Available online at www.sciencedirect.

com

ScienceDirect
Procedia Materials Science 3 (2014) 1111 1116

20th European Conference on Fracture (ECF20)

Modeling load-displacement curve and pop-in effect

in nanoindentation tests
Pavel anderaa,b, Jaroslav Pokludaa,b, Thomas Schberlc,d, Jana Hornkova,b*,
Miroslav erna,b,e
a
Brno University of Technology, Faculty of Mechanical Engineering, Technick 2, 616 69 Brno, Czech Republic
b
Brno University of Technology, Central European Institute of Technology, Technick 10, 616 00 Brno, Czech Republic
c
Department Material Physics, University of Leoben, Jahnstrasse 12, 8700 Leoben, Austria
d
Austrian Academy of Sciences, Erich Schmid Institute of Materials Science, Jahnstrasse 12, 8700 Leoben, Austria
e
Institue for Materials Physics, Academy of Science of CR, ikova 22, 662 62 Brno, Czech Republic

Abstract

The nanoindentation test of a single crystal of tungsten is simulated by a multiscale model based on a nonlinear elastic finite
element analysis coupled with both ab initio calculations of the ideal shear strength and crystallographic considerations. The
onset of microplasticity, associated with the pop-in effect identified in experimental nanoindentation tests (creation of first
dislocations), is assumed to be related to the moment of achieving the value of the ideal shear strength for the copper crystal
under a superimposed hydrostatic stress. The calculated value of the critical indentation depth is in a very good correspondence
with that of the experimentally observed pop-in on the load-displacement curve. The value of the Young modulus of tungsten
received from the reduced modulus of elasticity of the original Hertzs model is also in an excellent agreement with experimental
data. This offers us a possibility to assess the concentration of alloying and impurity elements in the surface and sub-surface
layers.

2014 Published by Elsevier Ltd. Open access under CC BY-NC-ND license.

2014 The Authors. Published by Elsevier Ltd.
Selection and peer-review under responsibility of the Norwegian University of Science and Technology (NTNU), Department
Selection and peer-review under responsibility of the Norwegian University of Science and Technology (NTNU), Department of
of Structural Engineering
Structural Engineering.

Keywords: Nanoindentation; Ab initio calculation; Ideal shear strength; Tungsten crystal; Finite element analysis

* Corresponding author. Tel.: +420-541142866; fax: +420-541142842.

E-mail address: hornikova@fme.vutbr.cz

2211-8128 2014 Published by Elsevier Ltd. Open access under CC BY-NC-ND license.
Selection and peer-review under responsibility of the Norwegian University of Science and Technology (NTNU), Department of Structural Engineering
doi:10.1016/j.mspro.2014.06.181
1112 Pavel andera et al. / Procedia Materials Science 3 (2014) 1111 1116

1. Introduction

The nanoindentation is considered to be a very promising experimental approach to measuring the incipient
plasticity in crystals containing defects, e.g. Gken and Kempf (2001), Ciu and Ghan (2002), or even the ideal
(theoretical) shear strength id since the stressed volume beneath the sharp indenter may be dislocation-free, e.g.
Lilleodden et al. (2003), Krenn et al. (2002) and Hornkov et al. (2008). The local shear component of the stress
reaches its maximum value at certain (not very large) penetration depth of the indenter into the bulk. The value of
this stress can approach the ideal shear strength id and, consequently, it can be high enough to nucleate dislocations.
This process might be detected as a pop-in on the nanoindentation loaddisplacement curve. The nanoindentation
can also yield important information on mechanical properties and chemical composition of surface layers when
taking a change of the reduced elasticity modulus Er from the original Hertzs theory into account.
A relevant model of the nanoindentation test must be based on joined approaches on three different levels:
(i) atomistic (calculation of id); (ii) mesoscopic (crystallography); (iii) macroscopic (finite element analysis of
stressstrain response). In particular, the influence of the compressive (nearly hydrostatic) stress h beneath the
indenter on the ideal shear strength value, i.e. the function id(h), is to be considered along with both the
nonlinearity and the anisotropy of the constitutive stressstrain relation.
The main aim of this article is to present a multiscale model of the nanoindentation test in a single crystal of
tungsten based on a nonlinear elastic finite element analysis coupled with both ab initio calculations of the ideal
shear strength and crystallographic considerations. The developed procedure can be easy adapted to other bcc
crystals as, e.g., iron.

2. Experimental data and scales of the model

The experiments have been realized on a Hysitron Triboscope (Hysitron Inc., MN, USA), where the indentation
device has been mounted on the scanner head of an atomic force microscope (Dimension D3100,Veeco, Plainview,
NY, USA) instead of the original standard cantilever holder. A spheroconical indentation tip of the radius
R = 850 nm and the angle = 70o was used in experiments. A careful statistics of load-displacement curves was
performed based on a set of 100 nanoindentations applied in the [111] crystallographic direction - see Schberl
(2012) for more detail. The pop-in effect associated with a discontinuity of the load-displacement curve P vs. h is
depicted in Fig.1. The related penetration depth of the nanoindenter is hpi = 87.7 nm and the loading force Ppi = 8050
N.

