Research Article: Enhancing Fatigue Performance of Sandwich Composites With Nanophased Core
Research Article: Enhancing Fatigue Performance of Sandwich Composites With Nanophased Core
Research Article: Enhancing Fatigue Performance of Sandwich Composites With Nanophased Core
Journal of Nanomaterials
Volume 2010, Article ID 712731, 8 pages
doi:10.1155/2010/712731
Research Article
Enhancing Fatigue Performance of
Sandwich Composites with Nanophased Core
Copyright © 2010 S. Zainuddin et al. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
We report fatigue performance of sandwich composites with nanophased core under shear load. Nanophased core was made from
polyurethane foam dispersed with carbon nanofiber (CNF). CNFs were dispersed into part-A of liquid polyurethane through a
sonication process and the loading of nanoparticles was 1.0 wt%. After dispersion, part-A was mixed with part-B, cast into a mold,
and allowed to cure. Nanophased foam was then used to fabricate sandwich composites. Static shear tests revealed that strength and
modulus of nanophased foams were 33% and 19% higher than those of unreinforced (neat) foams. Next, shear fatigue tests were
conducted at a frequency of 3 Hz and stress ratio (R) of 0.1. S-N curves were generated and fatigue performances were compared.
Number of cycles to failure for nanophased sandwich was significantly higher than that of the neat ones. For example, at 57% of
ultimate shear strength, nanophased sandwich would survive 400,000 cycles more than its neat counterpart. SEM micrographs
indicated stronger cell structures with nanophased foams. These stronger cells strengthened the sub-interface zones underneath
the actual core-skin interface. High toughness of the sub-interface layer delayed initiation of fatigue cracks and thereby increased
the fatigue life of nanophased sandwich composites.
that by infusing a small percentage of nanoparticles in the was carried out in three steps; the first was the dispersion of
foam, the static properties of sandwich structures can also be nanoparticles into liquid polyurethane, the second was cast-
enhanced under flexural loading [19]. Similar trend has been ing of the foam (core materials), and the final was fabrication
demonstrated when nanophased sandwich structures were of sandwich panels using CIRTM. In addition, a number
tested under compression and high strain rate loadings [20]. of sandwich panels were also made with neat polyurethane
As far as particles are concerned, vapor-grown carbon foam without having any nanoparticle infusion.
nanofibers (CNFs) are drawing significant attention due
to their high strength, modulus, and relatively low cost
2.1. Dispersion of Nanoparticles into Liquid Polyurethane.
[21, 22]. These particles are synthesized from pyrolysis of
The steps used for dispersion of nanoparticles in liquid foam
hydrocarbon or carbon monoxide in the gaseous state, in
are shown in Figure 1. The liquid foam has two parts: part A
presence of a catalyst [23, 24]. As opposed to carbon nan-
(Diphenylmethane Diisocyanate) and part B (Fluorocarbon
otubes (CNTs), CNFs do not have tubular structure—rather
blown Polyol). Part A was selected for infusion of nanopar-
they have carbon fiber-like structure with diameter in the
ticles since it is less reactive than part B. Carbon nanofibers
nanometer range and a good aspect ratio. Carbon nanofibers
(CNFs) were first measured to have 1% by weight of part-
have been used in this investigation as reinforcement. One of
A plus part-B (step 1). It was observed that beyond 1.0 wt%
the main reasons to use CNF as reinforcement was of course
loading, agglomeration increased significantly and the cell
the cost but more than that was the acicular aspect of CNF.
structures were collapsing. In our earlier investigations [5,
Carbon nanofibers having large aspect ratio would allow
11, 20] nanoparticle loading also remained within 1–3 wt%.
more entanglement with polymer chains at the mesophase
The mixing was carried out in a Sonic Vibra Cell ultrasonic
stage of the foaming process. This entanglement of CNFs
liquid processor (Ti-horn, 20 kHz, 100 W/cm2 ) for about 30
with the polymer would introduce interfacial tension when
minutes at 5◦ C temperature (step 2). At this time it was visu-
stresses are applied and allow large deformation—a property
ally observed that nanoparticles were uniformly dispersed in
that would be desirable under shear and fatigue loading.
