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Thin Solid Films 447 448 (2004) 399405

Finite element analysis of substrate effects on indentation behaviour of


thin films
Zhi-Hui Xu*, David Rowcliffe
Department of Materials Science and Engineering, Royal Institute of Technology, Stockholm S-100 44, Sweden

Abstract
The substrate effects on indentation behaviour of thin films are analysed using finite element (FE) method. There is no
universal critical penetration depth beyond which the substrate effects come in. The critical penetration depth is dependent on the
combination of the film and the substrate and more sensitive to differences in the elastic properties than in the plastic properties
of the filmysubstrate system. The FE simulation results of the effects of the substrate on the elastic modulus and the hardness of
the filmysubstrate system have also been compared with the empirical models of Doerner and Bhattacharya, respectively.
2003 Elsevier B.V. All rights reserved.
Keywords: Finite element method; Indentation; Thin films

1. Introduction
The rapid development and application of thin film
or coating technology requires an accurate measurement
of the mechanical properties of thin films. Nanoindentation is a popular technique used to evaluate the
mechanical properties of thin films due to its capability
of deforming materials on a very small scale and
measuring the mechanical properties in situ. When
determining the mechanical properties of thin films, it
is very important to distinguish the film properties from
the substrate effects. Basically, there are two ways to
determine the film properties without the influence of
the substrate. One is by making a shallow indentation
so that the substrate effects can be neglected. This
requires that the penetration should be kept within a
certain critical depth beyond which the influence of
substrate comes in. It is obvious that such an approach
may be only applicable to relatively thick films, e.g.
films with the thickness above micrometer. The other
way is by deriving the film properties through empirical
or analytical models. This approach is especially useful
for the cases where the film thickness is at the nanometer
level and it is unlikely that the effects of the substrate
can be avoided for such a thin film.
*Corresponding author. Tel.: q46-8-790-8340; fax: q46-8-10-0411.
E-mail address: zhihui@met.kth.se (Z.-H. Xu).

Various models have been developed to study substrate effects and derive film properties from the composite response of a filmysubstrate system. Theoretical
and empirical elastic analyses w15x of indentation on a
layered medium are available and can be used to
determine the elastic property of the film from the
composite properties of the filmysubstrate system, provided the mechanical properties of the substrate are
known. Similarly, the plastic properties of the film can
also be estimated using the empirical models based on
FE analyses w6x and rule of mixtures w710x. However,
a prerequisite of determining the film properties using
these models is that the mechanical properties of the
substrate must be known in advance.
Much research work has been done to investigate the
indentation behaviour of thin films and determine the
critical penetration depth. Once the critical penetration
depth is known, the mechanical properties can be simply
determined by making indentation within the critical
depth and no knowledge of the substrate properties is
needed. A well-known empirical rule for hardness measurement of hard films on soft substrates is that the
penetration depth should be smaller than one tenth of
the coating thickness in order to avoid substrate effects
w11x. However, this rule of thumb has been proven not
to be a universal law w1218x. For example, several FE
simulations of a conical indenter penetrating different
filmysubstrate systems show that, for a soft film on a
hard substrate, the critical penetration depth for hardness

0040-6090/04/$ - see front matter 2003 Elsevier B.V. All rights reserved.
doi:10.1016/S0040-6090(03)01071-X

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Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405

