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Adhesion of nickel–titanium shape memory alloy wires to thermoplastic materials: theory and

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2012 Smart Mater. Struct. 21 035022

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IOP PUBLISHING SMART MATERIALS AND STRUCTURES
Smart Mater. Struct. 21 (2012) 035022 (17pp) doi:10.1088/0964-1726/21/3/035022

Adhesion of nickel–titanium shape

memory alloy wires to thermoplastic
materials: theory and experiments
F C Antico1 , P D Zavattieri1 , L G Hector Jr2 , A Mance2 , W R Rodgers2
and D A Okonski2
1
School of Civil Engineering, Purdue University, West Lafayette, IN 47907-2051, USA
2
GM Research and Development Center, Warren, MI 48090-9055, USA

E-mail: zavattie@purdue.edu

Received 15 September 2011, in final form 16 January 2012

Published 17 February 2012
Online at stacks.iop.org/SMS/21/035022

Abstract
We present a combined experimental/theoretical study aimed at enhancing adhesion between a
NiTi wire and a thermoplastic polyolefin (TPO) matrix in which it is embedded. NiTi wire
surfaces were subjected to the following surface treatments prior to pull-out tests: (i) treatment
with an acid etch or chemical conversion coating and (ii) application of a surface
microgeometry to enhance mechanical interlocking between the wire and the TPO matrix.
Nanometer to micron-scale NiTi wire surface features were examined with atomic force
microscopy. The extent to which each treatment increased the pull-out force was quantified.
Existing theoretical models of wire pull-out based upon strength of materials and linear elastic
fracture mechanics are reviewed. Results from a finite element model (FEM), wherein the
NiTi/TPO matrix interface is modeled with a cohesive zone model, suggest that the interface
behavior strongly depends on the cohesive energy. The FEM model properly accounts for
energy dissipation at the debonding front and inelastic deformation in a NiTi wire during
pull-out. We demonstrate that residual stresses from the molding process significantly
influence mode mixity at the debonding front.
(Some figures may appear in colour only in the online journal)

1. Introduction such as thermoplastic vulcanizate (TPV) and thermoplastic

The fabrication and application of shape memory alloy (SMA)
wire-reinforced polymer matrix composites for actuators has
gained significant importance during the last decade [1–4].
The capabilities of these smart composites, especially impact
resistance, high-temperature mechanical properties, shape
control, fatigue resistance, and vibration and buckling
response, have been demonstrated [5–9]. Considerable effort
has been focused on applying knowledge acquired in
laboratory settings directly to industrial applications [8].
Shape recovery makes these alloys good candidates for
actuators in transportation industries since they can be
activated via applied stress and temperature change and
do not substantially contribute to vehicle mass. Typical
automotive applications employ thermoplastic polymers,
olefins (TPO), which require manufacturing processes such
as injection molding, compression molding or extrusion
techniques. Although the high temperatures and pressure
levels required for these processes make embedding
SMA wires particularly challenging, a recent study has
shown that an efficient procedure to fabricate these
composites is by a combination of extrusion and injection
molding [87]. Figure 1(a) shows composite films made
of a nickel–titanium (NiTi) wire-reinforced thermoplastic
vulcanizate using extrusion molding. A subsequent step where
the film is overmolded using standard injection molding yields
a composite material with the NiTi wires located at very
specific locations, typically eccentric from the neutral plane
of the composite (figure 1(b)). These types of composites
are ideal for bending actuation in automotive applications.

0964-1726/12/035022+17$33.00 1 c 2012 IOP Publishing Ltd Printed in the UK & the USA

Smart Mater. Struct. 21 (2012) 035022 F C Antico et al

10 cm 10 cm

(a) (b)

5 cm
(c) (d)
Figure 1. SMA-reinforced thermoplastic composites for actuation devices. (a) Resulting extruded film with embedded NiTi wires using
two different thermoplastic vulcanizates. (b) Composite material made from overmolding the extruded film using a standard injection
molding process. This technique enables better control of the position of the NiTi wires. Bending of the composites is achieved due to shape
recovery of the prestrained NiTi wires located off of the neutral plane. (c) and (d) Cyclic experiments showing bending actuation of
SMA/thermoplastic composites. Shape recovery can be obtained by temperature-induced martensitic-to-austenitic transformation (e.g. via
electrical current). The white background shows the expected deflection (vertical axis) of the composite as a function of the current
(horizontal axis) that flows through the SMA.

Bending can be achieved by inducing shape recovery to
prestrained NiTi wires that are embedded in the polymeric
matrix at different locations through the thickness of a thin
specimen. If the NiTi wire is bonded to the matrix, it
transmits forces to the matrix inducing a distributed bending
moment to the entire composite. Figures 1(c) and (d) show
the type of bending actuation that can be obtained from these
materials under thermal cyclic loading. Non-trivial challenges
associated with actuator fabrication processes and a lack
of optimal component designs are barriers to wide-scale
implementation of SMA materials in transportation industries
in general. A significant barrier is load and displacement
transfer from NiTi shape memory wires to a polymer matrix;
this is primarily controlled by chemical and mechanical
bonding at the interface between these two materials.
Nickel–titanium shape memory alloys typically have low
surface energies which limits their ability to effectively bond
to other materials. To make matters worse, TPV and TPO
also have low surface energies. Poor interfacial adhesion due
to the lack of sufficient chemical and/or mechanical bonding
between NiTi and polymeric materials results in premature
failure and insufficient actuation response.
Much of the extant literature on shape memory
materials focuses on quantifying material properties [10]
with minimal attention to adhesion in actuators. Poor
interfacial bonding due to low surface energies can be
addressed through mechanical interlocking [2, 11–16, 22–24],
chemical treatments [17–19] or by simply neglecting
adhesion and facilitating the sliding of the SMA material
and anchoring it at the ends of the specimen (e.g. by
inserting it in tubes with internal low adhesion/friction
surfaces) [20, 21]. Adhesion enhancements via mechanical
interlocking in SMA actuators have been investigated
with only the most rudimentary means such as hand
sanding, sandblasting [11] or wire twisting [12, 13]
to alter otherwise smooth surfaces [11–13]. While these
approaches help to alter the smooth surface of the SMA and
improve mechanical interlocking between the wire and the
matrix, these methods are either impractical or prone to leave
impurities and debris. The existing literature does not address
repeated actuation [7] or fatigue of devices using SMA.
However, the degradation of polymers through repetitive
heating of an SMA has been identified as a critical obstacle
to increasing the durability of these materials [14, 25].
Chemically functionalizing NiTi wire surfaces to enhance
adhesion to polymeric materials is attractive from the
standpoint that additional mechanical fixtures can be avoided.
This idea, which is the basis of aluminum sheet conversion

