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DOI: 10.1016/j.actamat.2015.07.006

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 Acta Materialia 98 (2015) 242253

Contents lists available at ScienceDirect

Acta Materialia
journal homepage: www.elsevier.com/locate/actamat

Multiscale modeling of the mechanical behavior of IN718 superalloy

based on micropillar compression and computational homogenization
A. Cruzado a,1, B. Gan a,1, M. Jimnez a, D. Barba a, K. Ostolaza b, A. Linaza b, J.M. Molina-Aldareguia a,
J. Llorca a,c,, J. Segurado a,c
a
IMDEA Materials Institute, C/Eric Kandel 2, 28906 Getafe, Madrid, Spain
b
Industria de Turbo Propulsores, 48170 Zamudio, Bizkaia, Spain
c
Department of Materials Science, Polytechnic University of Madrid, E.T.S. de Ingenieros de Caminos, 28040 Madrid, Spain

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

Article history: A multiscale modeling strategy is presented to determine the effective mechanical properties of polycrys-
Received 8 June 2015 talline Ni-based superalloys. They are obtained by computational homogenization of a representative
Revised 2 July 2015 volume element of the microstructure which was built from the grain size, shape and orientation
Accepted 2 July 2015
distributions of the material. The mechanical behavior of each grain was simulated by means of a crystal
Available online 23 July 2015
plasticity model, and the model parameters that dictate the evolution of the critical resolved shear stress
in each slip system (including viscoplastic effects as well as self and latent hardening) were obtained
Keywords:
from compression tests in micropillars milled from grains of the polycrystal in different orientations
Multiscale modeling
Ni-based superalloys
suited for single, double (coplanar and non coplanar) and multiple slip. The multiscale model predictions
Crystal plasticity of the compressive strength of wrought IN718 were in good agreement with the experimental results.
Micropillar 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Computational homogenization

1. Introduction Polycrystalline IN718 presents a strength well above 1000 MPa,

Polycrystalline IN718 is a NiFe based superalloy strengthened
with c0 and c00 precipitates, which is widely used for structural
applications up to 650700 C because of its good castability and
weldability, high mechanical properties and corrosion resistance
[1]. The microstructure of IN718 is made up by a c phase (Ni FCC
solid solution) which contains a dispersion of nm-sized
c0 -Ni3(Al,Ti) and c00 -Ni3Nb coherent precipitates within the grains
together with lm-sized metal carbides and d phase (Ni3Nb) parti-
cles at grain boundaries [24]. The c0 phase presents an ordered
cubic (FCC) L12 structure, while the c00 phase shows a body centered
tetragonal (BCT) D022 structure [5] and forms thin ellipsoidal
disc-shape precipitates. The c00 phase (which provides most of the
strengthening [6]) is a metastable form of Ni3Nb, which tends to
stabilize to the orthorhombic d phase with the D0a structure
preferentially at grain boundaries [7]. The volume fractions of
c0 and c00 phases are in the range 35% and 1020% respectively,
depending on the bulk alloy composition, the heat-treatment and
the degree of element segregation. In general the weight fraction
of (c00 + c0 + d) is around 20% [8].
Corresponding author at: IMDEA Materials Institute, Spain.
E-mail address: javier.llorca@imdea.org (J. Llorca).
1
These authors contributed equally to this work.
large ductility (>30%), a marked tension-compression strength
differential [9], softening under cyclic loading conditions [10] and
signicant losses of strength above 650 C. These properties are con-
trolled by the microstructural features of the material (grain size,
precipitate size and volume fraction, etc.) but physically-based
models capable of establishing a quantitative relationship between
the microstructure and the mechanical properties are scarce. This is
important from the fundamental viewpoint as well as from perspec-
tive of including the microstructural features into the design of
structural components.
Most of the models for the mechanical behavior of polycrys-
talline IN718 are phenomenological [9,10]. More recently, Fisk
and Lundbckl [11] proposed a physically-based ow stress model
to evaluate the residual stresses obtained during welding and heat
treatment of IN718. The parameters of the dislocation-based model
were obtained from the stressstrain curves of the polycrystalline
material at different temperatures, taking into account the
strengthening effects of precipitates. Following this work, Fisk
et al. [12] developed a model that includes the evolution
(nucleation, growth and coarsening) of precipitate size and volume
fraction in order to simulate the aging process of IN718. These
models [11,12] were a rst attempt to link the microstructure with
the macroscopic mechanical but the connection of the single crys-
tal deformation with the macroscopic ow was carried out through

