3 Investigation of Crack Propagation . . . . . . . . . . . . . . . . . . . . . . 35
5.3 Preparation of Lamellae with the Focused Ion Beam (FIB) Workstation for Trans-
mission Electron Microscope Analyses . . . . . . . . . . . . . . . . . . . . . . . . 40
5.3.1 Characteristics of the Leo 1540XB Focused Ion Beam Workstation . . . . 40
5.3.2 In-Situ Lift-Out of Lamellae at the Focused Ion Beam Workstation . . . . 40
5.3.3 Characteristics of the Transmission Electron Microscope . . . . . . . . . . 41
5.3.4 Characteristics of the Scanning Transmission Electron Microscope . . . . 41
5.3.5 Electron Back Scatter Diraction . . . . . . . . . . . . . . . . . . . . . . . 41
6 Results 42
6.1 Fracture Toughness and Crack Propagation . . . . . . . . . . . . . . . . . . . . . 42
6.1.1 Titanium Aluminide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.1.2 Tungsten . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
6.2 Fractography and Deformation Structures . . . . . . . . . . . . . . . . . . . . . . 47
6.2.1 Titanium Aluminide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
6.2.2 Tungsten . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
6.2.3 EBSD-Investigations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
7 Discussion 63
7.1 Crack Propagation Investigations . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
7.1.1 Size of the Cyclic Plastic Zone . . . . . . . . . . . . . . . . . . . . . . . . 63
7.1.2 R-Curves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
7.1.3 Evaluation of the Obtained Values for Fracture Toughness . . . . . . . . . 65
7.2 Procedure to Lift Out TEM-Specimens on the FIB Workstation . . . . . . . . . . 65
7.3 Surface Damage Caused by Ion-Thinning of Samples for TEM . . . . . . . . . . . 67
7.4 Deformation Structures in High Nb-Containing TiAl . . . . . . . . . . . . . . . . 70
7.4.1 Crack Origin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
7.4.2 Propagating Crack . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
7.5 EBSD-Investigations of Tungsten . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
8 Conclusion 78
Bibliography 78
A Optical Micrographs of the Fatigue Pre-Cracks 82
B Diagrams Obtained from the Fracture Experiments 85
C In-Situ Lift-Out of Lamellae at the FIB Workstation 93
C
Kurzfassung
Untersucht wird das Auftreten von Verformungsstrukturen, welche beim Bruch bei Raumtem-
peratur einer TiAl-Legierung und von Wolfram entstehen. Die Proben f ur die Messungen
der Bruchz ahigkeit wurden unter Mode I-Belastung gepr uft und die R-Kurven aufgezeichnet.
Die Experimente wurden an CT-Proben durchgef uhrt. Um das Verst andnis f ur die Vorg ange
beim Bruch von semispr oden Materialien zu vertiefen, werden die Ver anderungen der Mate-
rialstrukturen in unmittelbarer N ahe der Bruchober ache untersucht. Eine hoch Nb-h altige
TiAl-Legierung und rekristallisiertes technisches reines Wolfram werden f ur die Untersuchun-
gen verwendet. Beide Materialien brechen vergleichsweise spr od bei Raumtemperatur. Die
Bruchz ahigkeiten von TiAl-Legierungen und Wolfram zeigen ein typisches R-Kurven-Verhalten,
d.h. die Bruchz ahigkeit nimmt mit fortschreitendem Riss zu. Proben f ur Untersuchungen mit
dem Transmissions-Elektronenmikroskop wurden aus verschiedenen Stellen der Bruchober ache
mittels in-situ lift-out Technik auf einer focused ion beam workstation herausgenommen. Daf ur
wurde diese neue Technik zur Probenherstellung etabliert. TEM Analysen wurden durchgef uhrt,
um das m ogliche Auftreten von Verformungsstrukturen wie verformungsinduzierten Zwillingen
und Versetzungen, welche von der Rissspitze emittiert werden, zu untersuchen. Zum Vergleich
wurden Proben f ur das TEM aus dem unverformten Material auf herkommliche Weise hergestellt.
Um durch plastische Verformung an der Rissspitze hervorgerufene Orientierungsunterschiede
nahe der Bruchober a feststellen zu k onnen, wurden EBSD-Untersuchungen durchgef uhrt.
1
1. Abstract
The appearance of deformation structures generated during fracture at room temperature in
a TiAl alloy and tungsten is investigated. The R-curves under mode I loading were recorded.
The experiments were performed on CT-specimens. In order to improve the understanding
of fracture processes in semi-brittle materials the change in the substructure in the immediate
vicinity of the fracture surface is investigated. A high Nb-containing TiAl alloy and recrystallized
technical pure tungsten are chosen for this study as model materials. Both materials fracture in
a relatively brittle manner at room temperature. The fracture toughness of the TiAl alloy and
the tungsten exhibits a typical R-curve behavior i.e. the fracture toughness increases with crack
extension. Samples for transmission electron microscope analyses were taken out at dierent
parts of the fracture surface by in-situ lift-out technique at a focused ion beam workstation.
This new technique for sample preparation was established. TEM analyses were carried out
to investigate possible deformation structures like mechanically induced twins or dislocations
emitted from the crack tip. For comparison, specimens for TEM of the undeformed material
were fabricated by conventional methods. EBSD-investigations were carried out to determine
the change of orientations near the fracture surface due to plastic deformation caused by crack
propagation.
2
2. Introduction
The fracture toughness of many brittle structural materials is greater than predicted by the
Grith theory. It is well known that plastic deformation that occurs at the crack tip is the
reason for this increase in fracture toughness [1]. Such a plastic deformation is caused by
the generation, multiplication and motion of dislocations and/or the formation of deformation
twins. The extent of the inuence of plastic deformation that occurs at a crack tip in high-Nb
containing TiAl and recrystallized W is investigated in this diploma thesis. New techniques like
the focused ion beam technology are used for the preparation of specimens from selected regions
of the fracture surface for transmission electron microscope analyses.
An important aspect of a cleavage fracture analysis in such semi-brittle materials is the mobility
of dislocations. Static dislocation population does not produce eective toughening. Mobile
dislocations consume energy irreversibly when they are displaced against the lattice friction.
The fracture toughness of the material increases and a residual strain is left in the wake of the
crack [2]. Hence, deformation structures like dislocations and/or deformation twins are located
in the vicinity of the fracture surface if plastic deformation occurred at and in the vicinity of
the crack tip.
In recent years -TiAl-bases alloys have been subject of extensive investigations to improve the
mechanical and thermal properties, among others especially the fracture toughness at low and
high temperatures. TiAl alloys may be used to replace the heavier nickel-base super alloys for
applications in advanced energy conversion systems. Demands for higher strength coupled with
good oxidation resistance have led to high Nb-containing TiAl alloys which contain between 5
at% and 10 at% Nb [3]. Concerning fracture toughness, evidence has been given that crack tip
plasticity can lead to an appreciable enhancement in fracture resistance of two-phase materials
[4]. It is expected that the mobility of dislocations essential for crack tip plasticity depends
strongly on alloy composition, phase distribution, grain size and impurity concentration. The
dislocation mobility seems to be determined by localized pinning and jogs. This leads to strongly
bowed out dislocations between the pinning centers [5]. The aim of this study is to investigate
such deformation structures by means of transmission electron microscope analyses.
Polycrystalline tungsten was originally developed for radiation containment and have been used
extensively in penetrator applications as a result of their good combination of mechanical and
thermal properties [6]. In this study a recrystallized tungsten is investigated to determine the
contribution of crack tip plasticity for intergranular brittle fracture. According to Margevicius
et al. it is likely that grain boundary fracture of polycrystalline tungsten absorbs a considerable
amount of the fracture energy and reduces the stress concentration at the crack tip [7].
3
3. Theoretical Background
3.1 Brittle Fracture
3.1.1 Characteristics of Brittle Fracture
The two investigated materials recrystallized polycrystalline tungsten and globular high Nb-
containing TiAl break brittle predominantly at room temperature. Brittle fracture occurs if a
material breaks without previous plastic deformation, i.e. without any movement of dislocations.
The energy absorbed during crack propagation is very low. The crack propagates unstably, it
grows without increase of the applied stress. It can propagate at very high velocities up to the
speed of sound.
It can be distinguished between two types of brittle fracture. Intergranular brittle fracture oc-
curs when the crack growth resistance R of the grain boundaries is smaller than R of the grains.
Trans- or intragranular brittle fracture is based on breaking the atomic bonds in the lattice along
certain crystallographic directions and is the most frequent type of failure in body-centered cu-
bic and hexagonal metals at low temperature; it is also called cleavage crack. Macroscopically
transgranular brittle fracture shows a brilliant fracture surface. Theoretically the cleavage planes
should be perfectly planar, but lattice defects as dislocations, inclusions etc. interact with the
crack and create structures in the material and the fracture surface. Furthermore the propaga-
tion of the cracks in dierent grains also requires the formation of steps. A fracture surface can
show characteristics of both the inter- and intragranular type.
3.1.2 The Grith Concept
The fracture behavior of ideal brittle materials can be described by the Grith Theory. It
approaches crack propagation from the continuum viewpoint. Griths idea was to model a
static crack as a reversible thermodynamic system. Inclusions or other inhomogeneities can be
regarded as such cracks in materials. The important elements are dened in gure 3.1. An
elastic body B containing a plane-crack surface S of length 2a is subjected to loads applied at
the outer boundary A. Grith sought the conguration that minimized the total free energy
of the system. The crack would then be in a state of equilibrium, and thus on the verge of
extension [2].
For the propagation of a crack, the energy provided by the elastic stress eld U
el
and the applied
forces which displace the outer loading points U
w
must be at least as big as the energy necessary
for the creation of the crack surface U
s
[8]:
d(U
el
U
w
)
da