2
Smart Mater. Struct. 21 (2012) 035022
coating treatments with chemical coupling agents, was
applied by Smith et al [19] to improve adhesion between
NiTi wires and plexiglass. They noted improvements in
adhesive strength of up to 100% with silane coupling agents.
While this is encouraging, silane coupling agents must be
hydrolyzed before use, and the hydrolyzed solutions have
finite lifetimes. Chemical coupling agents function in several
ways. They can directly bond to a polymer matrix by
R
reacting with functional groups in the polymeric matrix; they
can incorporate themselves into the polymer matrix due to
the similarity of their structure to that of the polymer; or
they can interact through van der Waals bonding with the
polymeric matrix. Oxide surface functionalization using a
R
coupling agent typically requires hydroxyl groups (−OH)
on the NiTi surface. Phosphorus-containing compounds [26]
and organosilane-coupling agents react with oxide/hydroxide
groups and bind to metal oxide surfaces via a condensation
reaction. A heating step may be employed after treatment with
the coupling agent in order to ensure complete condensation.
In this paper, we explore two experimental methodologies
for improving adhesion between a NiTi SMA in wire form
and a polymeric matrix. These are: (i) functionalizing a NiTi
wire surface with a chemical conversion coating or coupling
agent or (ii) application of a surface microgeometry to an
NiTi wire surface for enhancement of mechanical interlocking
between the wire and the polymer matrix. Although prior
work has focused on enhancing NiTi wire adhesion in carbon
fiber-reinforced polymers with acid etching [17] and silane
coupling agents [18, 19], it appears that organophosphorus
compounds have yet to be extensively explored in cases
where an inexpensive polymeric matrix, such as thermoplastic
polyolefin (TPO), is required. There is indeed evidence from
both the theoretical [27] and experimental [28, 29] literature
that organophosphorus compounds will react with surface
oxides and hydroxides on NiTi alloys. However, the extent
to which these compounds improve NiTi wire adhesion with
a polymeric matrix has not been investigated. Atomic force
microscopy (AFM) and wire pull-out tests in conjunction with
numerical models are used to examine and quantify NiTi
wire/TPO matrix interactions.
The remainder of this paper is organized as follows.
The NiTi wire surface treatments are detailed in section 2
followed by AFM measurements in section 3. Mechanical
pull-out tests of wire–polymer adhesion due to the surface
treatments, and the theoretical and computational models
employed to interpret the results are described in sections 4
and 5, respectively. The paper concludes with a summary
of the major observations from the experiments and FEM
simulations.
2. Surface treatments
Nickel–titanium (NiTi) shape memory alloy wires, known
by the Flexinol
R
trademark, and manufactured by Dynalloy,
Inc. [30] were used in this study. These wires exhibit
a Young’s modulus increase of a factor of 2.6 and a
dimensional change of up to 4–5% (depending on the
amount of prestrain) when heated. If deformed, a wire can
3
F C Antico et al
return to its original shape after it is heated to 90 ◦ C,
the transformation temperature required for shape recovery
(i.e. the martensite-to-austenite phase transformation). The
Young’s modulus of the martensitic (cold) phase is 30 GPa,
and in the austenitic (hot) phase it is 80 GPa. Additional
information on the physical properties and deformation
response of NiTi shape memory alloys is in [31, 32].
Currently, Flexinol
wires are manufactured specifically
for use in actuators for high cycle applications. All wires
were ‘trained’ through a thermo-mechanical cyclic process
by the manufacturer prior to subsequent surface treatment.
See [32–35] for representative applications and for more
details on the thermo-mechanical behavior of Flexinol
wires. Typically these wires exhibit a dark surface due to
their natural oxide layer which is (approximately) 400 nm
thick [36]. Whether the NiTi wire surface oxide was grown
prior to wire drawing or after drawing is not known for certain
without AFM examination.
2.1. NiTi wire preparation
Surface contaminants were removed from the wires through
sequential treatment with acetone, 2-propanol and xy-
lene [17]. The wires were then air dried and briefly soaked
in deionized water. Each cleaned NiTi wire was immersed in
a 3% hydrofluoric acid (HF)/15% nitric acid (HNO3 ) solution
until the surface oxide was removed (a 20 min process). The
HF ensured dissolution of the otherwise insoluble titanium
oxide on the NiTi. Drying was avoided since it allows
formation of a strong oxide film that is difficult to convert
into a surface rich in hydroxyl groups. The wires were
instead soaked in deionized water after etching and after
each subsequent step, and then immersed in 1 M sodium
hydroxide (NaOH) for 20 min to force the oxide groups to
reform as hydroxides. Some (or most) of these hydroxides
were present as surface-O–Na species (i.e. when exposed to a
highly alkaline solution). Hence, a 5 min soak in concentrated
H2 SO4 was used to remove the sodium ions and to leave a
surface rich in −OH groups available for reaction with the
coupling agent. Ultrasonication followed each step.
Once the new oxide/hydroxide layer formed, each
NiTi wire was soaked in an aqueous solution of 1%
phenylphosphonic acid (PPPA, R–P(=O)(OH)2 , R=C6 H5 )
at 298 K for 20 min. Another set was subject to a 20 min
soak, with ultrasonication in 5% PPPA. Additionally, hand
sanding (180 grit sand paper) of the wires was used to
apply a directional microgeometry. The NiTi wires that were
embedded into the polymeric matrix had diameters ranging
from 380 to 750 µm and embedded lengths, le , ranging from
70 to 90 mm.
2.2. Phenylphosphonic acid (PPPA) coupling agent
The phosphorus atom (P) in PPPA contains a double bond
to an oxygen atom (=O) and the P is also bonded to two
hydroxyl (OH) groups that possess acidic hydrogen atoms.
Although we chose R=C6 H5 , in principle any organic group
that is compatible with −OH groups is possible, and it will
Smart Mater. Struct. 21 (2012) 035022
(a) (b)
(c)
(d)
Figure 2. (a) Hydrogen bond between the oxide–hydroxides on the
NiTi surface and the phosphonic acid. (b) Condensation (produces
water) which results in bonded P(=O)R groups. (c) Surface −OH
groups on NiTi. (d) Polymer and NiTi substrate interface with
coupling agent (P–O bonds to NiTi surface not shown). In the
present study, R=C6 H5 .
determine the extent of bonding with a polymer. The hydroxyl
units (i.e. the OH groups) will initially be attracted to polar
oxide and hydroxide groups on oxide surfaces. Interaction
between the metal oxide surface and the PPPA will first occur
through hydrogen bonding. Although moderately strong,
these bonds are not as strong as the bonds formed through
a subsequent heat treatment. The P end is bound to the NiTi
oxide–hydroxide via a condensation reaction as illustrated in
figure 2(a). The resulting P–O bonds are shown schematically
in figure 2(b). The process of applying the coupling agent
to an as-received NiTi wire surface required removal of the
native oxide/hydroxide layer (via acid etching) followed by
controlled re-growth of the surface oxide. This generated an
ample number of surface −OH groups for bonding. Once this
was completed, the re-grown NiTi oxide was treated with the
coupling agent.
The TPO polymeric matrix is a saturated hydrocarbon
material that offers little opportunity for bonding or polar
interactions. Polarizable substances, such as aromatic phenyl
rings, will interact with TPO. This occurs due to the
high polarizability of the electrons in delocalized p-orbitals.
Electrons in these orbitals are more easily polarized than
4
F C Antico et al
those in σ bonds (for example). However, an ample supply
of surface −OH groups must be available (see figure 2(c))
to achieve effective coverage with the coupling agent. The
completed reaction, which shows the coupling agent at
the interface between the polymer and NiTi material, is
schematically detailed in figure 2(d). The solvents used
were histological grade acetone, reagent grade 2-propanol
and reagent grade xylene (mixed isomers). Reagent grade
sodium hydroxide (Baker), nitric acid, sulfuric acid (VWR)
