In Situ Deformation Experiments:
TEM for volume observations is emphasized in
Technical Aspects
In situ deformation experiments in plasticity involve
observing microstructural changes in a given speci-
men in the course of deformation. Various techniques
have been used relying on surface or volume obser-
vations. The most simple is certainly the double-etch
pit technique by which the first measurements of ve-
locities of individual dislocations were achieved in
semiconductors. Other in situ observations have been
made by optical microscopy (Neuhauser et al. 1975),
transmission electron microscopy (TEM) (Couret
et al. 1993), scanning electron microscopy (Allais
et al. 1994), and atomic force microscopy (AFM)
(Small et al. 1995, Coupeau et al. 1998).
Figure 1 illustrates the complementarity of optical
microscopy (Neuhauser et al. 1995) and AFM (Small
et al. 1995) in observing slip-line formation at differ-
ent scales. AFM has the highest spatial resolution
since it allows one to resolve slip lines of 0.1 –0.2 nm
height. Optical microscopy, coupled with a high-
speed camera, allows one to observe slip-line forma-
tion within 10 ms, which corresponds to dislocation
velocities in the ms
1 range. On the contrary, AFM
requires a much longer time between successive
images.
50 µm
(a) t = 0.02 s
(b) t = 0.06 s
1 µm
(e) (f)
Figure 1
Complementarity between optical (a–d) and AFM (e–g) in situ straining experiments in observing slip-line formations.
Plessing J, Sculke M 1990 Portevin-LeChatelier effect and observation of slip band growth in Cu–Al single crystals. J.
Mech. Beh. Met. 2, 231–54.
The complementarity of X-ray topography and
Figs. 2 and 3. Both methods allow one to identify
dislocations unambiguously using classical visibility
criteria. Similar events of nucleation and propagation
of dislocations at a crack-tip can be observed as a
function of time in silicon (Michot et al. 1994) and in
a Ti3Al intermetallic alloy (Legros 1994) (Fig. 2).
Both methods provide consistent dependencies of
dislocation velocity on stress in Si (Fig. 3). The ob-
servation of individual dislocations by X-ray topog-
raphy, the resolution of which is limited, is, however,
restricted to very small dislocation densities.
This article is restricted to the description of some
technical aspects concerning in situ deformation ex-
periments performed inside the transmission electron
microscope. Section 1 will be devoted to straining
experiments for which a tensile stress is applied to the
sample whereas more complex situations will be de-
scribed in Sect. 2.
1. TEM In Situ Straining
Hirsch et al. (1956) were the first to observe some
movements of dislocation in aluminum crystal heated
under the electron beam in a microscope operating at
100 kV. Two years later, Wilsdorf (1958) performed
(c) t = 0.18 s
(d) t = 0.60 s
(g)
1
In Situ Deformation Experiments: Technical Aspects

Figure 2
Complementarity between X-ray topography and TEM to observe nucleation and propagation of dislocations at a
crack-tip: (a) silicon; (b) Ti3Al. Reproduced from (a) Loyola de Oliviera M A 1994 Emission et d!evelopment de
dislocations en t#ete de fissure dans le silicium. Analyse tridimensionnelle de l’interaction dislocation/fissure. Ph.D.
Thesis, INPL de Nancy and (b) Legros M 1994 Etude par d!eformation in situ des m!ecanismes de d!eformation de Ti3Al
et Ti–24Al–9Nb. Ph.D. Thesis no. 1739, Universite! P. Sabatier, Toulouse, France.