dU
s
da
, (3.1)
4
CHAPTER 3. THEORETICAL BACKGROUND
B
A
2a
S
da da
Figure 3.1: Assumed geometry and loading condition used in the Grith concept
G =
d(U
el
U
w
)
da
, (3.2)
R =
dU
s
da
= 2. (3.3)
The system becomes unstable when
G R. (3.4)
Instead of using the crack resistance R, the critical energy release rate G
c
is utilized frequently
G
c
R. (3.5)
In case of plane strain state, the stress intensity factor K is dened as
K =
G E
(1 )
2
. (3.6)
The material breaks under pure mode I loading (e.g. tension loading of a crack) when
K K
Ic
(3.7)
where
U
el
is the strain potential energy per unit thickness stored in the elastic medium
_
J
m
,
U
w
the potential energy per unit thickness of the applied loading system
_
J
m
,
U
s
the free energy per unit thickness expended in creating new crack surfaces
_
J
m
,
the surface energy per unit area
_
J
m
2
,
a the crack length [m],
G the energy release rate
_
J
m
2
,
5
G
c
the critical energy release rate
_
J
m
2
,
R the crack resistance per unit area
_
J
m
2
,
K the stress intensity factor [MPa
m], and
K
Ic
the critical stress intensity factor for mode I loading [MPa
m].
K and G are loading parameters. R, G
IC
and K
Ic
are characteristic parameters of the material.
K
Ic
is usually called fracture toughness.
3.2 Ductile Fracture
3.2.1 Characteristics of Ductile Fracture
There are dierent denitions for ductile fracture. From the fractographic point of view the
fracture surface shows a typical dimple structure. From the physical point of view, besides
breaking of atomic bonds, other irreversible processes take place, e.g. dislocation movement or
generation of twins, phase transformations etc. In this study we will focus on the physical point
of view.
A fracture process is called ductile when a material breaks after plastic deformation. The energy
absorption of ductile fracture is bigger than in case of brittle fracture. The energy absorbed
creates and multiplies dislocations and forms deformation twins. Compared to the formation of
twins the motion of dislocations is relatively slow. This is the reason why ductile cracks grow
slowly compared to brittle cracks. The propagation can be stable, it can resist further extension
unless the applied stress is increased. Macroscopically ductile fracture does not show a brilliant
fracture surface like brittle fracture. On the microscopic level ductile fracture surfaces appear
rough and irregular. The surface consists of many microvoids and dimples.
3.3 Ductile versus Brittle Behavior
Some materials show characteristics of both ductile and brittle fracture. Below a certain tem-
perature the brittle-to-ductile transition temperature (BDTT) they behave brittle and above
ductile.
3.3.1 General Considerations
Brittle to ductile transition is directly related to the temperature dependency of the energy
absorbed during crack propagation. A material tested at a certain temperature can show char-
acteristics of both brittle and ductile fracture like cleavage planes on the fracture surface and
dislocations when the bulk material is examined with the transmission electron microscope.
The ductile versus brittle behavior of a material can be described on the basis of the magni-
tude of the critical local stress intensity factor k
Ic
relative to local stress intensity factor for
the emission of dislocations k
Ie
. For k
Ic
< k
Ie
, an unstable brittle crack growth without crack
tip deformation is expected. For k
Ic
k
Ie
, crack tip deformation and brittle crack growth are
expected to occur concurrently. For k
Ic
> k
Ie
, dislocations are generated at the crack tip before
the crack can grow, therefore the fracture process is ductile [1]. A more detailed description of
the conditions for the emission of dislocations from the vicinity of a crack tip is given in section
3.5.
6
3.3.2 R-Curve
In ideal brittle materials the crack resistance R is twice the surface energy (equation 3.3)
and is independent of the actual crack length, the type of load and the stress state. In metals
which show a microductile fracture behavior, the stress intensity factor K for crack propagation
is approximately constant. Therefore the critical stress intensity factor K
Ic
is used for the
characterization of materials which fail in a microductile way.
In some non-ideal or, as they are often called, semi-brittle materials the crack resistance R
depends on the actual length of the propagated crack and the stress state. Therefore the critical
stress intensity factor K
Ic
describes the fracture behavior in an insucient way. The R-curve
represents the dependence of the crack resistance R and the critical stress intensity factor K
Ic
on the crack extension a respectively. The criterion for fracture can be determined by a
combination of the R curve and the G curves versus a as a function of the load as depicted in
gure 3.2. As long as G intersects with the R-curve below point I, the crack does not propagate.
The initial critical stress intensity factor for mode I loading K
iIc
represents the stress intensity
where the rst crack propagation is observed. Between I and the critical point II the growth
is stable under the load G
2
. From point II on the crack propagates unstable if subjected to a
load equal or greater than G
3
. The maximum critical stress intensity factor for mode I loading
is K
Icmax
, which can be determined in a load controlled experiment only for very long cracks
where the slope dG/da is very low in the critical case [8].
G,R
da
a
0
R(non-idealbrittlematerial)
G
3
R(idealbrittlematerial)
G
2
G
1
II
I=K
iIc
K
Icmax
Figure 3.2: Schematic representation of an R-curve for an ideal brittle material and a non-ideal
brittle material; G versus a curves for dierent applied load for a given initial crack length a
0
3.4 Dislocations
Movement of dislocations is the main mechanism which causes plastic deformation. In general
it is distinguished between two types of dislocations: the edge and the screw dislocation. The
atomic arrangements of such dislocations are depicted in gures 3.4.1 and 3.4.1.
3.4.1 Geometry and Coordinate Systems of Dislocations
The Burgers vector b of an edge dislocation is perpendicular to the line of the dislocation. For
convenience a coordinate system is chosen whose z axis coincides with the tangent vector l of the
dislocation line. The edge dislocation propagates in positive x direction. In case of a positive
edge dislocation (gure 3.3(a)), the extra half-plane of atoms extends in the negative y direction
7
and the Burgers vector b has a positive value. The extra half-plane of atoms of a negative edge
dislocation (gure 3.3(b)) extends in the positive y direction and the Burgers vector b has a
negative value.
b
x
z
l
t
y
(a) Positive edge dislocation
b
x
y
z
l
t
(b) Negative edge dislocation
Figure 3.3: Schematic representation of edge dislocations in a simple cubic crystal
In case of a screw dislocation, the Burgers vector b is parallel to the line of the dislocation.
The tangent vector l of the dislocation is chosen to point in the positive z direction. The screw
dislocation propagates in positive x direction. The screw dislocation is called left-handed if value
of the Burgers vector b is positive (gure 3.4(a)). It is called right-handed if the value of the
Burgers vector b is negative (gure 3.4(b)).
x
z
b
y
t
l
(a) Left-handed screw dislocation
z
x
y
t
b l
(b) Right-handed screw dislocation
Figure 3.4: Schematic representation of screw dislocations in a simple cubic crystal
Mixed dislocations (gure 3.5) consist of both edge and screw dislocation parts. Thus, the
Burgers vector b of a straight dislocation of mixed character makes some arbitrary angle with
the dislocation line l itself. If the z axis coincides with the dislocation line l at an arbitrary
point and the x axis is placed in the slip plane of the dislocation, the Burgers vector b can be
written as
b = b
x
i +b
z
k, (3.8)
where
b
x
is the component of the Burgers vector in the x direction,
8
b
z
the component of the Burgers vector in the z direction,
i the unit vector in x direction, and
k the unit vector in z direction.
x
y
z
l
b
t
Figure 3.5: Schematic representation of a mixed dislocation in a simple cubic crystal
3.4.2 The Dislocation Core
The stress eld of a dislocation can be described by a linear elastic theory except in a very
small regime in the vicinity of the defect which is called dislocation core. The denition of the
core radius of a dislocation is somewhat imprecise, hence it is more correct to use the physically
better dened dislocation width.
When an extra half-plane of atoms is created by the presence of an edge dislocation of Burgers
vector b, the atoms in the planes above (a) and below (b) the slip plane are displaced by u as
shown in gure 3.6. The displacement dierence u between two atoms on adjacent sites above
and below the slip plane can be calculated as
u = u
b
u
a
,
where
u is the displacement dierence [m],
u
a
the displacement of an atom above the glide plane [m], and
u
b
the displacement of the adjacent atom below the glide plane [m].
The width of the dislocation core w is dened as the distance over which the displacement
dierence u is greater than half of its maximum value (gure 3.7). Computer simulations
usually nd core widths w between b and 5b, depending on the interatomic potential and the
crystal structure [9].
9
a
b
u
b
u
a
y
x slip
plane
b
Figure 3.6: Displacement of atoms at an edge dislocation
Du/b
x
w
+0,5
-0,5
-0,25
+0,25
Figure 3.7: Displacement dierence
3.4.3 Movement of Dislocations
Motion on a slip plane i.e. glide is called conservative motion. The slip plane has to contain
both the line vector l and the Burgers vector b of the dislocation. Slip planes are usually planes
with the highest density of atoms. Screw dislocations can switch from one slip plane to another
since the Burgers vector b and the line vector l are parallel. This process is called cross slip.
Another moving mechanism of dislocations is climb, which is called nonconservative motion.
Since the process of climb requires diusion, it is more likely to occur at elevated temperatures.
3.4.4 Intersection of Dislocations
A dislocation moving in an glide plane is referred to as gliding dislocation. These dislocations
are intersected by dislocations which traverse the glide plane. The latter are called forest dislo-
cations. The forest dislocations are not necessarily perpendicular to the slip plane [9].
The structures of the intersected forest and gliding dislocations are determined by their Burgers
vectors b. Since the dislocation shears the material on either side of the slip plane through
a displacement equal to its Burgers vector b, a forest dislocation cut by a gliding dislocation
henceforth contains a step. This step is parallel to the Burgers vector b of the gliding dislocation.
In most cases the gliding dislocation also contains a step after intersecting the tree dislocation.
The resulting structures can be classied as kinks or jogs.
Kinks displace the dislocation on the same slip plane. Thus it does not impede glide of the line
10
of both edge and screw dislocations. Jogs move the dislocation from one slip plane to another.
Therefore jogs may impede further glide of the dislocation.
The intersection of a left-handed and a right-handed screw dislocation (gure 3.8f) produces
two steps. Since the Burgers vector b and the line vector l of the step are perpendicular, the
structures have edge character. In both cases the Burgers vector b does not lie in the slip plane
of the dislocation, therefore the resulting structures are called jogs and are immobile. The jogs
can move anyhow: by a conservative process along the line of the screw dislocation or by a
non-conservative process e. g. climb at elevated temperatures.
An example for a mobile jog is the intersection of two edge dislocations with perpendicular
Burgers vectors b (gure 3.8a). The gliding dislocation does not contain a step, since the line
vector l of the gliding dislocation is parallel to the Burgers vector b of the tree dislocation. The
step in the tree dislocation is a jog with the Burgers vector b lying in the slip plane of the tree
as well as the gliding dislocation. Together with the line vector l, the jog of the tree dislocation
lies in the slip plane of the gliding dislocation. This is not the same slip plane as the one of the
tree dislocation, but motion must be possible on this plane since the movement is not inhibited
for the gliding edge dislocation [10].
jog
kink
kink
jog
kink
kink
jog
jog
jog kink
b
l
b
b
b
b
b
b
b
l
l
l
l
l
l
l
a)
b)
c)
d)
e)
f)
Figure 3.8: Dislocation intersections: vertical forest dislocations intersected by horizontal gliding
dislocations; the gliding dislocations move from left to right
3.4.5 Forces on Dislocations
The total force on a curved dislocation consists of three parts:
forces which result from line tension,
chemical forces, and
forces arising from applied stresses or stresses induced by other dislocations.
When a dislocation is located near a surface or interface, the image force also becomes important.
Line Tension
A dislocation which is free to move containing a bulge will straighten and shorten itself. A
dislocation loop tends to decrease in radius and ultimately disappear, thus any curved dislocation
segment (gure 3.9) must be subjected to a force. This force produces the line tension T which
acts in a direction tangential to the dislocation line. The segment experiences a downward force
11
equal to 2T sin , where is the angle the tangent to an end of the segment and the horizontal
x direction. In order to be in equilibrium, an additional force F
l
must act on the segment in the
positive y direction. The line tension is given by the approximate expression [10]
T
Gb
2
4
log

5b
, (3.9)
where
T is the line tension [N],
G the shear modulus [MPa],
b the length of the Burgers vector [mm], and
the radius of curvature of the dislocation line [mm]
x
y
b
r
T T
F
l
q
Figure 3.9: Force on a curved dislocation segment
Forces Arising from Ordinary Stresses: The Peach-Koehler Equation
For the following calculations the coordinate system as depicted in gure (3.10) is used.
y
x
z
t
zx
t
xz
t
xy
t
yx
t
zy
t
yz
s
x
s
y
s
z
dislocationline
slipplane
Figure 3.10: Stresses on a volume element of a dislocation gliding in the depicted slip plane
12
The force on the dislocation F due to externally applied stress can be described by the Peach-
Koehler equation [10]55
F = t G, (3.10)
G = b,
=
_
_
x

xy

xz
yx

y

yz
zx

zy

z
_
_
,
b =
_
_
b
x
b
y
b
z
_
_
,
t =
_
_
t
x
t
y
t
z
_
_
,
where
F is the force on the dislocation per unit length
_
N
m
,
t the unit vector parallel to the dislocation line [1],
the stress tensor [MPa], and
b the Burgers vector [m].
z
x
y
t
b l
F
(a)
b
F
x
z
l
t
y
(b)
Figure 3.11: Forces on a screw (a) and an edge (b) dislocation due to external stress
13
Chemical Force
The chemical force (gure 3.12) arises from the existence of a nonequilibrium concentration
of lattice vacancies or interstitial atoms within the crystal. Only at the dislocation line itself
vacancies can be created or destroyed.
According to the Peach-Koehler Equation, an edge dislocation experiences a downward force
under a tensile stress
x
. Since vacancies are free to diuse away from the dislocation, it can
move downwards. This motion is called negative climb (gure 3.13). When the dislocation
moves, it creates more and more vacancies. However, since there is no other place than the
dislocation line where vacancies can be destroyed, the vacancy concentration must increase as the
dislocation continues to move downwards. Eventually vacancy creation becomes such a dicult
process that the dislocation will be unable to continue motion unless the stress
x
is increased.
The excess vacancy concentration has produced a chemical force F
c
equal in magnitude but
opposite in direction to the force F [10].
F
c
F
s
x
s
x
Figure 3.12: Chemical force on a dislocation
positiveclimb
negativeclimb
Figure 3.13: Dislocation climb: creation or annihilation of vacancies
Image Force
The image force becomes important when a dislocation is located near the surface. Dislocations
move towards free surfaces since there the strain energy of the material is reduced. When the
dislocation reaches the surface, it is eliminated from the crystal and its self-energy vanishes. The
reduction of energy is not a sudden process which occurs just at the moment the dislocation
arrives at the surface, the energy diminishes gradually with decreasing distance to the surface.
This results in a force on the dislocation which can be described by an image dislocation similar
to the force on a charge in the vicinity of a metal surface. An image dislocation (gure 3.14)
14
is a virtual dislocation of opposite sign at the other side of the surface, therefore an attractive
force exists between the dislocations respectively between the dislocation and the surface [10].
solid
freesurface
d d
dislocation
imagedislocation
F
i
F
i
Figure 3.14: A dislocation and its virtual image dislocation
3.5 Dislocation Emission from Cracks
Crack tip deformation at very small loads occurs primarily by emitting dislocations from the
crack tip. This is reasonable in view of the fact that the stress is highest at the crack tip and
other sources of dislocations are absent in the vicinity [1].
3.5.1 Elastic Considerations
Stresses and Forces on Dislocations in the Vicinity of a Crack Tip
For cracks of mode I type, the plastic zone consists of edge dislocations on slip planes inclined by
angle to the crack plane. Those slip planes activated at the crack tip are systems of maximum
crack tip Schmid factor. For a dislocation with Burgers vector b a distance r ahead of the crack
front there exists an attractive image stress
i
Gb/r and a repulsive stress
a
K/
r due
to the applied external loading. The generated dislocations induce crack blunting as they move
away from the crack tip, leaving behind a dislocation free zone (DFZ) between the crack tip and
the plastic zone. According to Bilby et al [11], dislocations must overcome the friction stress
f
of the lattice in order to glide along the slip plane. The distance at which the stress on the
dislocation equals the friction stress for the rst time is indicated by r
0
.
The shear stress on an edge dislocation on a slip plane that is making an angle with the crack
plane is given by
r
=
k
I
(8r)
1
2
sin cos(
2
)
Gb
4(1 )r

