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INTERFACE FRACTURE
Michael Lane
IBM T. J. Watson Research Center, Yorktown Heights, New York 10598;
email: mwlane@us.ibm.com
INTRODUCTION
0084-6600/03/0801-0029$14.00 29
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0i = (ξ + χ + ζ )0o , 1.
INTERFACE FRACTURE 31
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Indentation tests (Figure 3a) are characterized by the use of a sharp-rigid tip
indenting a film (or films) on a rigid substrate. The original mechanics for a single
film were derived by Marshall & Evans (19) and indicate that the driving force for
delamination, or the strain energy release rate, G, has three contributing energies
that are required for its calculation. The required measurements are the residual
stress of the film, the indentation depth that allows for calculation of the indentation
stress, and the diameter of the resultant delamination. One advantage of this test is
that the interface of interest undergoes no processing after its initial creation, which
allows for the determination of the interfacial adhesion of the virgin interface.
However, for ductile films or well-adhering interfaces, the film of interest may
deform plastically prior to the buildup of sufficient elastic strain energy, resulting
in no delamination (20). In order to address this issue, a highly stressed overlayer
film may also be deposited (21). The overlayer adds an additional driving force
through its residual stress and is typically a refractory metal with a high-yield stress
that reduces plastic deformation. Kriese & Gerberich (21) extended the analysis
of indentation of a single film to include the case of multiple films on a single
substrate. Interface adhesion measurements utilizing the superlayer indentation
test have captured effects of interfacial chemistry and plasticity (22–24), but the
scatter in the data collected can be large [at times up to an order of magnitude
(18)]. A further limitation of the indentation test is that methods to measure the
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INTERFACE FRACTURE 33
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However, the DCB sample can be placed in a special loading configuration (32–
34) that allows the interface fracture energy to be determined over the complete
range of phase angles, as has been done in a number of glass epoxy systems
(35–38). Load relaxation techniques can be used to measure the effects of the
environment (39), and the samples can also be used to address issues of fatigue
loading on the interface (40), making this particular test the most flexible reviewed.
However, there are several drawbacks to this test. First, the sandwiched fracture
mechanics specimens are often made either by a diffusion bonding procedure or
with an epoxy. The diffusion bonding procedure often involves high temperatures
for extended periods of times [400◦ C in the case of Cu diffusion bonding (17)]. This
introduces the possibility of altering the interface during the sample preparation
step. In the case of an epoxy bond, care must be taken to design the stack structure
so that plasticity in the bond layer is eliminated (41), otherwise measurements of
the interface fracture energy will include plasticity in the epoxy bond layer. The
sample preparation of the sandwiched fracture mechanics specimens can be tedious
and often requires polished side face of the samples if the substrate is brittle, e.g.,
Si, to eliminate fracture of the substrate before interfacial delamination occurs.
Finally, Becker et al. (42) have shown that, for the four-point flexure geometry, the
limit of validity of the mechanics-derived strain energy release rate depends on
the amount of plastic energy dissipation, which is a function of the ductile layer
thickness.
The driving force for formation, and therefore the energy that must be overcome
during fracture, of an interface is the release of energy when intimate contact is
established between the materials that form the interface (43, 44). The simplest
description of the physical interaction between two materials is the work of adhe-
sion, 0 o. If clean surfaces are brought into contact, the energy is released according
to (e.g., 44):
0o = γ1 + γ2 − γ1–2 , 2.
where γ 1 and γ 2 are the free energies of the relaxed surfaces of each constituent
of the bimaterial interface, and γ 1–2 represents the energy of the relaxed interface.
Note this is simply the Griffth criteria for fracture (45) applied to interfaces, and 0 o
is the reversible work released per unit area of interface formed by two free surfaces.
This section discusses the factors that affect the work of adhesion and, in particular,
deals with the effects of interfacial segregants, bond density, and bond energy.
Rice & Wang (46) formally described the effect of segregants to an interface
on the work of adhesion as
X¡ ¢
Go = 0o − 1goi − 1gso ci , 3.
i
INTERFACE FRACTURE 35
segregant per unit area of interface, and 1go is the Gibbs free energy of segregation
for the interface (i) and a free surface (s).
