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Received 22 June 2007; received in revised form 30 August 2007; accepted 1 September 2007
Available online 18 October 2007
Abstract
This study is about the origin of systematic deformation-induced crystallographic orientation patterns around nanoindents (here of
single crystalline copper; conical indenter) using the following approach: first, the rotation pattern is investigated in three-dimensions
(3D) using a high-resolution 3D electron backscattered diffraction (EBSD) technique (EBSD tomography) which works by a serial sec-
tioning and EBSD mapping procedure in a scanning electron microscopy-focused ion beam cross-beam set-up. Second, the problem is
modeled using a crystal plasticity finite element method which is based on a dislocation density-based constitutive model. Third, the
results were discussed in terms of a geometrical model which simplifies the boundary conditions during indentation in terms of a com-
pressive state normal to the local tangent of the indent shape. This simplification helps to identify the dominant slip systems and the
resulting lattice rotations, thereby allowing us to reveal the basic mechanism of the formation of the rotation patterns. The finite element
simulations also predict the pile-up patterning around the indents, which can be related to the dislocation density evolution.
2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
1. Introduction we must also state that a detailed simulation does not nec-
essarily replace a firm understanding of the main mecha-
The observation of deformation-induced crystallo- nism which is responsible for the fact that such patterns
graphic lattice rotations caused by nanoindentation has exist at all. In other words, although good agreement was
recently attracted attention [1–8]. These orientation obtained in a previous experimental and theoretical study
patterns were observed experimentally [1–4,7] and also in of this phenomenon [4], it remains unclear why these defor-
corresponding simulations [4,6]. Concerning the experimen- mation-induced patterns consist of multiple narrow zones
tal work, it is important that the same rotation patterns of alternating crystalline rotations and counter-rotations
were identified by using three different types of techniques of equal magnitude in close sequence. In this paper, we
performed by different groups, namely, synchrotron wide- therefore try to elucidate the general crystallographic prin-
angle Bragg diffraction [1], electron backscattered diffrac- ciple behind these patterns. For this purpose, we take the
tion (EBSD) in two [7] and three dimensions [4], and following approach: first, the rotation patterns are investi-
transmission electron microscopy (TEM) [2,3]. The visco- gated by a high-resolution three-dimensional (3D) EBSD
plastic crystal plasticity finite element simulations which technique (EBSD tomography) for a nanoindent performed
we published recently [4] could also capture some important by a conical indenter with a spherical tip in a copper single
features of the experimentally observed orientation pat- crystal. Next, we conduct advanced crystal plasticity finite
terns. However, irrespective of some success along this line, element simulations which are based not on a viscoplastic
formulation but on a dislocation density-based constitutive
*
Corresponding author. Tel.: +49 211 6792 333. model [9,10]. Finally, the results are discussed in terms
E-mail address: d.raabe@mpie.de (D. Raabe). of a geometrical model which simplifies the boundary
1359-6454/$30.00 2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.actamat.2007.09.001
32 N. Zaafarani et al. / Acta Materialia 56 (2008) 31–42
conditions imposed during indentation in terms of a com- slip system a are treated as functions of the statistically
pressive state normal to the local tangent of the indent stored dislocation density, qSSD. In Ref. [9] it is shown that
rim. This simplified assumption allows one to identify the the mobile dislocation density can be approximated by
dominant slip systems and the crystallographic principle 2k B T pffiffiffiffiffiffiffipffiffiffiffiffiffiffi
behind the resulting reorientations. The finite element sim- qMa ¼ qFa qPa ð2Þ
c1 c2 c3 Gb3
ulations also predict the pile-up patterning around the
indents which can be related to the dislocation density where c1, c2 and c3 are material constants, kB is the Boltz-
evolution. mann constant, T is the absolute temperature and G is the
shear modulus. The quantities qFa and qPa denote the
2. Modeling and simulation forest dislocation density and the density of parallel dislo-
cations, respectively. Both measures are calculated as
2.1. Motivation projections of the statistically stored dislocation density
qSSD on the slip system a. Based on the cutting process
The deformation and reorientation patterns caused by of the forest dislocations, the average dislocation velocity
nanoindentation motivate the use of a crystal plasticity can be calculated as
finite element approach for obtaining a better understand- Q ðjsa j spass;a ÞV a
ing of this phenomenon. The crystal plasticity finite va ¼ ka m0 exp cut ð3Þ
kBT
element method allows one to study the activation of
certain slip systems at different stages of indentation, the where
pffiffiffiffiffiffiffi
change of the crystal orientation, and the formation of spass;a ¼ c1 Gb qPa ð4Þ
pile-up or sink-in patterns around the indent [11]. The
strength of the method lies particularly in properly map- is the shear stress required to move a dislocation past the
ping the strong kinematical influence of crystalline anisot- other parallel dislocations.