4 10
6
r
c
e
3
2
sin
4r
2
+r
2
c
e
3
, (3.11)
where
the rst term is induced by the applied stress intensity K
I
,
the second term is caused by the image force, and
the third represents the eect of crack blunting.
15
r
t
f
r
0
r
1
totalstress
imagestress~r
-1
crackstress ~r
-1/2
t
rf
dislocationfreezone
Figure 3.15: Schematic representation of the shear stress
r
acting on a dislocation in the
vicinity of a crack tip as a function of the distance r from the crack tip
The applied stress exerts a repulsive force on the dislocation and hence will tend to drive
the dislocation away from the crack tip. This stress is opposed by the image stress and the
blunting contribution, which both work against the emission of dislocations. The force on a
single dislocation due to a shear stress
r
can be described by
F
r
=
r
b
10
3
.
Derived from equation 3.11, the force on an edge dislocation can be written as
F
r
=
k
I
b
10
3
(8r)
1
2
sin cos(
2
)
Gb
2
4 10
3
(1 )r

4 10
3
br
c
e
3
2
sin
4r
2
+r
2
c
e
3
. (3.12)
As shown in gure (3.15) and according to equation (3.12), there is always an attractive force
for small values of r
c
and a repulsive force for larger values of r at a sucient load. On the basis
of purely elastic eects and for r
c
< r
0
, a crack will always be mechanically stable against the
spontaneous emission of a dislocation. For values r > r
0
the dislocation already sees a repulsive
elastic force and will move away from the crack tip until =
1
at r = r
1
(gure 3.15). For
values of r smaller than the core width of the dislocation and crack, the elastic approximation
breaks down. Therefore Rice and Thomson [12] assumed that a dislocation is spontaneously
emitted if r
0
r
c
[13, 1]. According to this theory, the dislocation is assumed to be suddenly
well formed and no allowance is made for its gradual build-up [14]. If the shear stress
r
at r
c
in equation (3.11) is substituted with the friction stress
f
, the critical stress intensity factor k
Ie
for the emission of a dislocation is given as
k
Ie
=
_
f
+
Gb
4(1 )r
c
+
4 10
6
r
c
e
3
2
sin
4r
2
+r
2
c
e
3
_
(8r)
1
2
sin cos(
2
)
, (3.13)
where
16
r
is the shear stress on the edge dislocation [MPa],
F
r
the force per unit length on the edge dislocation
_
N
mm
,
k
I
the local crack tip stress intensity factor (mode I) [MPa],
b the Burgers vector [m],
r the distance on the slip plane between the dislocation and the crack tip [m],
r
c
the core radius of the dislocation [m],
the angle between the crack plane and the slip plane [1],
G the shear modulus [MPa],
the Poissons ratio [1], and
the surface energy
_
J
m
2
.
According to equation (3.13) the minimum value for the critical stress intensity factor for dislo-
cation emission for mode I k
Ie
is found for a value of approximately 70
(gure 3.16). It has to

be pointed out that the calculations describe the stress, the force on a dislocation respectively,
and not the stress eld in the material contributed by the dislocations.
f
r
x
Figure 3.16: Emission of dislocations from a crack tip under mode I loading
Reduction of the Local Stress Intensity Factor Caused by the Emission of Dislocations
The emission of dislocation blunts the crack and reduces the crack tip stress eld, hence it is
more dicult to emit dislocations from a blunted crack than from a sharp crack. This decrease
in the local stress intensity factor caused by the stress eld of a dislocation is called dislocation
shielding of the crack tip. The local stress intensity factor for mode I loading k
I
is given as
k
I
= K
I
+k
Id
, (3.14)
where
k
I
is the local crack tip stress intensity factor for mode I loading [MPa
m],
17
K
I
the global stress intensity factor for mode I loading [MPa
m], and
k
Id
the stress intensity factor for mode I loading contributed by the dislocation [MPa
m].
The stress intensity factor for mode I loading induced by a dislocation k
Id
emitted along an
inclined slip plane is given as
k
Id
=
3Eb
4(1
2
)(2r)
1
2
sin cos(
2
) (3.15)
where
k
Id
is the stress intensity factor for mode I loading contributed by a dislocation [MPa
m],
E the Youngs modulus [MPa],
b the Burgers vector [m],
the Poissons ratio [1],
r the distance between the dislocation and the crack tip on the slip plane [m], and
the angle between the crack plane and the slip plane [1].
It should be noted that, for 0 < < 2 and k
Id
< 0, a dislocation emitted in one of these direc-
tions always shields the crack tip from the applied stress intensity. The dislocation shielding by
crack tip deformation is therefore a mechanism by which the fracture toughness of a material is
raised. When a number of dislocations are emitted from the crack tip, the stress intensity factor
for mode I loading contributed by a dislocation k
Id
is inuenced by the mutual interactions of
these dislocations.
3.5.2 The Dislocation Free Zone Concept
A consequence of the dislocation emission from the crack tip is the presence of the dislocation
free zone between the crack tip and the plastic zone. It was experimentally observed and theo-
retically veried.
If the stress on a dislocation is bigger than the friction stress
f
(between r
0
and r
1
in gure
3.15), it forces the dislocation out of the immediate crack environment. Thus, the zone between
r
0
and r
1
is free of dislocations. The stress in this dislocation free zone is greater than the yield
stress
y
, but, due to partial dislocation shielding, lower than the stress at the crack tip without
the emission of dislocations.
The plastic zone is located behind the dislocation free zone. As depicted in gure 3.17, the stress
in the plastic zone is equal the friction stress
f
because no work hardening is assumed. The size
of the plastic zone depends on the ratio of the applied stress
a
to the friction stress
f
. The
number of the dislocations in the plastic zone is N
max
. In case of a pure plastic crack, where
no dislocation free zone exists (gure 3.18(b)), the crack tip can be regarded as being shielded
completely from the applied global stress intensity factor K.
Figure 3.17 shows the stress distribution in a slip band after emission of few dislocations. In the
vicinity of the crack tip the dislocation free zone where the local stress intensity factor describes
the stress eld is located. In the following plastic zone the mean stress is equal to the friction
18
DFZ plasticzone elasticzone
t
f
t
a
r
t
rf
Figure 3.17: Stress elds in the dislocation free zone (DFZ), the plastic zone and the elastic
zone. The stress elds around the dislocations are also drawn in;
f
. . . friction stress ,
a
. . .
applied stress
stress. On the atomistic scale the stress eld of the dislocations is drawn in. The plastic zone is
then surrounded by the elastic zone.
In principal cracks can be classied in three dierent types:
the elastic crack,
the plastic crack, and
the elastic-plastic crack.
Between the elastic crack and the plastic crack, we have a wide range of elastic-plastic cracks
(gure 3.18(c)) in which a dislocation free zone is part of the crack tip equilibrium conguration.
The elastic-plastic crack can be dened as a crack in which the crack tip stress eld is relaxed
by a certain amount due to crack tip deformation but not to the full extent, so that the value
of the local crack tip stress intensity factor k
I
is less than the applied stress intensity factor K
but greater than zero [1]. Once the applied stress
a
, the friction stress
f
and the number of
dislocations in the plastic zone are assigned, the length of the dislocation free zone and of the
plastic zone are determined. The sizes of both zones may vary with the crack speed [15].
It should be noted that the stress eld of the dislocations in the dislocation-free-zone model is
valid only for thick specimens [16]. Since the specimens used are much bigger than the size of
the plastic zone, the considerations are valid for this study.
19
(a) Elastic crack, k = K
pz
(b) Plastic crack, k = 0
pz
dfz
(c) elastic-plastic crack, 0 < k <
K
Figure 3.18: Classication of cracks based on the distribution of dislocations; pz. . . plastic zone;
dfz. . . dislocation free zone
3.6 Deformation Twinning
Besides movement of dislocations mechanical twinning can play an important role in plastic
deformation in general and especially at the crack tip of semi-brittle materials.
Deformation twinning is a process in which a region of a crystal undergoes a homogeneous shear
that changes the original crystal structure in a new orientation. The two single crystals of the
same species but in dierent orientations are called twin components. The mirror plane along
which the lattice points are shared in twinned crystals is called the coherent composition plane.
The other interfaces between the twin and the matrix are incoherent. Deformation twinning
can be induced by plastic deformation and plays an important role in face-centered cubic and
hexagonal crystals. Deformation twinning leads to a characteristic change of the orientation.
The twinned region describes a rotation of 180
by a straight line perpendicular to the compo-

sition plane. Besides the reection across a mirror plane, twins can also be generated by the
rotation around an axis (twin axis) or the inversion through a point (twin center) in the crystal
[9, 17].
The geometry of a twin system can be described by the composition plane and the displacement
direction or the displacement plane. The composition plane lies perpendicular to the displace-
ment plane, the straight intersection line indicates the displacement direction (gure 3.19). A
composition plane cannot run parallel to a mirror plane of the crystal structure because in that
case both twin components would have the same orientation [19].
The twin systems of the face-centered cubic, body-centered cubic and hexagonal structure are
listed in table 3.1.
Table 3.1: Twin systems of fcc, bcc and hcp structures
lattice structure composition plane deformation direction displacement plane
fcc {111} 112 {110}
bcc {112} 111 {110}
hcp
_
1012
_
1011
_ _
1210
_
20
composition
planes
displacement
direction
displacement
direction
composition
planes
displacement
direction
displacement
direction
displacement
plane
Figure 3.19: Arrangement of atoms in a twin; composition planes, displacement directions and
displacement plane
Another possibility to represent the orientation relation of a twin system are pairs of axis and
angles. They describe the possible rotations of the lattice of the matrix by dierent angles in
order to achieve the determined orientation of the twin. The axis-angle pairs for a face-centered
cubic lattice are depicted in table 3.2.
Table 3.2: Axis-angle pairs for a fcc lattice
Axis Angle
110 70.53
110 109.47
111 60
111 180
210 131.81
211 180
311 146.44
3.7 Transmission Electron Microscope Analyses

The transmission electron microscope (TEM) is a useful tool to analyze the deformation in a
crystal. There are dierent ways to characterize the deformation:
the direct observation of dislocations and twins or the
indirect examination from the change of crystal orientation.
One possibility to determine the crystal orientation is the evaluation of Kikuchi patterns. Such
a pattern consists of an arrangement of pairs of Kikuchi lines. If at least three pairs of Kikuchi
lines are dened in a diraction picture, they can be used to determine the orientation of a
crystal of a thin sample in a transmission electron microscope.
3.7.1 Origin of Kikuchi Lines
In thin TEM-specimens elastic diraction of electrons is the dominant process. The elastic
diraction occurs at the Coulomb eld of the nucleus. Since the mass of the nucleus is much
21
bigger than the mass of an electron, hardly any energy is transferred from the electron to the
nucleus. The elastic diraction leads to discrete diraction maxima in crystalline specimens.
With increasing thickness of the specimens, inelastic scattering of electrons becomes more and
more important. For the inelastic process, deection of the incoming electrons occurs at electrons
of the shell. In this case there is a certain energy transfer from the beam electrons to the electrons
of the shell. The diraction is diuse and the intensity decreases with increasing angle from the
primary electron beam I
0
as depicted in gure 3.20.
angle
I
I
a
I
b
a
b
Figure 3.20: Intensity of the inelastically scattered electrons as a function of the angle between
the primary electron beam and the scattered electrons
The primary electron beam I
0
produces a cone of inelastically scattered electrons in every point
in the lattice. The energy of the inelastically scattered electrons can be considered as constant.
These inelastically scattered electrons can be regarded as new primary beams I
0
and can produce
new Bragg reections on planes. Planes which are nearly parallel to the incident beam diract
electrons on both sides as depicted in gure 3.21. The diracted electrons have dierent energies
ergo the electron beams of both sides of the plane have dierent intensities. The result is a dark
and a bright Kikuchi line. The lines which appear in the diraction pattern are actually conic
sections due to the fact that the diraction cones are cut by the screen [20].
22
q
q
a
b
latticeplane
TEM-specimen
I
0
I
0
bright
line
dark
line
b-a=2q
I
a
I
b
screen
Figure 3.21: Kikuchi lines: The drawing is not scaled. In reality the angles , and are very
small and the distance between the specimen and the screen is large compared to the thickness
of the specimen
3.8 Remark to the Mechanical Tests: Fatigue Crack Growth under
Cyclic Compression
The generation of pre-cracks for fracture mechanics investigation is relatively dicult. The
method of cyclic compression is one possibility and was used to produce fatigue pre-cracks in
this study. A short description of the bascics of the method is given below.
In the case of small scale yielding and for cyclic tension the stress intensity factor range K and
the yield stress
y
of the material determine the cyclic deformation around the crack tip [34].
This is also valid for a notched specimen provided that the notch root radius is much smaller
than the size of the cyclic plastic zone. In the latter case it makes no dierence whether one has
cyclic tension or cyclic compression as long as the notch surfaces do not contact each other [22].
Cyclic compression tests can be performed at constant load amplitude. Each load cycle leads to
a cyclic plastic strain in the cyclic plastic zone which causes the crack initiation. According to
Irvin the size of the monotonic plastic zone is
=
K
2
max