measurement may be approximately 30% w6x, 20% w12x


or 50% w13x of the coating thickness while for a hard
film on a soft substrate it may be 20% w6x, 15% w14x,
10% w15x, or 7% w16x of the coating thickness depending
on the combinations of the filmysubstrate systems. A
recent analysis of nanoindentation on both soft and hard
coatings also shows that the ratio of the critical penetration depth to the coating thickness for hardness measurement can be 20% for a gold film on a nickel substrate,
40% for an aluminium film on a glass substrate in the
soft coating cases w17x, and 20% for both a diamondlike carbon film on M2 steel substrate and an alumina
on a nickel substrate in the hard coating cases w18x. It
is obvious that the critical penetration depth depends on
the mechanical properties of both film and substrate,
such as, the ratio of the yield strength of substrate to
that of film, aYsss y sf, the ratio of the elastic modulus
of substrate to that of film, aEsEs yEf , and the indenter
geometry. Therefore, a systematic study of the influence
of aY and aE on the substrate effects would be very
helpful for determining the mechanical properties of
films.
In the present paper, FE method is employed to
investigate substrate effects on the measurement of the
mechanical properties of different combinations of thin
film systems, that is, the substrate is either plastically
harder or softer than the film or elastically stiffer or
weaker than the film.
2. Finite element modelling
In this study, nanoindentation of a layered sample by
a pyramidal indenter is simplified by the axisymmetric
indentation of a specimen with a thin film that is
perfectly adherent to a semi-infinite substrate by a rigid
conical indenter. The simulation has been carried out
using ABAQUS. The included half-tip angle of the
conical indenter is 70.38, which gives the same area
function as a Berkovich or Vickers indenter normally
used in experiments. A frictionless contact is defined
between the surface of the indenter and that of the
specimen. The thickness of the film, t, is 300 nm. The
size of the model is 38 000=30 000 nm with totally
3078 elements and 3178 nodes, which is large enough
to simulate the semi-infinite specimen. Roller boundary
conditions are applied on the axis of symmetry and the
bottom surface of the specimen separately. Since a large
local deformation occurs directly under the indenter,
very fine elements with the width from 5 to 20 nm are
employed in the contact region according to the penetration depths. This feature accurately accounts for the
pileup or sinking-in of the contact surface and consequently, accurately estimates the contact area of indentation. Farther away from that area, a progressive coarser
mesh is used.

The materials of the film and the substrate are


modelled as isotropic elastic-perfectly-plastic von Mises
solids. Constant Poissons ratios, nfsnss0.28, are used
for both film and substrate since the effect of Poisson
ratio on indentation is very small w19x. The mechanical
properties of the film are fixed with elastic modulus,
Efs100 GPa, and yielding strength, sfs1 GPa. By
changing the mechanical properties of the substrates,
various film and substrate combinations with different
aY and aE have been considered. The substrate can be
either stiffer (aE)1) or weaker (aE-1) than the film
depending on the value of aE, or it can be either harder
(aY)1) or softer (aY-1) than the film depending on
the value of aY.
The indentation process has been simulated by gradually applying a downward and an upward displacement
on the rigid indenter. At a given depth the corresponding
indentation load is determined directly from the reaction
force on the rigid indenter. The indentation hardness H
is determined by
Hs

Pmax
Ac

(1)

where Pmax is the maximum indentation load, Ac is the


projected contact area and Acspa2 for conical indenter,
a is the contact radius obtained directly by checking the
contact status of the nodes on the surface under the
maximum load. This allows the pileup or sinking-in
effect occurring at the surface to be taken into account.
The reduced modulus Er is calculated by
Ers

yp S

2 yAc

2
1 1yni2 1yncom
s
q
Er
Ei
Ecom

(2)

(3)

where S is the contact stiffness determined by a linearfitting of the initial part of the unloading curve, Ei and
ni are the elastic modulus and Poissons ratio of the
indenter, and Ecom and ncom are the composite elastic
modulus and Poissons ratio of the film and substrate
system.
3. Results and discussion
3.1. Substrate effects on the loadpenetration depth
curves
The loadpenetration depth curves of different filmy
substrate systems and the bulk film with 0.3t and 1.2t
penetrations are shown in Fig. 1. Fig. 1a shows the 0.3t
penetration curves of the elastically homogenous filmy

Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405

Fig. 1. Loadpenetration depth curves for different filmysubstrate systems and a bulk film with 0.3t and 1.2t penetration. (a) elastically
homogeneous filmysubstrate systems (aEs1) 0.3t penetration. (b)
elastically homogeneous filmysubstrate systems (aEs1) 1.2t penetration. (c) plastically homogeneous filmysubstrate systems (aYs1) 0.3t
penetration.

substrate system (aEs1) with different aY. As can be


seen, at very shallow penetration the curves of the filmy
substrate systems with either harder or softer substrates
coincides well with that of the bulk film, which shows

