Microelectronics Reliability 53 (2013) 443–451

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Microelectronics Reliability
journal homepage: www.elsevier.com/locate/microrel

Application of nanoindentation technique for investigation of elasto-plastic

properties of the selected thin film materials
Artur Wymysłowski ⇑, Łukasz Dowhań
Faculty of Microsystem Electronics and Photonics, Wrocław University of Technology, Wrocław, Poland

a r t i c l e i n f o a b s t r a c t

Article history: Nanoindentation is one of the most known method for investigating the properties of thin films. The
Received 23 June 2012 materials can be assessed by means of elastic mechanical properties (hardness and Young’s modulus).
Received in revised form 7 October 2012 However, the author’s research work shows that it is possible to obtain the elastic as well as the plastic
Accepted 23 October 2012
material behavior of the investigated thin layer. It can be done by using the nanoindentation experiment
Available online 24 November 2012
and the numerical simulations.
This paper focuses then on investigation of thin metal layers by nanoindentation with a support of
numerical methods, such as finite element method and numerical optimization processes. Additionally,
the 3-level, full factorial design of experiment (DOE) process was applied. In order to carry out such
experiment 27 samples were prepared and taken into account: three different materials with three dif-
ferent thickness’s values sputtered on three different substrates. The results were then processed by the
numerical methods in order to achieve more information about the materials – mainly the plastic
behavior.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction yield stress [4,5]. In case of electronic packaging, mechanical prop-

The microelectronic industry still aspires to the miniaturization
of the designed devices and to improvement of their functionality
and reliability. The main role in this process play the thin film
materials that should challenge the devices’ requirements. Nowa-
days, there are many research works in progress referring the
investigation of thin film materials with low dielectric constant
(low-k) or metallic layers used in novel on-chip interconnects. It
is a known fact that such thin layers are characterized by different
mechanical properties than their bulk equivalents [1,2]. The
mechanical properties of the thin layers are changed mainly due
to the fact that they are deposited on a substrate using the thin-
film deposition technology, e.g. magnetron sputtering. This leads
to the intrinsic mechanical stresses that are in such layer. The
stresses appear due to the CTE mismatch during the deposition,
the grain growth after this process, the phase transformation, etc.
[1,3].
The goal of the current paper is to focus on the problem of thin
film materials used in electronic packaging and aspect of reliability
prediction using numerical methods. In case of numerical methods
it is required to use appropriate material models as e.g. elasto-plastic
(bi-linear, nonlinear, etc.) to be able to predict properly the reliability
parameters as e.g. fatigue. There are in fact a number of papers that
focus on one aspect of material properties of thin layers as e.g.
⇑ Corresponding author.
E-mail address: artur.wymyslowski@pwr.wroc.pl (A. Wymysłowski).
erties play the main role in the reliability aspects of the prototyped
devices. Knowing the basic mechanical properties of thin layers
such as elastic–plastic behavior it is possible to predict and avoid
many types of failures: degradation, cracking, delamination, buck-
ling or fatigue. Therefore, there are many research works being
made in reference to development of measurement methods
which are able to characterize the mechanical properties of thin
layers. The known methods, presented in the literature are: wafer
curvature measurement, beam bending, bulge test, microtensile
testing, AC technique and nanoindentation [2,6,7]. However, many
of them are still under investigation and are not available commer-
cially or have still limited measurement possibilities. One of the
method that is widely used is nanoindentation. The results pre-
sented in this paper base on this method and are obtained by the
nanoindentation equipment – Hysitron TriboIndenter.
Nanoindentation method is mainly used for extraction of elastic
properties of the thin films. Nanoindentation technique was intro-
duced in 1992. The goal was to measure apart from the material
hardness H, additionally the elastic (Young’s) modulus E of the
investigated material. The hardness of the investigated material
is measured by indenting the surface with a known force F using
an indenter of a selected shape. The remained indentation print
of the indenter on the material surface is used as a measure of
hardness. Initially the material hardness was usually measured
by loading an indenter of specified geometry onto the material
and measuring the dimensions of the resulting indentation. The
measurement is done by indenters of various shapes thus leading

0026-2714/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.microrel.2012.10.009
444 A. Wymysłowski, Ł. Dowhań / Microelectronics Reliability 53 (2013) 443–451

obtained after the indentation also carries the information about

the plasticity of the indented thin film. Such curve can be therefore
analyzed numerically in order to obtain as well the plastic behav-
ior. Some more description of the nanoindentation method, ap-
plied measurement technique and analysis methods along with
the developed algorithms can be found in our previous papers
[13,14].