2
y
(1 2)
2
, (3.16)
where
is the size of the monotonic plastic zone [m],
K
max
the maximum stress intensity factor [MPa
m],
y
the yield stress [MPa], and
23
Dw
w
s forK=K
max
s forK=K
min
-s
y
s
y
s
x
(a) Cyclic tension
Dw
w
s forK=K
min
s forK=K
max
s
y
-s
y
s
x
(b) Cyclic compression
Figure 3.22: Schematic stress distribution in front of a sharp notch in case of cyclic tension and
cyclic compression
the Poisson ratio [1].
According to Rice the size of the cyclic plastic zone can be written as
=
K
2
4
2
y
(1 2)
2
, (3.17)
where
is the size of the cyclic plastic zone [m], and
K
max
the stress intensity factor range [MPa
m].
An advantage of the cyclic compression over the cyclic tensile tests is that the part of the ampli-
tude where the crack is open decreases until the crack arrests. The size of the monotonic plastic
zone
0
, which appears in the rst cycle of the compression test at K = K
max
, represents the
upper limit of the length where the crack arrests. The size of the cyclic plastic zone
0
, which
appears in the rst cycle of the compression test at K = K
min
, represents the lower limit of the
length of the arrested crack. The shape of the crack depends on the number of cycles N, the
stress intensity factor range K and the stress ratio R =
K
min
K
max
[22].
24
4. Materials
4.1 High Nb-Containing Globular Titanium Aluminide
Intermetallic -TiAl based alloys are potential candidates for advanced applications in aerospace,
automotive and related industries since research and development on -alloys have progressed
signicantly within the last two decades. However, for widespread application of -alloys
a further improved balance between room temperature ductility, fracture toughness, high-
temperature strength and oxidation resistance is required [23]. The properties listed below
make them suitable for high temperature applications [24]:
high melting point of up to 1600
C,
low density of 4 g/cm
3
,
high elastic modulus of up to 180 GPa,
low diusion coecient, and
good resistance against oxidation and corrosion.
Compared with standard TiAl alloys, high Nb-containing TiAl alloys have a very high yield
strength
y
of about 1000MPa at room temperature [3].
4.1.1 Fabrication of Globular Titanium Aluminide
The investigated material with the composition Ti-42Al-7.5Nb (B, Si, C) was fabricated by
B ohler Schmiedetechnik GmbH & CoKG by conventional ingot metallurgy methods. The cast
ingots were vacuum arc remelted, the resulting TiAl rods had a diameter of 90 mm. To prevent
damage of the surface, a steel encasement was welded around the rod. The space between the
TiAl rod and the steel protection was evacuated. During the extrusion at 1250
C, the diameter
of the TiAl rod decreased to 26 mm, respectively to 30 mm with steel encasement. According to
the equation
r
= ln(r
0
/r), the reduction of the diameter corresponds to a deformation strain
of 124 %. The material cooled down to room temperature in silicon akes to ensure a smooth
cooling. To reduce the residual stresses of the material, it was annealed at 1000
C.
4.1.2 Phase Diagram and Microstructure
The quasi-binary section of the ternary Ti-Al-Nb diagram for a Nb concentration of 8 % was
determined by Chen et al. [25] (gure 4.1).
The microstructure of conventional TiAl-alloys can be divided into ve basic types, depending
on the heat treatment [5, 26, 27].
25
CHAPTER 4. MATERIALS
Figure 4.1: Quasi-phase diagram showing the eect of 8% Nb addition on the phase realtionship
of near- TiAl alloys (solid lines). The binary TiAl phase diagram is drawn in dotted lines for
reference 4.1
The as-cast microstructure is usually coarse and consists of columnar grains. The -TiAl
lamellae with interspersed
2
-Ti
3
Al platelets are surrounded by interdendritic Al rich
regions (gure 4.2(a)).
Heat treatment in the middle of the two-phase + region at about 1200
C leads to a
duplex microstructure which is composed of grains and lamellae colonies and a few small
2
precipitates at the grain boundaries of the grains (gure 4.2(b)). In such two-phase
grains, the lamellae have a dened orientation relation:
(111) || (0001)
2
[110] || [1210]
2
For generating a Nearly lamellar microstructure cast -alloys are heat-treated slightly
below the transus temperature. This leads to mainly lamellar grains. Besides the existing
small quantity of grains, boron proved to be very benecial for obviating uncontrolled
growth of grains (gure 4.2(c)).
Hot working and subsequent heat treatment at a temperature slightly above the eutectoid
one ( 1125
C) leads to near- microstructures consisting of equiaxed grains and ne
2
grains or precipitates at grain boundaries (gure 4.2(d)).
26
Fully-lamellar microstructures are generated when annealing the material in the -region
and cooling quickly. Since a phase does not exist, the grain growth is not inhibited. The
grain sizes are between 100m and 500m (gure 4.2(e)).
(a) (b) (c)
(d) (e)
Figure 4.2: Types of microstructures of two-phase -TiAl
The investigated material Ti-42Al-7.5Nb is a duplex-type material. The microstructure is de-
picted in gures 4.3, 4.4 and 4.5. The bright elongated particles are Titanium-Niobium Borides
(Nb, Ti) B
2
. It is suggested that Nb reduces the stacking fault energy [28] which can explain
the signicant number of twins visible in the micrographs. The darker regions are -grains.
The lamellar structure in the remaining grains results from the
2
and lamellae which have a
thickness of 200 nm.
4.1.3 Alloy Elements
Although it has been demonstrated that the alloy composition signicantly aects the mechanical
properties, the role of various alloy elements is not suciently clear. Nevertheless, certain rules
have been empirically established and can be used as guidelines. The content of Al of 42 at% is
relatively low for two-phase TiAl alloys for structural applications where the Al contents usually
are between 46 at% and 49 at%. In general, a reduction in aluminium content tends to increase
the strength level, but reduces ductility and oxidation resistance. Alloying with Nb generally
decreases the - and -transus temperatures and contracts the -phase eld as depicted in gure
4.1. Nb improves the oxidations resistance of the phase but does not change the constitution
for concentrations up to 8 at%. This modication leads to a signicant structural renement,
which is the most important source of the high yield strength of the material [3, 32]. Nb
27
Figure 4.3: Microstructure of the extruded Ti-42Al-7.5Nb (B, Si, C) parallel to the extruding
direction
is distributed in equal amounts to the
2
and phases [25]. Atom location by channeling
enhanced microanalysis studies showed that Nb preferentially substitutes for Ti [29]. Additions
of 1-2 at% Nb are required in order to achieve sucient oxidation resistance. The lamellar
constituents of the microstructure
2
and exhibit very ne lamellar spacing. This results
in a dense arrangement of interfaces, which impede dislocation glide and mechanical twinning.
Other investigations showed an activation of twinning, an observation that suggests that the
stacking fault energies of TiAl are lowered by Nb additions [28]. A decrease in stacking fault
energy furthermore has a positive eect on the creep strength at high temperatures since cross
glide of screw dislocations is inhibited. B, which builds Titanium-Niobium Borides (Nb, Ti) B
2
,
acts as grain rener, is used for stabilizing the microstructure during casting, high temperature
service and improves workability. It is assumed that C increases the creep resistance, but reduces
ductility. The addition of Si forms Ti
5
Si
3
, which stabilizes the lamellar structure [30].
4.1.4 Lattice Structures
The atomic arrangements in the ordered L1
0
structure (face-centered tetragonal) of -TiAl
and in the hexagonal DO
19
structure of
2
-Ti
3
Al are described in gure 4.6 [5]. For some
considerations the ordered L1
0
structure (fct) of -TiAl can be regarded as a face-centered cubic
structure since the ratio c/a lies between 0.98 and 1.02 [31]. The lattice parameters for -TiAl
and
2
-Ti
3
Al according to the database PC-PDF 2.14 are listen in table 4.1.
28
Figure 4.4: Microstructure of the extruded Ti-42Al-7.5Nb (B, Si, C) perpendicular to the ex-
truding direction
4.1.5 Fracture Properties and Deformation Structures
Due to the strongly ordered nature and the directional bonding of the compounds, Titanium
Aluminides suer like other intermetallics from brittleness at low and ambient temperatures,
which makes processing dicult. Intergranular fracture and cleavage are the dominant fracture
mechanisms in duplex microstructures, while interfacial delamination, translamellar fracture
and decohesion of lamellar colonies are the most important failure processes in lamellar alloys.
The brittleness of the material may in part be attributed to the plastic anisotropy of the -TiAl
and
2
-Ti
3
Al phase. In view of the observed cleavage fracture, it is supposed that unfavorably
orientated grains or lamellae may provide easy crack paths. Once nucleated on [111]
planes,
the cracks are subjected to high tensile stresses and can rapidly grow to a critical length. The
temperature dependence of the near material suggests that crack tip plasticity can also lead
to appreciable toughening although dislocations experience a high glide resistance [24].
The L1
0
structure provides more than ve independent slip systems, but in the phase of
two-phase alloys glide of superdislocations is dicult [5], which leads to a signicant plastic
anisotropy because no glide component in the c-direction of the tetragonal unit cell is provided.
In grains that are unfavorably oriented for glide of 1/2 110] dislocations, high constraint stresses
can be developed, which can easily exceed the fracture stress [5].
Electron microscope studies have revealed that crack tips in -TiAl can be eectively shielded
by mechanical twins [28]. Especially in high Nb-containing alloys (5-10% Nb) with a relatively
29
(Ti,Nb)B
2
g/a
2
grains
g grains
Figure 4.5: Microstructure of the extruded and annealed Ti-42Al-7.5Nb (B, Si, C) parallel to
the extruding direction
low Al content tested at room temperature, an abundant activation of mechanical twinning has
been recognized [32]. This reduction of the interfacial energy might be a reason why the lamellar
structure of high Nb-containing alloys exhibits extremely ne lamellar spacings. Twin nucleation
in these alloys is certainly supported by the ne scale of lamellar microstructure which provides
a high density of nucleation sites for mechanical twins [3].
30
Table 4.1: Lattice parameters for -TiAl and
2
-Ti
3
Al
phase a [
A] c [
A]
-TiAl 3.976 4.049
2
-Ti
3
Al 5.775 4.638
c
a
Titanium
Aluminium
(a) L1
0
structure (face-centered tetragonal, fct) of -
Tial
a
c
(b) Hexagonal DO
19
structure of
2
-
Ti
3
Al
Figure 4.6: Atomic arrangements of -TiAl and
2
-Ti
3
Al in the unit cell
4.2 Recrystallized Tungsten
Due to the high melting point and the high mass the refractory metal tungsten is used in
the lighting industry, as material for shielding of radiation and for armor piercing projectiles.
Tungsten carbides are widely used as cutting tools. Selected thermal and mechanical properties
of tungsten are listed below.
very high melting point of 3422
C
high density of 19.3g/cm
3
high Youngs modulus of 400MPa
good resistance against corrosion
4.2.1 Fabrication of the Investigated Tungsten
The investigated pure tungsten was fabricated by Plansee AG by powdermetallurgical methods.
The diameter of the sintered rod of 45 mm was reduced by forging and rolling to a diameter of
25 mm. According to the equation
r
= ln(r
0
/r), the reduction of the diameter corresponds to
a deformation grade of 58 %.
After the fabrication of the CT-specimens and production of fatigue pre-cracks, the samples
were annealed at 1700
C for one hour in a hydrogen atmosphere to generate a recrisallized

microstructure.
31
4.2.2 Microstructure
The microstructure of recrystallized pure tungsten is depicted in gure 4.7.
Figure 4.7: Microstructure of recrystallized pure W
4.2.3 Lattice Structure
Tungsten is a body-centered-cubic metal (gure 4.8). The lattice parameter a is 3.17