and 98+% PPPA were also used, as was deionized water.
2.3. Wire embedding process
Following surface treatment, the NiTi wires were embedded
into TPO by injection molding. Following this procedure,
the wires were exposed to the same manufacturing process
as the composites shown in figure 1. The mold was used
to produce dogbone-shaped specimens. Each dogbone was
4 mm thick, 167 mm long (excluding the crimped wire ends)
and 10 mm wide at its center (20 mm wide at its ends).
Two dogbone specimens per molding cycle were produced,
each with a straight gauge section. Wire expulsion from the
polymer matrix had to be prevented to allow measurement
of the interfacial strength of the polymer/NiTi interface [11]
in the mechanical pull-out tests. Additional wire prestrain
was deemed unnecessary. A two-step embedding process was
subsequently developed. In the first step, the end of the wire
that protruded from the specimen was crimped. The crimp was
attached to the mold. A small weight was affixed to the other
end of the wire which was to be embedded in the polymer.
The weight was intended to minimize wire bending or kinking
during injection molding and mitigate the fluid drag force
to keep the wire straight. In addition, the weight geometry
helped to keep the wire from moving to the surface of the
solidified polymer, irrespective of the wire surface treatment.
Nevertheless, the effectiveness of the weight was found to be
largely dependent upon the wire surface treatment. After the
embedding process, the portion of the specimen containing
the weight was carefully cut without affecting the interface
between the wire and the polymer.
3. Surface characterization
3.1. Optical observations
Figure 3 shows three molded specimens. Figure 3(a) shows
a NiTi wire with no surface treatment. Roughly 50% of the
wire penetrated the specimen surface (dark region along the
center of the gauge section moving from left to right across
figure 3(a)). This shows that the wire moved during molding,
even with the weight, and suggests that wire/TPO polymer
adhesion was insufficient. It should be mentioned that
one-half of the specimens with no surface treatment exhibited
this type of behavior. Only those specimens with uniform
embedding were considered for the subsequent pull-out tests.
The hand-sanded SMA wire, shown in figure 3(b), shows
improved embedding. However, some of the wire is still
faintly visible on the right-half of the specimen in figure 3(b).
Smart Mater. Struct. 21 (2012) 035022
Untreated
(a) Wire through
the polymer
Hand-
sanded
(b) Embedded
NiTi wire
5% PPPA
(c)
Figure 3. (a) Untreated NiTi wire which is not properly embedded
in the TPO matrix—a portion of the wire surface penetrated one
surface of the specimen; (b) a hand-sanded NiTi wire is still not
properly embedded in the TPO matrix and (c) 5% PPPA treatment
facilitates proper positioning of the wire within the TPO matrix,
which is indicative of improved wettability with the TPO.
On the other hand, the NiTi wire treated with 5% PPPA
(figure 3(c)) displays the most uniform embedding within
the TPO matrix, which suggests greatly improved adhesion
between the wire and TPO3 . Additionally, none of these
specimens showed wire penetration to the surface. These
observations were consistent with additional molding tests in
which the same treatment procedures were repeated.
3.2. AFM analysis
The ultrasharp AFM probe, model TESP-HAR from Veeco
Instruments, consisted of a silicon cantilever doped with Sb.
The tip radius is nominally less than 10 nm and the tip height
is 10–15 µm, with a front angle of 5◦ and a side angle of 5◦ .
The cantilever thickness, length and width are 4 µm, 125 µm
and 30 µm, respectively. The cantilever stiffness is 42 N m−1 .
All wire surfaces were scanned with a Digital Instruments
D3100 AFM in tapping mode. Typical scanning speeds ranged
from 0.5 kHz (10 µm s−1 ) to 1.5 kHz (30 µm s−1 ). For
the majority of images gathered from the present work, a
0.7 kHz scanning speed was used. All scans were gathered
over a 10 µm × 10 µm area with 512 × 512 pixels2 . Scans
over larger areas provided no useful information beyond that
reported herein. Great care had to be exercised in establishing
AFM scan parameters so as to avoid a myriad of scan artifacts
that precluded acquisition of quantitative surface topography
data. Several wires with as-received and hand-sanded (180 grit
sandpaper was used) surfaces, along with some treated with
the PPPA coupling agent, were scanned with the AFM.
3 ‘Uniformly embedded’ implies that the wire remains straight inside the
polymer with a fixed distance to the TPO surface along its length. By use of
the term ‘not properly embedded’, it is meant that the wire is curved and its
distance to one of the surfaces, along the thickness, of the specimen varies
such that, in most cases, part of the wire was visibly exposed.
5
F C Antico et al
3.2.1. As-received NiTi wire surface topography. Figure 4(a)
shows an oblique view of an as-received NiTi wire surface.
Areas of bright contrast represent roughness values that
are high relative to the deepest recessions in the surface
(denoted by regions of dark contrast). Height values are
reported in nm in the key, with the total roughness height
range being 0–451.2 nm. Die marks are indicated with the
dotted arrows. Note the die marks on the planar portion of
the surface follow the white arrow in the upper right of
figure 4(a): this denotes the drawing direction. This surface
also contains a series of randomly positioned cracks. The
orientations of crack openings are mostly transverse to the
drawing direction, suggesting that the cracks originated from
one of two possible mechanisms during drawing. In the first
mechanism, crack nucleation resulted from local adhesion of
the wire surface oxide (either natural oxide or re-grown oxide)
to the drawing die surface due to local lubricant starvation
(leading to a stick–crack–slip phenomenon). Alternatively, a
condition of mixed-film lubrication may have existed at the
die–wire interface wherein load transfer occurred through
locally entrapped lubricant films. The thickness of these
films is impacted by the drawing speed. Those areas of
the wire surface beneath the films were in unconstrained
deformation which creates conditions conducive to surface
crack nucleation and growth. This process is very similar
to that which generates transverse micro-cracks on rolled
aluminum sheet, for example [37]. However, the surface
damage shown in figure 4(a) may have resulted from the
wire training process (as-received wires are typically black;
manufacturer specifications are such that the oxide thickness
is in excess of 400 nm [34]). What this fails to answer is
whether or not the existing oxide was grown prior to drawing
or after drawing. This issue is resolved by the longitudinal die
marks in figure 4(a) due to sliding of the wire surface over
the die surface. Note that these marks could not have resulted
from any amount of training subsequent to drawing, and this
suggests that the as-received wire surface oxide was grown
prior to drawing. The die marks are indicative of the finish on
the die used to manufacture the wires. A cursory examination
of the die marks in figure 4(a) reveals peaks in the 10–30 nm
range. This suggests that the die surfaces were reasonably well
polished (the wavelength of green light is ∼550 nm), and such
a smooth finish may have contributed to the aforementioned
lubricant starvation mechanism during wire drawing. Section
profiles along a line normal to the drawing direction revealed
a nominal peak-to-valley excursion (representing the distance
from the mean surface plane to the bottom of the measured
cracks) of 282.6 nm. The nominal slope of the crack walls was
58.3◦ . The highest regions of the surface are plateau-shaped,
indicating that the surface has a good bearing area [38].
It is unlikely that the majority of the surface cracks fully
penetrated the oxide layer.
3.2.2. Hand-sanded NiTi wire surface topography. Fig-
ure 4(b) is a representative AFM surface plot of an NiTi
wire surface topography from hand sanding. The surface
is irregular with jagged peaks corresponding to displaced
material and embedded debris that are good sites for
Smart Mater. Struct. 21 (2012) 035022 F C Antico et al