401

that the substrate effect is small and negligible. With


further increase of the penetration, the curves of the
filmysubstrate systems start to deviate from that of the
bulk film. As expected, the harder substrates raise the
curves to high load while the softer substrates lower
them. The unloading curves for the film on harder
substrate coincide with one another and are parallel to
that of the bulk film. For the film on softer substrate,
the unloading curves deviate from one another and are
not parallel to that of the bulk film. This difference of
unloading curves can be more clearly seen in the 1.2t
penetration curves shown in Fig. 1b. The difference
between the film on harder substrate system and the
film on softer substrate system is due to the difference
in deformation behaviour. For the film on harder substrate, the deformation is mainly concentrated in the
film while for the film on softer substrate, the film is
bent into the soft substrate and the major deformation
occurs in the soft substrate. The in-plane plastic shear
strain field of the film on softer substrate system with
aYs0.125 and aEs1 during the unloading process
shows the existence of a reverse plastic shear deformation caused by the bending effect. This reverse plastic
deformation results in a decrease of the slope of the
unloading curve and the unloading process is not simply
elastic as is normally assumed for bulk materials. The
loadpenetration depth curves with 0.3t penetration of
the plastically homogenous filmysubstrate system (aYs
1) with different aE are shown in Fig. 1c. Similarly, the
stiffer substrate raises the curves while the weaker
substrate lower them. The unloading curve shows a
steadily decreasing slope with the decrease of aE, that
is, the substrate becomes progressively weaker.
As shown above, with the increase of the penetration
depth the substrate effects gradually come in and the
loading curves of the filmysubstrate system will deviate
from that of the bulk film. Comparing the loading
curves of the filmysubstrate systems with that of the
bulk film, a deviation point can be determined. The
absolute value of the deviation point depends on how
large the deviation is allowed. Here 1% deviation of the
loadpenetration curves of the filmysubstrate system
from that of the bulk film is chosen, which may represent
the critical penetration depth where the substrate effects
are negligible. A ratio of the critical penetration depth
to the coating thickness, h1%, is defined here to represent
the negligible substrate effects and the variation of h1%
with aY and aE is shown in Fig. 2. Cases with elastically
or plastically homogenous filmysubstrate systems and
cases with inhomogeneous systems are included. As can
be seen, there is no universal critical penetration depth
for all filmysubstrate systems. The critical penetration
depth depends on the combination of the filmysubstrate
systems. For the elastically homogeneous cases (aEs1
in Fig. 2a), h1% is constant (h1%s24%) and independent of aY for the film on harder substrate systems (aY)

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Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405

(h1%s0.005). In fact, the substrate effects are more


influenced by the elastic property difference in the filmy
substrate system than by the plastic property difference.
This elastic property dominance is clearly shown by
comparing the two cases of the inhomogeneous systems
(aEs2 in Fig. 2a and aYs0.5 in Fig. 2b). For the case
with aEs2, h1% has the same value as that of the
plastically homogeneous case (aYs1, aEs2) and is
independent of aY. For the case with aYs0.5, h1%
coincides with that of the plastically homogeneous case
(aYs1) very well except for the point aEs1 which
gives the same value of the elastically homogeneous
case (aEs1) at aYs0.5. The sensitivity of the substrate
effects to the elastic properties difference is easy to
understand considering that elastic deformation is a far
field deformation while plastic deformation is a local
deformation.
3.2. Substrate effects on the elastic modulus

Fig. 2. Variation of h1% with aY and aE. (a) elastically homogenous


(aEs1) and inhomogenous (aEs2). (b) plastically homogenous
(aYs1) and inhomogenous (aYs0.5).

1) while increases with the increase of aY for the film


on softer substrate systems (aY-1). For the plastically
homogeneous cases (aYs1 in Fig. 2b), h1% increases
with the increase of aE for the film on weaker substrate
systems (aE-1) and is almost independent of aE (h1%s
3%) for the film on stiffer substrate systems (aE)1). It
is clear that the softer or the weaker the substrate is, the
smaller the h1% value is and the earlier the substrate
effects come in during indentation.
It should be noted that the critical penetration depth
is more sensitive to the elastic property difference in the
filmysubstrate system than the plastic property difference. As shown in Fig. 2a,b, the h1% values of the
elastically homogeneous film systems (aEs1 in Fig.
2a) are much higher than that of the plastically homogeneous systems (aYs1 in Fig. 2b). This means that
the system with the plastic property difference allows
more penetration without the influence of the substrate.
For example, in the case of the film on hardest substrate
system with aYs8 in Fig. 2a, the penetration depth can
be about one-fourth of the coating thickness (h1%s
0.24) without any influence from the substrate; while in
the case of the film on weakest substrate system with
aEs0.125 in Fig. 2b, the substrate effects occur almost
as soon as the indenter starts to penetrate the film