A.
Figure 4.8: Body-centered cubic crystal structure of tungsten
4.2.4 Fracture Properties and Deformation Structures
In this type of W the cohesive strength is usually reached before the signicant sliding of disloca-
tions occurs at room temperature. Therefore brittle fracture is the principal rupture mechanism.
According to Grith, surfaces with the lowest surface energies should appear as favored cleav-
age planes. The dominance of {100}-cleavage planes cannot be explained on this basis, since
surfaces with {011}-cleavage planes have the lowest surface energy. Therefore the Grith crite-
rion can only be regarded as a necessary condition and not as a fracture criterion [36]. Cracks
tend to propagate on {100}-cleavage planes because in contrast to {011}-planes a multitude of
32
crack front directions is possible. This approach does not consider the surface energy and the
activating of dislocations, results were obtained from atomistic simulations [35].
Investigations [21] have given K
Ic
values at room temperature for SENT-bending specimens
with crack propagations parallel and perpendicular to the axis of the elongated grains. Brittle
fracture lead to the relatively low values of 12.7 MPa
m for the perpendicular and 8 MPa
m
for the parallel specimens. The fracture surface of the perpendicular specimens consisted of
30% intercrystalline and 70% transcristalline cracks. The fracture surfaces of the parallel spec-
imens were 100% intercrystalline. It has to be pointed out that the material investigated was
as-fabricated and not recrystallized respectively.
Cracks along grain boundaries in polycrystalline tungsten usually propagate very quickly. Only
very few dislocations were generated during the crack propagation. Some dislocation activity
may occur when a grain boundary crack is held up at a barrier such as a triple point. In some
instances dislocations are attracted to the crack ank as the crack propagates [1].
33
5. Experimental Method
5.1 Denomination of the Specimen
The specimens are denominated as follows.
WRCT Wolfram Recrystallized Compact Tension
TGCT Titanium Aluminide Globular Compact Tension
For the characterization of the fatigue pre-cracks, the faces of the specimens were denominated
with A and B. The two halves of the broken specimens were denoted with t for top and b for
bottom.
5.2 Crack Propagation Investigations
5.2.1 Specimens
The tungsten and the titanium aluminide CT-specimens with the specimen width W = 12mm
were manufactured in the workshop belonging to the department. The geometry of the samples
according to ASTM E 399 standard [33] is depicted in gure 5.1.
1
6
,
2
0,9
3
3
,
3
3
,
3
3
3
1
6
,
2
6
12
Figure 5.1: Dimensions of the used CT-specimen, W = 12mm
The coarse notch of 2mm width and 5mm depth was produced with a diamond cutting
disc. A ner notch of 400m width and 1mm length was fabricated with a diamond wire
34
CHAPTER 5. EXPERIMENTAL METHOD
saw. With a razor and diamond gilding paste a ne cut of 40m width and a few hundred m
depth was produced. The ne razor-cut notch is necessary to produce a short fatigue pre-crack
with a relatively small load amplitude. It is important that the root of the notch is in the middle
of the CT-specimen (gure 5.2). If the notch is too short, it will be dicult to produce a fatigue
pre-crack. If the notch is too long, the sample will break under cyclic compression from the back
side of the sample because of the brittleness of the material.
5.2.2 Producing the Fatigue Pre-Crack
The fatigue pre-cracks were produced by the method of cyclic compression at constant load with
a frequency of 100 Hz. This method has some advantages compared to cyclic tension, especially
in brittle materials. For more detailed information about cyclic compression please read section
3.8.
F
cycl
F
cycl
Figure 5.2: Loading of the CT-specimen for initiation of a fatigue pre-crack
A short fatigue pre-crack acts as an ideally sharp crack for the crack propagation experiment.
It is important that the plastic zone of the pre-crack is small and that the crack is short re-
spectively. A large plastic zone would have an undesired inuence on the propagation of the
crack in the propagation experiments. In this case the experiment would give K
I
-values for the
predeformed material with residual tensile stresses in front of the pre-crack which may aect the
measured fracture resistance at small crack extensions. The calculated stress intensity factor K
I
at the beginning of the propagation of the crack in a material with a large compression fatigue
plastic zone might be smaller than K
I
for a material with a small plastic zone.
Tables 5.1 and 5.2 show the necessary stress intensity factor ranges K
I
, the number of load
cycles and the average lengths (mean value of sides A and B) of the fatigue pre-cracks a
fc
.
An example for a fatigue pre-crack is depicted in gure 5.3. The micrographs of the fatigue
pre-cracks for all specimens are listed in appendix A.
5.2.3 Investigation of Crack Propagation
The crack propagation experiments were performed on a Type 1386 ZWICK tensile testing
machine at constant crosshead speed. The crack propagation was measured with the potenial
method. The dependence of the load F and the potential drop U as a function of time t was
35
Table 5.1: Production of fatigue pre-cracks: globular TiAl specimens
specimen K
I
[MPa
m] load cycles a
fc
[m]
TGCT3 21 10000 25
TGCT5 20 10000 30
TGCT6 20 10000 20
TGCT7 21 20000 25
Table 5.2: Production of fatigue pre-cracks: recrystallized tungsten specimens
specimen K
I
[MPa
m] load cycles a
fc
[m]
WRCT2 20 10000 23
WRCT3 20 10000 40
WRCT4 18 10000 35
recorded.
The Potential Method
At the top and bottom of the specimens holes of 1.3 mm diameter were drilled. For the current
feed silver-coated copper pins of 1.3 mm in diameter were soldered on cables and pressed into the
drilled holes. The cables were connected with a source that provided the samples with constant
current. A device which reversed the polarity with a frequency of 1 Hz was used to compensate
the thermoelectric eect. This eect causes a potential drop due to a drop in temperature.
Thus, temperature dierences during the experiment change the measured potential and would
have made the results useless.
Thin copper wires were welded on the side faces of the specimens. The voltage was measured
with a nano-voltmeter. A good isolation of linkage was essential to obtain good results. The
experiments were controlled by a computer program [37], which processed the data and produced
log les. The arrangement of the current feed and the points for the measuring of the voltage are
depicted in gure 5.4. Before loading the specimens and starting the experiments, the computer
program which controlled the polarity-reversing device was started and the samples were fed
with alternating current for a few minutes. This ensured that the temperature dierence during
the actual experiments were small. Temperature compensation was not required.
The potential method [39] was used to determine the crack propagation. The idea behind this
technique is that the electric resistance of the specimen changes when a crack propagates and
when the area which the current traverses decreases respectively. According to the equation
R =
l
A
, (5.1)
where
R is the electric resistance [],
the specic resistance [ m],
l the length [m], and
A the cross section where the current traverses
_
m
2
,
36
Figure 5.3: Example of a fatigue pre-crack produced by cyclic compression
d
w
I
~
V
F
F
Figure 5.4: Experimental arrangement for determination of the crack propagation
the resistance R grows when the area decreases. According to Ohms law, the potential drop U
grows at constant current I because the resistance R increases. An example for a voltage-time
curve is given in gure 5.5. The voltage-time curves for all specimens are listed in appendix B.
With the Johnson equation (equation 5.2) it is possible to calculate the actual crack length a
from the measured potential drop. The accuracy depends on many factors [37]. In the performed
experiments the accuracy was better than 10m.
a =
2W
arccos
_
_
_
cosh
d
w
2W

_
cosh
_
U
U
0
arccosh
cosh
d
w
2W
cos
a
0
2W
__
1
_
_
_
, (5.2)
where
W is the specimen width [mm],
d
w
the distance between the points for voltage measuring [mm],
U the actual voltage measured [V ],
U
0
the voltage measured at da = 0 [V ],
37
TGCT5
0,532
0,533
0,534
0,535
0,536
0,537
0,538
0,539
0,54
0 50 100 150 200 250 300
t [s]
U
[
m
V
]
Figure 5.5: Example for a potential drop as a function of time
a
0
the length of the non-propagated crack at t = 0 [m], and
a the length of the propagated crack [m].
The calculated values of the crack length a at small crack extensions may be overestimated and
the fracture resistance at small crack extensions may be underestimated respectively. The reason
for this is that the shape of the specimen changes by elastic deformation when is is loaded. This
deformation causes the change in the electric resistance R [38].
Crack Propagation Experiments
The experiments were performed at constant crosshead speed. The force was measured with a
load cell. The parameters for the crack propagation experiments are listed in tables 5.3 and 5.4.
An example for a load-time curve is given in gure 5.6. The at part of the curve results from
the alignment of the linkage when loaded. The load-time curves for all specimens are listed in
appendix B.
Table 5.3: Parameters for the crack propagation experiments for TiAl-specimens
specimen a
0
[MPa
m] d
w
[mm] I [A] v [m/min]
TGCT3 4.125 1.65 1.5 150
TGCT5 4.13 1.7 1.5 150
TGCT6 4.22 1.6 1.5 150
TGCT7 4.425 1.6 1.5 150
Calculation of the R-Curves
The dependence of the stress intensity factor K
I
on the time t was calculated according to the
ASTM E 399 standard [33] as
K =
F f (a/W)
B
W
, (5.3)
38
TGCT5
0
100
200
300
400
500
600
700
800
900
0 50 100 150 200 250 300
t [s]
F
[
N
]
Figure 5.6: Example for an loading curve
Table 5.4: Parameters for the crack propagation experiments for W-specimens
specimen a
0
[MPa
m] d
w
[mm] I [A] v [m/min]
WRCT2 4.483 1.7 6 80
WRCT3 3.96 1.7 6 80
WRCT4 4.315 1.7 6 80
where
K is the stress intensity factor [mm],
F the load [N],
B the specimen thickness [mm],
W the specimen width [mm],
f (a/W) the factor [1], and
a the length of the propagated crack [mm].
The factor f (a/W) can be calculated as
f (a/W) =
(2 +a/W)
_
0.76 + 4.8a/W 11.58 (a/W)
2
_
+ 11.43 (a/W)
3
4.08 (a/W)
4
(1 a/W)
3/2
,
(5.4)
where
f (a/W) is the factor [1],
a the length of the propagated crack [mm], and
W the specimen width [mm].
39
Together with the Johnson equation, which gives the dependence of the crack propagation a
as a function of time t, the R-curves can be determined. An example for an R-curve is given in
gure 5.7. The R-curves for all specimens are listed in chapter 6.
R-Curve TGCT5
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
Figure 5.7: Example for a measured R-curve of TiAl
5.3 Preparation of Lamellae with the Focused Ion Beam (FIB) Work-
station for Transmission Electron Microscope Analyses
5.3.1 Characteristics of the Leo 1540XB Focused Ion Beam Workstation
The CrossBeam Leo 1540XB Focused Ion Beam Workstation combines the SEM (operating with
the ultra high resolution GEMINI eld emission column) with the CANION FIB column into
one integrated system. The live SEM imaging capability during FIB operation mode gives full
control when preparing samples for the TEM. A multi-channel gas injection system can be used
to deposit materials like tungsten or platinum. The SEM can be operated at an acceleration
voltage between 5kV and 25kV , the FIB between 10kV and 30kV . The FIB operates with a
gallium liquid metal ion source. The ions can be used for milling or depositing. The available
ion current ranges from 5pA to 20nA. A micromanipulator which controls a ne tungsten needle
diameter at the tip: 2m is used for lifting out the TEM-samples.
5.3.2 In-Situ Lift-Out of Lamellae at the Focused Ion Beam Workstation
The specimen holder was tilted to 54
so that the ion beam was perpendicular to the surface of

the sample. The desired structure ( 15m2m) was coated with a tungsten layer of about
1m height. Above and below the structure ditches ( 40m 40m 15m) were cut out.
Between the ditches the coated lamella remained. After tilting the sample to 10
, the lamella
was cut out at two sides. The specimen holder was tilted back to 54
and the ne tungsten