pffiffiffiffiffiffiffi
ropy during plastic straining, which as a rule also leads ka ¼ c2 = qFa ð5Þ
to the prediction of the correct tendency in the resulting
is the jump width of the mobile dislocations related to the
orientation changes. This has been shown in a number of
density of forest dislocations qFa.
studies [4,11–16] where predictions obtained by the crystal
The activation volume, Va, resulting from the steps
plasticity finite element method were compared in detail
(kinks) created by the cutting process can be expressed as
with corresponding micromechanical experiments with
respect to strain, texture and forces. Conventional crystal V a ¼ c 3 b2 ka ð6Þ
plasticity models (e.g. [17,18]) use viscoplastic hardening
The quantities m0 and Qcut in Eq. (3) are the attack
laws as a good compromise between computation speed
frequency and the activation energy for the forest cutting
and predictive reliability. The shortcoming of such visco-
process, respectively.
plastic formulations is the absence of an internal variable
The evolution of the statistically stored dislocation den-
concept beyond the incorporation of the crystal orienta-
sity describes the hardening on each slip plane. The evolu-
tion. More advanced variants of the crystal plasticity finite
tion Eq. (7) includes multiplication ðq_ þ Þ and annihilation
element method, therefore, replace the viscoplastic consti-
ðq_ Þ terms for the statistical density of dislocations, qSSD,
tutive description by dislocation-based models [9,10,19–
in the form of a rate formulation,
26]. Since it is likely that some dislocation effects which
cannot be readily captured by viscoplastic hardening laws q_ SSD ¼ q_ þ1 þ q_ þ2 q_ 1 q_ 2 ð7Þ
may play a substantial role in nanoindentation of single þ1 þ2
where q_ and q_ are the production rates of qSSD due to
crystals, we use in this study an advanced crystal plasticity the interaction with forest dislocations and dipole forma-
finite element method which is based on dislocation rate tion, respectively.
formulations for the simulation of nanoindentation.
c4 1
q_ þ1 ¼ c_ a ð8Þ
2.2. A physically based crystal plasticity model b ka
c5
2.2.1. Theory q_ þ2 ¼ d dipole qM c_ a ð9Þ
b
The model which was introduced in Refs. [9,10] adopts
c4 and c5 are fitting parameters,
the Orowan equation as a kinematic equation on each slip
pffiffiffi
system to establish a connection between the shear rate and Gb 3
the mobile dislocation density d dipole ¼ ð10Þ
16pð1 mÞðjsa j spass;a Þ
c_ a ¼ qMa bva ð1Þ
is the critical distance for dipole formation [24] and m is the
where c_ a is the shear rate on slip system a and b is the mag- Poisson’s ratio. The rates q_ 1 and q_ 2 are the non-
nitude of the Burgers vector. The mobile dislocation thermal and thermal annihilation rates of the dislocations,
density, qMa, and the velocity of the dislocations, va, on a respectively.
N. Zaafarani et al. / Acta Materialia 56 (2008) 31–42 33
3. Experimental procedure
Table 1
Summary of crystal constants and parameters used in the model
Material constant Unit Value Parameter Unit Value
Shear modulus, G GPa 75.4 For passing stress, c1 – 0.1
Burgers vector, b m 2.56 · 1010 For jump width, c2 – 1.95
Attacking frequency, m0 s1 1010 For obstacle width, c3 – 0.3
Activation energy of slip, Qcut J 6.33 · 1019 For lock formation, c4 – 0.037
Poisson’s ratio, m – 0.33 For dipole formation, c5 – 0.04
For athermal annihilation, c6 – 50
Initial dislocation density, q0 m2 5 · 1010
Fig. 4. Top view presenting the cutting planes relative to the indent
Fig. 2. The mesh used in finite element simulation (one quarter of the position.
mesh is not shown).