Fig. 1 The pop-in effect observed during the nanoindentation tests of a tungsten single crystal.
 Pavel andera et al. / Procedia Materials Science 3 (2014) 1111 1116 1113

A three-dimensional isotropic FEM analysis was performed using the finite element ANSYS code described in
ANSYS Users Manual (1992). A frictionless spheroconical indenter with the radius R =850 nm was pressed into a
substrate disc of thickness 100R (see Fig. 2). The size of the elements near the contact is an order of magnitude
smaller than the depth of penetration. Owing to the axial symmetry of the 3D indentation model, only 2D section
could be analyzed as also depicted in Fig. 2. The Young modulus Ed = 1141 GPa and the Poisson ratio d = 0.07
were considered for the diamond indenter whereas Et = 411 GPa and t = 0.29 for the tungsten crystal. The contact
surface in the vicinity of the indenter tip was created by a set of contact elements that comprised the surface of the
deformable body which was formed by contact pairs, i.e., the target surface and the contact surface. These
contact elements had the same geometric characteristics as the underlying elements of the deformable body. The
contact detection points were located at Gauss integration points interior to the contact surface elements. The contact
surface elements were constrained against penetration into the target surface at its integration points. However, the
target surface could, in principle, penetrate through into the contact surface. The code ANSYS updated tangential
contact stiffness based on current contact normal pressure and the maximum allowable elastic slip.

Fig. 2. The geometrical configuration of the model.

Fig. 3. The stressstrain response of the tungsten crystal to the uniaxial compression in the [111] direction.

The ab initio calculations of stress and energy were performed using a plane wave code VASP (Vienna Ab initio
Simulation Package) developed by Kresse and Furthmller (1996). This code uses projector augmented waves as
supplied with the code reported by Kresse and Joubert (1999) later on. The exchange-correlation energy was
evaluated using the generalized-gradient approximation (GGA) of Perdew et al. (1996). The energy cut-off of the
1114 Pavel andera et al. / Procedia Materials Science 3 (2014) 1111 1116

plane-wave expansion was increased to 300 eV in order to obtain a reliable stress tensor. The solution was
considered to be self-consistent when the energy difference of two consequent iterations was smaller than 0.01 meV.
From the series of convergence tests, 212121 MonkhorstPack k-point in the Brillouin zone mesh was found
satisfactory to reach the required precision and convergence. Both the nonlinearity and the anisotropy of the stress
strain elastic response were taken into account by the uniaxial compression stressstrain curve calculated by the
above mentioned method for the [111] direction in the tungsten crystal - see Fig. 3. A multilinear approximation of
this curve was utilized in the ANSYS code procedure as an equivalent von Mises stressstrain dependence. The
function id(h) was also computed by means of the ab initio approach see Fig. 4.

Fig. 4. The ideal shear strength as a function of the superimposed hydrostatic stress.

Fig. 5. The shear stress r,max and the ideal shear strength id(h) as functions of the penetration depth h. The predicted penetration depth
hpi* = 85.9 nm at the pop-in corresponds to the intersection of these curves.

3. Results of the multiscale model and discussion

The global procedure simulates, step by step, the penetration of the indenter into the copper crystal. In order to
identify the appropriate crystallographic plane in which the latter condition for the dislocation emission (pop-in)
is firstly reached, the activity in the shear system 111> {110} was considered in the calculations. With regard to
the cylindrical symmetry of the 3D model, the stress tensor transformation was performed to obtain all possible
 Pavel andera et al. / Procedia Materials Science 3 (2014) 1111 1116 1115

positions of the crystallographic systems rotating relatively to the main coordinate system. This rotation enabled
us to compute, for a particular mesh node, the value of the resolved shear stress r as a function of the angle .
Simultaneously, the values of the hydrostatic stress h for that node were determined and the ratios r /id(h) were
computed. In the following, the value of r corresponding to maximum of the ratios r /id(h) was searched on the
whole circle (going through each node of the mesh). This value over all nodes, all angles and all shear systems
was denoted r,max. The values of r,max were related to each individual deformation step characterized by the
penetration depth h. As a result, the values of r,max and id(h) as functions of the penetration depth h are depicted
in Fig. 5. When the equality r,max = id(h) is reached (intersection of both curves in Fig. 5), the condition for the
pop-in is fulfilled. This corresponds to the depth hpi* = 85.9 nm which is in a very good agreement with the
experimental value hpi = 87.7 nm. Fig. 6 shows the calculated contours of the ratio r,max /id(h) as a function of
coordinates at the moment of the pop-in. The maximal value of this ratio lies within the red area, which is
slightly off the loading axis in agreement with other published models of the nanoindentation tests.

Fig. 6. Contours of the ratio r,max /id(h) for the indentation step related to the pop-in effect (hip* 85.9 nm) beneath the indenter.