needle was brought into contact with the lamella. After depositing tungsten on the contact
region, the lamella was cut out completely. The specimen holder was moved so that the lamella
was in the right position to mount it on the prepared TEM-grid. The contact area between the
lamella and the grid was coated, the needle was cut and moved out of the way. The lamella
was polished with low current on both sides until it was thin enough for the investigation in the
TEM.
40
A detailed illustrated description of in-situ lift-out of lamellae at the focused ion beam worksta-
tion is given in appendix C.
5.3.3 Characteristics of the Transmission Electron Microscope
The Philips CM12/STEM Transmission Electron Microscope can be operated with acceleration
voltages from 20kV to 120kV and beam currents from 2.5A to 100A. The vacuum level in the
specimen chamber in operating mode is 10
5
Pa. The valves are switched with compressed
air supplied by the air compression system of the department. The TEM is digitally controlled
by means of an integrated microprocessor system. Pictures can be taken with a 35mm camera.
The TEM is connected with a computer, where the fotos can be processed. The specimens must
have a diameter of 3mm. If smaller, they have to be mounted on a TEM grid.
5.3.4 Characteristics of the Scanning Transmission Electron Microscope
The Scanning Transmission Electron Microscope (STEM) is a built-in feature of the Leo 1540XB
Focused Ion Beam Workstation. It is operated at an acceleration voltage of 30kV . With the
STEM it is possible to produce brighteld images, a diraction operational mode is not possible.
5.3.5 Electron Back Scatter Diraction
Electron back scatter diraction (EBSD) analisis was performed on a Leo 1525 scanning elec-
tron microscope equipped eld-emission cathode and an EDAX orientation imaging microscopy
(OIM) system. The combination provides a comprehensive solution available for analyzing ori-
entations related aspects of crystalline microstructures.
41
6. Results
6.1 Fracture Toughness and Crack Propagation
In materials which show a microductile behavior, the stress intensity for crack propagation
is more or less constant. Therefore usually the critical stress intensity factor K
Ic
is used to
characterize the fracture toughness. In materials which show a pronounced R-curve behavior,
the critical stress intensity factor K
Ic
describes the fracture behavior only insuciently. Thus,
besides the R-curve, following stress intensity factors are used to characterize the fracture prop-
erties of the investigated materials [38]:
K
iIc
describes the initial deviation of the R-curve. Since the determination of this value
can be problematic, it was dened as the stress intensity factor for a crack extension of
10m similar to the yield stress R
p0.2
in a --diagram. It has to be stated that this
determination of K
iIc
is not standardized in contrast to the yield stress R
p0.2
. At this
extension the crack grows slowly.
K
I50
represents the stress intensity factor for a crack extension of 50m. This value makes
it easier to draw conclusions from the inuence of the microstructure.
K
Imax
describes the maximum stress intensity factor. Usually it is reached just before the
sample fails. At this extension the crack grows fast.
6.1.1 Titanium Aluminide
The experiments were performed at room temperature at a crosshead speed of 150m/min. The
calculated stress intensity factors are listed in table 6.1 below. A horizontal hyphen indicates
that the sample failed before the crack reached an extension of 50m.
Table 6.1: Results of R-curve-experiments for TiAl
specimen K
iIc
[MPa
m] K
I50
[MPa
m] K
Imax
[MPa
m]
TGCT3 6.2 9.1 9.3
TGCT5 5.5 7.8
TGCT6 6.2 6.5
TGCT7 8.4 12 13.2
42
CHAPTER 6. RESULTS
R-Curve TGCT3
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
Figure 6.1: R-curve of the specimen TGCT3
R-Curve TGCT5
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
43
CHAPTER 6. RESULTS
R-Curve TGCT6
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
R-Curve TGCT7
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
6.1.2 Tungsten
The experiments were performed at room temperature at a crosshead speed of 80m/min. The
fracture toughness also exhibits an R-curve behaviour as in the case of TiAl. The R-curves and
calculated stress intensity factors are listed in table 6.2 below.
44
CHAPTER 6. RESULTS
Table 6.2: Results of R-curve-experiments for W
specimen K
iIc
[MPa
m] K
I50
[MPa
m] K
Imax
[MPa
m]
WRCT2 3 4.4 5.7
WRCT3 3.3 4.5 6.4
WRCT4 3 3.7 5.9
R-Curve WRCT2
0
1
2
3
4
5
6
7
0 100 200 300 400 500 600
da [mm]
K
[
M
P
a
m
1
/
2
]
Figure 6.5: R-curve for the specimen WRCT2
R-Curve WRCT3
0
1
2
3
4
5
6
7
0 100 200 300 400 500 600
da [mm]
K
[
M
P
a
m
1
/
2
]
45
CHAPTER 6. RESULTS
R-Curve WRCT4
0
1
2
3
4
5
6
7
0 100 200 300 400 500 600
da [mm]
K
[
M
P
a
m
1
/
2
]
46
CHAPTER 6. RESULTS
6.2 Fractography and Deformation Structures
To interpret the structures in the material with the TEM, it is essential to know where exactly
they were located and in which direction the crack propagated. In this section the fracture
surfaces and the location of the cut-out lamellae are described and selected TEM-images are
depicted.
6.2.1 Titanium Aluminide
The fracture surface of the globular Titanium Aluminide (gures 6.8 and 6.9) shows the char-
acteristics of transgranular cleavage fracture. A continuous crack path cannot be determined
since the structures are very ne. On smaller scale nucleation sites for parts of the crack can be
seen as well as the paths of propagation of such cracks.
It is dicult to specify the length of the fatigue pre-crack, because mostly its fracture surface
does not show the usual corrugated surface, i.e. the dierence in the surface texture of the
fracture surface is not as pronounced as in the case of other metals.
Figure 6.8: SEM-picture (top view) of the fracture of the globular TiAl surface at large crack
extensions
47
CHAPTER 6. RESULTS
Figure 6.9: SEM-picture (top view) of the fracture surface of the globular TiAl at a crack
propagation of about 20m
48
CHAPTER 6. RESULTS
Microstructure of the Undeformed Material
The TEM sample of the undeformed TiAl was fabricated by conventional methods (polishing,
dimpling and ion-etching). The microstructure consists of lamellar /
2
grains and grains.
The particles visible in the STEM-picture (gure 6.10) and the TEM-picture (gure 6.11) may
be Titanium-Niobium Boride (Nb, Ti) B
2
precipitations.
Figure 6.10: STEM-picture of the globular TiAl; in the middle and on the right side of the
picture the microstructure consists of grains; on the left side /
2
grains and a part of a crack
can be seen
49
CHAPTER 6. RESULTS
Figure 6.11: TEM-picture of the globular TiAl; the microstructure consists of mostly /
2
lamellae, some small regions and presumptively Titanium-Niobium Borides (dark)
50
CHAPTER 6. RESULTS
TEM-Investigations of the Origin of the Crack
The selected structure is located at a crack extension of about 10m behind the end of the fatigue
pre-crack. SEM-pictures of the structure on the fracture surface analyzed and TEM-pictures of
the lamella lifted out are depicted in gures 6.12 - 6.16.
Figure 6.12: Origin of the crack in TiAl: SEM-picture (top view) of the region of the crack surface
where the lamella was lifted out (circle); the long arrow indicates the macroscopic direction of the
crack; the short arrow indicates the direction of the crack on smaller scale; the two parallel lines
describe the approximate length of the fatigue pre-crack; the tungsten protection was deposited
parallel to the short arrow as depicted in gure 6.13
51
CHAPTER 6. RESULTS
Figure 6.13: Origin of the crack in TiAl: SEM-picture (inclined view from the left) of the
deposited tungsten protection (below the arrow); the arrow indicates the direction of the crack
on small microstructural scale; the dashed line indicates the end of the pre-crack
Figure 6.14: Origin of the crack in TiAl: TEM-picture of the lamella; the arrow indicates the
direction of the crack; the tungsten protection layer (about 1m high) is located between the
polished windows and the arrow
52
CHAPTER 6. RESULTS
500nm
Figure 6.15: Origin of the crack, TiAl: TEM-picture of the left part of the window on the left
side of the lamella of gure 6.14; the arrow indicates the direction of the crack; the line in the
W-layer is parallel to the fracture surface
53
CHAPTER 6. RESULTS
1 m m
Figure 6.16: TiAl, origin of the crack: TEM-picture of the window in the middle of the lamella
of gure 6.14; the arrow indicates the direction of the crack on small microstructural scale; the
parallel line is parallel to the fracture surface
54
CHAPTER 6. RESULTS
TEM-Investigations at Large Crack Extension
The structure chosen for investigation is located in the middle of the fracture surface at a crack
extension of about 2.8mm. SEM-pictures of the fracture surface analyzed and TEM-pictures of
the lamella lifted out are depicted in gures 6.17 - 6.21.
Figure 6.17: Advanced crack in TiAl: SEM-picture (top view) of the region of the crack surface
where the lamella was lifted out (circle); the long arrow indicates the macroscopic direction of
the crack; the short arrow indicates the direction of the crack on smaller scale; the tungsten
protection was deposited parallel to the short arrow as depicted in gure 6.18
Figure 6.18: Advanced crack in TiAl: SEM-picture (inclined view from the left) of the de-
posited tungsten protection (below the arrow); the arrow indicates the direction of the crack on
microstructural scale
55
CHAPTER 6. RESULTS
10 m m
Figure 6.19: Advanced crack in TiAl: TEM-picture of the lamella; the arrow indicates the
direction of the crack; the tungsten protection layer (about 1m high) is located between the
polished windows and the arrow
56
CHAPTER 6. RESULTS
500nm
Figure 6.20: Advanced crack in TiAl: TEM-picture of a detail of the window on the left side
of the lamella of gure 6.19; the arrow indicates the direction of the crack; the parallel line is
parallel to the fracture surface
57
CHAPTER 6. RESULTS
1 m m
Figure 6.21: Advanced crack in TiAl: TEM-picture of the window in the middle of the lamella
of gure 6.19; the arrow indicates the direction of the crack; the parallel line is parallel to the
fracture surface
58
CHAPTER 6. RESULTS
6.2.2 Tungsten
The fracture surface of the recrystallized pure tungsten (gures 6.22 and 6.23) shows the char-
acteristics of intergranular fracture. Only few regions of transcrystalline fracture can be seen.
At some locations, the crack split up in two paths. However, further propagation occurred only
on one crack path, the other path stopped in the material. A gap at grain boundaries, where
the crack split up, is clearly visible.
Figure 6.22: SEM-picture (inclined view) of the fracture surface of the recrystallized pure tung-
sten; on the left side gaps at grain boundaries and parts of transcrystalline fracture can be
seen
Figure 6.23: SEM-picture (top view) of the fracture surface of the recrystallized pure tungsten
59
CHAPTER 6. RESULTS
Microstructure of the Undeformed Material
The TEM specimen of the undeformed tungsten (gure 6.24) was fabricated by conventional
methods (polishing, dimpling and ion-etching).
Figure 6.24: STEM-picture of W; grain and presumptively subgrain boundaries can be seen; the
dark spots could be preparation artefacts
60
CHAPTER 6. RESULTS
TEM-Investigations of Tungsten
The quality of the obtained W samples for TEM/STEM investigations is unsatisfactory due to
excessive ion damage of the surface during polishing the lamella in the FIB. Nevertheless, one
STEM-picture of such a sample is depicted in gure 6.25.
Figure 6.25: STEM-picture of a grain boundary in the recrystallized pure tungsten; the sample
only demonstrates the excessive ion damage
6.2.3 EBSD-Investigations
Electron back scatter diraction was performed on lamellae to obtain information about changes
in crystal orientation near the fracture surface due to plastic deformation at the crack tip. It
was not possible to investigate the TiAl because the quality of the diraction patterns was not
good enough for the analysis. Hence, only tungsten was investigated with EBSD.
EBSD-Investigations of Tungsten
The orientation map depicted in gure 6.26 was recorded from a tungsten lamella at the crack
origin. It does not show signicant changes in the cystal orientation as depicted in gure 6.27.
The scan was performed on one grain which exhibits a (111) orientation parallel to the sample
surface.
61
CHAPTER 6. RESULTS
Figure 6.26: Orientation map of the region below the fracture surface of recrystallized tungsten;
the color code gives the orientation in relation to the sample normal; the black part on the
left side is the protection layer; the crack propagated parallel to the white line in the indicated
direction; the red line indicates the path of the misorientation prole (gure 6.27)
Figure 6.27: Misorientation prole calculated from the orientation map (gure 6.26)
62
7. Discussion
7.1 Crack Propagation Investigations
7.1.1 Size of the Cyclic Plastic Zone
When producing the fatigue pre-crack, it is important that the size of the cyclic plastic zone is
small compared to the crack length, since the subsequent crack propagation experiments should
not be inuenced by the plastic zone of the fatigue pre-crack.
With the equation 3.17
=
K
2
4
2
y
(1 2)
2
,
the size of the cyclic plastic zone can be determined.
High Nb-Containing TiAl
The fatigue pre-crack in TiAl was produced in the annealed material. Following material pa-
rameters are used:
the stress intensity factor range for producing the fatigue pre-cracks in TiAl K =
20MPa
m,
the Poisson ratio of = 0.3 and
a typical value for the yield strength of high Nb-containing TiAl
y
= 900MPa
m [3].
This leads to a size of the cyclic plastic zone of about 6m for the high Nb-containing TiAl.
Recrystallized Pure Tungsten
The fatigue pre-crack in tungsten was produced in the as-worked material. The recrystallization
heat treatment was performed afterwards. Thus, the material parameters for the as-worked
tungsten must be applied for the estimation of the size of the cyclic plastic zone. Following
material parameters are used:
the stress intensity factor range for producing the fatigue pre-cracks in W K = 20MPa
m,
the Poisson ratio of = 0.3 and
a typical value for the yield strength of pure tungsten
y
= 1000MPa
m [43].
This leads to a size of the cyclic plastic zone of about 5m for the as-worked tungsten.
63
CHAPTER 7. DISCUSSION
Remarks
Both estimations of the sizes of the plastic zones can be regarded as suciently small for the
considerations concerning the inuence of the cyclic zone on the origin of the crack in this study.
With the modied equation 3.17
=
K
2
2
y
(1 2)
2
,
the size of the plastic zone for the actual fracture experiment can be determined, i.e. the
extension of possible deformation structures can be estimated (table 7.1). For the following
calculations
y
= 1000MPa and = 0.3 is assumed.
Table 7.1: Extension of the plastic zone for dierent values of K
Ic
K
Ic
[MPa
m] [m]
5 1.3
10 5.1
15 11.5
7.1.2 R-Curves
The fracture resistances of both investigated materials show pronounced R-curve behaviour, i.e.
the fracture resistances grow with increasing crack extension as depicted in the example in gure
7.1.
R-Curve TGCT3
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
Figure 7.1: Example of an R-curve
Some of the determined R-curves have a somewhat uncommon shape. The zig-zag shape at small
crack propagations (marked with the red circle in the diagram) can be explained by changes in
the heat ow from the sample (heated by the current) to the linkage due to an increased contact
between the sample and the bolts which transfer the force from the linkage to the sample (CT-
specimens) when starting to load. A change in the temperature of the sample leads to a variation
in the measured potential which is used to calculate the crack propagation. This may also be
64
the reason for sudden jumps in the R-curve at larger crack extensions.
The slope of the curve marked with the red ellipse is usually larger than calculated for the
R-curves in this study. This can be explained by the underestimation of the fracture resistance
at small crack extensions due to the elastic part of the deformation which contributes to the
voltage drop but not to the crack propagation.
7.1.3 Evaluation of the Obtained Values for Fracture Toughness
For values of fracture toughness of high Nb-containing TiAl at room temperature no data
was available. The standard literature values for fracture toughness at room temperature for
duplex-type TiAl with the composition Ti-47Al-1Cr+Nb, Mn, Si, B lie between 10MPa
m and
15MPa
m [5]. They are signicantly higher than those obtained in this study for the specimens
TGCT3, TGCT5 and TGCT6 (gure 7.2). The relatively high value for the specimen TGCT7
and the large scatter cannot be explained at the moment.
Table 7.2: Results of the crack propagation experiments for TiAl
specimen K
iIc
[MPa
m] K
I50
[MPa
m] K
Imax
[MPa
m]
TGCT3 6.2 9.1 9.3
TGCT5 5.5 7.8
TGCT6 6.2 6.5
TGCT7 8.4 12 13.2
The room temperature values for the initial fracture toughness K
iIc
of recrystallized tungsten
(mean value 3.1MPa
m) are signicantly lower than those obtained by Riedle [21] for single
crystals (6.5MPa
m). Compared with the values for K