http://dx.doi.org/10.1016/j.actamat.2015.07.006
1359-6454/ 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
 A. Cruzado et al. / Acta Materialia 98 (2015) 242253
the Taylor factor and this simplication limited the scope of the
approach as microscopic stress and strain elds within each grain
were not considered.
Polycrystalline homogenization [13] offers an alternative
approach for developing models of the mechanical behavior based
on the microstructure. Within this framework, the grain structure
is considered through the denition of a representative volume
element (RVE), while the single-crystal behavior is accounted for
by a crystal plasticity model. In particular, computational homog-
enization models [14,15] (based on the resolution of a boundary
volume problem on an RVE using either nite elements or fast
Fourier transform) can account for the inuence of the grain size,
shape and orientation distributions on the mechanical properties.
The accuracy of these models is strongly dependent on the
single-crystal behavior, which can be represented by a
physically-based constitutive model [1619] or by simpler phe-
nomenological crystal plasticity (CP) model [2022]. In any case,
the determination of the single-crystal behavior still remains the
main issue in polycrystalline homogenization. Different
approaches can be used to obtain the single crystal properties:
from a multiscale bottom-up approach ranging from the heteroge-
neous subgrain microstructure to the grain mesoscale [18], to an
inverse analysis strategy in which the single crystal behavior is
chosen to reproduce the results of a set of mechanical tests in poly-
crystals [1923] or of a set of indentation tests in single crystals
[24,25]. Neither strategy is fully convincing as multiscale modeling
strategies are not yet mature enough and the extrapolation of the
parameters obtained by inverse analysis strategies to other scenar-
ios (different from the one used in the inverse analysis) can be
questioned.
In this investigation, an alternative approach is proposed to
obtain the single-crystal behavior based on the use of micropillar
compression tests within individual grains from the polycrystalline
microstructure [2628]. Micropillar compression allows the direct
determination of the single-crystal stressstrain behavior without
the need of complex inverse analysis, as in the case of inverse anal-
ysis strategies based on indentation. However, it is well known that
the mechanical behavior of micropillars might be affected by their
size [29], and this approach would only be reliable if the micropillar
(a)
Carbides
250 m
(c)
phases
20 m
Fig. 1. Microstructure of wrought IN718 superalloy. (a) Optical image showing the homogeneous distribution of metal carbides throughout the sample. (b) Inverse pole gure
showing the grain orientation distribution. (c) SEM micrograph showing the decoration of grain boundary by d phase. (d) TEM micrograph showing the distribution of c0 and
c00 precipitates within the grain.
243
behavior is size independent and representative of the single crystal
behavior within the polycrystalline material. This hypothesis seems
reasonable in the case of IN718 because the internal length scale
controlling the strength, i.e., the c00 + c0 precipitate spacing, is much
smaller than the micropillar dimensions.
The multiscale modeling approach based on micropillar com-
pression tests and computational homogenization is developed
and validated on a precipitation-hardened coarse-grain IN718
wrought alloy. The room temperature single-crystal behavior was
experimentally measured by compressing single-crystal micropil-
lars machined by focused ion beam (FIB) out of individual grains
with different crystallographic orientations. The results of these
tests were used to calibrate a CP model of the c-Ni phase that
accounts for the effect of the c00 + c0 precipitation hardening.
Finally, the polycrystal behavior was obtained by computational
homogenization of an RVE of the microstructure that accounted
for the actual grain size, shape and orientation distributions. The
multiscale model predictions were in good agreement with the
macroscopic response of the polycrystal.
2. Experimental methodology
2.1. Microstructural characterization
The microstructure of the IN718 wrought alloy was character-
ized by optical microscopy, scanning electron microscopy (SEM),
using a FEI Helios Nanolab 600i instrument, and electron backscat-
ter diffraction (EBSD) in an Oxford AZTEC system. The microstruc-
ture was mainly composed of c phase grains, with negligible
amounts of dispersed metal carbides (<1 vol.%), Fig. 1a. The average
grain size was 95 lm and the grain orientations presented a ran-
dom crystallographic texture, as shown in the inverse pole gure
(IPF) map of Fig. 1b. Negligible amounts of d phase particles
(<1 vol.%) were found, all decorating the grain boundaries
(Fig. 1c). Transmission electron microscopy analysis, performed
using a JEOL 3000F instrument, revealed the presence of profuse
amounts of c0 and c00 precipitates in the interior of the grains with
sizes below 50 nm (Fig. 1d).
(b)
125 m
(d)
phases
phases
20 nm
244 A. Cruzado et al. / Acta Materialia 98 (2015) 242253
Based on the microstructural observations, the metal carbide
and d phase content was rendered negligible and the material
was modeled as a polycrystalline aggregate of c grains, containing
a ne dispersion of c0 and c00 precipitates. Thus, the micropillar
compression tests in single crystals provided the mechanical
response of the c0 and c00 strengthened c-Ni phase.
2.2. Mechanical characterization
The compressive stressstrain behavior of the wrought IN718
alloys was determined using a universal testing machine. Tests
were conducted at room temperature and a constant strain rate
of 5.0  104 s1 on cylindrical specimens 6 mm in diameter and
9 mm in length.
2.3. Micropillar compression tests
The CP model of the single crystal was calibrated from the
results of micropillar compression tests machined out of individual
grains within the polycrystal. The micropillars were milled in the
center of selected grains (Fig. 2a) by means of FIB (FEI Helios
Nanolab 600i) following an annular milling strategy, with a nal
polishing step using a current of 230 pA to minimize FIB
surface damage. Special care was taken to ensure that the resulting
pillars were completely embedded in individual grains to avoid
grain boundary effects. The crystallographic orientation of the
pillars was determined by EBSD (Fig. 2b). A wide range of crystal-
lographic orientations were tested, and they are shown in the
reduced inverse pole gure (IPF) of Fig. 2b. Plastic deformation in
FCC c-Ni phase occurs on the octahedral {1 1 1} h1 1 0i slip
systems and the micropillar orientations were selected to promote
single slip, double (coplanar and non-coplanar) and multiple slip.
Fig. 2. (a) SEM micrograph of polycrystalline IN718 with the micropillars machined out in the center of various grains. (b) IPF showing the orientation of the micropillars.
Fig. 3. (a) SEM micrograph of a micropillar machined from the IN718 polycrystalline specimen. (b) Cross-section of the micropillar showing the upper and lower diameter
and the height.
The micropillar aspect ratio (length/diameter) was 2.4 to avoid
buckling during compression [30] and the micropillar diameter
was varied between 1 and 18 lm to determine the range of
micropillar sizes that rendered a size independent response. One
of the as-milled micropillars, with 5 lm in diameter and 12 lm
in length, is depicted in Fig. 3a. The annular milling parameters
used resulted in a minimum taper (<1.5) of the pillars, as shown
in the FIB cross-section of Fig. 3b.
Most of the pillars were compressed using a circular diamond
at punch of 10 lm in diameter inside an instrumented nanoin-
dentation system (Hysitron TI950). Tests were carried out in dis-
placement control at three different strain rates (104, 103 and
102 s1). Only pillars with diameter <7 lm (which constitute the
majority of the results included in this paper) could be compressed
in this system because of the at punch diameter. Larger pillars (up
to 18 lm in diameter) were tested in a Micromaterials Nanotest
system (maximum load of 500 mN) with a circular diamond at
punch of 30 lm in diameter. The experimental loaddisplacement
curves were corrected for the extra compliance associated with the
elastic deection of the matrix at the base of the pillar using the
Sneddon correction [31]. They were transformed in either engi-
neering stressstrain curves or engineering resolved shear stress
strain curves from the initial length and upper diameter of the pil-
lar and the initial Schmid factor calculated from the crystallo-
graphic orientation of the pillar.
3. Multiscale modeling strategy
3.1. Crystal plasticity model
A detailed description of the CP constitutive model and its
implementation is provided in [14]. It is briey outlined here for
completeness. The CP model is based on the multiplicative
 A. Cruzado et al. / Acta Materialia 98 (2015) 242253 245