Part-A. We varied the sonication parameters time, frequency,
Uniform dispersion of nanoparticles poses another prob-
and intensity many times to come up with 30 minutes,
lem in the preparation of nanocomposites. Due to high sur-
20 kHz, and 100 W/cm2 , respectively as optimum parameters
face energy, nanoparticles tend to agglomerate and produce
for the system. After each trial, foam was made and looked
unwanted stress concentration which may act as a precursor
under SEM to check the cell structures—if they were broken
for failure. High-intensity ultrasonic waves have been used
or collapsed, parameters were changed until we came up with
successfully to get uniform dispersion of nanoparticles [25,
the best possible cell structure. In order to avoid temperature
26]. Ultrasound waves generate nonlinear effects in the
rise during sonication, external cooling was applied for the
liquid, namely transient cavitation and acoustic streaming
entire period of irradiation. External cooling was applied
[27–30]. Acoustic cavitation involves formation, growth,
through an NESLAB RTE Series refrigerated bath. After infu-
pulsating, and collapsing of minute bubbles, producing
sion of nanoparticles, the modified Part-A was mixed with
transient (in the order of microseconds) microhot spots
Part-B at a ratio of 48 : 52 by weight using a mechanical stir-
that can reach temperatures of about 5000◦ C, pressure
rer at 2500 rpm for about 30 s (step 3). The mixture was then
of about 1000 atm, and heating and cooling rates above
cast into a mildly preheated steel rectangular mold. After
1010 K/s [31]. Strong acoustic impact coupled with local
about 8-9 hours, the cast foam (step 4) was demolded and
high temperature effects accelerates intrinsic mixing of
postcured for about 20 minutes at 80◦ F. The density of the
polymer and nanoparticles and can break the agglomerated
foam in both categories was measured to be around 0.08 g/cc.
particles by damaging the Coulomb and Van der Waals forces
resulting in a homogenous dispersion.
Mechanical behavior of foam cores for simple stress states 2.2. Sandwich Fabrication. CIRTM process was employed
such as uniaxial tension or compression has been studied to fabricate the sandwich panels. Both the top and bottom
extensively [32–35]. Only a limited number of investiga- face sheets were infused simultaneously during the CIRTM
tions have dealt with multiaxial behavior [36, 37]. In this process. A schematic of the co-injection process is shown
study, polyurethane foam properties have been modified by in Figure 2. Dry fabric preforms with required orientations
dispersing nanoparticles through sonic cavitation. Sandwich were first laid out on the top of a flat aluminum tool. The
panels were then fabricated using the nanophased foam as fabric used in this investigation was plane weave S2-Glass
core materials through the CIRTM process. In parallel, con- fibers. Three layers of fabrics were used for each face sheet.
trol sandwich panels were also made using neat polyurethane The core was then placed on the top of the bottom face
foam. Response of these sandwich structures under static and sheet fabrics, and upon which the preforms for the top
cyclic shear loading are described in the paper. face sheets were stacked. Two types of core materials were
used during the fabrication; one was neat polyurethane, and
the other was dispersed with CNF. After stacking, infusion
2. Materials and Manufacturing of lines were installed and the assembly was vacuum bagged.
Sandwich Composites Before infusion the system was debulked for several hours.
SC-15 epoxy resin (Part-A: epoxy, Part-B: Hardener, Alkyl
Materials used for making two categories of sandwich com- Polyamine) manufactured by Applied Poleramic, Inc. was
posites are shown in Table 1. The manufacturing of panels used in this study due to its low viscosity (300 cps) and longer
Journal of Nanomaterials 3
Stirrer
Mixture of Mixture of
part A and part A, part B
CNF and CNF
(a) (b) (c) (d)
Figure 1: Schematic of manufacturing of nanophased PU foam: (a) step 1; (b) step 2; (c) step 3; (d) step 4.
pot life (6 hours). After the resin infusion, the vacuum was
kept on until the complete cure took place. No additional
adhesives were used for the skin-core bonding, since it
developed during the cure process. It is to be noted here
that the surfaces of the nanophased foams had to be sanded
prior to setting them up in the CIRTM mold. This allowed
better adhesion between the core and the skin. Several panels
were fabricated in this manner and were machined for shear
characterization.
Property Neat Polyurethane Foam Sandwich 1% CNF Polyurethane Foam sandwich % Improvement
0.55 0.83
0.64 0.81 +33
Shear Strength (MPa)
0.66 0.78
Ave.: 0.61 ± 0.014 Ave. : 0.81 ± 0.02
11.7 13.7
11.9 14.9
+19
Shear Modulus (Mpa) 12.4 14.4
Ave. : 12.0 ± 0. 35 Ave. : 14.3 ± 0.32
0.6 Neat polyurethane foam sandwich data for a minimum of three specimens in each category
of sandwich composites were generated at stress levels of
90%, 80%, 70%, 60%, and 50% of the ultimate static shear
0.4 strength.