Imax
at room temperature for swaged
polycrystalline tungsten obtained by Margevicius et al. [7],
12.6MPa
m for cracks propagating perpendicular to the elongated grains and

8.0MPa
m for cracks propagating parallel to the elongated grains,

the investigated recrystallized material also failed at lower fracture toughness (mean value
6.0MPa
m). The values calculated in this study are listed in table 7.3.
Table 7.3: Results of the crack propagation experiments for tungsten
specimen K
iIc
[MPa
m] K
I50
[MPa
m] K
Imax
[MPa
m]
WRCT2 3 4.4 5.7
WRCT3 3.3 4.5 6.4
WRCT4 3 3.7 5.9
7.2 Procedure to Lift Out TEM-Specimens on the FIB Workstation
Compared with earlier attempts of in-situ lift-out of lamellae for TEM investigations with the
Leo 1540XB FIB workstation, the success rate could be increased signicantly. With the new
method, taking out lamellae of a fracture surface and the following ion-beam thinning takes
approximately 12 hours in total. The success rate now is higher than 90% compared to about
10% with the conventional method. A detailed illustrated description of the new method is
65
given in appendix C.
The preparing and lifting out of lamellae from more or less rough fracture surfaces can be
regarded as dicult and above all time-consuming, because the topography of the surface makes
it necessary to remove a lot of material with the ion beam to manoeuvre the tungsten needle to
the desired location. Another diculty is the positioning of the gas injection system (GIS). If
the GIS is not located at the right position, deposition does not work which means that the ion
beam cuts instead of depositing a protective layer. Thus, it is advisable to try to deposit a layer
in the close surroundings (a few m) of the structure of interest, especially when connecting the
lamella with the tungsten needle.
In some cases the deposition of a tungsten protection layer on a certain structure of interest is
not possible because the inclination of the structure in the fracture surface is unfavourable for
deposition (gure 7.2).
Figure 7.2: Fracture surface of recrystallized tungsten; the tungsten needle and the tube of
the GIS for the deposition of tungsten are located near the lamella; the red circles indicate
regions where a deposition is not possible due to unfavourable location and/or inclination of the
structures of interest
Rotation or inclination of the whole specimen is limited because the GIS must be located very
close to the fracture surface and near (between 100m and 300m) the region where material
should be deposited (gure 7.3).
The small distance between the GIS and the fracture surface frequently produces so-called
stage-touches (electrical contact between the tube of the GIS and the surface) due to thermal
expansions of the GIS which must be heated for deposition. Although the temperature remains
more or less constant when maneuvering the GIS near the surface, very small temperature
dierences produced by the thermostat provoke such thermal expansions. Stage-touches are
especially dangerous when connecting the tungsten needle with the lamella. Even very small
movements of the sample caused by the impingement with the GIS lead to material deposition
at an undesired location.
Generally, moving the tungsten needle towards the lamella with the micromanipulator works
66
Figure 7.3: Fracture surface of recrystallized tungsten; on the right side the cuts produced by
the wire saw and the razor blade can be seen; three of the ve tubes of the GIS and the tungsten
needle are visible
well. As mentioned above, grains which are much higher than the frature surface sometimes
inhibit the positioning of the needle. In such a case, the grain must be removed by the ion beam
which can take up to few hours, depending on the size of the grain. Another possibility would be
the rotation of the sample holder which usually is not possible, since it leads to contact between
the GIS and the fracture surface.
An annoying problem is that the software does not always work properly. Among others, this
can be one reason for failure. Besides smaller diculties like crashes of the main program, the
ion beam scanning control the so-called scan generator occasionally shows malfunctions.
Thus, the ion beam sometimes does not stop cutting when reaching the specied nishing line.
7.3 Surface Damage Caused by Ion-Thinning of Samples for TEM
It is well known that ion-thinning leads to surface damage like amorphisation. It has been shown
in many studies [40, 41, 42], that the degree of the damage depends on the incident angle of the
ions and the ion energy. Besides the amorphisation, the energy input of the Ga ions may have
a signicant inuence on the deformation structures in the material if the lamella is very thin.
During ion-thinning of the lamella, the high voltage of the SEM was set to 5kV 7kV which
made it possible to stop milling when the thickness of the sample was suciently thin for TEM
analyses. When the ion-thinned part of the lamella appeared very bright in the SEM, it was
thin enough for TEM investigations with the highest acceleration voltage possible (120kV ).
It is assumed that the thickness of the damaged surface layer is about 10nm. If the whole lamella
has a thickness of 50nm or even less, the thickness of the damaged layer is not small compared
to the overall thickness. In this case, the contribution of the damaged surface layers on both
sides of the lamella ( 20nm damage) is not negligible, because the remaining undamaged
material is only 30nm thick.
67
The TiAl lamellae are thicker than the W lamellae, which makes it possible to analyze the TiAl
with the used Philips CM12/STEM at 120kV . Nevertheless, it is too thin to obtain Kikuchi
lines and determine the orientation of the material. In case of tungsten, which must be very thin
for TEM investigations with 120kV , the contribution of the damaged layer is too big, i.e. the
pictures cannot be evaluated due to excessive ion-induced damage. Micrographs of TiAl (gure
7.4) and W (gure 7.5) as well as a brighteld picture of ion-beam induced damage in FeAl [41]
(gure 7.6) are depicted below for comparison.
500nm
Figure 7.4: TEM-micrograph of TiAl: the extent of ion damage is relatively low, especially in
the middle and on the left side of the thinned window
68
Figure 7.5: STEM-micrograph of W: excessive ion-beam induced damage
Figure 7.6: Brighteld TEM image of ion-beam induced damage of FeAl particles [41]
69
7.4 Deformation Structures in High Nb-Containing TiAl
In this section the TEM-pictures of the investigated TiAl fracture surfaces are analyzed. The
recrystallized tungsten cannot be investigated successfully with TEM, since the ion-damaged
surface layers are too thick and the thickness of the undamaged material is too thin for TEM
analyses.
7.4.1 Crack Origin
Two selected TEM-images of the material at the origin of the overload crack are depicted in
gures 7.7 and 7.8. Both pictures do not show signicant characteristics of microplastic defor-
mation like twinning or dislocations. It is supposed that the microstructure of the investigated
details depicted below shows grains, since it does not exhibit a lamellar structure. Evaluable
diraction patterns could not be obtained. It is assumed that the specimen was too thin for
Kikuchi lines and maybe also damaged too much by the ion beam for good results. Thus, the
orientations of the microstructure cannot be analyzed completely with the Philips CM12/STEM
TEM. A TEM with a higher acceleration voltage would make investigation of thicker specimens
possible. In such a case the ratio of the ion-damaged layer to undamaged material would be
smaller and therefore the results better, especially for tungsten.
The obtained results which show only a minor degree of deformation structures in the material
at the origin of a crack contradicts investigations [28, 32, 44] which have revealed, that crack
tips in TiAl can eectively be shielded by mechanical twins and that an abundant activation
of mechanical twinning takes place.
7.4.2 Propagating Crack
Two selected TEM-images of the material from the fracture surfaces of the crack at larger crack
extensions are depicted in gures 7.10 and 7.11. The crack propagated from the right to the left
side of gure 7.10 and furthermore from the right to the left side of gure 7.11 as it can be seen
in gure 7.9.
The microstructure depicted in gure 7.10 presumptively shows grains or subgrains and a
Titanium-Niobium Boride particle in the middle of the ion-thinned window. It is assumed that
the lamellae on the left side are deformation twins, since no dened grain boundary between
the lamellae and the grain is visible. It has been shown for bcc Fe single crystals [45], that
twinning dislocations can be emitted in backward direction of the crack propagation too.
The microstructure depicted in gure 7.11 presumptively shows a /
2
grain with the typical
lamellar structure. It is assumed that the dark parts of the lamellae are deformation twins which
propagate in the backward direction of the crack like in gure 7.10. A reason for the formation
of such twins in this region could be a stress concentration near the surface step where the dark
structures seem to originate from. The structures reach about 500nm into the material, which
corresponds to about one third of the size of the calculated plastic zone calculated at the end of
subsection 7.1.1. To prove the existence of deformation twins, further TEM-investigations must
be carried out to determine the orientation relation of the depicted structures.
70
500nm
Figure 7.7: Origin of the crack in TiAl: TEM-picture of the left part of the window on the
left side of the lamella of gure 6.14; the arrow indicates the direction of the crack on small
microstructural scale; the indicated line is parallel to the fracture surface; it is supposed that the
depicted detail is a grain because no lamellar structure is visible; no signicant deformation
structure is visible in this region
71
1 m m
Figure 7.8: Origin of the crack in TiAl: TEM-picture of the window in the middle of the lamella
of gure 6.14; the arrow indicates the direction of the crack on the microstructural scale; the
drawn-in line is parallel to the fracture surface; it is supposed that the depicted detail is a
grain because it does not exhibit a lamellar structure; the orientation and lattice type of the
textured structure in the middle of the thinned window could not be determined in this study
72
10 m m
Figure 7.9: Advanced crack in TiAl: TEM-picture of the lamella; the arrow indicates the
direction of the crack on the microstructural scale
73
1 m m
Figure 7.10: TiAl, advanced crack: TEM-picture of the window in the middle of the lamella
of gure 6.19; the arrow indicates the direction of the crack on the microstructural scale; the
drawn-in line is parallel to the fracture surface; it is supposed that the major part of the thinned
area consists of grains or subgrains; the lamellae on the left side of the polished window
could be deformation twins; the particle in the middle of the thinned area is presumptively a
Titanium-Niobium Boride particle
74
500nm
Figure 7.11: Advanced crack in TiAl: TEM-picture of a detail of the window on the left side of
the lamella of gure 6.19; the arrow indicates the direction of the crack on the microstructural
scale; the indicated line is parallel to the fracture surface; it is assumed that the depicted detail
shows a /
2
grain which exhibits the typical lamellar microstructure
75
7.5 EBSD-Investigations of Tungsten
The orientation map and the corresponding misorientation prole (gures 7.12 and 7.13) were
recorded and calculated from a lamella lifted out at the origin of the crack in polycrystalline
pure tungsten. The map as well as the prole do not show signicant changes in the crystal
orientation in tungsten. This leads to the conclusion that at least in this part of the material no
measurable deformation due to crack propagation occurred, since this would result in a gradient
in the orientation. This result corresponds to Margevicius et al. who stated that crack tip
plasticity does not signicantly contribute to the fracture toughness of polycrystalline tungsten
at room temperature [7].
Figure 7.12: Orientation map of the region below the fracture surface of recrystallized tungsten;
the color code gives the orientation in relation to the sample normal; the black part on the
left side is the protection layer; the crack propagated parallel to the white line in the indicated
direction; the red line indicates the path of the misorientation prole (gure 6.27)
76
Figure 7.13: Misorientation prole calculated from the orientation map (gure 6.26)
77
8. Conclusion
In this study the deformation structures in the vicinity of the fracture surface resulting from
semi-brittle fracture in recrystallized pure tungsten and high Nb-containing two-phase TiAl
were investigated. Therefore fracture mechanics experiments were performed and the R-curves
recorded. Lamellae for TEM investigation were lifted out in-situ from the fracture surfaces by
means of a FIB workstation. On tungsten EBSD-scans were carried out near the fracture surface
to determine the degree of plastic deformation due to crack propagation.
From the results following conclusions can be drawn:
It is assumed that plastic deformation occurs to a certain degree in high Nb-containing
two-phase TiAl at least at large crack extensions, since deformation twins are presumably
visible.
The EBSD investigations of W lead to the conclusion that no signicant plastic occurs
near the fracture surface.
The in-situ lift-out of lamellae from a fracture surface at the FIB workstation is a powerful
method to investigate the material from dened regions. Nevertheless, ion-thinning should
be performed with an acceleration voltage of less than 10kV to minimize the damage of
the surface layers.
An acceleration voltage of 120kV at the TEM is not high enough to obtain good results
for tungsten. For investigation at such a voltage, the tungsten lamellae must be very thin
which results in an unfavourable ratio of the ion-damaged layer to the undamaged part.
To specify the extent of plastic deformation due to crack propagation in TiAl and W and
its eect on the fracture toughness further experiments must be carried out.
78
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allen: Risse, Phasengrenz achen, Dissertation, Max-Planck-Institut f ur Metallforschung,
Stuttgart
[36] Gumbsch P. (2003) Brittle Fracture and the Brittle-to-Ductile Transition of Tungsten, Jour-
nal of Nuclear Materials Vol. 323, 304
[37] Tabernig B. (2000) Das Erm udungsverhalten Teilchenverst arkter Aluminiumlegierungen,
Dissertation, Montanuniversitt Leoben
[38] H ock M. (2003) R-Kurvenverhalten der Bruchz ahigkeit in -TiAl Basislegierungen, Diplo-
marbeit, Montanuniversitat Leoben
[39] Brantner H.-P. (1996) Bruchz ahigkeit Teilchenverstrkter Aluminiumlegierungen, Diplomar-
beit, Montanuniversitat Leoben
[40] McCarey F. P. et al (2001) Surface Damage Formation During Ion-Beam Thinning of
Samples for Transmission Electron Microscopy, Ultramicroscopy Vol. 87, 97
[41] Munroe J. M. and Cairney J. M. (2001) Preparation of Transmission Electron Microscope
Specimens from FeAl and WC Powders using Focused-Ion Beam Milling, Materials Char-
acterization Vol. 46, 297
[42] Nakahara S. (2003) Recent Development in a TEM Specimen Preparation Technique Using
FIB for Semiconductor Devices, Surface and Coatings Technology Vol. 169-170, 721
[43] D ummer T. et al. (1998) Eect of Strain Rate on Plastic Flow and Failure in Polycrystalline
Tungsten, Acta Materialia Vol. 46, No. 17., 6267
[44] Appel F. (2005) An Electron Microscope Study Of Mechanical Twinning and Fracture in
TiAl Alloys, Philosophical Magazine Vol. 85, Nos. 2-3, 205
[45] Farkas D. (2005) Twinning and Recrystallisation as Crack Tip Deformation Mechanism
During Fracture, Philosophical Magazine Vol 85, Nos. 2-3, 387
81
A. Optical Micrographs of the Fatigue
Pre-Cracks
(a) Side A (b) Side B
Figure A.1: Fatigue cracks of the specimen TGCT3
82
APPENDIX A. OPTICAL MICROGRAPHS OF THE FATIGUE PRE-CRACKS
Figure A.5: Fatigue cracks of the specimen WRCT2
83
APPENDIX A. OPTICAL MICROGRAPHS OF THE FATIGUE PRE-CRACKS
84
B. Diagrams Obtained from the
Fracture Experiments
Summary of the load vs time, potential drop vs time and the determined R-curves of the crack
propagation experiments.
85
APPENDIX B. DIAGRAMS OBTAINED FROM THE FRACTURE EXPERIMENTS
R-Curve TGCT3
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
TGCT3
0
200
400
600
800
1000
0 100 200 300 400 500
t [s]
F
[
N
]
TGCT3
0,506
0,508
0,51
0,512
0,514
0,516
0,518
0 100 200 300 400 500
t [s]
U
[
m
V
]
Figure B.1: R-curve, load-time curve and potential drop-time curve for the specimen TGCT3
86
TGCT5
0
100
200
300
400
500
600
700
800
900
0 50 100 150 200 250 300
t [s]
F
[
N
]
TGCT5
0,532
0,533
0,534
0,535
0,536
0,537
0,538
0,539
0,54
0 50 100 150 200 250 300
t [s]
U
[
m
V
]
R-Curve TGCT5
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
87
R-Curve TGCT6
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
TGCT6
0
100
200
300
400
500
600
700
0 50 100 150 200 250
t [s]
F
[
N
]
TGCT6
0,663
0,6635
0,664
0,6645
0,665
0,6655
0,666
0,6665
0,667
0 50 100 150 200 250
t [s]
U
[
m
V
]
88
R-Curve TGCT7
0
2
4
6
8
10
12
14
0 20 40 60 80 100
da [mm]
K
[
M
P
a
m
1
/
2
]
TGCT7
0
200
400
600
800
1000
1200
1400
0 100 200 300 400 500
t [s]
F
[
N
]
TGCT7
0,576
0,578
0,58
0,582
0,584
0,586
0,588
0,59
0,592
0,594
0 100 200 300 400 500
t [s]
U
[
m
V
]
89
R-Curve WRCT2
0
1
2
3
4
5
6
7
0 100 200 300 400 500 600
da [mm]
K
[
M
P
a
m
1
/
2
]
WRCT2
0
100
200
300
400
500
600
0 50 100 150 200 250 300 350
t [s]
F
[
N
]
WRCT2
0,0755
0,076
0,0765
0,077
0,0775
0,078
0,0785
0,079
0,0795
0 50 100 150 200 250 300 350
t [s]
U
[
m
V
]
Figure B.5: R-curve, load-time curve and potential drop-time curve for the specimen WRCT2
90
R-Curve WRCT3
0
1
2
3
4
5
6
7
0 100 200 300 400 500 600
da [mm]
K
[
M
P
a
m
1
/
2
]
WRCT3
0
100
200
300
400
500
600
700
0 100 200 300 400 500
t [s]
F
[
N
]
WRCT3
0,066
0,068
0,07
0,072
0,074
0,076
0,078
0 100 200 300 400 500
t [s]
U
[
m
V
]
91
R-Curve WRCT4
0
1
2
3
4
5
6
7
0 100 200 300 400 500 600
da [mm]
K
[
M
P
a
m
1
/
2
]
WRCT4
0
100
200
300
400
500
600
0 100 200 300 400 500
t [s]
F
[
N
]
WRCT4
0,074
0,076
0,078
0,08
0,082
0,084
0,086
0 100 200 300 400 500
t [s]
U
[
m
V
]
92
C. In-Situ Lift-Out of Lamellae at the
FIB Workstation
In this study the in-situ lift-out of lamellae for transmission electron microscope analyses with
the focused ion beam workstation was performed for the rst time with a high success rate. A
short illustrated description of the steps of the procedure is given below.
Ensure that a tungsten needle is mounted. Insert the specimen holder with the clamped
aperture. The lamella will be connected with this aperture which serves as a specimen
holder for the TEM. The aperture has a diameter of 3mm and is 50m thick. The hole
has a diameter of 1mm. Approximately a quarter of the aperture is cut out (gure C.11).
Evacuate the chamber.
Start the EHT when the pressure reaches 9 10
5
mbar and the FIB gun when the pressure
is down to 5 10
5
mbar.
Control the coincidence of the FIB scans with the movable crosshair for the currents that
will be used. The reference current is 50 pA. Adjust the FIB beam shift correction if
necessary. It can be useful to note the spot sizes of the dierent currents to get an idea of
the actual precision of the ion beam.
The part of the aperture, the lamella will be connected to, must be at to ensure good
contact. Bring the aperture in position (stage tilted to 54
) and save the position in the