decomposition of the deformation gradient, F, into its elastic Fe and hardening modulus at large strains and ca is the accumulated shear
plastic part Fp according to strain in all slip systems, which is given by
Z tX
F Fe Fp 1
ca jc_ a jdt 10
The plastic velocity gradient Lp in the intermediate (relaxed) 0 a
conguration is dened as the sum of the shear rates, c_ a , on all
the slip systems a according to 3.2. Single-crystal CP constitutive model
N slip
1 X
Lp F_ p Fp c_ a sa0  ma0 2 The CP model was implemented in a user subroutine UMAT for
a1 the c0 and c00 strengthened c-Ni phase. Slip trace analysis in poly-
where sa0 and ma0 are the unit vectors in the slip direction and the crystalline IN718 [33], as well as the micropillar compression tests
normal to the slip plane in the reference conguration respectively. that will be presented below, indicate that plastic deformation
The elastic strain is dened using the Green-Lagrange strain only took place in octahedral {1 1 1} h1 1 0i slip systems. This is con-
tensor, Ee, is expressed as sistent with the FCC structure of the c phase and it is presumably
due to the low volume fraction (<20%) of c0 and c00 small precipi-
1 eT e tates, as opposed to the high volume fraction (>50%) of large c0 pre-
Ee F F  I 3
2 cipitates observed in other Ni-based superalloys where
where I stands for the second order identity tensor. The symmetric pseudo-cubic systems operate [34]. Therefore, only the 12 octahe-
second Piola-kirchhoff stress tensor in the intermediate congura- dral {1 1 1} h1 1 0i slip systems were implemented in the CP model.
tion, S, is related with the Green-Lagrange strain tensor according to The single crystal elastic properties were obtained from literature
[21] and can be found in Table 1. The parameters that control the
S CEe 4 plastic deformation of each slip system s0 , ss , h0 , hs and qab were
where C stands for the fourth order elastic stiffness tensor on the obtained by comparison of the experimental stress-strain curves
single crystal. Thus, the resolved shear stress sa on the slip plane of micropillars of 5 lm in diameter in different orientations with
a is obtained as the projection of the Kirchoff stress on the slip sys- the nite element simulations of the micropillar compression tests
tem according to presented below.
 