the first true in situ tensile experiments at room tem-
perature, again in a 100 kV electron microscope, and
provided evidence for several dislocation processes
that had been previously hypothesized. These types of
experiments were not pursued after these pioneering
works since at that time it was believed that the spec-
imen thickness observable in transmission was too
small to give information relevant to the macroscopic
behavior of materials. At the end of the 1960s, oper-
ation of high-voltage microscopes in Japan and France
made it possible to conduct new in situ studies of dis-
location behavior in b.c.c. and f.c.c. metals (Fujita
1986, Furubayashi 1969, Louchet and Kubin 1975,
Caillard and Martin 1975). Since then, this technique
has been incessantly used and improved (Couret et al.
1993). Most of the in situ deformation experiments
conducted in the past few decades have been per-
formed with commercial low-voltage microscopes op-
erating at 200 kV (see In Situ Straining Experiments:
Examples of Results). This is partly due to the quality
of the pictures and to the ease of operating these in-
struments that allows easier and better control of the
image conditions and minimizes experimental artifacts.
1.1 Straining Holders
Many different straining holders have been designed in
the 1970s for high-voltage electron microscopes. An
overview of these systems can be found in the pro-
ceedings of a conference held in Halle (see, e.g., Mess-
erschmidt and Appel 1979) and in those of a seminar
held in Nagoya (see, e.g., Imura 1993). Although most
of these holders are no longer in operation, their prin-
ciples can still be discussed. They are top- or side-entry
and their mode of straining can be soft or hard. The
advantages of these systems are compared below.
Top-entry straining holders were designed in Osaka,
Nagoya, and Halle (Imura and Saka 1976, Messersch-
midt and Appel 1979, Fujita 1986, Imura 1991). They
offer ample space for the experimental setup and high
thermal and mechanical stability. Side-entry systems
were designed in Toulouse and ONERA-Paris (Martin
et al. 1975, Valle et al. 1979). They allow one to intro-
duce samples rapidly, thanks to a short pumping time.
Straining can be achieved by screws, piezoelectric
elements, or dilatation, for example, by heating a wire
thus allowing the expansion of a spring (Messersch-
midt and Appel 1979). Hard devices allow one to
impose the strain rate whereas soft devices yield
a constant load. The former are better adapted to
materials exhibiting plastic instabilities, and more
generally to materials with a large stress–strain rate
dependence such as intermetallic alloys. As a matter of
fact, in soft devices to which a constant load is ap-
plied, a very small local increase of stress due to crack
initiation induces a very large increase of strain-rate

2
 In Situ Deformation Experiments: Technical Aspects

10−1
 (µm s−1)

10−2

10−3

10 100

(MPa)

Figure 3
Dislocation velocity in Si single crystals as a function of resolved shear stress. Comparison between X-ray topography
and high-voltage electron microscopy. Reproduced from Louchet F 1981 On the mobility of dislocations in silicon by
in situ straining in a high-voltage electron microscope. Phil. Mag. 43, 1289.

leading to early sample destruction. On the contrary,
hard systems allow one to control the strain-rate and
to perform relaxation tests at the microscale.
The most recent and still available straining devices
are under operation in Osaka (Komatsu et al. 1994),
in Toulouse (Couret et al. 1993, Pettinari et al. 2001),
and in Grenoble (Pe! lissier and Debrenne 1993). The
former is a top-entry holder adapted to a 3 MV elec-
tron microscope. Heating is achieved by electron
bombardment of jaws and specimen, providing tem-
peratures as high as 1720 K that enable investigations
of the plasticity of sapphire. Those in Grenoble and
Toulouse are side-entry holders fitted to 300 kV and
200 kV electron microscopes, respectively. Some spe-
cific aspects of in situ straining experiments in the
TEM are addressed further.
1.2 Determination of the Sample Temperature
The microsample temperature is generally difficult to
measure directly because of its small size. The tem-
perature is then either taken equal to that of the jaws
or calibrated, as shown below.
In most devices, heating or cooling is transmitted
by the jaws, which in turn requires samples to be
firmly clamped in order to ensure good thermal con-
tact. This method is, however, difficult to apply to
brittle materials (semiconductors, ceramics, quasi-
crystals). Indeed, such samples tend to break easily
before the brittle-to-ductile transition temperature is
reached, and this may occur either in the course of
mounting onto the holder or else during the heating
procedure as a result of differential thermal expan-
sion. These samples must be loosely fixed to the jaws,
and subsequently radiation-heated inside a tungsten-
wired microfurnace. The sample temperature is cal-
ibrated from the in situ observation of the melting of
various samples with a high vapor pressure such as
In, Bi, Al, Cu, Ag (Couret et al. 1993). Senda et al.
(2004) showed that the thin parts of TEM samples
melt at a slightly lower temperature than the thicker
ones, and that the heating effect of the electron beam