stage point list.
Cut the edge of the aperture in order to obtain a vertical at plane.
Find the structure on the surface of the sample which has to be worked out and take
pictures at dierent magnications. It might be useful to take pictures with the SEM with
the specimen holder tilted to 0
and 54
.
If the structure does not appear horizontal in the SEM image, rotate the sample holder.
Find the point of coincidence at the surface where the beams of the FIB and the SEM
intersect and save the position in the stage point list.
Open the valve for tungsten and heat the gas injection system (GIS). When the working
temperature is reached, move it towards the surface. It can be necessary to use the buttons
x, y and z of the GIS panel to position it manually near the selected structure.
Try to deposit the material on a small area in the surroundings of the structure.
93
APPENDIX C. IN-SITU LIFT-OUT OF LAMELLAE AT THE FIB WORKSTATION
Figure C.1: A tungsten layer protects the surface from the incoming Ga ions
If the deposition worked well, deposit a layer of about 1 m height and 2 m thickness
(gure C.1).
Park the GIS, switch o the heating and close the valve.
Dig suciently big ditches with a high current on both sides of the lamella. There should
be a security space of some m between the deposited material and the nishing line of
the cutting window since high currents usually have relatively big diameters of the ion
beam (big spot sizes).
Remove the remaining material of the security space with a lower current which has a
smaller spot size. The raw lamella should be about 1 or 2 m thick (gure C.2).
Move the z axis to a lower value and tilt the sample holder until an angle of -10
is reached.
Find the point of coincidence and save the position in the stage point list.
Cut out the lamella perpendicular (only on one side!) and parallel to the surface. The
cut-out areas should have a width of a few m to have enough space to manoeuvre the
lamella later (gure C.3).
Recall the position where the sample holder is tilted by 54
. Check if the lamella was cut

out properly.
Move the tungsten needle towards the lamella with caution. To obtain a plane at the tip
of the needle parallel to the lamella, it can be necessary to cant o the tip of the needle.
Heat the GIS. When the working temperature is reached, move it towards the surface
(gure C.4).
Try to deposit the material on a small area in the surroundings of the lamella.
94
Figure C.2: Remaining lamella of 1 or 2 m thickness
If the deposition worked well, bring the needle in contact with the lamella.
Deposit a layer on the contact surface of the needle and the lamella (gure C.5).
Withdraw the GIS manually some steps of 25 m and cut out the lamella completely.
Lift out the lamella by moving the sample downwards along the M axis. If the sample
is at a safe distance, it can be moved downwards along the z axis until the lower limit is
reached (gure C.6).
Park the GIS.
Recall the position of the sample holder, where the aperture is at a safe distance from the
point of coincidence.
Move the sample along the z axis until the aperture is positioned a few 25 m away from
the lamella.
Bring the GIS in position.
Move the sample holder along the x, m and z axes until the lamella touches the aperture
slightly.
Bring the GIS manually in a close position.
Try to deposit the material near the lamella on top of the aperture.
If the deposition worked well, deposit a layer on the contact surface of the lamella and the
aperture (gure C.7). If not, adjust the position of the GIS manually until deposition is
possible.
95
Figure C.3: Lamella cut out at two sides
Withdraw the GIS manually some steps of 25 m and turn o the heating.
Cut o the needle parallel to the lamella (gure C.8) and withdraw the needle carefully
and completely.
Park the GIS and close the valve.
Tilt the sample holder by 55
and nd the point of coincidence. Save the position in the

stage point list.
Polish the front side of the lamella with a current of 50 pA (gure C.9). Make sure that
no articial structures are produced by the ion beam.
Rotate the sample holder by 180
to polish the back side of the lamella, tilt it by ap-

proximately 57
and nd the point of coincidence. Save the position in the stage point
list.
Depending on the size and the expected residual stresses of the lamella, either polish the
whole lamella or a few small windows (gures C.10 and C.11).
After closing the valve of the GIS and switching o the EHT and the FIB gun, the sample
holder must be brought into horizontal position.
Delete your entries from the stage points list.
Take the sample out of the vacuum chamber, release the screw of the aperture holder and
take the aperture with the lamella out carefully using the vacuum tweezers. Insert the
aperture with the lamella in the sample holder for the TEM.
96
Figure C.4: GIS in position for deposition of tungsten
Figure C.5: Tungsten needle connected with lamella by the deposition of a tungsten layer, top
view
97
Figure C.6: Lift-out of the lamella
Figure C.7: Connecting the raw lamella with the edge of the aperture
98
Figure C.8: Cutting o the tungsten needle, top view
Figure C.9: Polished front side of the lamella
99
Figure C.10: Small ion-thinned windows at the back side of the lamella
Figure C.11: Aperture and lamella (marked with circle)
100

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Investigation of Deformation Structures

Resulting from Semi-Brittle Fracture in

(gure 3.16). It has to

by a straight line perpendicular to the compo-

3.7 Transmission Electron Microscope Analyses

C) leads to near- microstructures consisting of equiaxed grains and ne

C for one hour in a hydrogen atmosphere to generate a recrisallized

m for the perpendicular and 8 MPa

so that the ion beam was perpendicular to the surface of

and the ne tungsten

m). Compared with the values for K

m for cracks propagating perpendicular to the elongated grains and

m for cracks propagating parallel to the elongated grains,

) and save the position in the

. Check if the lamella was cut

and nd the point of coincidence. Save the position in the

to polish the back side of the lamella, tilt it by ap-

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