Interfacial delamination cracking shapes and stress states during

wedge indentation in a soft-film-on-hard-substrate

system—Computational simulation and experimental studies
Lei Chen
Department of Mechanical Engineering, National University of Singapore, Singapore 117576; and
Center for Advanced Computations in Engineering Science (ACES), Department of Mechanical Engineering,
National University of Singapore, Singapore 117576
Kong Boon Yeap and Kai Yang Zenga)
Department of Mechanical Engineering, National University of Singapore, Singapore 117576
Chong Min She
Academy of Frontier Science, Nanjing University of Aeronautics and Astronautics, Nanjing 210016, China
Gui Rong Liu
Center for Advanced Computations in Engineering Science (ACES), Department of Mechanical Engineering,
National University of Singapore, Singapore 117576; and Singapore-MIT Alliance (SMA), Singapore, 117576

(Received 24 January 2011; accepted 16 May 2011)

The shapes of the interfacial delamination crack and stress states during wedge indentation in
a soft-film-on-hard-substrate system were investigated systematically using the three-dimensional
(3D) finite element simulation and wedge indentation experiment. In the simulation, a traction–
separation law was used to characterize the failure behaviors of the interface. The effects of the wedge
indenter tip length and the film thickness on the onset and growth of interfacial delamination were
analyzed. It was shown that a two-dimensional (2D) to 3D transition of stress states occurred
depending on the ratio of indenter length to film thickness. Furthermore, the interfacial delamination
process by wedge indentation was conducted experimentally, and comparisons between the
computational and experimental results yielded quantitative good agreement. Finally, a straightfor-
ward criterion based on the curvature of the delamination crack front was proposed to indicate the
transition of stress states during the interfacial delamination. A guideline was therefore proposed to
classify the 2D and 3D stress states for extracting the interface adhesion properties.

I. INTRODUCTION and wedge indentation experiments,13–15 have been

Thin film structures are widely used in many tech-
nologically important application areas, including mi-
croelectronics and optoelectronics devices, magnetic
data storage, medical devices, and many more.1,2 An
important issue in all of the thin film/substrate systems is
the adhesion of the interface between the film and
substrate since the interfacial delamination may lead to
a system failure even though the film and substrate still
satisfy the technical requirements. This issue has there-
fore attracted a great deal of attention in recent years.3–5
For ultrathin films, the thickness of the films is usually
in the order of few hundred nanometers. Therefore, it is
difficult to measure their interfacial adhesion properties
using conventional mechanical testing techniques, such as
tensile and bending tests. On the other hand, nanoin-
dentation techniques,6–9 such as spherical,10 conical,11,12
a)
Address all correspondence to this author.
e-mail: mpezk@nus.edu.sg
DOI: 10.1557/jmr.2011.175
proven very effective in the investigation of interfacial
delamination of thin film systems. During the nanoinden-
tation tests, the interfacial delamination can be reflected
and identified by characteristic changes in the indentation
load–displacement curves (P–h curves). For example,
Swain and Men
cik10 demonstrated various responses in
the indentation load–displacement curves caused by the
interfacial delamination during spherical indentations.
Later on, Drory and Hutchinson16 developed a conical
indentation analysis to assess the interface toughness.
Furthermore, a wedge indentation method has been de-
veloped.14,15,17 Recently, Yeap et al.18,19 adopted the
wedge indentation method and focused ion beam (FIB)
technique to determine the interfacial toughness of the
ultrathin continuous film on substrate [low-dielectric con-
stant (low-k) films on silicon (Si) substrate]. Compared to
spherical and conical tips, the wedge indenter is capable of
producing high driving force, and thus it does not penetrate
into the substrate for inducing the interface crack. In
addition, the delamination crack is eventually propagated
into the surface and, therefore, can be relatively easily