3
In Situ Deformation Experiments: Technical Aspects
is fairly small. All these effects are taken into account
in the calibration. Melting temperatures plotted as a
function of the input power fall on a single curve
which can be used to estimate the temperature of the
thin parts of any sample within 7101. In situ tem-
perature jumps can be performed with a much better
relative accuracy of the order of 711, but one should
keep in mind that the local stress varies during the
transient because of differential thermal expansion.
1.3 Determination of the Local Stress
Observations are usually made in the vicinity of thin-
edged holes perforated at the center of microsamples.
Figure 4 shows that the stress distribution is rather
complex in these zones in direction and intensity
(Coujou et al. 1990). The local stress is, however,
Figure 4
Orientation of the major principal axis in a microsample
for a specimen in which the hole is at the center.
(a)
Figure 5
Example of measurement of the radius of curvature of moving dislocations.
4
concentrated in the two opposite areas where the hole
rim is parallel to the tensile direction. Since the cor-
responding local stress is parallel to the macroscopic
stress, the operating slip systems that appear first can
be predicted from the application of the Schmid law
to the whole sample. However, the magnitude of
the local stress cannot be easily predicted because the
intensity of the stress concentration depends on the
sample shape and its distance from the hole, and also
because elastic calculations, as in Fig. 4, are no more
valid after a substantial amount of plastic strain. The
local stress is then measured using the smallest avail-
able stress sensors, the dislocations themselves. Dis-
locations indeed behave like elastic strings with a line
tension T# defined as the dependence of the elastic
energy of a bowing dislocation upon length, that is,
T# ¼ dE/dl. As an order of magnitude estimate, T#
amounts to the average elastic energy of dislocations
#
per unit length, TEmb 2
, where m is the elastic shear
modulus and b is the Burgers vector. Assuming that T#
is independent of the dislocation character, a dislo-
cation pinned at two extremities and subjected to a
shear stress t (namely to a force per unit length tb)
appears as an arc of circle with radius R ¼ T/tb # (this
condition can be extended to any situation where the
curved dislocation can be considered to be at equi-
librium), hence providing the local stress t from the
measurement of R (Fig. 5). (Significantly different
values of R can be measured under 7g diffracting
conditions, as the contrast changes from one side of
the dislocation to the other one. Average values are to
be used especially at high stresses (small R).) More
precise measurements can be made using an orienta-
tion-dependent line tension computed under aniso-
tropic elasticity (Vailhe! et al. 1997). The corresponding
(b)
 In Situ Deformation Experiments: Technical Aspects