An example of segregation is seen in the effect of nitrogen on the adhesion of
the Ta/SiO2 interface (47, 48). In this experiment a 2-nm Ta layer was deposited
on thermal SiO2 and different amounts of N (20, 30, or 40 at%) were diffused
to the interface. This resulted in an increase in the measured fracture energy by
∼150% owing to the addition of the nitrogen, and the increase may be understood
by consideration of the following reactions:
14 Ta + 5 SiO2 → 2 Ta2 O5 + 5 Ta2 Si—43.9 kcal/mol, 4a.
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INTERFACE FRACTURE 37
0o = N (1g M + 1g O − 1g M – O ), 7.
where N is the number of bonds per unit area, and 1g is the Gibbs free energy
of the pure metal, the oxygen-terminated Si surface, and the metal-oxygen bond,
respectively. Equation 7 is similar to that derived for the fracture resistance of bulk
glasses in a corrosive environment (55) if one notes that the chemical potential
(used in the bulk glass literature) is equivalent to the partial molar Gibbs free
energy.
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where E, ν, and σ ys are the elastic modulus, Poisson’s ratio, and yield strength of the
plastically deforming material, respectively. Ro scales with the plastic zone size.
The essential features of the unified model may be found in Figure 6 and
consist of a traction separation law, which determines the interfacial strength, the
Figure 6 Schematic representing the key features of the unified model. The major
dependencies are indicated in the text except for N, which is the strain-hardening
exponent for the ductile layer (65).
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INTERFACE FRACTURE 39
peak stress σ̂ , and a plasticity free zone of width D. The traction separation law
characterizes the interface fracture process and serves as an internal boundary
condition along the interface. A dimensionless separation parameter, λ, is defined
in terms of the normal, δ n, and tangential, δ t, displacements of the crack faces
across the interface:
sµ ¶ µ ¶2
δn 2 δt
λ= + c , 9.
δnc δt
where δnc and δtc are critical interface displacements. When λ = 1, the tractions drop
to zero, crack advance occurs, and the fracture energy is determined by
1 c
0o = σ̂ δ [1 − λ1 + λ2 ], 10.
2 n
where λ1, λ2, σ̂ , and δnc are detailed parameters in the traction separation law and
may be found in References (62, 65). The delamination is separated from the active
plastic zone by an elastic layer of thickness, D, the purpose of which is to embed the
debond tip in an elastic region so that the high stresses at the debond tip necessary
for atomic separation can be obtained (64). Therefore the interface is characterized
by the adhesion energy and peak separation stress, 0 o and σ̂ , and the plasticity
free zone of width D. Simulation results indicate that the ductile layer deformation
properties and film thickness, cohesive properties, and elastic layer thickness have
the most significant effect on interface fracture resistance (e.g., 63, 65).
A problem in determining the effect of any one parameter on the extent of plastic
energy dissipation in a given system is the number of independent variables in the
model. In order to accurately gauge the effect of any one variable on a given system,
the others must be fixed by experimental measurements. One attempt to do this is
found in the experimental study of the fracture resistance of the TiN/SiO2 interface
with different thicknesses of a ductile Al-Cu layer (17, 48, 69). In this experiment,
the thickness of the elastic layer, D, was set by the thickness of the TiN layer,
and an estimate of the work of adhesion was made by extrapolation to zero Al-Cu
layer thickness. This left only the peak interface separation stress and the yield
properties of the Al-Cu layer as variables. The results of the interface fracture
energy measurements along with simulations of the fracture process from both the
unified model (65) and a multiscale continuum/FEM model (63) are presented in
Figure 7. Both models accurately predict the observed behavior, and an important
ratio emerges from the unified model. As the ratio of the ductile layer thickness,
hAl-Cu, to the modeling length scale (given in Equation 8, Ro ∼ 1 µm in the current
example) approaches four, increases in toughening owing to additional increases in
metal layer thickness are not expected. Thus for a fixed value of D and metal yield
stress, limits to the toughness enhancement owing to plastic dissipation can be
expected, as was predicted (65). However, the utility of the simulations is limited
because accurate values of the work of adhesion, 0 o, were not determined and a
constant value of the yield stress of the Al-Cu layer was assumed, even though the
thickness of the film varied by over an order of magnitude. Note that data from
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Figure 7 Interface debond energy as a function of Al-Cu layer thickness. The lines
represent fits of various models to the data. In the rising portion of the curve, the plastic
zone (represented by a black rectangle) size is larger than the Al-Cu layer thickness.