J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
Materials Research Society 2011 2511
http://journals.cambridge.org Downloaded: 04 Feb 2015 IP address: 129.93.16.3
L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system
observed from the surfaces around the wedge indentation
impression, making the interpretation of the experimental
phenomena easier. Thus, it is considered as a potential
powerful experimental method to determine interfacial
properties. However, deriving interfacial adhesion proper-
ties from the wedge indentation is still a challenging issue
because analytical methods are generally not feasible for the
explanation of the indentation test results.18,19 Therefore,
finite element (FEM) simulations are often used to interpret
the experimental results.20–23
In view of simulating the interfacial delamination
processes induced by a wedge indentation, many studies
have used a traction–separation law24,25 (cohesive zone
model) to describe the adhesive and failure behaviors of
the interface between film and substrate. In the traction–
separation law, interfacial properties are characterized by
two parameters: interfacial strength, rs, which is the peak
traction (stress) to separate an interface, and interfacial
energy, C0, which is the work-of-separation per unit area
of the interface. An advantage of using this traction–
separation law to simulate the wedge indentation process
is that it is not necessary to make assumptions that
interfaces are fully bonded, fully debonded, or precracked
because the interfacial delamination criterion is inherently
included in the traction–separation law. Thus, it can
capture and predict both the onset and propagation of
interfacial delamination during a wedge indentation pro-
cess. Most of these works, however, were limited in the
two-dimensional (2D) simulation of indentations. In fact,
the mechanics of indentation may be in a three-dimen-
sional (3D) stress state unless the indenter is long enough
compared to the other characteristic system dimensions,
such as the film dimension or indentation depth.
On the other hand, recent experiments by Yeap
et al.18,19 on continuous film [BlackDiamond (BD) film
on Si substrate] have showed that the stress state near the
ends of the wedge indenter in the length direction (hereafter
refers to the “end of the wedge indenter”) changes from
a plane strain condition to a 3D strain status, and the contour
of the interfacial crack front also changes gradually from
a narrow strip shape to an elliptic shape as the film thickness
or indentation depth increases. It is known that the growth
contour of the interfacial crack should be a straight line if
the indentation is in the plane strain state. The appearance of
the elliptical-shaped contour of the interfacial crack indi-
cates that the wedge indentation is in 3D stress state.
Therefore, it is necessary to perform 3D FEM modeling
of interfacial delamination by wedge indentation to interpret
experimental phenomena or determine the interfacial prop-
erties. Recently, She et al.26 conducted a 3D FEM simula-
tion to study the interface cracking of a ductile thin film
subjected to wedge indentation. Their work only focused on
the effect of the length of the wedge indenter on interfacial
crack shapes and stress states under different indentation
depths, whereas the film thickness was fixed. Moreover, the
2512 J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
http://journals.cambridge.org Downloaded: 04 Feb 2015
evaluation of the stress states during indentation was based
on the value of hardness calculated by using the Oliver and
Pharr’s27 method; however, the hardness values are not
directly related to the interfacial delamination process, in
addition, the hardness values from wedge indentation are
not well-defined as the indenter shape is difficult to be
determined for wedge indentations. Furthermore, a thorough
comparison between the simulation and experimental
results has not been done in the work by She et al.26
Following the previous works,18–20,26 this study further
investigates the effects of wedge indentation length and film
thickness to the stress states of the wedge indentation-induced
interfacial delamination in a soft-film-on-hard-substrate
(SFHS) system using the 3D FEM simulation, and followed
by a detailed comparison with the experimental results. To
compare with the experimental results, the simulation in this
work specifically uses the properties of the BD-film/Si-
substrate systems. Different from the previous work by She
et al.,26 the effects of both the wedge indenter length and
the film thickness on the interface delamination processes are
analyzed. It is shown that a 2D to 3D transition of stress states
occurs depending on the ratio of indenter length to film
thickness. Furthermore, the interfacial delamination process
by wedge indentations is also studied experimentally with
the wedge indenters of different lengths as well as the
samples with different film thicknesses, and the results from
simulations are found to be in good agreement with the
experimental results. Compared to the evaluation of stress
states by hardness values,26 a more straightforward criterion
based on the curvature of the delamination crack front is
introduced to indicate the transition of stress states during the
interfacial delamination. Finally, a guideline was therefore
proposed to classify the 2D and 3D stress states for extracting
the interface adhesion properties.
II. COMPUTATIONAL MODEL
A. Cohesive zone model
A cohesive zone model28 is used to simulate the
interfacial delamination process during wedge indentation.
A single mode traction–separation law is first introduced
[Fig. 1(a)], and d1, d2, and d3 are the separations in the
normal, first, and second shear directions, respectively.
Likewise, t1, t2, and t3 are the tractions in these three
directions. t10 , t20 , and t30 represent the peak values of
tractions, i.e., strengths, when the separation is either purely
normal to the interface or purely in the first or second shear
direction. d01 5 t10 =K, d02 5 t20 =K, and d03 5 t30 =K are the
quantities that represent the critical separations at the onset
of delamination in these three single mode conditions,
where K is “penalty stiffness.” The area under the single
mode traction–separation curve, corresponding to the re-
spective (Mode I, II, or III) fracture toughness (GIC, GIIC,
and GIIIC, respectively), defines the final separations, df1 , df2 ,
and df3 corresponding to complete failure.
IP address: 129.93.16.3
 L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system

However, the wedge indentation problem requires the mixed-mode separation corresponding to damage initi-
a mixed-mode implementation of this cohesive model. ation and total failure, respectively, and dmax
m is the maximum
Therefore, the traction–separation law proposed by mixed-mode separation during the loading or unloading
Tvergaard and Hutchinson24,25 is used to combine the process. The Macauley operator〈〉is defined as:
normal and shear displacements into a single parameter for 
0; x , 0
the mixed-mode effects. As shown in Fig. 1(b), the total Æxæ 5 : ð4Þ
mixed-mode separation, dm, is given by: x; x $ 0

dm 5 ðd21 þ d22 þ d23 Þ1=2 : ð1Þ It should be noted that if the maximum mixed-mode
separation meets the condition of d0m . dmax
m , the traction–
The constitutive equation for mixed-mode loading is separation law remains reversible. Nevertheless, for
defined as: d0m , dmax
m , an irreversible unloading path is used so that
unloading occurs linearly toward the origin of the traction–
ts 5 Dsr dr ; s;r 5 1; 2; 3 ; ð2Þ separation plane [Fig. 1(b)].24,25
The maximum nominal stress failure criterion29 is used
where Dsr is the damaged elasticity matrix, which has the to predict the onset of delamination. Due to the fact that the
form: compressive normal tractions do not affect the onset of
8 delamination, it can be expressed as:
>
> 
dsr K dmax # d0m  
>
< h i m Æt1 æ t2 t3
Dsr 5 dsr ð1  dÞK þ Æd 1æ 
d0m , dmax max o ; o ; o 5 1 : ð5Þ
f
d1 ds1 dK m , dm
>
>
t1 t2 t3
>
: ;
ds1 
d1r Æd 1æ
d1 K dmax
m $ dm
f
Assuming interfacial strength, rs 5 t1o 5 t2o 5 t3o , Eq. (5)
dfm ðdmax
m  dm Þ
0
ð3Þ
can also be written as:
d5 ; d 2 ½0; 1
dmax f
m ðd m  dm Þ
0
maxfÆt1 æ; t2 ; t3 g 5 rs : ð6Þ

where  dsr is the Kronecker delta function, K is the “penalty In addition, a linear failure criterion is used to predict
stiffness,” d is the damage evolution function, d0m and dfm are delamination propagation under mixed-mode loading as:
GI GII GIII
þ þ 51 : ð7Þ
GIC GIIC GIIIC

Assuming interfacial energy (toughness), C0 5 GIC 5

GIIC 5 GIIIC, we have:
GI þ GII þ GIII 5 C0 ; ð8Þ

where the quantities GI, GII, and GIII refer to the work
done by the traction and its conjugate separation in the
normal, first, and second shear directions, respectively.