1 eT e
sa C F F  I : sa0  ma0 5 3.3. Finite element model of micropillar compression
2
The crystal is assumed to behave as an elasto-viscoplastic solid The FE model used for the simulation of the micropillar com-
in which the plastic slip rate for a given slip plane system follows a pression tests is shown in Fig. 4. The model represents the geome-
power law dependency try of the micropillars with 5 lm in diameter, including the radius
 a 1=m of curvature of the llet (approximately r = 1.5 lm) and the taper
js j angle b  1.5, as measured in Fig. 3b. Including the taper is crucial
c_ a c_ 0 sgnsa 6
sac because it is has been shown that neglecting taper might result in
an overestimation of the elastic modulus and of strain hardening
where c_ 0 stands for the reference strain rate, sac is the critical
and an increase of the apparent yield stress [35].
resolved shear stress (CRSS) of ath slip system at the reference
The micropillar and the supporting material were modeled as a
strain rate and m the rate sensitivity parameter.
single crystal. Eight node lineal brick elements (C3D8 with full
The evolution of the CRSS of a given slip system a, sac , is
integration in Abaqus [36]) were used for discretization. The total
expressed as,
number of elements in the model was 15359 elements, following
X
s_ ac hab jc_ b j 7 a mesh convergence analysis. The at punch was modeled as a
b rigid body, with a lateral stiffness of 10 lN/nm, which approxi-
mately corresponds to the lateral stiffness of the indenter used in
where b stands for any slip system. hab is the strain hardening mod-
the experiment [37]. The contact between the at punch and the
ulus due to self and latent hardening, which can be expressed in a micropillar head was modeled according to a Coulomb friction
simplied manner according to
hab qab h 8

where qab are the interaction coefcients that represent the inu-
ence of the hardening between different slip systems, and h corre-
sponds to the self hardening modulus. The evolution of the self
hardening was described according to the Voce hardening model
proposed in [32],
 
h0 hs ca
hca hs h0  hs exph0 ca =ss s0 9
ss  s0
where h0 is the initial hardening modulus, s0 the initial yield shear
stress, ss the saturation yields shear stress, hs the saturation

Table 1
Elastic constants of the cubic IN718 single crystal [21].

C11 (GPa) C12 (GPa) C44 (GPa)

259.6 179 109.6
Fig. 4. Finite element model of the micropillar compression tests.
246 A. Cruzado et al. / Acta Materialia 98 (2015) 242253
Fig. 5. Log-normal grain size distribution of polycrystalline IN718 (solid line) and
the corresponding grain size distribution in the RVE of the microstructure.
model, with a friction coefcient of 0.1 [37]. The base of the sup-
porting material was fully constrained, while a at punch was
moved in the vertical direction at a constant speed.
3.4. Computational homogenization framework
The effective behavior of polycrystalline IN718 was obtained by
computational homogenization of an RVE of the microstructure.
The grain size distribution in the polycrystal was measured from
a cross-section that included approximately 300 grains. The exper-
imental 2D grain size distribution was transformed to a 3D distri-
bution assuming spherical grains. The open source software
StripStar [38] was used to this purpose. The 3D grain radii distribu-
tion was then approximated by a lognormal function (r = 0.70862,
l = 3.65) by means of the LevenbergMarquadt algorithm (correla-
tion coefcient of 0.93) and is shown in Fig. 5. The mechanical
behavior of each crystal in the RVE was given by the CP model pre-
sented in Sections 3.1 and 3.2. The cubic RVEs were generated from
the Voronoi tessellation of a set of points, which divided the initial
volume in a number of polyhedral [39]. A Monte Carlo algorithm
was developed to generate the position of the set of points used
Fig. 6. Finite element model with 130000 elements of an RVE containing 210 grains following the lognormal distribution in Fig. 5. A cross-section of the RVE parallel to one of
the cube faces is shown to the right, showing the periodicity of the microstructure.
for the tessellation, so the grain size distribution in the RVE fol-
lowed the experimental grain size distribution (Fig. 5). The details
of the algorithm developed can be found in Appendix A.
The Voronoi tessellation was carried out with Neper [40] from
an extended cloud of points obtained by a periodic copy in the
three directions of space of the point distribution obtained by the
Monte-Carlo method in order to preserve the periodicity of the
microstructure in the RVE. The nal shape of the RVE was not cubic
because grains intersecting the cube faces were not cut and copied
into the opposite face but were maintained in their positions. This
strategy avoided meshing problems related with the development
of very small grains near the cube surfaces. The periodic RVE was
nally meshed with the open source program Gmsh [41].
10-node quadratic tetrahedral elements (C3D10 with full integra-
tion in Abaqus [36]) were used for the discretization and the mesh
quality was very high (only 0.26% of distorted elements). Because
the texture in the material was negligible, the grains orientations
were randomly generated in the rotation group SO3. Finite element
models of RVEs containing from 20 to 472 grains and 615 to 26007
elements per grain were created to analyze the inuence of ele-
ment size and number of grains in the numerical results. One of
them, which includes 210 grains, is depicted in Fig. 6.
The generated RVEs are periodic along the axes of the original
cube of length L although they do not have a cubic shape because
grains are not limited by the faces of the original cube to avoid dis-
torted elements. Nodes A and B in the same location of opposite
surfaces can be grouped in pairs of periodic nodes and the initial
distance between them is given by xB  xA LAB , where
LAB = (L,0,0), (0,L,0) or (0,0,L) depending of the surface orientation.
Uniaxial compression of the RVE was simulated by applying peri-
odic boundary conditions to each node pair according to
  ILAB
uB  uA F 11
where F  stands for prescribed macroscopic deformation gradient
and uA and uB the displacement vectors of the paired nodes. If some
components of the far-eld deformation gradient are not known a
priori (mixed boundary conditions, as in uniaxial compression),
the corresponding components of the effective stresses are applied
instead following the strategy presented in [23].
4. Results
4.1. Effect of pillar size
The effect of pillar size on the experimental stressstrain
response was assessed by performing tests on pillars with
 A. Cruzado et al. / Acta Materialia 98 (2015) 242253 247