(a) (b)

(c) (d)
Figure 4. (a) AFM height Image of an as-received NiTi wire surface across a 10 µm × 10 µm surface area showing die marks along
plateau regions with cracks. Surface cracks suggest an oxide layer prior to wire drawing. (b) AFM image height of hand-sanded NiTi wire
surface. (c) AFM height images of NiTi surface with 5% PPPA. (d) Phase contrast image corresponding to height image (c).

mechanical interlocking. The bottom part of the image shows
a substantially unidirectional topography and is indicative
of the sanding direction. The irregular array of peaks and
valleys resulting from the grit particles effectively extended
the surface area which is beneficial for mechanical adhesion
with a polymeric matrix during the embedding process.
The hand-sanded wires are brighter in appearance than the
as-received wire surfaces due to removal of the oxide layer.
In addition to data of the type shown in figure 4(b), we also
scanned portions of the hand-sanded surfaces that contained
isolated debris particles.
3.2.3. PPPA treatment. Measurement of NiTi wire surfaces
with the 5% PPPA coupling treatment initially proceeded with
the AFM scan parameters established for the as-received and
hand-sanded NiTi wires. Topography slope images revealed
high frequency ringing that snakes along valley regions of
the treated wire surface. Previous experience with other
chemically treated metal surfaces led to the conclusion that
these features are due to locally excessive sticking between the
oscillating AFM probe and the surface. Hence, the chemistry
of the treated surface differs from that of the as-received and
hand-sanded surfaces since the probe is momentarily adhered
to the sample surface while the body of the cantilever deflects,
thereby jerking the probe away from the sample surface and
instantaneously altering its oscillation amplitude [39]. This
behavior was noted in all initial scans of the chemically
treated wire surfaces for which the initial scan parameters
(established for the as-received and hand-sanded wires) were
used. Adjustment of the cantilever oscillation amplitude, so
as to apply greater force to the wire surface with each tap,
significantly diminished scan artifacts.
Figure 4(c) is a representative AFM surface plot of an
NiTi wire surface following treatment with 5% PPPA. Notable
aspects of this image are its substantially different appearance
from the as-received and hand-sanded height images, e.g. its
2.10 µm maximum roughness height (approx. the extreme
roughness heights of 451.2 nm and 560.2 nm in figures 4(a)

6
Smart Mater. Struct. 21 (2012) 035022
and (b), respectively). This resulted from the acid etch
treatment prior to application of the 5% PPPA coupling agent.
Figure 4(d) is a phase contrast image corresponding to the
height and slope images in figure 4(c). Comparison (not
shown) of height and slope images with the phase image
show that the latter contains contrast features that are not
readily apparent in the former two images. Selected regions
that show contrast unique to the phase image in figure 4(d)
are labeled A–F. Figure 4(d) suggests that phase contrast
measured from the treated NiTi wire was not largely mitigated
by surface topography, but rather through local variations in
probe surface adhesion. Amplitude distribution plots derived
from AFM height data revealed that the 5% PPPA coupling
treatment gave a surface that has negligible skewness (i.e. it is
primarily a Gaussian distribution). The transition from air to
surface is more gradual in the chemically treated wire surfaces
than in the as-received and hand-sanded wire surfaces. This
is advantageous from the standpoint that the surface slopes
are less extreme and offer less resistance to liquid polymer
wetting than would be the case with that in figure 4(b).
3.3. Roughness comparison
Ten areas of each surface type (i.e. as-received, hand-sanded
and chemically treated) were separately scanned on selected
NiTi wires. The data from each was used to compute the
arithmetic mean roughness (Ra ).
Figure 5 shows that as-received NiTi wire surfaces are the
smoothest, with a mean Ra of 36.41 nm (standard deviation of
5.12 nm). Wire surfaces treated with 5% PPPA have the largest
Ra values, with a mean Ra value of 222.10 nm and the widest
spread of roughness values (standard deviation of 76.9 nm).
The hand-sanded surface roughness values are intermediate
to those of the as-received and chemically treated wire
surfaces with a mean value of 66.66 nm (standard deviation
of 35.732 nm). We also computed the root-mean-square
roughness (Rq ) and the extreme peak-to-valley excursions
(1z). The values of Rq follows the same trend as that
for the Ra with the chemically treated NiTi wire surfaces
having the greatest spread of values, and the as-received
wire surface having the smallest spread of values. The
mean Rq for the NiTi wires treated with 5% PPPA was
287.68 nm (standard deviation of 46.72 nm), while the mean
values for the as-received and hand-sanded NiTi wires were
51.26 nm (standard deviation of 6.79 nm) and 92.89 nm
(standard deviation of 47.86 nm), respectively. The mean 1z
for the treated wires is 2.21 µm with a standard deviation
of 493.94 nm. The mean 1z for the hand-sanded wires is
considerably smaller at 765.01 nm with a standard deviation
of 336.16 nm. Close to this value is the mean for the
as-received wires at 638.99 nm with a standard deviation of
153.79 nm.
4. Pull-out tests
In tensile pull-out, the pull-out force is defined as the applied
force to initiate debonding between an NiTi wire and a TPO
matrix. This test methodology has been used to measure
interfacial adhesion in fibrous composites, for example, and
7
F C Antico et al
Figure 5. Arithmetic mean roughness (Ra ) values from 10
specimens of each surface type.
the mechanics of debonding is well understood [40–43].
Tensile pull-out testing of NiTi wires embedded in polymeric
or composite matrices has been reported in [11, 12, 17, 19,
44–46]. In this study, the wires are tested at room temperature.
It is believed that this type of test represents the worst-case
scenario for the NiTi/TPO interface. Here, the wire thinning
caused by the stress-induced martensitic detwinning of the
NiTi contributes to an opening mode in the interface, helping
prevent any additional energy dissipation mechanisms that
may be triggered by mechanical interlocking due to the
roughness of the interface.
4.1. Test configuration
The inset in figure 6 is a schematic of the pull-out test
and a typical force–displacement curve is also shown. This
configuration ensures that the specimen does not experience
lateral compressive stress. A monotonically increasing force,
F, is applied to the crimp at the end of the wire until
debonding is triggered. This test effectively captures the peak
(or maximum force, Fmax ) to pull the wire out of the polymer.
Each specimen (i.e. a NiTi wire embedded in TPO) was first
cut through its gauge section exposing one end of the wire.
The specimens were cut to have the same embedded wire
length le = 90 mm. However, a few specimens with le =
70 mm were also measured. The free end of the NiTi wire was
loaded with a monotonically increasing force. The following
final set of TPO specimens with embedded NiTi wires were
investigated in the pull-out tests.
(1) As-received wires (five specimens with le = 90 mm and
seven specimens with le = 70 mm).
(2) Hand-sanded wires (four specimens with le = 70 mm and
four specimens with le = 90 mm ).
(3) Pre-treated wires with acid only (oxide/hydroxide layer,
see section 2.1) (five specimens with le = 90 mm).
Smart Mater. Struct. 21 (2012) 035022
Table 1. Test matrix with mean forces recorded for each treatment for pull-out specimens with le = 90 mm. The untreated-wire specimens
require the lowest pull-out force, while those treated with 5% PPPA require the highest pull-out forces. The maximum value achieved with
the untreated NiTi wires is even lower than the maximum values from tests of the treated wires.
Number of specimens
Treatment tested (le = 90 mm) Mean force ± stand. dev. (N)
Untreated 5 16.2 ± 5.1
Hand-sanded 4 22.7 ± 2.0
Acid 5 21.0 ± 2.8
1% PPPA 8 22.0 ± 2.6
5% PPPA 8 22.4 ± 3.1
Figure 6. Typical load–displacement curve obtained from the
experiments. Inset figure: schematic of pull-out specimen
containing an embedded NiTi wire.
(4) Wires with fresh oxide/hydroxide layer followed by
treatment with 1% PPPA (eight specimens with le =
90 mm and one specimen with le = 70 mm).
(5) Wires acid etched and then treated with 5% PPPA (eight
specimens with le = 90 mm).
Three distinct regions can be observed in the
force–displacement curve: an initial portion in which the force
increases to point I, a plateau in the force between points II
and III, and a final decaying portion down to zero force. The
translucency of the TPO allowed observation of debonding of
the NiTi wire from the polymer matrix. Wire deformation and
debonding started at the wire/matrix interface from the force
application end before the force achieved its maximum value
in figure 6. The axial deformation observed in the wire at force
levels equal to or greater than Fmax indicates that the wire
was undergoing detwinning. Finally, the wire breaks free of
the TPO matrix (point IV) as the debonding process becomes
unstable. Thinning of the wire in the transverse direction also
contributed to wire debonding from the TPO.
The progression of the debonding process is schemati-
cally depicted in figure 7. Each inset in figure 7 shows the
relative position of the image above it with respect to the
entire NiTi/TPO specimen. The region where a NiTi wire
8
F C Antico et al
Max. force
Min. force recorded (N) recorded (N)
6.9 22.2
19.2 24.3
18.9 26.4
18.1 25.7
18.0 28.0
debonded from the TPO is referred to as the debonding
process zone (denoted by the light gray region labeled
‘Debonding process zone’ in figure 7(a)). Figure 7(b) depicts
the debonding process zone advancing deeper into the TPO
as the applied pull-out force increases during loading stages
I–II. Meanwhile, large axial deformation in the wire is still
observed near the debonding process zone. The debonding
front finally reaches the specimen end opposite that of the
applied force as shown in figures 6 (inset) and 7(c), with
complete debonding shown in figure 7(d).
4.2. Experimental results
Table 1 reports the pull-out forces (newtons) obtained in the
experiments. Due to the large number of experiments, the
table only shows mean force values associated with each
treatment. The mean maximum pull-out forces and equivalent
tensile stress (with their standard deviations) were plotted in
figure 8. The red dots denote those pull-out specimens with
le = 90 mm, whereas the green squares are associated with
the shorter pull-out specimens (le = 70 mm). This data shows
that the maximum mean pull-out force for all of the tests was
within the standard deviation regardless of NiTi wire surface
treatment. However, as seen in table 1, the wires treated
with 5% PPPA required the largest pull-out force achieved
in a single test. In contrast, the untreated wires required the
smallest pull-out forces, although a single specimen with an
untreated wire reached a maximum force close to that of the
treated wires. The forces required with the treated wires were,
in general, higher than those associated with the untreated
wires. The pull-out results suggest that the various treatments
lead to an improvement in adhesion of the NiTi wires to the
TPO matrix.
5. Theoretical models
Wire pull-out forces typically need to be interpreted through
appropriate models to obtain the effective wire/matrix
properties. Previous studies have used analytical models based
on strength of materials and linear elastic fracture mechanics
(LEFM) to convert pull-out forces to interfacial strength or
adhesion energies [11, 14–16, 47–50]. In section 5.1, we
briefly review relevant analytical models and discuss the
extent to which they apply to the pull-out tests in this study.
Both analytical expressions based on LEFM and strength of
materials are presented in section 5.1. Finally an FEM that
Smart Mater. Struct. 21 (2012) 035022 F C Antico et al