B. Model description
Considering a wedge indentation of a typical film–
substrate system, as illustrated in Fig. 2, the indenter is
a wedge-shaped tip with an inclusion angle, 2h; and the
wedge length is 2Wmi. Due to its symmetry along the
y-axis and x-axis, only a quarter of the system is modeled
in the 3D simulations. The boundary conditions applied to
the system are such that:

ux ð0; y; zÞ 5 0
uy ðx; 0; zÞ 5 0 ; ð9Þ
uz ðx; y; 0Þ 5 0
FIG. 1. Schematic diagram showing the traction–separation law used for
finite element (FEM) simulation: (a) single mode; (b) mixed mode.

J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011 2513
http://journals.cambridge.org Downloaded: 04 Feb 2015 IP address: 129.93.16.3
L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system
where ui (i 5 x, y, z) is the displacement in the x, y, or z
directions. Loading is imposed to the indenter under
displacement-controlled conditions as:
uz ðx; y; zÞ 5  h ; ð10Þ
where h is the indentation depth, which is to be at
maximum of 1.0 time of the film thickness.
In this simulation, all the parameters in the length scales
are normalized by a length, D0 5 1lm, for convenience.
The geometric values (Fig. 2) are chosen as following: the
thickness of substrate is hs 5 4 D0, and the width of the
system is taken to be Wfs 5 10 D0. To capture the 2D to 3D
stress state transition, the thickness of film hf and the length
of wedge intender Wmi are varied as: hf / D0 5 0.1, 0.3, 0.5,
0.7, 1.0 and Wmi / D0 5 0.5, 1.0, 2.0, 3.62, respectively. For
simplicity, the wedge indenters are assumed to be rigid
bodies with an inclusion angle of 2h 5 120°.
Both thin film and substrate are considered to be
isotropic and are modeled as elastoplastic materials based
on J2 theory, and the stress–strain relation is:
 strength of the film and the length scale.
r=E r # ry
e5   1=N ; ð11Þ
ry =E r=ry r . ry
where ry is the yield strength, and N is the strain hardening
exponent. In this article, we only present the simulations
for the thin film of which elastic modulus, hardness, and
yield strength are lower than those of the substrate, known
as SFHS system. In this way, as the yield strength of
substrate is very high, during the simulation, the substrate
almost deforms elastically and nearly no plastic deforma-
tion occurs in substrate. These conditions are based on the
experimental observation reported earlier.18,19 The prop-
FIG. 2. Schematic diagram showing the geometries and material
parameters of the wedge indentation on a film/substrate system. The
coordination system is indicated in the diagram, and h denotes the
indentation depth.
2514 J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
http://journals.cambridge.org Downloaded: 04 Feb 2015
erties of low-k film (BD)18,19 are used as film properties,
and its elastic modulus and hardness can be determined by
a normal indentation with standard Berkovich indenter tip,
which will be described in detail in “Experimental pro-
cedure.” However, the yield strength and strain hardening
exponent cannot be determined directly from the indenta-
tion experiment. Therefore, Johnson’s analysis30 was used
to estimate the yield strength after acquiring the elastic
modulus and hardness of the film, and the values of yield
strength and strain hardening exponent can be adjusted by
matching the simulation and experiment curves before
the onset of interfacial delamination.20 The substrate is
assumed with the properties same as those of silicon, and
the yield strength of the substrate is estimated from its
hardness values. The detailed material parameters are
tabulated in Table I.
The interface adhesion properties are determined from
the interface energy–strength contour developed in an earlier
study20; these values are: the interfacial strength of rs / ryf 5
0.5 and the interfacial energy value of C0 / ryfD0 5 0.006,
again, the interfacial properties are normalized by the yield
The 3D FEM simulations are performed with displace-
ment control using the commercial software ABAQUS.
The interface is modeled with 3D cohesive elements with
six nodes and three integration points (COH3D6); and the
film and substrate are modeled with four-node linear
tetrahedron elements (C3D4). The sizes of the elements
within the indentation contact area are refined carefully
because of the strong stress gradient and difficult con-
vergence. The detailed FEM model is shown in Fig. 3. To
accommodate the stress gradient and requirement of
convergence, the size of the minimum elements in the
film, he, near the end of the wedge tip is set to be lower than
0.02 times the length scale D0 5 1 lm, and he increases
with the distance from the indenter with a ratio 5.0 in the
x-direction and 10.0 in the y-direction and z-direction. The
radius rmi of the chamfer curve of the indenter is artificially
set as rmi / D0 5 0.05. Each FEM model contains at least
83,658 elements and 15,555 nodes. The validation and
convergence of the mesh size described above have been
confirmed in the simulations.
The master-slave contact mechanism is applied be-
tween the wedge indenter and the film. Friction is not
considered, and small sliding conditions are adapted. The
contact algorithm used in this analysis is augmented
Lagrange method. The maximum indentation depth during
simulation is kept less than the film thickness. In this
simulation, the piling-up and the sinking-in during the
indentation on soft films are not considered for simplicity.
In addition, residual stress in the film and film radial cracks
are not included. As it will be discussed later in this article,
the film radial crack affects the delamination crack shape
only near the two ends of the wedge indenter, and the crack
front shape is not affected by the radial crack in the films.
IP address: 129.93.16.3
 L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system
TABLE I. Material properties of film and substrate used for simulation.
E (GPa) Poisson’s ratio, v
BD 12.6 0.34
Substrate 112.4 0.28
BD, BlackDiamond.
FIG. 3. The three-dimensional (3D) FEM mesh used in the simulations.
III. EXPERIMENTAL PROCEDURE
The BD films investigated by wedge indentation experi-
ments have various thicknesses of 100, 300, 500, 700,
1000, and 1200 nm, respectively. To study the interfacial
delamination process, wedge indentation experiments are
conducted by using diamond wedge tips with 120° in-
cluded angle and two wedge lengths of l 5 2Wmi 5 4.06 lm
and l 5 2Wmi 5 7.24 lm using a commercial nanoindenter
machine (UMIS-2000H; CSIRO, Sydney, Australia). The
lengths of the wedge tips were measured from scanning
electron microscope images. The indentation test consists of
three segments: (i) loading to the predefined maximum load
in 20 s, (ii) holding at the maximum load for 5 s, and
(iii) unloading to 30% of the maximum load in 20 s. For
every case, 20 indentation tests are performed at the
indentation load, which leads to the interface crack kinking
to the film surface.18,19 Field-emission scanning electron
microscopy (FESEM) (JEOL JSM-5700F; JEOL Corpora-
tion, Tokyo, Japan) is used to capture the plane view images
of the delaminated area. In addition, an FIB (Quanta 2003D;
FEI Company, Hillsboro, OR) is used to make cross-
sectional cuts at the middle of the wedge indentation
impression to view the interfacial delamination profile
(not shown in this article). The details of experiments and
analyses are presented earlier.18,19