Fig. 7. CRSS vs. strain curves of micropillars of different diameter oriented for single slip tested in compression. (a) Diameter range from 1 to 7.5 lm. (b) Diameters of 6 and
18 lm.

diameters in the range 118 lm at an average strain rate of parameters were obtained from the behavior of micropillars of
103 s1. To this end, micropillars with different size were milled 5 lm in diameter.
in grains with the same or similar crystallographic orientation
(close to either h2 4 5i or h2 3 5i) to rule out any plastic anisotropy
4.2. Calibration of the CP model
effects. They were favorably oriented for single slip with Schmid
factors (SF) of 0.452 and 0.445 for the orientations h2 4 5i and
As shown in Fig. 7, the slope of the initial loading decreases with
h2 3 5i respectively. The critical resolved shear stress (CRSS) vs.
micropillar diameter, leading to a much more compliant response
strain curves of 4 micropillars with diameters between 1 and
than that found upon unloading. While the unloading slope yields
7.5 lm are plotted in Fig. 7a and the corresponding SEM
the correct elastic modulus, it is well known that the initial loading
micrographs of the deformed micropillars are shown in Fig. 8ad,
slope in a micropillar tests is strongly affected by asperities of the
which conrmed that plastic deformation took place by single slip.
surface and/or incorrect alignment between the at punch and the
The micropillar of 1 lm in diameter presented a stiffer
head of the pillar [37]. This misalignment induces a stress concen-
initial response and a higher CRSS while the CRSSstrain behav-
tration at the initial contact point of the micropillar, which leads to
ior of the micropillars with diameters between 3 lm and 7.5 lm
early yielding and to the apparent reduction of the initial loading
were practically identical, except for a slight reduction in the slope
stiffness while the unloading slope is free for this artifact once full
of the initial loading slope with pillar diameter, that will be
plastic contact has been established between the at punch and
discussed in more detail in the next section. In all cases, the
the pillar. Unfortunately, this experimental uncertainty makes it
CRSSstrain curves displayed unloading events as a result of
difcult to establish the onset of plastic yielding from the stress
dislocation bursts, upon which the high frequency feedback loop
strain curves, and this information is necessary to calibrate the
of the system reacts relaxing the load to maintain the prescribed
parameters of the CP model. This limitation can be overcome fol-
displacement rate.
lowing the strategy proposed by Kupka et al. [26] to obtain the
In addition to these tests, two new pillars with 6 and 18 lm in
evolution of the stress with the plastic strain in micropillar com-
diameter were milled in grains with h3 2 6i (SF = 0.467) orientation.
pression tests. To this effect, the experimental strain er was rst
The CRSSstrain curves are plotted in Fig. 7b and the SEM micro-
corrected by subtracting the elastic strain, which was obtained for
graphs of the deformed micropillars are depicted in Fig. 8e and f,
each stress level from the unloading slope Sunload according to
showing single slip. These micropillars were tested in a different
nanoindentation system, as described in Section 2.2, due to the r
large load required for the 18 lm pillar. The dynamic response of
e1 r er  12
Sunload
this system was not fast enough to unload the pillar in reaction
The original and the corrected stress-strain curves are shown in
to the dislocation bursts, resulting in repeated pop-in events,
Fig. 9a for the case of a micropillar of 3 lm in diameter oriented for
instead of load relaxations. Except for this, the CRSSstrain curves
single slip in the [3 2 5] direction. After this correction, the unload-
measured in these micropillars were indistinguishable from those
ing segment of the stressstrain curve appears as a vertical line.
measured in micropillars with diameter between 3 and 7.5 lm.
Afterwards, the initial yield point (ry , e1y ) was determined as the
These results conrm the hypothesis that the micropillar response
point at which the maximum slope of the loading curve decreased
can be regarded as independent of the micropillar diameter, and
by 20% with respect to the initial slope, and the corrected plastic
representative of the single-crystal bulk behavior, at least for
strain free of the initial loading artifacts-was given by
micropillars with diameters above 3 lm in the case of IN718.
This behavior presumably occurs because the internal length scale ep r e1 r  e1y 13
controlling the strength, i.e. the c00 + c0 precipitate spacing, is much
smaller (of the order of 50 nm) than the micropillar dimensions. and the corresponding stressplastic strain curve can be found in
However, the CRSSstrain curves in Fig. 7a also showed a clear size Fig. 9b.
effect of the type the smaller the stronger in micropillars of 1 lm The CRSSplastic strain curves corresponding to the micropillar
in diameter. The origin of this behavior is intriguing but is beyond compression tests were obtained using this procedure and they
the scope of this paper. Based on these results, the CP model were used to determine the parameters of the CP model as follows.
248 A. Cruzado et al. / Acta Materialia 98 (2015) 242253

(a) (425) (b) (325)

500 nm 1
m
m

(c) (235) (d) (245)

1.5 m 2 m
(e) (326) (f) (326)

1.5 m 10 m

Fig. 8. SEM micrographs of micropillars with different size deformed in the single slip condition. (a) 1 lm oriented in [4 2 5]. (b) 3 lm oriented in [3 2 5]. (c) 5 lm oriented in
[2 3 5]. (d) 7.5 lm oriented in [2 4 5]. (e) 6 lm oriented in [3 2 6] and (f) 18 lm oriented in [3 2 6].