bowed dislocations have complex shapes varying ho-
mothetically with stress that can be compared with
observations. Taking into account all sources of inac-
curacy, in particular those involved in measuring R
itself, the local stress is estimated with an accuracy of
720%. Local and macroscopic stresses are compared
in Sect. 1.6.
1.4 Trace Analysis at Foil Surfaces
In principle, a moving dislocation generates a step of
interatomic height where the dislocation intersects
the two sample surfaces. In real experiments, dislo-
cation-emergence and subsequent surface-step is hin-
dered by an oxide layer formed during or just after
the sample preparation. This results in a residual
elastic field along the crystal/oxide interface, and this
in turn is at the origin of a trace contrast. Since traces
and emerging dislocations have homothetical elastic
strain fields, their conditions of observation (visibil-
ity/invisibility) are similar. In some materials (e.g.,
Al), traces disappear in a few minutes under the effect
of the electron beam, probably because of an en-
hanced relaxation of the oxide layer.
Traces are very useful to determine dislocation
paths. Two rectilinear traces correspond to a motion
in a single plane whereas wavy traces correspond to a
more complex motion (Fig. 6). When a dislocation
switches from a glide plane to another (cross-slip), the
intersection of the two planes yields the direction of
the Burgers vector (Figs. 6(a) and 6(b)). In case of
extensive cross-slip and for the same reason, the two
wavy traces can be superimposed upon a translation
parallel to the Burgers vector direction noted B (Figs.
6(c) and 6(d)). In case of climb, the two traces cannot
be superimposed by any translation. Under such con-
ditions, the close inspection of the two traces allows
one to reconstruct the whole dislocation motion in
three dimensions and, in case of cross-slip, to deter-
mine the Burgers vector direction.
1.5 Possible Thin-foil Artifacts
The problem of the relevance of in situ experiments to
reproduce the bulk behavior of materials has been
addressed and discussed in several articles (Martin
and Kubin 1978, Couret et al. 1993, P!elissier and
Louchet 1993). Various possible thin-foil artifacts
have to be checked carefully (see below). In addition,
irradiation effects may also take place, although they
are often negligible in TEM operating below the irra-
diation threshold of the material investigated. The
main thin-foil artifacts are as follows:
(i) Image stresses: The self-energy of a dislocation
decreases rapidly as it approaches a free surface where
its elastic strain field vanishes. The stress field re-
quired to produce this effect is roughly that of a
‘‘mirror’’ dislocation of opposite sign and arranged
symmetrically with respect to the nearest surface. The
magnitude of the image stress is accordingly of the
order of mb/4pd, where d is the distance to the surface.
It can be neglected when it is much smaller than the
local applied stress as deduced from the dislocation
radius of curvature R, namely when 4pd4R, or dXR.
(ii) Pinning at free surfaces: The formation of the
traces requires some work due to the back-force re-
sulting from the dislocation impinging on the two
surfaces. This force which amounts to a small fraction

d
h

B Ss
b
Si B

(a) (b)

B Ss
b B
d Si
(c) (d)
Figure 6
Traces left by moving dislocations. The two sample surfaces are referred to as Ss and Si, and B is parallel to the
dislocation Burgers vector.

5
In Situ Deformation Experiments: Technical Aspects
of mb2, must be much smaller than the total force
applied to the moving dislocation, tbl, where l is the
dislocation length. Taking l E e, the sample thickness
yields the condition ecR.
(iii) Geometrical effects: Dislocations emerging at
free surfaces tend to lie perpendicular to the sample
plane in order to reduce their length and thus, their
total energy. This tendency is enhanced by the rapid
elimination of dislocations parallel to the surfaces on
account of the image forces (see (i) above).
(iv) Initiation of dislocation mechanisms at surfaces:
Cross-slip is often considered to be more easily ini-
tiated at free surfaces. In the same way, single-kink
nucleation at a surface should be easier than kink-pair
nucleation in the sample interior. These effects have
been sometimes observed (Mompiou et al. 2004) but
their influence is less significant than expected, prob-
ably because of the presence of the oxide layers that
hinder core transformations involved in cross-slip.
Artifacts are of course the strongest in very thin
foils used in high resolution and (to a lesser extent) in
weak-beam observations. They are, however, fairly
minor for sample thicknesses larger than 300 nm.
The conditions, dXR and ecR (explained above),
are approximately equivalent. When they are satis-
fied, it is easy to find mobile dislocations that do
not interact significantly with the surfaces. Further
arguments may help neglect thin-foil effects such as
(i) when the same dislocation behavior is observed in
samples strained along the same axis but cut in dif-
ferent planes, (ii) when the temperature dependence
of the local flow-stress deduced from dislocation radii
of curvature is the same as in conventional mechan-
ical tests (Fig. 7), and (iii) when the dislocation