J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
http://journals.cambridge.org Downloaded: 04 Feb 2015
Yield strength, ry (GPa) Strain hardening exponent, N
1.47 0.25
4.70 0.25
IV. RESULTS AND DISCUSSION
A. Computational predictions
1. Basic model behavior
In view of simulating the interfacial delamination
processes induced by a wedge indentation, 2D plane
strain models have been well established earlier.20–23
However, generally speaking, the wedge indentation
induces a 3D stress state unless the indenter is long enough
compared to the other characteristic lengths, such as the
film dimension and the indentation depth.
In this study, 3D stress state is modeled with the length
of the wedge tip less than the width of the sample (Fig. 2),
i.e., Wmi , Wfs. For comparison, 2D plane strain models
are also modeled with the length of the wedge tip greater
than or equal to the width of the sample, i.e., Wmi $ Wfs.
Figure 4 compares the indentation deformations, film
buckling, and interface crack profile for the SFHS system
under both the 2D plane strain condition (Wmi 5 Wfs) and
3D stress state condition (Wmi 5 0.2Wfs 5 2D0; other
parameters were described in “Model description” at the
indentation depth of h 5 0.8hf, where the film thickness is
hf 5 0.5D0. In both cases, the interfacial properties are
taken to be the same as rs / ryf 5 0.5 and C0 / (ryfD0) 5
0.006. To better show the difference of crack profiles in the
2515
IP address: 129.93.16.3
L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system
y-direction (Fig. 2) between the 2D and 3D models, the
crack line path under 2D plane strain condition is extruded
along the y-axis to the area crack profile as shown on the
right side in Fig. 4(a). It appears that during indentation, as
the indentation depth increases, the stress in the x-direction
rxx (Fig. 2) induced by the indenter simultaneously
increases, causing a large displacement in the x-direction
within the film. Meanwhile, the deformation within the
substrate remains small and cannot accommodate this
large deformation. The mismatch between substrate and
film deformation leads to the interfacial crack propagation
in the x-direction. When rxx exceeds a critical value,
buckling occurs and the film lifts off from the substrate.
For the 2D plane strain case, the rxx is nearly the same along
the y-direction (Fig. 2). As a consequence, the crack front is
almost parallel to y-axis as shown in Fig. 4(a). Note that the
crack front contours are obtained when the damage evolu-
tion function in Eq. (3) is unit (d 5 1), which also means:
!1=2
dmax
m d21 d22 d23
5 þ þ 51 : ð12Þ
dfm ðdfm Þ2 ðdfm Þ2 ðdfm Þ2
On the other hand, the 3D case possesses nonuniform
distribution of the resistance to interfacial delamination
along the y-direction. In this simulation, the resistance to
interfacial delamination includes two parts: the plastic
dissipation and the interfacial toughness (cohesive en-
ergy). As shown in Fig. 4(c), higher plastic strain is
observed in the region at the “end of wedge indenter.”
This means more plastic dissipation is required in this
region. Although we assume the cohesive energy is the
same everywhere during the simulation, the resistance to
interfacial delamination at the “end of wedge indenter” is
larger than that along the side of the indentation. There-
fore, the growth of crack front at the end of indenter is
slower, and the crack front is not straight-sided but
elliptical in shape as plotted in Fig. 4(b). Similar results
were also observed in earlier experimental works.18,19
2. Effects of indenter length and film thickness
It is known that the global behavior of interfacial
delamination process during wedge indentation can be
depicted from the characteristics of the indentation load–
displacement (P–h) curve. Thus, the effects of indenter
length and film thickness on the P–h curves are system-
atically investigated in this study.
a. Effect of indenter length
Figure 5 shows the P–h curves as the function of the
indenter lengths of Wmi / D0 5 0.5, 1.0, 2.0, and 3.62. It is
found that while increasing the indenter length Wmi / D0,
the corresponding P–h curve gradually approaches the
case of 2D plane strain condition for a given indentation
2516 J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
http://journals.cambridge.org Downloaded: 04 Feb 2015
depth. This observation indicates that the indenter length is
one of the key parameters controlling the 2D to 3D
transition of stress states. It is also noted that if the indenter
length is shorter, the critical indentation depth at the onset
of the interfacial delamination becomes deeper, and the
corresponding indentation load is higher. Therefore, when
comparing the 2D FEM simulation results with the wedge
indentation experiments, if the wedge tip used in experi-
ments is not long enough (3D), then for the given
interfacial properties, the 2D simulated critical indentation
load will be lower than the experimentally measured one
(3D) as indicated in Fig. 5. On the other hand, at a given
critical load, the interfacial properties determined from the
simulation will be higher than the experimentally deter-
mined values. These are consistent with previous 2D FEM
simulation results.20 One of the possible reasons for this is
the energy consumption, i.e., the resistance to interfacial
delamination at the two ends of the indenter is larger than
that at the side of the indentation impression as stated in
“Basic model behavior.” It is easily understood that the
energy consumption at the ends of indenter accounts for
higher percentage with decreasing the length of the in-
denter. Hence, the shorter indenter will cause a delay in the
interface delamination, and the overall indentation load will
increase with decreasing the length of the indenter.
b. Effect of film thickness
The P–h curves have also been obtained by solely
varying the thicknesses of the film from hf / D0 5 0.3, 0.5
to 0.7 as shown in Fig. 6. It is found that an increase in film
thickness increases both critical indentation load and
indentation depth for the onset of delamination. This
means that it requires a large driving force to initiate the
delamination for thicker film. One likely explanation for
this characteristic is that the thicker film may serve as
a buffer layer, which reduces the driving force and
therefore delays the delamination, resulting in an increase
in both critical indentation load and depth.
It is worthwhile noting that by comparing Figs. 5 and 6,
it is found that the decrease of indenter length and the
increase of film thickness lead to the same directional
change of the P–h curves, i.e., the increase of critical
indentation depth and load for delamination. Since the
dimension of the specimen is infinite compared to the film
thickness and indenter length, it is reasonable to conclude
that in addition to the effects on the P–h curves, decreasing
indenter length and increasing film thickness have the
same effects on the whole interfacial delamination pro-
cess, including the delamination crack shapes and stress
states, and thus the film thickness can be considered as
another key parameter that dictates the 2D to 3D transition
of stress states during wedge indentation.
For axisymmetrical indentations, it is common to use
the ratio of the contact radius to film thickness. As
IP address: 129.93.16.3
 L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system