Fig. 9. Correction of the stressstrain curves of the micropillar compression tests to obtain the stressplastic strain curve. (a) Original and corrected stressstrain curve
according to Eq. (12). The yield point is indicated in the corrected curve. (b) Stressplastic strain curve obtained from Eq. (13). The results in this gure correspond to a
micropillar of 3 lm in diameter oriented for single slip in the [3 2 5] direction and tested at an average strain rate of 103 s1.

According to Eq. (6), the actual CRSS in a given slip system a, sas , where c_ a0 and sac stand for the reference strain rate and the CRSS in
depends on the shear strain rate c_ a in the form the system a at the reference strain rate. The rate sensitivity expo-
 a nent m was obtained from the CRSSplastic strain curves at average
c_ 1 sa
ln ln j sa j 14 strain rate of 102 s1 in h1 2 3i micropillars and at 103 s1 and
c_ a0 m sc 104 s1 in h2 3 5i micropillars oriented for single slip (SF = 0.467
 A. Cruzado et al. / Acta Materialia 98 (2015) 242253 249

Fig. 10. (a) CRSS vs. plastic strain of micropillar oriented for single slip tested at different strain rates at room temperature. (b) Strain rate sensitivity parameter m of IN718 at
room temperature as obtained from micropillar compression tests.

Fig. 11. Experimental and simulated CRSS vs. plastic strain curves of compression tests of micropillars of 5 lm in diameter oriented for single slip. (a) Average strain rate
103 s1, micropillar orientation [2 3 5]. (b) Average strain rates 102 s1 and 103 s4, micropillar orientation [1 2 3] and [2 3 5].

Table 2
Self hardening and latent hardening parameters of the Voce law.
s0 (MPa) ss (MPa) h0 (GPa) hs (GPa)
465.5 598.5 6.0 0.3
and SF = 0.451 for h1 2 3i and h2 3 5i, respectively), Fig. 10a. The
average strain rate in each slip system can be computed as the aver-
age strain rate of the micropillar divided by the Schmid factor and
the corresponding CRSS was taken as the one at a plastic strain of
0.04. The choice of the plastic strain to determine the CRSS was
not very critical as the CRSSplastic strain curves were practically
parallel for plastic strains >0.02. These results (normalized by the
shear strain rate and the CRSS for the tests carried out at an average
strain rate of 103 s1) are plotted in Fig. 10b in bilogarithmic coor-
dinates. The strain rate sensitivity parameter m = 0.017 was
obtained from the inverse of the slope, the straight line tted by
the least squares method to these experimental data, according to
Eq. (14). This result indicates that strain rate sensitivity of IN718
at room temperature is very small and it is not surprising that linear
regression shows a relative poor correlation index with the experi-
mental data.
qab The second step to calibrate the crystal plasticity model was to
obtain the parameters of the Voce law each slip system, namely h0 ,
1
s0 , ss and hs . To this end, the nite element model of the micropil-
lar compression test, presented in Section 3.3, was used to simulate
the stressstrain curve of h2 3 5i micropillars, oriented favorably for
slip with a SF = 0.451 at an average strain rate of 103 s1. The
experimental CRSS vs. plastic curve is plotted in Fig. 11a together
with the results of the numerical simulation obtained with the
parameters shown in Table 2. It is worth noting that the values
of the initial and saturation CRSSs (s0 and ss ) obtained from the
nite element simulation of the micropillar are slightly below
the ones that would be directly obtained from the CRSSplastic
strain curve and the Schmid factor because the numerical model
accounts for the geometrical strain hardening introduced by the
tapering of the micropillar as well as for lattice rotation during
the test. The numerical model can also take into account the slight
inuence of the strain rate on the mechanical response of the
micropillars, as shown in Fig. 11b, in which the results of the
numerical simulations are compared with the CRSS vs. plastic
250 A. Cruzado et al. / Acta Materialia 98 (2015) 242253

Fig. 12. (a) Simulated stress vs. plastic strain curves of micropillars oriented for single slip (h2 3 5i) and double slip (h4 1 4i) obtained with qab = 1 and 2. (b) Experimental and
simulation results of micropillars oriented in h0 1 2i (non co-planar double slip) and in h4 1 4i (co-planar double slip). Simulations were carried out with qab = 1. (c) SEM of a
micropillar deformed along h0 1 2i showing non coplanar double slip. (d) SEM of a micropillar deformed along h4 1 4i showing coplanar double slip. All simulations and
experiments in this gure were carried out in micropillars of 5 lm in diameter at an average strain rate of 103 s1.