(MPa)
Low purity Ti
High purity Ti
T (K)
Figure 7
Stress measurements in two titanium ingots containing
low and high densities of impurities.
6
substructures are similar to those observed post
mortem in the material deformed by conventional
mechanical tests. These requirements are generally
satisfied in high-strength materials (small R) where
dislocations are either subjected to high frictional
forces or strongly anchored by a high density of pin-
ning points, as well as in light materials where the
observable thickness is large (large e, large d allowed).
Another strong limitation of in situ experiments, in
alloys heated above 80% of their melting tempera-
ture, is the rapid oxidation and evaporation of light
elements in the microscope vacuum. Evaporation is
strongly enhanced by the electron beam in sapphire
heated at 1200 1C where complete sample perforation
is accomplished after a few minutes of observation
(Castaing and Caillard, unpublished result).
1.6 The Role of the Microscopist: How to Avoid
Subjective Interpretations
Any TEM observation (not only in situ) is subject to
the choice of ‘‘representative’’ dislocation structures
or mechanisms, and to the role these are assigned in
explaining mechanical properties. In order to avoid
subjective interpretations, it is suggested (i) to obtain
a sufficiently large number of experimental results
allowing for statistical analyses, (ii) to consider all
events and aspects of dislocation motion with similar
care, and (iii) to cross-check for possible artifacts. It
must be kept in mind that several successful in situ
experiments are necessary to obtain a sufficiently
good overview of dislocation behavior at various
temperatures in a given material.
2. Other In Situ Deformation Experiments in
TEM
2.1 Nanoindentation
A new in situ deformation technique in TEM has
been developed recently (Minor et al. 2001). It allows
one to observe the contact between a nano-indentor
and a sample transparent to electrons. Details on the
technique can be found in Stach et al. (2001). Wedge-
shaped silicon substrates are fabricated through bulk
silicon micromachining techniques. The material to
be studied is subsequently deposited on a silicon
wedge, as shown in Fig. 8.
With this technique, one can apply very high
stresses to a tiny area, and record stress-penetration
curves as a function of the corresponding substruc-
ture evolution. It is suited to brittle materials that
cannot be deformed in tension.
In Al with a grain size of 250–400 nm, it was shown
that the nucleation of dislocations can be associated
with the ‘‘pop-in’’ response typical of nanoinden-
tation of metals whose grain size is larger than the
contact area of the indentor (Fig. 9). The stress
 In Situ Deformation Experiments: Technical Aspects

actually increases till a few dislocations are emitted

Diamond indenter
from the indentation. Then, the stress remains con-
stant and a small amount of displacement is recorded.
Dislocations subsequently stop and the stress increas-
es again. The experiments also showed a significant
contribution of grain-growth and grain-coalescence
Electrons AI to deformation (Jin et al. 2004).
Experiments in Al with a grain size smaller than
200 nm are more difficult to interpret because the
150 nm minimum sample thickness along the direction of
observation is necessarily much larger than the grain
size.
In addition to the limitations mentioned above, the
Silicon substrate small sample width may affect the stress distribution
around the indentor. This effect is, however, of minor
importance in the qualitative studies reported up to
now.
Figure 8
Cross-section of a sample for an in situ nanoindentation 2.2 Straining Experiments in Environmental Cells
experiment. The 250 nm thick Al film was deposited on a
silicon wedge. Reprinted with permission from Minor The effect of gas–solid interaction on deformation
A M, Morris J W, Stach E A 2001 Quantitative in situ mechanisms and mechanical properties can be analy-
nanoindentation in an electron microscope. Appl. Phys. zed by performing in situ straining experiments
Lett. 79, 1625. Copyright 2001, American Institute of under controlled environment. An environmental cell
Physics. adapted to a JEOL 4000EX has been designed at the

30
Al (113)
In situ
25

20
Al (110)
Force (µN)

15 Al (133)
Al (111)
10

D
5 C
Al (111)
B
0
0 5 10 15 20 25 30
A Displacement (nm)

(a) (b) (c) (d)

75 nm
[101]

Figure 9
Force–displacement curve and representative micrographs from an Al grain indented in situ. Reprinted with
permission from Minor A M, Morris J W, Stach E A 2001 Quantitative in situ nanoindentation in an electron
microscope. Appl. Phys. Lett. 79, 1625. Copyright 2001, American Institute of Physics.