Fig. 6. Misorientation maps (absolute lattice rotation) underneath the indentation at different cross sections, comparison between experimental and
simulation results. (The seemingly shallower indent near the center is due to the edge effects and milling-induced curvature.)
The measurements reveal a pronounced deformation- ity finite element model shows that it succeeded in captur-
induced crystal rotation pattern underneath the indent, as ing fine details of the crystallography of the rotation
reported previously [4]. The alternating rotation and reori- patterning (Fig. 7b1–b4). Concerning the absolute values
entation zones are arranged directly underneath the indent. of the rotation angles about the ½1 1 2 axis, a maximum
The measurements show that at the sides of the nanoindent rotation angle of 14 was observed in the experiment.
only very small crystallographic rotations took place. The The corresponding maximum in the dislocation-based crys-
pattern underneath the indent near the center section can tal plasticity model is about 23. This deviation could be
be characterized by six rotation zones which are separated due to edge effects at the contact zone and milling-induced
by narrow rotation-free areas (Fig. 6a4). The maximum curvature caused by the ion beam so that no complete
values of the misorientation angles can be observed at the EBSD mapping could be made up to the actual contact
surface directly at the contact layer. interface. In this region, though, maximum rotation values
are likely to occur. Also, the lateral resolution of the mea-
4.2. Rotation patterns in axis-angle presentation surement which was conducted using a 80 nm step size was
probably not fine enough to capture all the effects at the
The orientation maps are also represented in the form of actual contact surface.
rotation angles about the ½1 1 2 crystal direction in the sam-
ple reference system (note that in Ref. [4] the axis rotation 4.3. Pile-up pattern formation around the indent
is given in the crystal coordinate system). The maps are
plotted on the ð1 1 2Þ planes in Fig. 7a1–a4 at different spac- The pile-up pattern surrounding the ½1 1 1 indent is
ing to the center of the indent. The maps reveal pro- characterized by a sixfold symmetry, as already reported
nounced lattice rotations about the ½1 1 2 axis below the by Wang et al. [11]. The simulations reveal the same pat-
indent and lower values at the rims of the indent. The mea- tern (Fig. 8). Comparing the pattern of the mobile disloca-
surements also show frequent and quite abrupt changes in tion density around the indent (Fig. 9) with the pile-up
the sign of the rotation direction along and near the surface reveals some common features. The mobile dislocations
when presented in the form of ½1 1 2 axis rotations. The are arranged around the indent in a pattern similar to the
rotations decrease further away from the contact zone. pile-up distribution. In fact, the peak values for the mobile
The comparison with the dislocation-based crystal plastic- dislocation density are found in almost the same positions
36 N. Zaafarani et al. / Acta Materialia 56 (2008) 31–42
Fig. 7. Comparison between crystal rotation about the direction ½1 1 2 in the sample reference system underneath the indentation at different cross sections
between experimental and simulation results (positive values mean counter clockwise rotation). Note that in [4] the axis rotation is given in the crystal
coordinate system.
Fig. 10. Development of mobile dislocation density around the indent on a f1 1 2g midsection at: (a) 10% indentation (0.1 lm depth) (b) 30% indentation
(0.3 lm depth) (c) 50% indentation (0.5 lm depth) and (d) 100% indentation (1 lm depth).
Fig. 11. SEM image of a serial section: (a) non-relaxed and (b) relaxed. 4.4. Effect of the free surface
as the maximum pile-ups. This observation reflects the One drawback of the FIB technique for serial sectioning
obvious connection between the local shear and the activity is that the method is destructive. This means that any error
of the mobile dislocations. in the milling procedure requires full repetition of the entire
38 N. Zaafarani et al. / Acta Materialia 56 (2008) 31–42
Fig. 12. Effect of free surface milling on the total crystal rotation at the center cross section.