Let us finally make a remark concerning the slope at the onset of the load displacement curve. The onset of this
curve can easily be described by the model originally proposed by Hertz (1881). According to this model, the
contact force P can be expressed as

4
P Er a h , (1)
3

where a is the radius of the contact circle (see Fig. 2). The slope of the P-h curve is proportional to the reduced
modulus of elasticity Er:

1 1 Q indenter
2
1 Q specimen
2

 . (2)
Er Eindenter Especimen

The comparison of the initial slopes of the experimental P-h curves and the theoretical ones obtained from the
numerical analysis based on the Herzian approach revealed an excellent coincidence as reported by Hornikova et al.
1116 Pavel andera et al. / Procedia Materials Science 3 (2014) 1111 1116

(2012). It can also be easily shown that the value of Especimen and, therefore, also the value of Er is a very sensitive
function of chemical composition of the surface layer. This means that a high content of alloying elements or
impurities with Youngs modulus substantially different from the basic material of the substrate (specimen)
significantly changes the initial slope of the P-h curve. This gives us a very simple potential tool for a measurement
of the concentration of alloying elements or impurities in the surface or sub-surface layers.

4. Conclusion

The nanoindentation test in the single crystal of tungsten was simulated by utilizing a multiscale analysis. The
onset of microplasticity, associated with the pop-in effect identified in experimental nanoindentation tests (creation
of first dislocation loops) is assumed to be related to the moment when the value of the ideal shear strength for the
tungsten crystal was reached. In particular, the influence of the hydrostatic stress on the ideal shear strength value,
the three-dimensionality of the nanoindentation test, the nonlinearity of the stressstrain relation, the orientation of
relevant crystallographic planes and the anisotropy of the elastic response of the crystal were considered in the
model. The mechanical characteristics of the perfect copper crystal were calculated using the ab initio approach. The
three-dimensional isotropic FEM analysis, based on the finite element ANSYS code, was used to simulate the
development of the stressstrain field in the substrate.
The computed value of the penetration depth related to the pop-in effect is very close to the experimentally
detected one. This means that the results of the nanoindentation test can serve as a sufficiently precise tool for an
experimental verification of theoretically determined values of ideal shear strength. Moreover, the slope at the onset
of the load displacement curve is a very sensitive function of a chemical composition of the surface layer. This
gives us a simple potential tool for a measurement of the concentration of alloying elements or impurities in surface
or sub-surface layers.

Acknowledgements

This research was supported by the Czech Science Foundation under the Project No P108/12/0144 and by the
European Regional Development Fund under the project CZ.1.07/2.4.00/17.0006 (Ceitec).

References

ANSYS Users Manual. Revision 5.0, IIV. 1992. Swanson Analysis System, Houston, USA.
Chiu Y. L., Ngan A. H. W., 2002. Time-dependent characteristics of incipient plasticity in nanoindentation of a Ni 3Al single crystal. Acta
Materialia 50, 1599-1611.
Gken M., Kempf M., 2001. Pop-ins in nanoindentations the initial yield point. Zeitschrift fr Metallkunde 92, 10617.
Hertz H., 1881. ber die Berhrung fester elastischer Krper, Journal fr die reine und angewandte Mathematik 92, 156-171.
Hornkov J., andera P., ern M., Pokluda J., 2008. Multiscale modelling of nanoindentation test in copper crystal. Engineering Fracture
Mechanics 75, 37553762.
Hornkov J., andera P., Pokluda J., 2012. Comparison of Solutions of Stress Field based on Hertzian and Combined Numerical-
Crystallographic Approaches beneath Nanoindenter. Key Engineering Materials 488-489, 395 398.
Krenn C. R., Roundy D., Cohen M.L., Chrzan D.C., Morris Jr. J. W., 2002. Connecting atomistic and experimental estimates of ideal strength.
Physical Review B 65, 134111.
Kresse G., Furthmller J., 1996. Efficient iterative schemes for ab initio total-energy calculations using a plane-wave basis set. Physical Review
B, 54, 11169.
Kresse, G., Joubert, D., 1999. From ultrasoft pseudopotentials to the projector augmented-wave method. Physical Review B 59, 1758 1775.
Lilleodden E. T., Zimmerman J. A. Foiles, S. M., Nix W. D., 2003. Atomistic simulations of elastic deformation and dislocation nucleation
during nanoindentation. Journal of Mechanics and Physics of Solids 51, 901-920.
Perdew, J. P., Burke, K., Ernzerhof, M., 1996. Generalized Gradient Approximation Made Simple. Physical Review Letters 77, 3865 3868.
Schberl T., 2013. Do we measure theoretical strength by instrumented indentation? In: ESIS TC2 Meeting, Oxford 2012. On-line
http://energy.materials.ox.ac.uk/uploads/ESIS%20TC2%20Workshop%202012/Presentations/Schberl%20Measure%20of%20theoretical%2
0strength.pdf.