7
In Situ Deformation Experiments: Technical Aspects

University of Illinois (Lee et al. 1991, Robertson and
Teter 1998). The experimental challenge is to mini-
mize the electron path throughout the gas and to
confine it to the sample volume to avoid degrading the
column and gun vacuum. This has been achieved by
reducing the gas outflow by using a series of apertures
placed above and below the specimen. Figure 10
shows a schematic cross-sectional view through the
objective section. A total of five apertures were used.
Above and below the specimen, two apertures are
located in the body of the cell and in the pole pieces,
respectively. An additional reduction of gas leak is
obtained by pumping the volume between primary
and secondary sets of apertures. The fifth aperture is
located in the lower section of the condenser lens
stack to confine gas flow to the gun chamber. Experi-
mental limitations are the maximum cell pressure,
which is less than one atmosphere, and the impossi-
bility of making high-angle diffraction experiments.
This technique allows one to perform high-tempera-
ture experiments with appropriate straining holders.
Maintaining stress and temperature as gas is being
introduced can be a constraint in this case.
With this instrumental setup, the effect of hydrogen
on dislocation mobility has been studied in a large
number of materials (see Birnbaum et al. 2000).
Introducing H2 into the environmental cell under con-
stant stress applied to the sample increases dislocation
mobility; moving dislocations speed up while immo-
bile dislocations begin to move. This result has been
interpreted as a shielding effect whereby elastic inter-
actions between dislocations and other elastic centers,
such as other dislocations, solute atoms, or precipi-
tates, are screened by the presence of hydrogen atoms.
2.3 Electromigration
Nucleation and coalescence of voids can take place in
thin metallic layers subjected to high current densities.
This phenomenon—called electromigration—which
severely limits the lifetime of integrated circuits is
the result of atomic transport driven by temperature
gradients. In the direction of the electron flow, holes
and hillocks form in regions where temperature is the
highest and lowest, respectively. These effects are
more pronounced in thin layers where the Joule effect
is stronger, especially where grain size is larger than
the layer thickness (bamboo structure). Electromigra-
tion can be observed in situ in TEM. From the first
experiments of Blech and Meieran (1967), several
in situ experiments have been carried out which are

Gas cabinet
M9
G1
RP C V3 G2
TMP C
RP D V7
V4
RP E TMP D SA
TMP A
V5 V1
cell
H2 N2 PA RP B
V6 G4 G3 Specimen
G7
V9 PA
G5 cell
M1 V8 SA
M7 TMP B
M8 G6 Pole-piece V2

RP B
M5 M2

M6 M4 M3
Pneumatic valve Turbomolecular pump
H2
Bubbler Manual valve Rotary pump
purifier
Pressure gauge Roughing tank

Figure 10
Schematic cross-sectional view of the objective lens section of the microscope column. Reprinted with permission from
Lee T C, et al. 1991 An environmental cell transmission electron microscope. Rev. Sci. Instrum. 62, 1438. Copyright
1991, American Institute of Physics.