2. Design of experiments
Fig. 1. Illustration of nanoindentation test with the Berkovivh tip (left) and the
remained print (right). The first step of this research was DoE analysis based on the 3-
level full factorial scheme. The selected factors were: thin film
material, thickness of this film and the substrate. For each factor
to a variety of tests and analytical definition of hardness value. The three levels were defined (Table 1).
indenter that is the most suitable for thin layer assessment is the The designed DOE process consisted therefore of 27 experi-
indenting test with the so-called Berkovich tip. It is a diamond ments and such amount of samples was prepared using the mag-
three-sided pyramidal indenter shape (Fig. 1). This kind of indenter netron sputtering deposition technique. Every sample was
tip assures high spatial resolutions [10]. measured 32 times with different load values. Additionally, the
The indentation area in the material depends on the indentation in situ scans of the remained print were performed. In order to ob-
depth. The simplified formula is given by: tain the stress–strains characteristics of the investigated materials
Aðhc Þ ¼ 24:56hc
2
ð1Þ only the elastic modulus was taken into account. It is a well know
fact in nanoindentation method that measured Young’s modulus of
After the test the loading/unloading curve in the function of the the thin layer is influenced by the interaction with the substrate
indentation depth is obtained (Fig. 2). material. In order to minimize the above influence a special tech-
Considering the unloading part of the curve it is possible to esti- nique was used. The above technique is based on making a number
mate the following elastic material properties: of indents with different depths and then by extrapolating the
measurement results of Young’s modulus values E0 [6]. Unfortu-
 Stiffness S nately the mean value E0 , which is normally given by the nanoind-
  enter after a series of measurements, due to the influence of a
dF 
S ¼   ð2Þ substrate, is not a good solution. The idea of the extrapolation tech-
dh F¼F max nique is given on Fig. 3.
Before the main experiment it was decided to measure with the
where Fmax is a maximum force during loading and unloading
nanoindentation technique the elastic properties, which is Young’s
indentation process,
modulus, of the selected substrates: silicon, glass and polycarbon-
 Hardness H
F max ate. The above data are included in Table 2 along with the litera-
H¼ ð3Þ ture equivalents.
Ac
The results of measurements and corresponding extrapolation
where Ac is the contact area and can be assessed on the hc depth of Young’s modulus values Em are presented in Figs. 4–6 (for better
value according to the relation (1), comparison the Y scale is the same). As it can be seen the polycar-
 Effective
pffiffiffiffimodulus of elasticity Eeff bonate substrate influenced the results the most. The obtained val-
p S ues are about 5 times smaller than in case of glass and silicon
Eeff ¼ pffiffiffiffiffi ð4Þ
2 Ac substrate. This is mainly caused by the high elasticity of polycar-
bonate (about 4.5 GPa).
where Eeff takes into account displacement in both materials:
The measurements were the initial stage to the numerical anal-
specimen and indenter.
ysis. The goal of this analysis was to obtain the plastic material
Using the nanoindentation test it is only possible to obtain the
parameters of the investigated thin-film materials. Nevertheless
elastic mechanical properties such as hardness and elastic
(Young’s) modulus. However, the loading/unloading curve
Table 1
Designed 3-level full factorial experiment.

Factor 1: thin film material Factor 2: thickness Factor 3: substrate

Silver 300 nm Glass
Copper 600 nm Silicon
Titanium 900 nm Polycarbonate

Table 2
The measured and literature values of Young’s modulus of the selected substrates
[16].