experiment. Another problem of the method lies in the fact in the finite element analysis. On the surface of the sample
that the approach steadily produces new free surfaces for along the ½1 1 2 crystallographic direction the rotations
EBSD characterization (Fig. 11). This might have a small about the ½1 1 0 axis indicate the mentioned phenomenon,
effect on the measured orientations compared with the as shown in Fig. 13a. Three regions are inspected by select-
(hypothetical) state of a bulk crystal without free surfaces. ing corresponding nodes (Figs. 13). Node (a) is chosen very
With the help of the FE simulation, the error caused by close to the center, where the crystal reveals a negative rota-
the free surface can be estimated. For this purpose, the tion. While node (c) represents the neighboring positive
boundary conditions were changed to mimic a free surface rotation area, node (b) stands for the cross-over region
(relaxed model). This approach simulates the effect of cut- between the two counter-rotated areas. This means that at
ting the surface free. The misorientation patterns predicted node (b) almost no crystal rotation is expected to take place.
in the two model variants are compared in Fig. 12. The While Fig. 14 reveals the evolution of the rotation about
comparison shows that, although the misorientation pat- the ½1 1 0 direction (x-axis) during the indentation, Fig. 15
tern remains almost unchanged, some deviations occur in represents the corresponding slip system activity. It can be
the absolute values. The difference varies between 5 and seen from Fig. 15a that close to the center the crystal
8% from the initial model (which is referred to here as undergoes a small positive rotation at the beginning of
the non-relaxed model variant). the indentation, which soon reverses its sense. Moving out-
wards from the center (Fig. 14b and c), the positive rota-
5. Discussion tion increases until it dominates the whole indentation
process. A likely interpretation of this observation is that
The phenomenon addressed in this paper is the gradual the crystal rotation behavior is influenced by two different
formation of systematic orientation patterns in the mechanisms. The first one is caused by the spatial rotations
deformed zone underneath an indent caused by conical due to the geometry of the indenter. This means that cer-
nanoindentation with a spherical tip. The patterns are par- tain rigid body rotations are imposed by the antisymmetric
ticularly characterized by systematic arrangements of rota- portion of the external displacement gradient tensor which
tion and counter-rotation fields, as presented in the figures is generated by the indentation process. The local crystallo-
above. These rotation- and counter-rotation patterns were graphic slip is responsible for the second kind of rotation.
confirmed both by the measurements and by the In a second approach to better understand the reason
simulations. for the rotation patterns we consider as a simple approxi-
The first approach to better understand the rotation pat- mation the compression force exerted by the indenter as
terns is to conduct a detailed analysis of some selected nodes the only loading source. This force acts almost perpendic-
N. Zaafarani et al. / Acta Materialia 56 (2008) 31–42 39
Fig. 13. Three nodes with different rotations on the ð1 1 0Þ plane are chosen for investigation: (a) ½1 1 0 rotations on a front view at the middle cross section
and (b) Same rotations on the surface of the crystal.
ular to the local contact surface tangent between tool and the indentation process the axis rotates towards the ½1 1 1
crystal (schematical image in Fig. 16). direction for all selected nodes (1 ! 2 in Fig. 16), before
The components of the contact force at the selected it reverses its motion towards the ½0 0 1 pole, (2 ! 3 in
nodes are extracted from the simulation results. Knowing Fig. 16). This confirms the results of Fig. 14.
the orientation of the crystal at each node allows the deter- The question that arises is: why does the compression
mination of the crystallographic direction of the loading axis reverse its sense of rotation? The answer can be given
axis during the whole indentation process. by monitoring the slip systems involved in the process. At
This is shown in the schematical image on the right-hand the beginning of the indentation three pairs of slip systems
side of Fig. 16, where a simplification is described which is are activated, as indicated in Fig. 15. Slip system pair (1)
used to track the changes in the single crystal kinematics consists of ½1 0 1ð1 1 1Þ and ½0 1 1ð1 1 1Þ, pair (2) of
during indentation in terms of a Sachs loading case under ½1 01ð1 1 1Þ and ½0 1 1ð1 1 1Þ and pair (3) of ½1 10ð1 1 1Þ
simple compression tangential to the local contact interface. and ½1 1 0ð1 1 1Þ. It is well known [30] that for a single crys-
In the projection shown in Fig. 16 the corresponding tal under compression the rotation of the compression axis
evolution of the compression axis is plotted for the various towards the slip plane normal of the active slip system is
nodes. For all nodes the compression axis lies on the the primary rotation. Therefore, and also from Figs. 16
½0 0 1 ½1 1 1 boundary. This is also expected due to the and 17, one can see that the slip system pair (1) causes
symmetry of the problem resulting in a rotation about the compression axis to rotate towards the ½1 1 1 pole fol-
the ½1 1 0 axis. The movement of the compression axis lowing the reorientation route (1 ! 2), leading to an initial
along the ½0 0 1 ½1 1 1 boundary results in simultaneous positive crystal rotation. However, this rotation reduces its
slip on pairs of two slip systems, as can be seen in Schmid factor and hence the shear activity is lowered, as
Fig. 15. It can also be observed that at the beginning of can be seen in Fig. 15a.