The variation of the ratio of the reduced modulus of


the filmysubstrate system to that of the bulk film, Er y
Erf, with aE under different penetration depths is shown
in Fig. 3. As expected, Er yErf increases with the increase
of the elastic modulus of the substrate, that is, increasing
aE. For a weaker substrate, Er yErf decreases with the
increase of penetration depth from 0.1t to 1.2t. While
for a stiffer substrate, Er yErf increases with the increasing penetration depth. The composite effective modulus
of the filmysubstrate system can be empirically modelled using an equation given by Doerner and Nix w1x.
1yn2com 1yn2f
1yn2s yatyh
s
e
1yeatyh.q
Ecom
Ef
Es

(4)

Combining Eq. (4) with Eq. (3) and considering for


bulk film ts`, we have

Fig. 3. The relationship of EryErf and aE with different penetration


depths and comparison of finite element results and Doerners model.

Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405

Fig. 4. Change of the ratio AcyAc0 calculated from the finite element
simulation with aE under different penetration depths.

1yn2f 1yn2i
q
Er
Ef
Ei
s
2
Erf 1ynf
1yn2s yatyh 1yn2i
e
q
1yeatyh.q
Ef
Es
Ei

(5)

For the rigid cone Eis` and nfsnss0.28 used in this


study, Eq. (5) becomes
Er
aE
s
yatyh
Erf aE1ye
.qeyatyh

(6)

Eq. (6) is plotted with the FE results in Fig. 3. As


can be seen, there is very good agreement between the
FE simulation results and Eq. (6). The best fittings for
the FE simulation results with different penetration
depths give as0.2, which agrees well with as0.25
obtained by Doerner and Nix for tungsten films on
silicon substrate indented with a Berkovich indenter w1x.
Eq. (5) is similar to the equation used by King w3x in
his numerical analysis of the different shapes of flatended punch indenting a layered isotropic elastic halfspace. Instead of the ratio of reduced modulus in Eq.
(5), the ratio of stiffness is used by King and the result
can be written as
1yn2f 1yn2i
q
S
Ef
Ei
s
2
S0 1ynf
1yns2 yatyh 1yni2
e
q
1yeatyh.q
Ef
Es
Ei

403

where Ac0 and Er0 are the contact area and the effective
modulus for bulk film. Clearly when Ac yAc0s1, a
combination of Eq. (5) and Eq. (8) gives Eq. (7). The
ratio of Ac yAc0 calculated from the FE simulation with
different penetration depths is plotted against aE in Fig.
4. As shown in Fig. 4, the ratio of Ac yAc0 is dependent
on aE. Ac yAc0 increases with increasing aE and is greater
than 1 when the substrate is stiffer and less than 1 when
the substrate is weaker. With the increase of penetration
depth, Ac yAc0 increases for stiffer substrates and decreases for weaker substrates. The changing of Ac yAc0 with
aE and the penetration depth could be the explanation
of why a constant a is obtained for the cone indenter
in this study whereas in Kings results a is dependent
on the indentation size.
The relation of Er yErf and aY with different penetration depths is shown in Fig. 5. As can be seen, for the
elastic homogeneous case (aEs1) Er yErf is independent
on the penetration depth and almost constant with the
increase of aY. For the elastic inhomogeneous case
(aEs2), Er yErf increases with increasing penetration
depth since the substrate is stiffer than the film. When
the substrate is harder than the film (aY)1), Er yErf is
almost constant and when the substrate is softer than
the film (aY-1), Er yErf decreases with decreasing aY.
This decrease of Er yErf is due to the reverse plastic
deformation induced by the bending effects during the
unloading process of indentation on hard film on soft
substrate system. As expected, the larger the difference
of plastic properties between the film and the substrate
and deeper the penetration depth, the bigger the bending
effects and, therefore, the larger the decrease of Er yErf.
3.3. Substrate effects on the hardness
The composite hardness of the filmysubstrate system
normalised by the hardness of the bulk film, HyHf,

(7)

where S is the unloading stiffness of the filmysubstrate


system and S0 is the unloading stiffness of the bulk
film. It should be noted that Eq. (7) is only valid for
the case of flat-ended punch where the contact area is
always constant. From Eq. (2) we have
S
s
S0

y AA EE
c

c0

r0

(8)

Fig. 5. The relationship of EryErf and aY with different penetration


depths.