(a) (b)

(c) (d)

Figure 7. Schematics of the wire pull-out process at different stages of the pull-out test as described in figure 6. Process of debonding
during the pull-out force: if the wire is in the twinned martensitic phase, then it first undergoes a stress-induced detwinning with strains up
to 4%. The white arrow in the NiTi wire denotes the applied force. Debonding starts in (I). A gap is left in the wake of the debonding front
caused by the thinning of the NiTi wire (b). (c) Debonding propagates toward the other end of the specimen until (d) complete debonding is
attained at (IV). Insets beneath each figure show the location where the debonding process zone takes place relative to the entire specimen.

represents the mechanical response of the pull-out specimens
under quasi-static loading is used to analyze the debonding
process (section 5.2).
5.1. Analytical model
According to Penn and Lee [47], wire debonding can
exhibit two distinct behaviors: (i) ductile behavior, where
the interface has a uniform stress distribution, i.e. a large
fracture process zone, and yielding of the matrix is the main
mechanism of deformation, and (ii) brittle behavior, where
the interface has a small debonding process zone compared
with the dimensions of the specimen (which is described by
LEFM), and a non-uniform stress distribution along the NiTi
wire/matrix interface.
When ductile interface debonding takes place, Fmax
is proportional to the embedded wire length (Fmax ∝ le ).
Accounting for the contact area between the wire and a
polymeric (e.g. TPO) matrix Fmax is defined as [51]:
Fmax = 2π rle τiy
where r is the wire radius and τiy is the shear strength
of the wire/matrix interface or polymeric matrix (whichever
is smaller). In brittle interfaces, where plastic deformation
around the interface is limited, Fmax is not proportional to le
because of the nonlinear shear stress distribution around the
interface: this tends to very large values of τiy near the ends
of the wire/matrix interface. Following Piggott [51], Penn and
Lee [47] showed that, if a failure criterion based on the energy
of the interface is assumed, then the following expression
provides a valid estimate of the critical strain energy release
rate, Gc (J m−2 ), or work of separation, in terms of Fmax :
2
[1 + csch2 (ns)]F max
Gc = 3
(2)
4π 2 r Ef
where, for the present case, Ef is the Young’s modulus of the
NiTi wire, s = (le − a)/r, a is the length of the debonded
(1) initial region, le is the embedded wire length when a = 0 and

9
Smart Mater. Struct. 21 (2012) 035022 F C Antico et al

manufacturer’s recommended value to guarantee durability

(∼180 MPa for Flexinol R
wires). For optimal actuation,
the design of the composite requires that the actuation
force, and therefore the tensile stress, be maximized without
exceeding the maximum recommended value. Evidently, this
requirement competes with the necessary strength level of
the wire/polymer interface to preclude debonding. Wires
that can be pulled out at tensile values lower than the
manufacturer level cannot exert the maximum force. On
the other hand, wires that need a higher tensile stress for
pull-out are safer for actuation applications. Figure 8 shows
the maximum values of the tensile stress in the NiTi wires
used in the present study compared with the manufacturer’s
recommended level. Only the chemically treated NiTi wires
exceed the recommended values, suggesting that the load
capacity of actuators with embedded wires can be maximized
Figure 8. Maximum pull-out force recorded for NiTi wires with with a suitable wire surface treatment. It should be mentioned
embedded length le = 70 mm (in green squares) and le = 90 mm (in that the values of pull-out force for the treated wire may
red circles). The mean values for each treatment are denoted by
symbols and the standard deviation is indicated by the error bars. be safe mostly for single actuation applications, i.e. where
The tensile stress is obtained from equation (6) for all the the force is applied once monotonically. We surmise that
experimental points. The horizontal dashed line denotes the the required pull-out forces for typical cyclic actuation
manufacturer’s recommended tensile stress of 180 MPa. applications should be higher than those reported here to
compensate for accumulated damage at the interface between
the NiTi and the polymer.
n is defined as [51]
Em
n2 = (3) 5.2. Finite element model
Ef (1 + νm )ln R