FIG. 4. The film deformations and crack front profiles with rs / ryf 5 0.5, C0 / (ryfD0) 5 0.006, Wmi / D0 5 2.0, and hf / D0 5 0.5 at indentation depth
of h 5 0.8hf: (a) two-dimensional (2D) plane strain condition with Wmi 5 Wfs; (b) 3D stress state with Wmi , Wfs; and (c) distribution of plastic strain
in the region near the indenter.

mentioned in “Computational model,” the pile-up or sink-
in during indentations is not considered in the present
FEM models. Accordingly, the contact radius a can be
readily estimated by the indentation depth, h and half of
the inclusion angle for wedge indenter tip, h (Fig. 2):
a 5 h tan h : ð13Þ
In that case, the ratio of contact radius to film thickness
can be expressed as:
a=hf 5 ðh=hf Þ tan h : ð14Þ
However, this ratio is only useful for 2D cases, i.e., in
the section normal to the length of the wedge indentation
impression, it does not, however, reflect what happened
along the length direction of the wedge indentation. Also,
for thin film system, this ratio may break down if the
contact radius is larger than film thickness. Therefore, in
this article, for the 3D analysis, we utilize the ratio of
indentation depth to film thickness instead of the ratio of
contact radius to film thickness with consideration of the
fixed value of h in Eq. (14).
B. Comparison between computations
and experiments
As discussed earlier, the 3D case of interfacial delami-
nation possesses an elliptical-shaped crack profile; therefore,
the indenter length and the film thickness are the two key

J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011 2517
http://journals.cambridge.org Downloaded: 04 Feb 2015 IP address: 129.93.16.3
L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system
FIG. 5. Indentation load–depth curves for a range of wedge indenter
lengths with a fixed film thickness of hf / D0 5 0.5.
FIG. 6. Indentation load–depth curves for a range of film thicknesses
with a fixed wedge indenter length of Wmi / D0 5 2.0.
dimensional parameters affecting the delamination crack
shapes and stress states. Therefore, the effects of those two
parameters on crack profile shape are investigated in this
simulation with the indenter length values of Wmi / D0 5
0.5, 1.0, 2.0, and 3.62 and film thickness in the range of
hf / D0 5 0.1, 0.3, 0.5, and 1.0. To compare with the
simulation results, a series of wedge indentation experiments
using the wedge tips with the lengths of l 5 4.06 and 7.24 lm
on the samples with the film thicknesses of 100, 300, 500,
and 1000 nm are conducted. Due to l 5 2Wmi, for the cases
with l 5 7.24 lm in experiments, the corresponding indenter
length in computation is Wmi 5 3.62D0 5 3.62 lm; likewise,
for l 5 4.06 lm in experiments, Wmi 5 2D0 5 2.0 lm.
Figure 7 superimposes the computational crack front profiles
on the FESEM plane view images of the experimental crack
profiles resulting from the wedge indentations with the two
wedge lengths on the sample with the film thickness of
300 nm. It can be easily noticed that the crack front profiles
2518 J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
http://journals.cambridge.org Downloaded: 04 Feb 2015
from computational simulation and experimental studies are
matched very well for most part of the crack front except the
delaminated region near the “end of the indentation impres-
sion.” This discrepancy is most likely due to the fact that the
crack propagation is not stable during the initial stage of
delamination, which just corresponds to the delaminated
region near indenter, as reported by Hutchinson and Suo.31
Another possible reason for this discrepancy is that the FEM
model does not account for the radial cracks near the ends of
the indenters, whereas the experiments clearly show the
cracks in these positions. Despite these, the shapes of crack
front profiles in experimental studies and computational
simulation follow the similar trend with the changes of the
indenter length, i.e., the longer indenter (l 5 7.24 lm) results
in a relatively straight-sided crack front and the shorter
indenter (l 5 4.06 lm) results in a more curved crack front.
Following this comparison, the computational and ex-
perimental crack front profiles are further compared on the
samples with different film thicknesses at a constant wedge
length of l 5 4.06 lm, and the results are shown in Fig. 8.
Again, the experimental crack front profiles are found to be
nearly identical to the computational ones except the small
region near the end of the indenter. In addition, the
numerical and experimental crack front profiles also yield
the same trend, i.e., the higher film thickness corresponds to
the more curved profile, and vice versa.
C. Stress state of interfacial delamination
1. A curvature-based criterion
In this study, we define the stress state as 2D when the
crack front is more or less straight and as 3D stress when
the crack front is curved. Therefore, the changes of crack
front from straight side to curved side indicate the changes
of stress state from 2D to 3D. To quantitatively investigate
this transition of stress states, the curvatures of the crack
front profiles are calculated with the following approaches.
First, all the points along the front of the delamination
crack and the corresponding coordinates are exported from
the FEM simulation or experimental results, and then
the commercial software (Matlab 7.0) is used to fit the
delamination crack front with a function, f(x). For the
purpose of low error, two kinds of fitting function are
utilized as shown in Fig. 9: (i) a ninth-order polynomial
function y 5 f (x) 5 a0 + a1x +. . .a9x9 for the relatively
straight crack front and (ii) an elliptical function
2 2
f ðxÞ5 ax2 þ by2 for the curved crack front. The curvature of
interfacial crack front, j, can then be determined using:
f 0ðxÞ
j5 h i3=2 : ð15Þ
1 þ ðf 9ðxÞÞ2
Based on Eq. (13), the lower curvature indicates that the
crack front is more close to the straight-sided shape with
IP address: 129.93.16.3
 L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system