strain curves measured at 102 and 104 s1 in micropillars ori-
ented for single slip in orientations h1 2 3i and h2 3 5i, respectively.
The previous simulations were carried out under the assump-
tion that qab = 1 (Eq. 8). The choice of qab was irrelevant in the case
of micropillars oriented for single slip, as shown in the simulations
depicted in Fig. 12a for a micropillar of 5 lm in diameter oriented
along h2 3 5i for single slip. Nevertheless, the contribution of latent
hardening was not negligible in the case of double slip and the ow
stress of micropillars oriented along h4 1 4i for double slip
depended on qab (Fig. 12a). The actual value of qab was obtained
from the mechanical response of micropillars oriented along
h4 1 4i and h0 1 2i. h0 1 2i micropillars showed activity in two non
coplanar slip systems, {1 1 1} h1 0 1i and {1 1 1}h1 0 1i, with a
SF = 0.49 (Fig. 12c), while the micropillar oriented in h4 1 4i
deformed in two coplanar slip systems, {1 1 1}h0 1 1i and
{1 1 1}h1 1 0i, with SF = 0.43 (Fig. 12d). The simulations carried
out with qab = 1 provided the best approximation to the experi-
mental data (Fig. 12b) indicating that IN718 follows an isotropic
hardening model.
The CP model of IN718 was validated by comparing the results
of the micropillar compression tests in different orientations with
actual experimental results. They are shown in Fig. 13a for
micropillars of 5 lm in diameter tested at an average strain rate
of 103 s1 along h1 2 6i (SF = 0.488) and h4 5 6i (SF = 371) orienta-
tions. Numerical simulations were very close to the experimental
results in h1 2 6i while the simulations in h4 5 6i orientation overes-
timated the experimental ow stress. This difference may be due
to the proximity of the h4 5 6i direction to the h1 1 1i orientation,
which is the stiffest and strongest orientation of the crystal.
Deformation along h1 1 1i leads to the formation of a shear band
(Fig. 13c), presumably as a result of the activation of a secondary
slip system during deformation, although the exact sequence of
events leading to this behavior is not known and is currently under
study. Finally, simulation of the deformation along h0 0 1i was very
accurate (Fig. 13b) although this orientation led to multiple slip
with the activation of 8 simultaneous slip systems (Fig. 13d).
Finally, the predictive capacity of the CP model can be assessed
by comparing the SEM of the deformed micropillar after compres-
sion along the h2 1 2i orientation (where both coplanar slip systems
are active) (Fig. 14a), with the corresponding predictions of the
nite element model (Fig. 14b). The model was able to reproduce
accurately the shape of the deformed micropillar as well as the
location of the slip band.
4.3. Computational homogenization
The CP model calibrated in the previous section was able to
reproduce the mechanical behavior of IN718 single crystals in dif-
ferent orientations, which include single, double (coplanar and non
coplanar) and multiple slip. This model was used as the constitu-
tive equation of the single crystals within a computational homog-
enization framework to obtain the effective properties of the
polycrystal.
A sensitivity analysis was rst carried out to assess the inu-
ence the mesh size and of the number of grains in the RVE on
the predictions of the effective response of the polycrystal.
 A. Cruzado et al. / Acta Materialia 98 (2015) 242253 251

(111) (001)
(c) (d)

Fig. 13. (a) Experimental and simulation results of micropillars oriented in h5 4 6i and h2 1 6i orientations. (b) Experimental and simulation results of micropillars oriented in
h0 0 1i orientation (c) SEM micrograph of a square micropillar deformed along h1 1 1i showing the formation of a shear band. (d) SEM micrograph of a micropillar deformed
along h0 0 1i showing multiple slip. All simulations and experiments in this gure were carried out in micropillars of 5 lm in diameter at an average strain rate of 103 s1.

Fig. 14. (a) SEM micrograph of micropillar of 5 lm in diameter deformed up to 0.2 in h2 1 2i orientation at an average strain rate of 103 s1. (b) Contour plot of the
accumulated plastic strain superposed to the deformed mesh obtained from the nite element model.