Material Measured Young’s Standard Literature Young’s

modulus (GPa) deviation modulus (GPa)
(GPA)
Silicon 169.88 0.65 168
Glass 70.64 0.42 68
Polycarbonate 3.41 0.05 1.3–10.5
Fig. 2. Result of nanoindentation test – loading/unloading curve.
 A. Wymysłowski, Ł. Dowhań / Microelectronics Reliability 53 (2013) 443–451
Fig. 3. Method of Young’s modulus extraction with extrapolation technique, where h is the indentation depth, tf is the thin film thickness, E0 is the measured Young’s modulus
and Em is the extrapolated Young’s modulus.
Fig. 4. Results of the investigated materials on a glass substrate.
Fig. 5. Results of the investigated materials on a silicon substrate.
the achieved results for Young’s modulus are characterized by very
small standard deviation. As it is marked in the Figs. 4–6 its value
445
Fig. 6. Results of the investigated materials on a polycarbonate substrate.
in all cases was lower than 1% of the mean value. The same the
both tip location and surface grains seemed to have small influence
on the final results. Another interesting behavior is in case of silver
deposited on silicon substrate, which shows the opposite trend
from all other tests (including silver on other substrates). Accord-
ing to the authors the above behavior could be explained by quality
of the deposited thin film by magnetron sputtering deposition
technology. Unfortunately the above was not confirmed by struc-
tural investigations or visual inspection due to e.g. grain size
distribution.
3. Numerical extraction of mechanical properties
Many materials used in microelectronics can be precisely de-
scribed by elastic and plastic parameters. Elastic behavior, as de-
scribed above, can be obtained directly after nanoindentation
test. The plastic part of the material’s characteristic can be exam-
ined by numerical analysis of the nanoindentation results. One of
the solutions is the finite element modeling and the numerical
optimization of such designed models in reference to experimental
data.
446 A. Wymysłowski, Ł. Dowhań / Microelectronics Reliability 53 (2013) 443–451
3.1. FE-model of nanoindentation test
In order to obtain the results in the optimization process, the
numerical FE-model of the nanoindentation test was prepared.
The model is fully parametric and was created in Abaqus software.
According to the research already done in the past, the model was
designed as a 2D axisymmetric part (Fig. 7) [13,14]. The 2D model
though less accurate that 3D model was found out to be a good
trade off between simulation accuracy and computing time.
Especially in case of multi-criteria optimization. In our case, multi-
criteria optimization in each instance required hundreds of simula-
tions in order to extract elasto-plastic material properties.
The applied FE-model consisted of 2585 elements. The elements
were defined according to the axisymmetric model as 4-node bilin-
ear quadrilateral structures with reduced integration (CAX4R). The
model consisted of three areas: the diamond tip (366 elements),
the thin film area (980 elements) and the substrate (1239 ele-
ments). The bottom of the substrate was pinned (all degrees of
freedom set to 0) and the left edge was defined as the axis of rota-
tion. The key aspect in the prepared model was the contact defini-
tion between the diamond tip and the thin layer. The contact was
defined as the surface-to-surface interaction with the ‘‘hard
contact’’ properties [9]. Additionally, the influence of friction coef-
ficient was tested and explored during the evaluation of the
FE-model and it did not have any significant effects on the final
results.
The indenter shape was designed according to the area function
in its complex form [10]:
2 1=2 1=4 1=8
Aðhc Þ ¼ C 0 hc þ C 1 hc þ C 2 hc þ C 3 hc þ C 4 hc þ C 5 hc
where the Ci coefficients were obtained in the calibration phase
from the nanoindentation equipment.
The material properties of the thin layer were defined as elastic
and plastic. The plastic behavior is described by the kinematic
hardening model. This model can properly describe the material
plastic behavior after applying the load and then releasing it
[12]. Such defined numerical model was applied to the optimiza-
Fig. 7. FE-model of the nanoindentation test.
tion process in order to analyze and compare the numerical results
to the experiments. The material properties were described by
elastic and plastic models. The plastic model was chosen as the
Ramberg–Osgood relation:
 nh
r r r
e¼ þa y ð6Þ
E E ry
where e – strain, r – stress, E – Young’s modulus, ry – yield stress, a,
nh – hardening parameters. However, the so-called yield offset a(ry/
E) in Eq. (6) can be represented as constant 0.002, which stands for
the 0.2% of the nominal material strain (before loading). Therefore,
the numerical loading/unloading curve was fitted to the measured
one by changing three material parameters: Young’s modulus, yield
stress and hardening module (Table 3).
The elastic modulus was changed from the minus 5% value of
the measured Young’s modulus Em to the plus value of Em (see
Fig. 4–6). The nominal value was set as the mean value. The elastic
values were taken individual for each investigated sample. The
plastic parameters were fixed as it is shown in Table 3.
As the output parameters, which are the optimization’s objec-
tives three criteria were defined. Criterion 1 and Criterion 2 refer
to the loading/unloading curve in order to find the best fit between
the numerical and experimental data (Fig. 8). Criterion 1 is the dif-
ference between the contact depths after unloading. Criterion 2 is
the difference between the depth values at maximal load. Criterion
3 refers to the pile-up effect and is defined as the difference be-
tween the heights of the experimental value (in situ scanning)
and the numerical (Fig. 9). The goal is to find the minimal values
1=16
of the selected criteria.
The presented optimization process is carried out by the self-
ð5Þ developed software (Fig. 10). It combines the FE-models with the
implemented numerical multi-objective algorithms.
In order to extract numerically the plastic behavior of the inves-
tigated material, the FE-model has to be analyzed by the optimiza-
tion algorithm. The goal of the optimization is to find the best fit
between the numerical and experimental data. The fitting is made
by changing the elastic and plastic material parameters in the
Table 3
Values of the selected input parameters.
Parameter Minimal Nominal Maximal
Young’s mod. (GPa) 5% Em Em +5% Em
Yield stress (MPa) 30 100 3000
Hardening mod. (MPa) 2 5 10
Fig. 8. Illustration of selected criterion 1 and criterion 2 for the multi-objective
optimization.
 A. Wymysłowski, Ł. Dowhań / Microelectronics Reliability 53 (2013) 443–451 447