FIG. 7. Comparison of crack front profiles from the experiments and simulations for the wedge indentations with two different lengths of the wedge
indenter tips on the same film.

FIG. 8. Comparison of crack front profiles from the experiments and simulations for different film thicknesses with the same wedge indenter tip.

FIG. 9. Schematic diagram showing the curve fitting for the crack front profiles.

J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011 2519
http://journals.cambridge.org Downloaded: 04 Feb 2015 IP address: 129.93.16.3
L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system
FIG. 10. The crack front contours at different normalized indentation
depths, h / hf.
FIG. 11. The curvature of crack front versus normalized indentation
depth at different lengths of the wedge indenter tips.
curvature of 0, i.e., the 2D plane strain solution and the
higher curvature approaches the curved shape or is
dominated by 3D stress state.
It is worth to mention here that the crack front is relatively
straight at the initial stage of crack growth as plotted in
Fig. 10, indicating that the state of crack growth is pre-
dominantly in the 2D plane strain condition at the beginning
of the delamination, whereas the straight front becomes
curved with further indentation and crack growth, indicating
the 3D stress state. Figure 11 shows the variations of the crack
front curvature, j, versus the normalized indentation depth,
h / hf, at different indenter lengths Wmi / D0 5 0.5, 1.0, 2.0,
and 3.62. It can be observed that for all the indenter lengths
used, as the indentation depth increases, the curvature, j,
2520 J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
http://journals.cambridge.org Downloaded: 04 Feb 2015
FIG. 12. The curvature of crack front versus normalized indentation
depth for the thin films with different film thicknesses.
FIG. 13. The curvature of crack front versus ratio of wedge tip length
to film thickness.
increases significantly at the initial stage of delamination.
When j reaches a certain value js, it becomes nearly
unchanged and stable. For example, at Wmi / D0 5 0.5, when
the curvature, j, reaches the value of 0.96 at h/hf ; 0.65, little
change is observed by further increasing the indentation
depth, i.e., js 5 0.96 (Fig. 11). These observations are
consistent with the findings of Hutchinson and Suo,31 i.e.,
steady-state conditions are reached when the dimensions of
interfacial crack significantly exceed the thickness of film.
Furthermore, effects of indenter lengths are investi-
gated, and the results on crack front curvature are shown
in Fig. 11. It is obvious that with the increase in indenter
lengths, the crack front curvature markedly decreases,
IP address: 129.93.16.3
 L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system