Numerical simulations were performed with three different mesh
sizes with 615, 2466 and 26007 nite element per grain in RVEs
containing 21 and 199 grains. The differences in the stress-strain
curve between the coarse and the ne meshes were always below
1% up to an applied strain of 20%. Similarly, simulations were car-
ried out with RVEs containing 20, 210 and 472 grains and 610 nite
elements per grain. The differences in the stressstrain curves
between the models were also very small (<1%).
Thus, the model with 210 grains and 610 nite elements pre
grain was selected to predict the mechanical behavior of the
IN718 polycrystal. The grain size distribution followed the
log-normal distribution measured experimentally and numerical
simulations were carried out with four different realizations of
the random grain orientation distribution. The differences in the
mechanical response calculated with different realizations were
below 1.3%, which indicates the error in the effective response of
the polycrystalline model for a given set of CP parameters.
The effective response obtained by computational homogeniza-
tion is compared with the experimental behavior in Fig. 15 in
terms of the true stresslogarithmic strain curves. The agreement
between them was fairly good: the maximum difference in the
compressive ow stress was below 4% and the strain hardening
252 A. Cruzado et al. / Acta Materialia 98 (2015) 242253
Fig. 15. Experimental result and numerical simulation obtained by computational
homogenization of an RVE of the true stressstrain curve in compression of IN718.
of the model and of the material was identical. This is remarkable
taking into account the scatter associated with the micropillar
compression tests was around 5%. Moreover, it should be high-
lighted the multiscale nature of the approach because all the ingre-
dients in the polycrystalline homogenization strategy were
obtained at lower length scales from the microstructure of the
polycrystal and the mechanical properties of the single crystals
within the polycrystal.
An interesting consequence of the accuracy of this prediction is
that grain boundaries do not contribute to the hardening of this
coarse grained polycrystal. If this mechanism were relevant here,
the simulated stressstrain curves (that do not account for slip gra-
dients) should have underestimated the experimental ow stress.
The physical reason of the negligible effect of grain boundaries is
probably the small distance between precipitates that controls
the plastic response of the material, and renders negligible the
strengthening contribution of grain boundaries for this grain size.
5. Conclusions
A multiscale modeling strategy has been developed to predict
the mechanical behavior of polycrystalline Ni-based superalloys.
The effective properties of the polycrystalline material were
obtained by computational homogenization of an RVE of the
microstructure that accounts for the grain size, shape and orienta-
tion distributions. The mechanical behavior of each grain is given
by a crystal plasticity model and the model parameters that dictate
the evolution of the CRSS in each slip system (including viscoplas-
tic effects as well self and latent hardening) were obtained from
compression tests in micropillars milled from grains of the poly-
crystal in different orientations suited for single, double (coplanar
and non coplanar) and multiple slip. The ability of the crystal plas-
ticity model to reproduce the mechanical behavior of micropillars
was validated by the accurate prediction of micropillar compres-
sion tests in different orientations and at various strain rates. In
addition, the model was able to capture the dominant deformation
mechanisms in the micropillars, including the formation of the slip
bands observed. It was demonstrated that mechanical behavior of
micropillars was size independent (and, thus representative of the
behavior of the material within the grains) for micropillars with a
diameter above 3 lm because the ow stress in this material was
controlled by the distance between nm-sized c0 and c00 precipitates
dispersed in the solid solution c face.
The mechanical behavior in compression of the polycrystal pre-
dicted with this multiscale strategy was in good agreement with
the experimental results and validated the whole strategy. The
methodology presented in this paper, together with the recent
advances in the characterization of the mechanical properties of
lm-sized specimen milled from grains and grain boundaries in
the polycrystal, presents a large potential to carry out virtual tests
of polycrystalline Ni-based superalloys to predict the inuence of
the microstructure on key macroscopic features. This includes,
among others, the strength differential, the effect of temperature
on the strength, the creep and the fatigue resistance, etc.
Acknowledgments
This investigation was supported by the MICROMECH, funded
by the European Union under the Clean Sky Joint Undertaking,
7th Framework Programme (CS-GA-2013-620078). TEM was car-
ried out in the National Center for Electron Microscopy of the
Complutense University of Madrid.
Appendix A.
An algorithm has been developed to generate the coordinates of
a set of N points p = pi that can lead by Voronoi tessellation to an
RVE whose grain size distribution follows a prescribed one. To this
end, it is necessary to minimize an error function O(p) dened as
X
N
Op jPDF exp V j  PDF p V j j DV A1
j1
where PDF exp and PDF p are the probability density functions of the
experimental and the target grain size distributions, respectively,
which indicate the probability for a grain to have a volume in the
range V j and V j DV, where DV V max V min =N and V max and
V min stand for the maximum and minimum grain sizes, respectively.
An iterative process based on the Monte Carlo method was used
to minimize O(p). Let p(k) the set of points at iteration k, that leads
to an error Opk higher than a prescribed value. The new set p(k+1)
is obtained by moving a random point pi in a random direction a
random distance Dx in the range between 0 and 3.5D, where D is
the average grain size of the experimental distribution. A new
Voronoi tessellation is carried for the set pk1 , and the error func-
tion Opk1 is computed from the new PDF p . Whether or not the
set pk1 is chosen as the starting point for the next iteration
depends on the parameter prob, which is given by
  
Opk1  Opk
prob min 1; exp  A2
A Op k
where A is a parameter, chosen equal to 0.02 in this case. If the error
is reduced, Opk1 6 Opk , prob = 1 and the set pk1 is chosen as
the starting point for the next iteration. On the contrary,
prob 2 0; 1 if the error increases and a random number is gener-
ated, r 2 0; 1. The set pk1 is chosen as the starting point for
the next iteration if r < prob; otherwise, the old set pk is again
used as the starting point. This algorithm, that is able to accept dis-
tributions that slightly increase the error, leads to an improvement
of the efciency of the Monte Carlo method. The process is repeated
until the error function Op is smaller than a prescribed tolerance.
This algorithm has been programmed in Matlab.
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