Fig. 9. Illustration of selected criterion 3 for the multi-objective optimization.

Fig. 10. Console window of self-designed optimization software.

processed FE-model. The numerical loading/unloading curve and
the pile-up are compared to their experimental equivalents which
carry the information about the plasticity [8,11] (detailed descrip-
tion of the numerical extraction method in [10]).
The multi-objective optimization scheme takes into consider-
ation more than one optimization criterion and therefore the result
becomes optimal in reference to several criteria at the same time
(in this case: loading/unloading curve and pile-up effect). In case
of a multi-objective optimization problems (usually complex)
there is a need for finding a compromise between different objec-
tive functions in order to find the optimal solution in reference to
all the selected objective functions. In contrast to the single objec-
tive optimization, the multi-objective optimization can be defined
as follows:
where fi(X) are the objective function and the F(X) is the optimiza-
tion criterion based on the set of m objective functions; X – vector of
optimization variables; ci – equality and inequality constraints
functions. The optimal solution can be formulated in a form of a
set, which is optimal in the Pareto sense. The set means that there
is not only one optimal solution but a whole set of solutions, which
are equally acceptable from an engineering point of view and equiv-
alent from mathematical point of view. The solution is optimal in
the Pareto sense, if there is not a better solution in reference to at
least one criterion without worsening the solution in reference to
all other ones. The idea of Pareto set is shown in Fig. 11. The values
x and y on the right hand-side represent the input space and the
f(x,y), g(x,y) ar0065 the objective functions dependent on these in-
put (x,y) values [13,14].

min FðXÞ ¼ ff1 ðXÞ; f2 ðXÞ; . . . ; fm ðXÞg

for X ¼ ðx1; x2; . . . ; xn ÞT 4. Results and discussion
ð7Þ
ci ðXÞ ¼ 0; i ¼ 1; 2; . . . ; m
As the results of the numerical material data extraction the
ci ðXÞ0; i ¼ m þ 1; . . . ; n optimal models with elastic and plastic behavior. The example
448 A. Wymysłowski, Ł. Dowhań / Microelectronics Reliability 53 (2013) 443–451

Fig. 11. Idea of the Pareto set.

fitted experimental and numerical curves for the 900 nm silver

thin film on glass is presented in Fig. 12.
The stress–strain material characteristics for all investigated
samples were obtained and given in Figs. 13–21 with the marked
yield stress ry (circle dot). Additionally, all results are shown in Fig. 14. Example stress–strains curves for the investigated silver thin films on
silicon substrate.
Table 4.
In all cases the titanium material has the highest yield stress
from all investigated materials. In case of polycarbonate substrate

Fig. 15. Example stress–strains curves for the investigated silver thin films on
polycarbonate substrate.
Fig. 12. Fitted experimental and numerical response of the silver thin-film on glass
substrate.