TABLE II. The interfacial crack front’s stress–strain conditions of BD/ and film thicknesses are simulated, and the variations of
Si systems in the experiments. the crack front curvature, j, with the ratio of two times of
The ratio of wedge indenter length to film thickness, 2Wmi / hf, are
Wedge BD film wedge length shown in Fig. 13 (the wedge indenter length in experiment
length, thickness, and film thickness, Stress–strain is two times of that in computational model, i.e., l 5 2Wmi,
l (lm) hf (nm) l / hf condition thus 2Wmi / h f or l / h f is used here for the comparison in
4.055 100 40.55 Plane strain “Comparison between computations and experiments”). On
7.240 300 24.13 Transition the basis of the above analysis, the crack front curvatures
7.240 500 14.48 Transition after delamination becomes stable, and the value of js is
4.055 300 13.52 Transition
7.240 700 10.34 Nonplane strain
calculated and compared. For convenience, js, however, is
4.055 500 8.11 Nonplane strain still denoted as j in Fig. 13, and it is clear that the crack front
7.240 1200 6.03 Nonplane strain curvature is found to decrease exponentially as the ratio of
4.055 1000 4.055 Nonplane strain wedge indenter length to film thickness increases.
The curvatures of crack front in experiments are also
computed by Eq. (13) and listed in Table II. For this
purpose, the FESEM plane view image of a wedge in-
dentation impression is first plotted in a transparent grid
paper, and the center of the wedge indentation impression
is then defined as the origin of the coordination. In this
way, the coordinates of the crack front points (more than
30 points for one crack front) can be obtained.
The measured curvatures are also compared with the
computational values to further confirm that the FEM
simulation can accurately determine the stress state
during interfacial delamination. Similar to the simulation,
the measured curvature, j, is also plotted as the function
of the ratio of indenter length to film thickness l / hf as
shown in Fig. 14. It is found that both the measured and
simulated curvatures are comparable and approximately
the same in magnitude if l / hf . 7. However, some
differences exist if l / hf , 7. These differences may be due
to the discrepancy of computational and experimental
crack front profiles for the delaminated region near the end
FIG. 14. Comparison of curvature of crack fronts from the experiments of the indentation impression, as discussed in “Compar-
and simulations versus ratio of wedge indenter length and film
thickness. ison between computations and experiments.” Another
possible reason for this difference is that the coordinates of
the points at crack front are obtained manually based on
especially for the case with Wmi / D0 5 3.62, the curvature the grid paper. This operation may introduce some errors
is lower than 0.1. However, the curvature is ;0.96 for the in the positions of crack front points and thus lead to the
case of Wmi / D0 5 0.5. The curvatures of crack front at the errors in the determination of the curvature.
fixed indenter length have also been compared by varying It is well known that when a curvature is lower than
the thin film thickness from hf / D0 5 0.1, 0.3, and 0.5 to 0.05, the curve can be considered as a straight line.32
1.0, and the results are shown in Fig. 12. On the contrary, Based on the qualitative comparison of the experimental
by increasing film thickness, the crack front curvature is observations and the FEM simulation (Fig. 14), it can be
significantly increased. Thus, it can be concluded that deduced that: (i) if l / hf . 40, the interfacial crack front is
increasing indenter length and increasing film thickness under plane strain condition; (ii) if 40 . l / hf . 20, the
lead to the opposite effects on the crack front curvatures or interfacial crack front is under the transition from plane
changes of the stress states, as discussed in “Effects of strain to nonplane strain condition; and (iii) for 1 / hf , 20,
indenter length and film thickness.” the interfacial crack front is under nonplane strain condi-
tion. It is, therefore, noted that if the 2D simulation is used
to extract the interfacial adhesion properties of thin film–
2. A guideline of stress state for extracting substrate systems under wedge indentation,20,21 the ge-
interfacial adhesion properties ometries of wedge indenter and film–substrate systems
To combine the effects of the indenter length and the should fulfill the ratio of 1 / hf . 40 to achieve the 2D
film thickness, more cases with different indenter lengths stress state in the wedge indentation experiments.