The plateau region indicates the plastic zone size has become smaller than the Al-Cu
layer thickness (17, 48, 69).
the double-cantilever beam geometry are also presented and illustrate the effect of
stress state on the plastic deformation in these samples (depicted schematically in
Figure 2) (48).
However, measurements of interface fracture energy have been made for ductile
metal films where the interface fracture energy did not change over a range of metal
layer thickness (18, 48, 69), which indicates that the constant interface fracture
energy is a measure of the work of adhesion of the interface, as there is no apparent
plastic energy dissipation. One of these systems has been modeled extensively with
the multiscale continuum/FEM approach developed by Lane and Lane et al. (48,
69). The system consists of the SiO2/TaN interface with Cu layers ranging from
0.03 to 18 µm in thickness. Delamination occurred along the SiO2/TaN interface
so that the thickness of the elastic layer, D, is set by the thickness of the TaN layer,
and the work of adhesion is set by the plateau value of the interface fracture energy
shown in Figure 8. This leaves only the peak interface separation stress, σ̂ , and
the metal yield stress as variables to fit the data. However, published Cu yield data
were used, leaving only the peak interface separation stress as a variable. For Cu
thicknesses where yield data were not available, the metal yield stress was used as
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INTERFACE FRACTURE 41
a fitting parameter but made to follow a Hall-Petch type relation (69). The solid
line in Figure 8 shows the fit for a peak interface separation stress equal to ESi/60.
With σ̂ determined, other modeling parameters were varied to access their effects
on plastic energy dissipation. The results may be summarized as follows:
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the debond tip propagation direction relative to the far-field applied loading may
change. This change in debond orientation results in a change of the near-tip stress
state and therefore a change in the debond driving force (70, 71). As the debond
moves it may either tilt or twist relative to its original path. The driving force for
the new orientation may be calculated by a tensor transformation of the original
far-field stress fields (72, 73). Plots of the tip driving force normalized by the far-
field driving force have been made for the special case of equal parts shear and
normal applied loading and serve as a useful guide for understanding the effect
(73). The results indicate that tilt or twist angles with a ratio of Gtip/Gapplied less
than 1 result in debond tip shielding, whereas ratios greater than 1 lead to debond
extension at driving forces reduced from that of a planar debond. Small changes
in propagation angle due to twist or tilt do not have a significant effect on the
macroscopic work of fracture.
The second increase in interface fracture energy due to nonplanarity may be
understood by consideration of the Griffith criterion for fracture, which indicates
the energy required to separate two surfaces depends on the total area of separation
(45). For a planar interface, this is simply the length of the debond times its width.
However, for a debond that deviates from a planar path, an increase in the total
debonded area occurs that results in a corresponding increase in interface fracture
energy that scales with the true debonded area over the planar area.
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EH2
χ= , 11.
λ0o
where H is the amplitude of roughness, λ the wavelength, E the elastic modulus,
and 0 o the work of adhesion. A number of important phenomena are captured by
this simple model. First, the shielding effect increases dramatically as the loading
mode tends toward pure shear loading, as has been observed experimentally in a
number of systems. Second, when the shielding parameter is ≤10−4, shielding is
only realized as the phase angle of loading approaches 90◦ (pure shear). Finally,
as the shielding parameter approaches 1, further increases in the amplitude of
roughness do not significantly enhance the interface fracture energy.
Cao & Evans (10) found that for a glass epoxy system the interface fracture resis-
tance increased according to a value of χ equal to ∼1 as the phase angle of loading
was changed. Ma et al. (74) and Clarke (75) demonstrated that the interface fracture
energy of TiN/SiO2 could be increased by 50% simply by roughening the interface
(Figure 10). In a similar experiment examining the TiN/SiO2 interface, Lane et al.
(48, 76) examined a range of interfacial morphologies and correlated the change in
interface fracture energy with changes in interfacial roughness. In this experiment,
the interfaces were characterized with atomic force microscopy (AFM) to deter-
mine the average amplitude and wavelength of the roughness. A model interface
similar to that described by Evans & Hutchinson was constructed on the basis of
the root mean square (RMS) roughness and the average roughness wavelength, as
determined in the AFM measurements. These model interfaces were then used to
predict the relative magnitudes of the increases expected from the debond kinking
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out of the interface, increased surface area, and roughness-related shielding. Re-
sults indicated that increases in interface fracture energy for the roughest interface
predicted by crack tip deflection and increased area were only 2.3 and 0.3%, respec-
tively. However, increases based on the asperity contact model properly captured
the 25% increase in interface fracture energy as measured (Figure 11). So, espe-
cially for thin film systems where the roughness is not sufficient to cause large
changes in the propagation direction or significant increases in debonded area,
asperity contact is the dominant mechanism that leads to increases in interface
fracture energy due to roughness.