r
where Em are νm are the Young’s modulus and Poisson’s ratio, A two-dimensional axisymmetric FEM was used to analyze
respectively, of the matrix and R is the radius of a cylinder the pull-out tests. The geometry of the computational domain
of polymeric material that surrounds the wire. To estimate a and boundary conditions are shown in figure 9(a). The nodes
lower bound for Gc (see equation (2)), R is approximated as located at x1 = 0 are constrained to move in the x1 direction
the minimum dimension of the cross section of the specimen to satisfy the axisymmetric condition. Nodes along part of the
(in the present case, this is 4 mm, which corresponds to the upper boundary of the polymer (at x2 = 70 mm in figure 9(a))
thickness of the specimen). For very short values of le , ns  le were also constrained to move in the x2 direction to properly
and equation (2) reduces to account for the constraints in figure 6. Given the dimensions
2 of the specimens and pull-out tests, the radius of the TPO
Fmax
Gc = . (4) matrix, R (see figure 9(a)), was set to 2 mm to be consistent
4π 2 r3 Ef sinh2 (ns) with the specimen thickness. Preliminary simulations showed
Alternatively, for large embedded lengths, equation (2) that an increase in R from 2 to 4 mm results in only 3.5%
reduces to variation in the values of Fmax . Hence, the axisymmetric
2 approximation has only a very minor effect on our FEM
Fmax
Gc = . (5) results. Additionally, models with embedded lengths of 70 and
4π 2 r3 Ef 90 mm were used to verify that Fmax is indeed independent of
the embedded length of a NiTi wire [47]. In fact, a difference
This is a useful approximation for rectangular specimen of only 1% in the maximum pull-out force was obtained
geometries with large embedded lengths and a small fracture between the two embedded lengths.
process zone (i.e. the LEFM approximation). However, The experiments revealed large deformations (i.e. up
LEFM may underestimate Gc when material nonlinearities are to 5%) in the wires along the axial or pulling directions.
important (as in the present study). This deformation can be attributed to detwinning of the
Another quantity of interest is the tensile stress in the martensitic phase4 (noted in figure 7) [52]. Numerous
NiTi wire, estimated as continuum models for SMA have been developed that make
Fmax use of macroscale plasticity (often with backstress, flow rules
σmax = . (6) and yield functions) [52, 53]. Here, the following nonlinear
π r2
The tensile stress in the wire becomes important for 4 This is because the wires undergo temperature-induced martensitic-to-
actuation purposes, especially when a high number of cycles austenitic phase transformation during the injection molding process and
is required. Stress levels in the wires should remain below the therefore they recover any prestrain from wire drawing.

10
Smart Mater. Struct. 21 (2012) 035022 F C Antico et al

(a)

(b)

(c)

Figure 9. (a) Schematic of the axisymmetric FEM geometry. The light region denotes the polymer matrix, while the dark region denotes a
NiTi wire. Here, le = 70 mm. r is the radius of the wire, R is the maximum radius of the TPO adopted, w is the radial dimension of the TPO
relative to the outer radius of the wire and a is the crack length. (b) Experimental uniaxial stress–strain curve (dotted line) and exponential
hardening law for NiTi (solid line; equation (7)). (c) Schematics of the initially elastic constitutive cohesive law employed to describe the
interface behavior. The red double arrow indicates any irreversible post-peak unloading–loading cycle [65].

isotropic hardening model [54] was used to represent NiTi
deformation in its martensitic phase at 298 K [55]:
pl
Y(εpl ) = Y∞ + (Y0 − Y∞ )e−βε .
The plastic strain is ε pl , Y(εpl ) is the radius of
the yield surface, Y0 is the initial yield stress, β is
a hardening parameter and Y∞ is used here to fit the
constitutive model in equation (7) with the experimental
stress–strain curve of the wire. While this model can
predict the overall effective response of the NiTi wire
under monotonically increasing stress conditions, it may not
accurately account for the reorientation of the martensitic
phase and microscale inhomogeneous deformation. As
discussed by Gao and Brinson [56], caution is required
here since the SMA deformation/stress response is based on
underlying mechanisms that differ from those associated with
a reversible plastic response. To apply this model to predict
the behavior of the NiTi wire in our particular case, we note
that the NiTi is always subjected to a monotonically increasing
load during pull-out testing and that most of the inelastic
deformation of the debonded wire takes place under uniaxial
stress conditions. Additionally, due to the large deformations
expected in a NiTi wire during the pull-out tests, our FEM
also accounts for finite deformations. Figure 9(b) shows the
(7) experimental true stress–strain curve of NiTi compared to
the fit response from the model. In this case, the stress is
σ = Y(εpl ) and the total strain is defined as εtot = ε pl + σ/Ef .
The experimental stress–strain curve corresponds to our own
measurements; however, it follows what others have reported
for Flexinol wires [57, 58]. The linear response of NiTi was
characterized assuming Ef = 30 GPa based on the information
from the manufacturer. The parameters adopted to match
the nonlinear response of the wire from our experimental
measurements are Y0 = 0.04 GPa, Y∞ = 0.023 GPa and
β = −100.
In our FEM study, only quasi-static monotonic loading
at constant temperature was modeled. It is assumed that the
wire is initially stress-free, in the fully martensitic phase
and that detwinning occurs only due to the applied stress
during loading. The TPO matrix is modeled as linear elastic,
an assumption that is valid since stress values are well
below the yield strength of TPO. Here Em = 0.736 GPa and

11
Smart Mater. Struct. 21 (2012) 035022
νm = 0.33 [59]. Each material is represented by a mesh with
four-noded quadrilateral elements.
The NiTi wire/TPO interface is modeled with a
cohesive zone model [60–64] to simulate crack initiation
and propagation. A potential-based cohesive zone model
implemented as triangular-shaped, four-node, zero-thickness
interface elements [65] is embedded between the wire and
the TPO matrix [65–71]. The formulation of these elements
is based on a non-dimensional effective displacement jump
(λ) that takes into account the current normal and tangential
displacement jumps at the NiTi wire/TPO interface estimated
from the FEM. Hence
s
 2  2
un ut
λ= + (8)
δn δt
where un and ut are the current normal and tangential
displacement jumps, respectively, at the interface estimated by
the FEM, and δn and δt are the corresponding critical values of
the displacement jump at which interface failure takes place.
The displacement jump is related to the normal and tangential
traction of the interface using a traction-separation law ([65])
for mode I and mode II, namely
1 − λ∗ un
 