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Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405

substrate is harder than the film (aY)1) and the


penetration is within the film (hyt-1). For hyt)1, a
clear substrate effect is observed and HyHf increases
with the increasing yielding stress of the substrate, that
is an increasing aY. When the substrate is softer than
the film (aY-1), HyHf is almost constant at shallow
penetration whereas it decreases with decreasing aY at
deep penetration. The softer the substrate and the deeper
the penetration, the smaller the hardness.
Bhattacharya and Nix w6x developed a non-dimensional relationship between the hardness of a filmysubstrate
system and the penetration depth. For soft film on hard
substrate, HyHf is given by
B h E 2z
H Hs B
Hs E w
s qC1y FexpxyaYaEC F |
DtG ~
Hf Hf D
Hf G y

(9)

For hard film on soft substrate, HyHf is given by


w

yaE Hf h
H Hs B
Hs E
s qC1y F exp y
Hf Hf D
Hf G
aY Hs t ~
y

Fig. 6. The relationship of HyHf and aE, aY with different penetration


depths. (a) HyHf changing with aE, (b) HyHf changing with aY.

changes with aE and aY under different penetration


depths as shown in Fig. 6. As shown in Fig. 6a, HyHf
increases with increasing aE when the substrate is
weaker than the film (aE-1). When the substrate is
stiffer than the film (aE)1), HyHf is almost independent
of aE. For the case of a plastically homogeneous filmy
substrate system (aYs1), HyHf is independent of the
penetration depth for aE)1 but decreases with increasing penetration depth for aE-1. For the case of a
plastically inhomogeneous filmysubstrate system (aYs
0.5), HyHf depends on the penetration depth since the
effect of the softer substrate comes in for a deep enough
penetration.
The relationship of HyHf and aY with different penetration depths is shown in Fig. 6b. The results of both
elastically homogeneous (aEs1) and inhomogeneous
(aEs2) filmysubstrate systems are plotted. The curves
for both cases at the same penetration depth shows
essentially the same tendency though the curve for the
inhomogeneous case is higher than that of the homogeneous case due to the effects of the stiffer substrate. As
shown in Fig. 6b, HyHf is almost constant when the

(10)

Eq. (9) and Eq. (10) are plotted with the FE simulation results of two cases with aYs4, aEs2 and aYs
0.25, aEs2 in Fig. 7. As can be seen, for soft film on
hard substrate (aYs4, aEs2), Eq. (9) predicts the
hardness of the filmysubstrate system to increase with
increase of the penetration depth. However, there is a
large discrepancy between the FE results and the prediction of Eq. (9) especially when the penetration depth is
large. Eq. (9) overestimates the hardness value of the
filmysubstrate system. While for hard film on soft
substrate (aYs0.25, aEs2), the hardness decreases with
the increase of the penetration depth and there is a good
agreement between the FE results and the prediction of
Eq. (10).

Fig. 7. Comparison of the finite element results of the filmysubstrate


systems with aYs4, aEs2 and aYs0.25, aEs2 and Bhattacharyas
model.

Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405

4. Conclusions
The substrate effects on the indentation behaviour of
thin films with different aY and aE are analysed by FE
simulations. It is found that there is no universal critical
penetration depth for measuring the mechanical properties of films. The critical penetration depth depends on
the combination of the mechanical properties of the film
and the substrate and is more sensitive to differences in
the elastic properties than in the plastic properties of the
filmysubstrate system. The substrate effects on the
elastic modulus of the filmysubstrate system can be well
defined by the empirical relationship Eq. (5). The
substrate effects on the hardness of the hard film on
soft substrate system can be estimated using Eq. (10)
but a large overestimation occurs when Eq. (9) is used
to estimate the substrate effects on the soft film on hard
substrate system.
Acknowledgments
The authors wish to thank the EC Standards, Measurements, and Testing Programme for financial support
under the Contract Number SMT4CT982249. The
financial support of Brinell Centre-Inorganic Interfacial
Engineering for Z.-H. Xu is gratefully acknowledged.

405

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