ENVIRONMENTAL EFFECTS
The mechanisms reviewed above have, for the most part, resulted in increases in
the macroscopic work of fracture. However, as in the case of the segregation of
species to certain interfaces, there are factors that can cause dramatic decreases in
the energy required to separate an interface. In particular, the environment can alter
the overall strength and reliability of an interface. A number of authors have noted
that certain interfaces, especially those where one of the materials composing the
bimaterial interface is SiO2, exhibit debond growth at applied driving energies
less than that required for critical fracture when the interface is delaminated in
a corrosive environment (e.g., 16, 77, 78). These authors have noted that this
behavior is similar to stress corrosion cracking in bulk glass systems. A large body
of work has focused on determining the mechanisms that control stress corrosion
in glasses, and detailed models have been developed to describe the controlling
processes (79–87). For simplicity, the discussion and examples herein are limited
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INTERFACE FRACTURE 45
to the effects of water on stress corrosion, but it should be noted that other corrosive
species (such as alcohols) can cause the same effect both in bulk glasses (e.g., 88)
and at interfaces (e.g., 77).
In bulk glasses, the environmental process leading to crack advance is a three-
step concerted reaction involving a water molecule and the strained Si-O bonds at
the crack tip (85–89). Plots of crack growth velocity versus crack driving energy
typically result in a sigmoidal shape (Figure 12), where changes in slope indicate
a change in the rate-limiting step for crack advance (e.g., 80, 82, 84). Region III is
dominated by critical fracture events and represents the interface fracture energy
in the absence of a corrosive species.
Region II, or the plateau region, is insensitive to crack driving force and the
rate-limiting step is found to be controlled by the diffusion of a reactive species to
the crack tip, so that the crack velocity is given by (80, 82, 84):
64 G a3o PH2 O
ν= ¡1¢ 1 , 12.
3π Eao ln ao x(2πmkT) 2
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Figure 12 Schematic representing typical velocity versus driving force (V-G curve)
behavior for bulk glasses. The schematic shows the four distinct regions that correspond
to distinct rate-limiting steps for crack advance (79, 82, 84).
where E is Young’s modulus, l is the mean free path of the water vapor, m is the mass
of the diffusing species, P is the partial pressure of water vapor, x is the num-
ber of water molecules absorbed per bond, ao is the bond spacing, and G is the
mode I driving energy. The plateau velocity in Equation 12 depends linearly on
the partial pressure of water vapor, and an example of this occurring at interfaces
can be found in Figure 13 (48, 78).
As the crack velocity slows, the diffusion of water to the crack tip is greater than
the rate of crack advance, and the rate-limiting step switches from one controlled
Figure 13 (a) V-G curves for the Ta/SiO2 interface showing the shift in Region II with
partial pressure of water. (b) Liner relationship between the average Region II velocity and
partial pressure of water vapor γ (48, 78).
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INTERFACE FRACTURE 47
where µSi-O∗ , µSi-O, and µH2 O − RTlnPH2 O are the chemical potentials of the reactive
complex (Si-(H2O)-O), the crack tip bond, and the corrosive species, respectively.
The crack velocity in this region can be found by (84)
· ¸
G − N[α(T) − RTlnPH2 O ]
v = vo Sinh , 15.
η
where N is the number of bonds per unit area, T is the absolute temperature, PH2O
is the partial pressure of water vapor, α(T) represents the chemical potential of
the Si–O bond and the reactive complex, G is the applied driving force for crack
propagation, and η and ν o are parameters related to the bonds being broken. The
numerator of the Sinh function in Equation 15 implies a corrosion threshold below
which crack growth stops. Equation 15 also indicates that both the position of the
threshold driving force and the position of Region I will shift as the logarithm of
the partial pressure of water vapor. This behavior has been observed for different
interfaces with a representative example given in Figure 14 (48, 78). Note that
Figure 14b represents the effect of both temperature and humidity and that tem-
perature has only a weak effect on the position of the corrosion threshold. This
is consistent with Equation 15 in that over the range measured, the temperature
changed by a maximum of 29%, while the natural log of the partial pressure of
water vapor changed by 150%.