Tmax
Tn = (9)
λ∗ δn (1 − λcr )
1 − λ∗ ut αTmax
 
Tt = . (10)
λ ∗ δt (1 − λcr )
Note that λ∗ is monotonically increased by following the
condition
λ∗ = max(λmax , λ) (11)
where λmax = λcr (initially) and λmax = λ if λ > λmax .
Also, Tmax can be regarded as the cohesive strength of the
interface only when normal opening displacement is applied
to the interface and τmax = αTmax as the cohesive strength
when only shear (tangential displacement) is applied to the
interface. The dimensionless parameter α is the normal to
shear strength ratio and λcr is the critical value of the effective
displacement jump where the normal or tangential traction
reach their maximum values. The values of δn and δt were
derived from the geometrical relation that links the strength
and the cohesive energy (or work of separation) of the NiTi
wire/TPO interface:
GIc = 12 δn Tmax , GIIc = 21 δt αT max . (12)
Here, GIc is the cohesive energy for mode I (i.e. when
pure normal opening displacement is applied to the interface)
and GIIc is the cohesive energy for mode II (only shear). The
strength and energy of the cohesive interface are characterized
based on information from the pull-out tests. In turn, it is
expected that all these cohesive properties will depend on
a specific surface treatment. Figure 9(c) shows the cohesive
traction-separation law for the shearing mode (equation (10)).
While the elastic and inelastic properties of NiTi and TPO are
known, the cohesive parameters in equations (8)–(12) must
be quantified. Another characteristic length of interest is the
debonding process zone length, lf ∝ Gc Ef /Tmax2 [72–74]. We
12
F C Antico et al
conducted a systematic parametric analysis of the variation of
the main cohesive parameters, namely Tmax , α, δn and δt .
Previous studies neglected residual stresses from in-
jection molding. Residual stresses may delay the onset
of interfacial debonding during wire pull-out due to the
additional compressive normal stresses on the wire–matrix
interface. The compressive normal stresses increase friction
forces along the wire/TPO interface [75, 76]. The specimens
produced in the present study have low NiTi wire/TPO
friction compared with adhesion (even for the hand-sanded
specimens). However, in the NiTi/TPO system residual
stresses must not be ignored. Figure 7 depicts a case with
no residual stresses showing that wire thinning behind the
debonding front leads to an important mode I contribution,
leaving a gap in the wake of the debonding front (figure 7(b)).
This mode I contribution helps lower pull-out forces during
debonding. However, residual stress from the injection
molding process may cause the matrix to partially close the
gap, reducing the mode I contribution. To study the impact
of residual stresses, we carried out a series of simulations
that address shrinkage of the TPO during the injection
molding process. From previous studies [77, 78], a good
indicator of the ratio of volume change due to thermal
loads is the thermal expansion coefficient. Assuming 2 ×
10−5 mm mm−1 ◦ C−1 [59] and a temperature change of
100 ◦ C (typical of injection molding), we simulated the TPO
shrinkage process that preceded the pull-out simulations.
Although TPO has very high thermal stability, (i.e. shrinkage
during the injection molding process is very small compared
with other thermoplastic polymers), our simulations revealed
that the residual stresses indeed reduced the mode I
contribution, leading to values of Fmax that are 10% higher
than those without residual stresses.
5.3. Results and discussion
We analyzed NiTi wire/TPO interface behavior with the
analytical models presented in section 5.1 and the FEM
described in section 5.2. The ductile model in equation (1) can
only be applied when the debonding process zone spans the
entire bond length (see section 5.1). From our experiments,
this is not the case. An NiTi wire debonds from the matrix
following an interfacial debonding propagation process (see
section 4.2), a process that is initiated from the polymer
surface closest to where the force is applied and propagates all
the way to the other end (see the debonding process zone in
figure 7(a)). Application of equation (1) to the forces reported
in figure 8 would have resulted in grossly underestimated
values of the shear strength, τiy (∼0.1–0.2 MPa), and hence
the ductile model is inadequate.
Based on LEFM, Penn and Lee [47] studied the
correlation between Fmax and le . For large le , Fmax is
independent of le . Even though the molded NiTi wire/TPO
specimens were expected to develop a small fracture process
zone, the characterization of the interface behavior with
LEFM is not straightforward since the NiTi mechanical
response, under the conditions stated above, is inelastic. This
model has been used by Jonnalagadda et al [11]. Following
Smart Mater. Struct. 21 (2012) 035022
Figure 10. Fmax versus Gc . Solid red line: FEM accounting for
inelastic behavior of NiTi considering residual stresses. Gray dashed
line: FEM accounting for inelastic behavior of NiTi assuming no
residual stresses. Green long-dashed line: FEM calculation
assuming a linearly elastic behavior for the NiTi. Blue
dashed–dotted line: LEFM analytical prediction. The horizontal
dashed lines denote the minimum and maximum values recorded in
table 1 (from our pull-out tests). Circular, triangular and square
symbols indicate discrete values of Fmax obtained from each set of
simulations, respectively.
this model, Fmax is plotted with Gc in figure 10 as the
blue dashed–dotted line. The horizontal black dashed lines
denote one standard deviation below the minimum mean force
and one standard deviation above the maximum mean force
measured in our pull-out experiments detailed in table 1 and
figure 8. This curve clearly shows that Gc ranges from 13
to 85 J m−2 for the peak forces reported in our experiments
following LEFM.
Finally, a series of FEM calculations using the model
described in section 5.2 was carried out for different values
of the cohesive zone parameters. To properly account for the
mixed mode conditions at the debonding front, τmax , Tmax , δn
and δt were individually studied to assess their effect on the
overall behavior of the specimen geometry show in figure 9.
Typical force versus displacement curves from the FEM are
similar to those shown in figure 6. Variations of the cohesive
parameters lead to different values of Fmax . Consequently,
we performed a systematic parametric numerical analysis
wherein calculated Fmax are compared with measured values
from our pull-out experiments (section 4.2, table 1 and
figure 8). Our first observation is that moderate variation of
Tmax and δn with respect to τmax and δt , respectively, affected
Fmax by less than 1%. Hence, the NiTi wire/TPO interface
behavior strongly depends on the mode II properties rather
than on the mode I properties. As such, we show results
for δn = δt and α = 1. This limited our analysis to only
two main parameters, namely Tmax = τmax and Gc = GIc =
GIIc = 21 δn Tmax . Our FEM simulations also suggest that, once
the debonding front advances, the pull-out force, at the Fmax
level, remains constant, and therefore it is independent of le
13
F C Antico et al
for sufficiently long embedded lengths (depicted in figure 6).
Therefore, our simulations are indicative of the complete
macroscale debonding process observed in our pull-out tests
(i.e. the debonding initiation, the detwinning of the wire,
debonding front propagation and the complete failure of a
specimen). Following these observations, we performed a
parametric analysis evaluating Fmax as a function of Tmax and
Gc . The solid red line in figure 10 shows the dependence of
Fmax on Gc including TPO residual stresses. Following [11,
15, 16], we considered values of Tmax in the 10–50 MPa
range. However, it was observed that varying Tmax from 10
to 50 MPa affected Fmax by no more than 1% (and up to
3% when Tmax is above 100 MPa). The overall geometry of
the molded specimen is thus insensitive to Tmax , while it is
highly dependent on Gc . The calculations shown in figure 10
assumed Tmax = 20 MPa.
Besides Tmax and Gc , the shape of the cohesive zone
model may be relevant (see figure 9(c)). Previous studies [79]
have shown that the shape of the cohesive zone model can
have a negligible influence on the overall response of an FEM
solution of pure-mode failure models (i.e. only mode I or only
mode II) with an adequate spatial discretization. However,
it was observed in [80, 81] that the local response close to
Fmax may vary, depending on the shape of the cohesive zone
model only when the cohesive zone length is comparable
to other relevant characteristic lengths. Some studies suggest
that the shape of the softening part [79] of the cohesive zone
model may affect the overall response of the numerical model
and that this can be neglected, depending on the relationship
between the stiffness of the TPO, NiTi and the cohesive
interface [79, 82, 83]. Here, a single cohesive zone model
was adopted to represent the pull-out response of an NiTi
wire embedded in a TPO matrix, regardless of the surface
treatment, based upon the observation that the response is
only dependent on the Tmax and Gc . Following Zavattieri
et al [69, 84, 85], this indicates that Tmax and Gc may both
be controlled by the adhesion mechanisms resulting from our
various NiTi wire surface treatments. Therefore, the effect of
the shape of the cohesive model on our simulation results can
be considered to be negligible.
Additionally, our simulations consider the residual
stresses from the injection molding process (open circles in
figure 10 represent discrete values of Fmax obtained from
these simulations). For comparison purposes, figure 10 also
includes predicted results without residual stresses (gray