J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011 2521
http://journals.cambridge.org Downloaded: 04 Feb 2015 IP address: 129.93.16.3
L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system
V. CONCLUSIONS
In this article, the wedge indentation-induced interfa-
cial delamination in an SFHS system is systematically
investigated using both 2D and 3D FEM simulations, and
the results of the simulation and experiment are com-
pared. In the simulation, a traction–separation law is used
to describe the interface failure behavior. The effects of the
wedge indenter length and the film thickness on the onset
and growth of interface delamination are analyzed. Para-
metric studies for curvatures of crack fronts show that a 2D
to 3D transition of stress states occurs depending on the
ratio of indenter length to film thickness. On the other
hand, the interfacial delamination process by wedge
indentation is also conducted experimentally for different
indenter lengths and film thicknesses, and the curvatures
of delamination crack front are measured to compare with
the computationally derived transition of stress states. The
results from simulations show good agreement with those
obtained in the indentation experiments. Based on the
qualitative comparison of the experimental observations
and computations, it is found that the ratio of wedge length
to film thickness should be larger than 40 (l/hf . 40) to
achieve 2D plane strain condition, and a guideline is
proposed to classify the 2D to 3D transition for extracting
the interface adhesion properties.
This work proposes a criterion based on the curvature of
the delamination crack front, and the stress states are
evaluated by the shapes of the interfacial crack. It is
expected that this method can be used to solve the
delamination problems in a wider range of thin film
systems, e.g., hard, stiff films on soft, compliant substrates.
A recent work has showed that the substrate deformation
could play a more significant role during the interfacial
delamination process for a hard-film-on-soft-substrate sys-
tem (RuO2 film on Si substrate)33; in addition, the substrate
cracking may occur if the indentation load is high. There-
fore, the proposed approach may need to be modified further
to consider the effect of substrate deformation or cracking,
when applied to hard-film-soft-substrate systems, which
will be studied and presented in a forthcoming contribution.
ACKNOWLEDGMENTS
This work is supported by National University of
Singapore under Academic Research Funds (R265-000-
190-112 and R265-000-190-133) and National Natural
Science Foundation of China (No. 50805079).
REFERENCES
1. J. Malzbender, J.M.J. den Toonder, A.R. Balkenende, and G. de
With: Measuring mechanical properties of coatings: A methodol-
ogy applied to nano-particle-filled sol-gel coatings on glass. Mater.
Sci. Eng., R 36, 47 (2002).
2522 J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
http://journals.cambridge.org Downloaded: 04 Feb 2015
2. M.D. Kriese, D.A. Boismier, N.R. Moody, and W.W. Gerberich:
Nanomechanical fracture-testing of thin films. Eng. Fract. Mech.
61, 1 (1998).
3. Y.G. Wei and J.W. Hutchinson: Mixed-mode fracture analyses of
plastically-deforming adhesive joints. Int. J. Fract. 93, 315 (1998).
4. M. Lane: Interface fracture. Annu. Rev. Mater. Res. 33, 29 (2003).
5. A.A. Volinsky and W.W. Gerberich: Nanoindentaion techniques
for assessing mechanical reliability at the nano-scale. Microelectron.
Eng. 69, 519 (2003).
6. M.D. Kriese, W.W. Gerberich, and N.R. Moody: Quantitative
adhesion measures of multilayer films: Part I. Indentation mechan-
ics. J. Mater. Res. 14, 3007 (1999).
7. M.D. Kriese, W.W. Gerberich, and N.R. Moody: Quantitative
adhesion measures of multilayer films: Part II. Indentation of
W/Cu, W/W, Cr/W. J. Mater. Res. 14, 3019 (1999).
8. X. Li and B. Bhushan: A review of nanoindentation continuous
stiffness measurement technique and its applications. Mater.
Charact. 48, 11 (2002).
9. D.B. Marshall and A.G. Evans: Measurement of adherence of
residually stressed thin films by indentation. I. Mechanics of
interface delamination. J. Appl. Phys. 56, 2632 (1984).
10. M.V. Swain and J. Men
cik: Mechanical property characterization
of thin films using spherical tipped indenters. Thin Solid Films 253,
204 (1994).
11. A.A. Volinsky, N.R. Moody, and W.W. Gerberich: Interfacial
toughness measurements for thin films on substrates. Acta Mater.
50, 441 (2002).
12. A.A. Volinsky, J.B. Vella, and W.W. Gerberich: Fracture toughness,
adhesion and mechanical properties of low-k dielectric thin films
measured by nanoindentation. Thin Solid Films 429, 201 (2003).
13. M.R. Begley, D.R. Mumm, A.G. Evans, and J.W. Hutchinson:
Analysis of a wedge impression test for measuring the interface
toughness between films/coatings and ductile substrates. Acta
Mater. 48, 3211 (2000).
14. M.P. De Boer and W.W. Gerberich: Microwedge indentation of the
thin film fine line-I. Mechanics. Acta Mater. 44, 3169 (1996).
15. M.P. De Boer and W.W. Gerberich: Microwedge indentation of the
thin film fine line-II. Experiment. Acta Mater. 44, 3177 (1996).
16. M.D. Drory and J.W. Hutchinson: Measurement of the adhesion of
a brittle film on a ductile substrate by indentation. Proc. R. Soc.
Lond., Ser. A 452, 2319 (1996).
17. J.J. Vlassak, M.D. Drory, and W.D. Nix: A simple technique for
measuring the adhesion of brittle films to ductile substrates with
application to diamond-coated titanium. J. Mater. Res. 12, 1900 (1997).
18. K.B. Yeap, K.Y. Zeng, H.Y. Jiang, L. Shen, and D.Z. Chi:
Determining interfacial properties of submicron low-k films on Si
substrate by using wedge indentation technique. J. Appl. Phys. 101,
123531 (2007).
19. K.B. Yeap, K.Y. Zeng, and D.Z. Chi: Determining the interfacial
toughness of low-k films on Si substrate by wedge indentation:
Further studies. Acta Mater. 56, 977 (2008).
20. L. Chen, K.B. Yeap, K.Y. Zeng, and G.R. Liu: Finite element
simulation and experimental determination of interfacial adhesion
properties by wedge indentation. Philos. Mag. 89, 1395 (2009).
21. W.Z. Li and T. Siegmund: An analysis of the indentation test to
determine the interface toughness in a weakly bonded thin film
coating substrate system. Acta Mater. 52, 2989 (2004).
22. Y.W. Zhang, K.Y. Zeng, and R. Thampurun: Interfacial delamina-
tion generated by indentation in thin film systems—a computational
mechanics study. Mater. Sci. Eng., A 319, 893 (2001).
23. M. Schulze and W.D. Nix: Finite element analysis of the wedge
delamination test. Int. J. Solids Struct. 37, 1045 (2000).
24. V. Tvergaard and J.W. Hutchinson: Toughness of an interface
along a thin ductile layer joining elastic solids. Philos. Mag. 89, 641
(1994).
IP address: 129.93.16.3
 L. Chen et al.: Interfacial delamination cracking shapes and stress states during wedge indentation in a soft-film-on-hard-substrate system
25. V. Tvergaard and J.W. Hutchinson: Effect of strain-dependent
cohesive zone model on predictions of crack growth resistance. Int.
J. Solids Struct. 33, 3297 (1996).
26. C.M. She, Y.W. Zhang, and K.Y. Zeng: A three-dimensional finite
element analysis of interface delamination in a ductile film/hard
substrate system induced by wedge indentation. Eng. Fract. Mech.
76, 2272 (2009).
27. W.C. Oliver and G.M. Pharr: An improved technique for determining
hardness and elastic modulus using load and displacement sensing
indentation experiments. J. Mater. Res. 7, 1564 (1992).
28. X.P. Xu and A. Needleman: Numerical simulations of fast crack
growth in brittle solids. J. Mech. Phys. Solids 42, 1397
(1994).
J. Mater. Res., Vol. 26, No. 19, Oct 14, 2011
http://journals.cambridge.org Downloaded: 04 Feb 2015
29. ABAQUS: User Manual, Version 6.9 (SIMULIA, Providence, RI,
2009).
30. K.L. Johnson: The correlation of indentation experiments. J. Mech.
Phys. Solids 18, 115 (1970).
31. J.W. Hutchinson and Z. Suo: Mixed mode cracking in layered
materials, in Advances in Applied Mechanics, Vol. 29, edited by
J.W. Hutchinsonand T.Y. Wu (Academic Press, Burlington, 1992),
pp. 63–191.
32. S. Kobayashi: Differential Geometry of Complex VectorBundles
(Princeton University Press, Princeton, NJ, 1987), p. 192.
33. J. Zhu, K.B. Yeap, K.Y. Zeng, and L. Lu: Nanomechanical
characterization of sputtered RuO2 thin film on silicon substrate
for solid state electronic devices. Thin Solid Films 519, 1914
(2011).
2523
IP address: 129.93.16.3