Fig. 13. Example stress–strains curves for the investigated silver thin films on glass Fig. 16. Example stress–strains curves for the investigated copper thin films on
substrate. glass substrate.
 A. Wymysłowski, Ł. Dowhań / Microelectronics Reliability 53 (2013) 443–451
Fig. 17. Example stress–strains curves for the investigated copper thin films on
silicon substrate.
Fig. 18. Example stress–strains curves for the investigated copper thin films on
polycarbonate substrate.
Fig. 19. Example stress–strains curves for the investigated titanium thin films on
glass substrate.
the titanium yield stress levels were 2 times lower (about
1300 MPa) than in case of glass or silicon substrate (about
2700 MPa). The yield stresses in case of copper and silver on glass
and silicon substrate sustain at approx. the same level (about
449
Fig. 20. Example stress–strains curves for the investigated titanium thin films on
silicon substrate.
Fig. 21. Example stress–strains curves for the investigated titanium thin films on
polycarbonate substrate.
500 MPa). The silver layers on polycarbonate also show such
behavior. The copper in this case, for all thickness values have
the yield stresses at about 250 MPa. It can be also noticed that
the hardening for silver is in every case higher than in copper
material. Figs. 22–24 show dependence or rather trend of the ex-
tracted material plastic properties for the both yield stress and
hardening parameter versus the thin film thickness.
It can be concluded that according to the Figs. 4–6 and 22–24
the measured elasto-plastic material properties and especially
the parameters for Young’s modulus and yield stress depend on a
substrate material. Additionally the general trend can be noticed
that the measured Young’s modulus is getting higher with the film
thickness while it is just the opposite for the measured yield stress,
which is getting smaller with the film thickness. Though the film
thickness seem to have a small influence on Young’s modulus in
comparison to the yield stress. It is worthy to underline that in case
of Cu it was already reported by some authors as e.g. Volinsky [15]
that both Young’s modulus and yield strength drop with an in-
crease of film thickness. The above difference can be due to:
– Measurement method, which in case of Young’s modulus was
based on extrapolation of measurements for different indenta-
tion depths,
450 A. Wymysłowski, Ł. Dowhań / Microelectronics Reliability 53 (2013) 443–451

Table 4
Numerical results for all investigated thin-films.

No. Thin film tf (nm) Sub E (GPa) ry (MPa) nh [1]

1 Ag 300 Glass 85.13 302.18 3.3
2 Ag 600 Glass 98.57 274.29 3.9
3 Ag 900 Glass 106.46 221.17 2.8
4 Cu 300 Glass 107.72 378.84 4.7
5 Cu 600 Glass 115.17 346.29 4.9
6 Cu 900 Glass 129.46 318.79 5.1
7 Ti 300 Glass 99.29 1583.42 6.6
8 Ti 600 Glass 109.35 1527.86 7.4
9 Ti 900 Glass 123.43 1497.21 8.3
10 Ag 300 Silicon 111.37 456.74 4.8
11 Ag 600 Silicon 101.38 364.32 4.1
12 Ag 900 Silicon 99.17 322.86 3.8
13 Cu 300 Silicon 117.13 462.54 4.5
14 Cu 600 Silicon 121.24 368.78 4.1
15 Cu 900 Silicon 122.11 311.53 4.9
16 Ti 300 Silicon 148.16 1914.46 6.3
17 Ti 600 Silicon 155.49 1858.62 7.2
18 Ti 900 Silicon 158.16 1713.85 9.8 Fig. 23. Yield stress and hardening parameter versus the film thickness for Ti on
19 Ag 300 Polyc 31.78 396.14 5.8 given substrates.
20 Ag 600 Polyc 38.19 346.37 5.2
21 Ag 900 Polyc 46.87 322.58 6.3
22 Cu 300 polyc 24.76 189.18 5.9
23 Cu 600 Polyc 26.92 149.61 6.4
24 Cu 900 Polyc 32.08 129.73 6.8
25 Ti 300 Polyc 24.37 684.96 5.7
26 Ti 600 Polyc 29.27 651.36 6.7
27 Ti 900 Polyc 36.13 636.24 7.4
Polyc substrate 3.41 47.37 6.1

Fig. 24. Yield stress and hardening parameter versus the film thickness for Cu on
given substrates.