dashed curve; triangular symbols represent discrete values of
Fmax obtained from these simulations), showing a difference
in force of about 10%. This difference indicates the effect of
an important mode I contribution when there are no residual
stresses, making it easy for the interface to debond under
combined mode I/II conditions. Ignoring residual stresses can
result in a 20–40% overestimation of Gc .
The FEM calculations allowed us to analyze the stress
state and deformation modes in the NiTi wire in great
detail. It was observed that the stress state along the wire
during the debonding process differs for wire material behind
the debonding process zone, where the wire is completely
debonded, and in locations where the wire is still bonded to
Smart Mater. Struct. 21 (2012) 035022
the TPO. The former is characterized by a state of uniaxial
stress during the entire debonding process. Before debonding
begins, the initially exposed portion of the wire (i.e. the
portion of the wire that comes out of the matrix) deforms
uniformly until the Fmax is reached. This confirms that the
details of the reorientation of the martensitic phase may not
be necessary in the initial elongation part as long as the
model can properly capture the uniaxial stress–strain response
depicted in figure 9(b). Once the debonding front propagates,
the exposed portion of the wire remains at constant uniaxial
stress (σmax in equation (6)), and only the newly liberated
wire deforms from its elastic regime to σmax . Any portion
of the wire that is still bonded to the matrix (ahead of
the debonding front) remains elastic at very low stress
levels; therefore, detwinning does not occur in those regions.
Rather, detwinning occurs only in a localized plane, oriented
perpendicular to the longitudinal axis of the wire, that follows
the debonding process zone as it propagates. This detwinning
zone divides the two regions of the wire previously described.
Since the wire stress state is well characterized (it is either in
its elastic regime when it is bonded to the matrix, or under
mostly uniaxial stress–strain conditions), and the detwinning
zone is well known at all times, we conclude that our model
described in section 5.2 is well suited for this very important
problem.
In contrast to the results obtained with LEFM, our FEM
suggests values of Gc in the range of 48–450 J m−2 for
the same pull-out forces obtained in the experiments. This
represents a difference of almost one order of magnitude
for each wire surface treatment, a discrepancy that can be
explained in terms of Gc . In the LEFM model, the NiTi
wire is assumed to undergo linear elastic deformation with
Ef = 30 GPa. According to the maximum tensile stresses
obtained in our pull-out tests (i.e. σmax ≈ 200 MPa for the
treated wires), the strains attained in the debonded part of
the wires are very small (i.e., εtot = 0.006) compared with
those obtained with our FEM and the nonlinear stress–strain
behavior shown in figure 9(b) (εtot = 0.03). These small
elastic strains predicted in the wire lead to an underestimated
elastic energy stored in the specimen available to advance the
debonding front. According to the fracture mechanics concept
of energy release rate [86], this ultimately represents much
lower values of Gc than those predicted by the FEM model.
To support these findings, we also carried out additional FEM
calculations (following a similar model to that described in
section 5.2) with the only exception that the NiTi behavior
was modeled with linear elasticity (the cohesive behavior
for the interface remains the same). For these new cases,
Fmax versus Gc is plotted with a green line in figure 10.
Open square symbols represent computed values of Fmax .
These results are similar to those obtained with the LEFM
model, indicating that the inelasticity of the stress-induced
detwinning in the martensitic phase of the NiTi is extremely
important in the debonding. Therefore, we conclude that
LEFM is not appropriate for modeling pull-out tests wherein
large inelastic deformation occurs in a NiTi wire.
Once the FEM was established and the Fmax versus Gc
curves developed, we proceeded to calculate Gc using the
14
F C Antico et al
Figure 11. Gc calculated for NiTi wires with embedded length
le = 70 mm (red squares) and le = 90 mm (red circles). The
standard deviation is used for the error bars. These results were
obtained using the FEM simulations considering residual stresses
(figure 10). For comparison purposes, the same values obtained with
the LEFM model are included as filled gray circles.
experimental values of Fmax reported in figure 8 for each
surface treatment. We employed the results obtained from our
FEM considering residual stresses (solid red line in figure 10).
The Fmax –Gc relationship follows a simple polynomial: Gc =
−36.20+0.84Fmax +0.55Fmax 2 (where force is in newtons and
−2
the energy is in J m ). The experimental mean and standard
deviation of Fmax were used to obtain the equivalent mean
values of Gc (with their equivalent standard deviations) as
shown in figure 11. Here, Gc increases (on average) from
the untreated condition, where it is least, to the 5% PPPA
treatment, where it is greatest. For comparison purposes,
the values of Gc obtained with the LEFM model were also
included in figure 11 in light gray. Figure 11 also shows
the cohesive energy for specimens with different embedded
lengths. Hence, the greatest adhesion is achieved with the
PPPA treatments.
6. Concluding remarks
We have considered methodologies for improving adhesion
between NiTi shape memory alloys in wire form and a
TPO polymer matrix. The methods included functionalizing
the NiTi surface with an organophosphorus treatment and
wire surface microgeometry roughening through sanding. We
observed that the wires that needed the highest pull-out force
Fmax were those treated with 5% phenylphosphonic acid
(PPPA), followed by those treated with 1% PPPA and the
hand-sanded specimens. The untreated wires had the lowest
pull-out forces. Since the TPO by itself allows no significant
chemical bonding with an NiTi wire surface, it is concluded
that the PPPA greatly improves the bonding and adhesive
strength at the interface between the NiTi and the TPO.
From our experimental results we also conclude that it
is possible to achieve wire tensile stresses that exceed the
Smart Mater. Struct. 21 (2012) 035022
manufacturer’s recommended values without debonding from
the polymer matrix, and hence design actuators could take
advantage of the maximum stresses possible from NiTi wires.
However, future effort should be aimed at understanding
the effect of cyclic loads and accumulating damage at the
interface to apply these treatments to actuators subject to a
high number of cycles. It should also be mentioned that the
pull-out tests in this study considered only wires at room
temperature. The temperature effect on the interfacial strength
and energy as well as the effect on the wire deformation
of the temperature-induced martensitic-to-austenitic phase
transformation must be explored in future studies.
Based upon an existing LEFM theoretical model with
Fmax as input, all NiTi wire surface treatments investigated
lead to a comparable improvement in computed cohesive
energy, Gc , of the wire–polymer matrix interface relative
to an untreated NiTi wire. However, we demonstrated that
this model is grossly inadequate. Through consideration of
the nonlinear stress–strain behavior of the NiTi wire and
residual stresses from molding in a refined FE model, we
find that the estimated values of Gc are not only significantly
higher than those predicted with LEFM, but they clearly
show that the PPPA treatment improves the adhesion of the
interface. Our models also showed that the residual stresses
from the manufacturing process have an important effect in
the debonding process by reducing the mode I contribution
caused by the thinning of the NiTi wire. Neglecting these
residual stresses can result in an overestimation of Gc from
20% to 40%. While the values of Gc reported are believed
to be qualitative in nature, they provide information that
qualitatively characterizes the treatments explored in this
work.
The decreasing contribution of mode I at room
temperature (the test temperature of interest in this study)
helps prevent additional damage mechanisms due to sliding,
friction and mechanical interlocking. To provide a more
definitive test of the different chemical and mechanical
treatments detailed here, future investigations should be
focused on wire pull-out experiments wherein the wire
is actuated (through a temperature-induced martensitic-to-
austenitic phase transformation), and when the wire is in the
austenitic phase and pull-out through an external force. The
consequences of such a study will reveal any increase in
Gc due to these additional energy dissipation mechanisms.
Along those lines, we suggest that improvements to
cohesive models should include characterization of the
NiTi surface topography at the micron level (see, for
example, [84, 85]), as well as atomistically informed cohesive
laws that properly account for the chemistry and physics
of the NiTi/organophosphorus/polymer interface. Indeed a
numerical model could be developed that accounts for all
of the aforementioned features of these composite materials
within the spirit of a multiscale computational modeling and
design [88]. The development of thermo-mechanical-based
cohesive models that account for the effect of microgeometry,
cyclic loads and temperature effects will be the focus of future
work.
15
F C Antico et al
Acknowledgments
The authors are grateful to Nancy Johnson and Alan Browne
for many stimulating discussions on shape memory alloys and
potential applications.
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