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
400
Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405
Pmax
Ac
(1)
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.
401
402
Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405
(4)
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)
(6)
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)
y AA EE
c
c0
r0
(8)
404
Z.-H. Xu, D. Rowcliffe / Thin Solid Films 447 448 (2004) 399405
(9)
yaE Hf h
H Hs B
Hs E
s qC1y F exp y
Hf Hf D
Hf G
aY Hs t ~
y
(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).
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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