40 N. Zaafarani et al. / Acta Materialia 56 (2008) 31–42
Fig. 14. The evolution of the total crystal rotation about ½1 1 0 during Fig. 15. The active slip systems during indentation at: (a) node a, (b) node
indentation at: (a) node a, (b) node b and (c) node c. b and (c) node c.
On the other hand, the two other slip system pairs (2) two rotation mechanisms equilibrate and the crystal
and (3) remain fully active with progressing indentation. reverses its sense of rotation. Route (2 ! 3) describes a
Each pair tends to rotate the compression axis according compression axis rotation in the positive direction around
to the route (2 ! 3) (Fig. 16), towards the ½0 0 1 pole, ½1 1 0, i.e. a negative crystal rotation occurs.
which lies on the great circle going through the two slip The same slip mechanism occurs for node (b). The differ-
plane normals of the pairs ð1 1 1Þ and ð1 1 1Þ. Position (2) ence with respect to node (a) is caused by the tip geometry.
for node (a) (see Fig. 16) in Fig. 15a is located where the By moving outward along the tip, the direction of the
N. Zaafarani et al. / Acta Materialia 56 (2008) 31–42 41
[10] Ma A, Roters F, Raabe D. Acta Mater 2006;54:2169–79. [22] Zehetbauer M. Acta Metall et Mat 1993;41:589–99.
[11] Wang Y, Raabe D, Klüber C, Roters F. Acta Mater 2004;52:2229–38. [23] Estrin Y, Tóth LS, Molinari A, Bréchet Y. Acta Mater
[12] Liu Y, Wang B, Yoshino M, Roy S, Lu H, Komanduri R. J Mech 1998;46:5509–22.
Phys Solid 2005;53:2718–41. [24] Roters F. Realisierung eines Mehrebenenkonzeptes in der Plasti-
[13] Casals O, Ocenasek J, Alcala J. Acta Mater 2007;55:55–68. zitätsmodellierung. 1999 Ph.D Thesis, RWTH Aachen [in
[14] Zaefferer S, Kuo JC, Zhao Z, Winning M, Raabe D. Acta Mater German].
2003;51:4719–35. [25] Roters F, Raabe D, Gottstein G. Acta Mater 2000;48:4181–9.
[15] Ma A, Roters F, Raabe D. Acta Mater 2006;54:2181–94. [26] Arsenlis A, Parks DM. J Mech Phys Solid 2002;50:1979–2009.
[16] Raabe D, Sachtleber M, Zhao Z, Roters F, Zaefferer S. Acta Mater [27] Granato AV, Lücke K, Schlipf J, Teutonico L. J Appl Phys
2001;49:3433–41. 1964:2732–45.
[17] Asaro RJ, Needleman A. Acta Metall 1985;33:923–53. [28] MSC. MARC user’s manual 2005, User Subroutines and Special
[18] Wu TY, Bassani JL. Proc Roy Soc A 1991;435:21–41. Routines, vol. D.
[19] Kocks UF. ASME J Eng Mater Tech 1976;98:76–83. [29] Konrad J, Zaefferer S, Raabe D. Acta Mater 2006;54:1369–80.
[20] Estrin Y, Mecking H. Acta Metall 1984;32:57–70. [30] Hosford WF. The mechanics of crystals and textured polycrys-
[21] Mughrabi H. Mat Sci Eng 1987;85:15–31. tals. Oxford: Oxford University Press; 1993.