In some systems, an alternative threshold regime has been observed (85) in
which the threshold occurs when the corrosive molecule can no longer reach the
debond tip because it is sterically hindered from doing so. In this case, the thresh-
old depends only on the crack opening displacement and the size of the corrosive
species and only very weakly on the environment. The data in Figure 13 have
been replotted in Figure 15 with the onset of the threshold region expanded, which
illustrates this phenomenon. As mentioned above, Region II behavior consistent
with that expected in bulk specimens is observed for the interface. However, there
is a transition from Region II directly to a threshold as GI is lowered, with the
position only weakly dependent on the test conditions. This transition to a steric
hindrance threshold was shown to be consistent with the formation of a Ta oxide,
the thickness of which depends on the time of exposure (determined by the plateau
velocity) and the test temperature, which blocked the water molecule from reaching
the debond tip by reducing the opening behind the debond tip according to (78)
√ r
2 GI 8y dH O
uop = ao + √ − tox − 2 , 16.
E π 2
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Figure 14 (a) Region I and threshold driving force dependence on the environment.
(b) Change in threshold driving force as a function of temperature and partial pressure
of water vapor, indicating that temperature has only a small effect (48, 78).
where the first two terms represent the opening expected for a linear elastic solid,
where ao is the bond spacing, GI is the mode I driving energy, and y is the position
behind the debond tip. This opening displacement is reduced by the length of a
hydroxyl (-OH) group, which accounts for the rupture process and is represented
by d H2 O /2 and the thickness of the oxide, tox. The onset of the steric hindrance
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INTERFACE FRACTURE 49
threshold is found by solving Equation 16 for GI. A plot of the change in measured
threshold driving energy found in Figure 15 and that predicted by Equation 16 can
be found in Figure 16.
Finally, Equation 14 indicates that the effective work of adhesion can be altered
by changing the environment in which an adhesion test is conducted. By doing
this, the relationship between the work of adhesion and plastic energy dissipation
can be explored. Figure 17 (48, 78) illustrates this by plotting the change in work of
adhesion, predicted by Equation 14, for the TaN/SiO2 interface versus the macro-
scopic work of fracture. The result is a straight line with a slope of ∼20, which
indicates that for every 1 J/m2 the work of adhesion is changed as the macroscopic
work of fracture changes by a factor of 20. This is consistent with predictions of
interface fracture models (69).
Figure 16 Predicted change in steric hindrance threshold (solid line) versus that
measured in Figure 15. The predicted change is based on the growth of an oxide layer
immediately following fracture of the Ta/SiO2 interface (48, 78).
Figure 17 Relationship between the macroscopic work of fracture and the work of
adhesion for the TaN/SiO2 interface with a 16.4-µm Cu layer adjacent to the interface.
As the effective work of adhesion is decreased (by increasing the moisture content in
the testing environment) the plastic energy dissipation in the ductile Cu layer is reduced
(48, 78).
50
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INTERFACE FRACTURE 51
speculated to control the diffusion (91, 92). Recently (93), work has focused on
deriving a relationship between the adhesion of the fast diffusion path and the ele-
ctromigration activation energy, the results of which are summarized in Figure 18.
The linear relationship between the work of adhesion and electromigration ac-
tivation energy has been predicted (93, 94) and should not come as a surprise,
since both diffusion and fracture involve, to one extent or the other, the breaking
of bonds. There are two implications of this. The most obvious is that interfa-
cial adhesion measurements can be used as a screening process to address other
interfacial phenomena that may require laborious and costly sample preparation
(as in the case of electromigration samples), so long as a link between the two
measurements can be established. The second perhaps more subtle implication is
that bond character controls these interfacial phenomena and that the measure of
the bond character would give the ultimate insight into the interfacial phenomena.
For example, consider the work of Muller and coworkers (95), who investigated
the effects of B segregation to Ni-Al grain boundaries with electron-energy loss
spectroscopy (EELS). Muller et al. showed that B segregation altered the electronic
structure of Ni in the grain boundaries of a Ni3Al intermetallic and correlated that
change to a change in fracture properties of the grain boundary. Later, Rosenberg,
working with Muller (96), demonstrated that EELS spectra revealed changes in
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SUMMARY
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