It can be noticed that the curves are similar and the total error
between simulation and tensile test results are around 10%. There-
fore it can be concluded that the elaborated and applied numerical

Fig. 22. Yield stress and hardening parameter versus the film thickness for Ag on
given substrates.

– Applied plastic material model, which in our case was based on

nonlinear Ramberg–Osgood relation (6),
– Extraction method, which in case of yield stress was supported
by FEM simulations.

5. Verification experiment

In order to verify the described methodology of extraction thin

film elasto-plastic properties, the verification experiment was car-
ried out. For this experiment the standard tensile machine was
used. The idea of this experiment was to compare the results ob-
tained for the bulk elastic–plastic material from the numerical cal-
culations to the results obtained during the standard tensile test.
The material taken for this experiment was the polycarbonate sub-
strate. The stress–strains curves for both the numerical and exper- Fig. 25. Comparison of the stress–strain curves obtained from the numerical
imental data are shown in Fig. 25. simulations and tensile test.
 A. Wymysłowski, Ł. Dowhań / Microelectronics Reliability 53 (2013) 443–451 451

Table 5 response to the experimental data as well as by taking the pile-

Properties for a bulk material [16,17]. up effect into account. As a result the stress–strains material char-
Material Young’s modulus (GPa) Yield stress (MPa) acteristics were obtained. In fact the nanoindentation analysis of
Ag 76.0 55.0 thin films refers to the mechanical properties of the bimaterial
Cu 110.0 33.3 structure – substrate and thin film. One of the possibilities to ex-
Ti 116.0 140.0 tract the date for thin film is to use numerical analysis to the exper-
imental results. Nevertheless, the difference between extracted
final material properties of the thin films, as marked in Table 4,
are probably due to the different formation and quality of prepared
Table 6
Literature properties for the selected thin films [17–19]. thin metal layers, which were made by magnetron sputtering
deposition and depend on e.g. substrate and thin film thickness.
Material Young’s modulus Yield stress (MPa) Film thickness (nm)
(GPa)
Acknowledgment
Ag 129.7 708.0 300
Cu 145.5 730.0 300
Ti 138.2 2992.3 300
The authors would like to acknowledge the WCSS (Wroclaw
Center for Networking and Supercomputing) for its numerical cal-
culation resources.

method used for the material data extraction of the thin-films

seems to be a promising one.
Additionally in order to verify the methodology it was decided
to compare the results with the corresponding material properties
for a bulk material (Table 5) and literature date for thin films (Ta-
ble 6). Nevertheless, it should be underlined that even for bulk
materials the measured material properties depend on a number
of parameters and can vary from experiment to experiment. The
above problem refers to the thin layer even more as the measured
material properties would depend on even more parameters as e.g.
deposition technology, film quality, residual stresses between sub-
strate and thin film, etc.
Taking into account Tables 5 and 6 it can be noticed that in case
of Young’s modulus and thin films of Ag and Cu and for glass and
silicon substrates results are comparable while in case Yield stress
and especially for Ti and polycarbonate substrate results differ
highly.
According to the literature example date included in Table 6 it
can be concluded that extracted elastic properties by using the
elaborated methodology are consistent for silicon and glass sub-
strate. Additionally in case of plastic properties it is worthy to
underline that values of yield stress seem to be two times lower
in case of our measurements.
6. Conclusions
The goal of the paper was to present the elaborated methodol-
ogy and preliminary results of the investigation of the elasto-
plastic properties of selected thin films deposited on substrates
with the standard nanoindentation technique. In fact this research
is based on the number of tools and techniques as: nanoindentation
measurements, numerical calculations including the FE-modeling
and the multi-objective optimization. For the initial stage of the
numerical process the 3-level full factorial DOE experiment was
carried out. It consisted of 27 samples that were prepared and
measured using the nanoindentation method. The results were
then analyzed and compared to the numerical responses. The
plastic behavior were obtained by fitting the numerical material
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