8
 In Situ Deformation Experiments: Technical Aspects
reviewed in the recent works of Okabayashi et al.
(1996) and Shih and Greer (1997). Electrical contacts
are established at each extremity of the layer. The
main difficulty is to observe the evolution of the layers
(or multilayers) in thermal contact with a silicon
substrate, but electrically isolated by an SiO2 layer.
Most experiments have been carried out in thin foils
where the Si substrate and the SiO2 layer have been
removed, which results in deep changes in the local
equilibrium temperatures. Under such conditions,
heating effects are estimated from the substructure
evolution (Vavra et al. 1981), or from the onset
of melting of some layers (Shih and Greer 1997).
According to Shih and Greer (1997), damage proc-
esses remain essentially the same as in layers deposited
on thick substrates, although they are strongly accel-
erated by higher local temperatures.
Observations of thick lines are, however, facilitated
by the use of high-voltage electron microscopes (Ta-
kaoka et al. 1993). In particular, side-view observa-
tions preserving a good thermal contact between the
layer and the substrate are possible (Fig. 11).
It is observed that grain boundaries are generally
more conducive to void nucleation. Fortunately, void
healing competes with void formation in order to
maintain electrical conductivity (Fig. 12).
2.4 Plasticity of Thin Layers under Thermal Stress
Electronic devices are submitted to thermal cycling,
producing high stresses in films due to differences in
thermal expansion coefficients during both, process-
ing and service. This effect is dramatic in very small
devices. In situ thermal cycling in the transmission
electron microscope allows one to identify the micro-
structural processes occurring during thermal cycling.
Electron beam
Electron flow
Al
TiN
Figure 11
Illustration of in situ observation of the
electromigration. Reprinted with permission from
Okabayashi H, Kitamura H, Komatsu M, Mori H 1996
Behavior of electromigration-induced gaps in a layered
Al line observed by in situ sideview transmission electron
microscopy. Appl. Phys. Lett. 68, 1066. Copyright 1996,
American Institute of Physics.
The processes involved during the thermal cycling of
electronic devices have been observed in situ on plan-
view specimens of ultra-thin copper films (Balk et al.
2003) and on cross-sectional samples of passivated Al
films on Si substrates (Legros et al. 2002). In both
cases, double-tilt heating stages were used.
Figure 13 shows plan-view and cross-sectional thin
foils suitable for in situ heating experiments. The
plan-view sample (Fig. 13(a)) was made from a wafer
that had previously been cycled. The Si substrate was
subsequently thinned by mechanical polishing. At-
tention had been paid to keep the copper film un-
touched (undamaged). A stable ring of Si still remains
around the dimpled region which forces the film into
compression tension during thermal cycling.
In cross-sectional thin foils (Fig. 13(b)), the two
pieces are glued film-to-film using a vacuum epoxy to
protect the film during polishing. The thin films are
oriented parallel to the tip of the wedge in the area
1 µm 1 µm
(a) (b)
(c) (d)
(e) (f)
Figure 12
In situ electromigration test showing the development of
voids to failure. Reproduced from Shih W C, Greer A L
1997 Transmission electron microscopy of Al–Cu
interconnects during in situ electromigration testing.
Thin Solid Films 292, 103.
9
In Situ Deformation Experiments: Technical Aspects
Electron transparent
200 nm Cu
Si
(a)
Si substrate
(A)
Film
Glue
Film
Remaining of
Si substrate (B)
(b)
Figure 13
(a) Plan-view and (b) cross-sectional thin foils for in situ
heating experiments. (a) Reproduced from Balk T J,
Dehm G, Artz E 2001 Dislocations and deformation in
thin films and small structures. Proc. MRS Symp. 673,
2.7.1–6, with permission from MRS. (b) Reproduced
from Legros M, Hemker K J, Gouldstone A, Suresh S,
Keller-Flaig R M, Artz E 2002 Microstructural
evolution in passivated Al films on Si substrates during
thermal cycling. Acta Mater. 50, 3435.
where the thin hole is parallel to the longitudinal axis
of the holder. The Si substrate, which supports the
thin film, is subsequently glued to a copper grip
adapted to the heating holder. This geometry repro-
duces the conditions encountered by the thermally
cycled entire wafer.
The validity of in situ results is first checked by com-
parison with observations obtained from dead samples.
Local stresses are then estimated from the curvature of
bowed dislocations and a fair coherence is found with
stress deduced from substrate curvature measurements.
The main limitation of this technique is in the distri-
bution of the stress produced by the temperature in-
crease. This stress is uni-axial in thin foils whereas it is
bi-axial in devices. Its magnitude too is 20–30% lower.
See also: In Situ Straining Experiments: Examples of
Results.
Bibliography
Allais L, Bornert M, Bretheau T, Caldemaison D 1994 Exper-
imental characterization of the local strain field in a heter-
ogeneous elastoplastic material. Acta Metall. Mater. 42, 3865
10
Balk T J, Dehm G, Artz E 2001 Dislocations and deformation
in thin films and small structures. Proc. MRS Symp. 673,
2.7.1–6
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