4.2. Fatigue Tests. Shear fatigue data for both neat and
nanophased sandwich composites are shown in Table 3. S- 1
N (stress versus number of cycles) diagram for the fatigue
tests is shown in Figure 6 The stress axis is normalized with
ultimate shear strength. Data shown in the S-N diagram are
the average values from Table 3. Under constant amplitude 0.8
loading many engineering materials exhibit a plateau in the
τ/τultimate
stress life plot typically beyond 106 cycles, which is also true
in this case. The fatigue limit is seen to be about 55% of
the ultimate strength for the nanophased specimen while it 0.6
is 50% for neat specimen. It is seen in Figure 6 and in Table 3
that at each stress level, the number of cycles to failure for
nanophased foam was significantly higher than that of neat
specimen. The failure process in both the nanophased and 0.4
neat sandwiches was similar to that of PVC foam sandwich 0 0.4 0.8 1.2
composites studied by one of the authors [4]. Fatigue failure Number of cycles ×106
modes are shown in Figure 7. Small cracks first appeared
near the core-skin interface that coalesced into several larger 1 % CNF sandwich composite
Neat sandwich composite
cracks and progressed along the interface. After propagating
for a relatively short distance, these larger cracks as seen Figure 6: S-N curves for neat and nanophased specimens. Stress
in Figure 7 kinked into the core and traversed through the ratio R = 0.1 and frequency = 3 Hz.
thickness of the core. This suggests that during fatigue as
well as in static loading, the weakest region in a sandwich
composite is the core-skin interface region which is prone During fatigue the scenario is somewhat different—large
to failure at the initial stage of the loading. These minute cracks kink into the core at multiple places and propagate
cracks coalesce into one or many major cracks depending at about 20–40◦ angle. Cracks kinking into the core in fact
on the type of loading. If it is quasi-static, usually there is signals the final failure event as the core shear process is
only one major crack. However in case of fatigue loading very quick. As seen in Figure 7, some of the shear cracks
the number of major cracks is several. During quasi-static reach the interface on the opposite side depending on the
loading, the major crack kinks into the core at a sharp energy available at the crack tip and resistance offered by the
angle and diagonally crosses the entire thickness of the core. embedded nanoparticles.
6 Journal of Nanomaterials
Interface
Fixed plate
Separation of
plates along the
fracture line
Fracture
Fracture crack
Moving plate
(a) (b)
Figure 7: (a) Schematic of crack formation in the core and (b) schematic showing the line along which final shearing occurs.
Table 3: Fatigue test data for neat and 1% CNF sandwich composites.
4.3. SEM Analysis. To investigate the dispersion of nanopar- derives its strength from its edges, walls, faces, and the
ticles and their effect on the foam microstructures, SEM entrapped gas. Nanophased core will provide more resistance
analyses were carried out on both neat and nanophased to crack propagation due to its hexagonal shape, relatively
foam as shown in Figures 8(a)-8(d). It was observed that thicker edges, and walls as seen in Figure 8(d). It is quite
as-received CNFs were agglomerated due to high surface possible that as the resin gets filled into the partially opened
energy as shown in Figure 8(a). Since the length of CNF is cells, it soaks the cell walls and edges up to a certain depth.
in the order of micron, it is possible to observe individual When the resin is cured, these soaked cells become stronger
CNF-dimensional parameters. The diameter of CNF was than the regular dry cells just underneath. A sub-interface
measured to be about 200 nm, which agrees with the data is therefore created between these so-called soaked and dry
sheet [38]. Embedded CNFs in the cell edges are shown cells, which are apparently weaker than the actual core-
in Figure 8(b). Figure 8(b) also indicates that the CNFs skin interface mentioned earlier. It is indicated in earlier
were well separated and dispersed. The micrographs (c) studies [11, 20] that nanoparticle acts as a catalyst during
and (d) show that both neat and nanophased foams have the foaming process and controls the rate of CO2 generation,
a fairly uniform distribution of regular cells. As seen in which in turn affects the cell wall and edge thicknesses. It
these figures, cell edges and walls are distinctly visible with is believed that more resins are absorbed in thicker edges
almost uniform cell structures throughout. It is observed and walls during the fabrication of sandwich composites.
in the micrographs that CNF nanoparticle has somewhat This will make the soaked region relatively stronger and
different effect on the microstructure of the cell as it was consequently delay the initiation of cracks in the nanophased
observed in earlier studies [5, 11, 20]. In the present case foams during fatigue. In particular, two phenomena will
the size of the cell does not change whereas the shape of the dominate the failure of the core during shear fatigue: (i)
cell has changed significantly—from spherical to pentagon cell stretching in the loading direction which gives rise
or hexagonal shape. It is well known that closed cell foam to initial interface cracks and (ii) kinking of the interface
Journal of Nanomaterials 7
5. Summary
(1) It is shown that shear strength and modulus of
nanophased sandwich composites can be increased
T-CAM 5kV 10μm ×1, 000
by about 30% by reinforcing the polyurethane core
material with 1 wt% loading of carbon nanofibers
(a) (CNFs)
(2) Significant improvements have also been observed
during fatigue loading under shear. In an average
sense fatigue limit (i.e., stress level to survive more
than 1 million cycles) of nanophased sandwich
composites was found to be around 55% of the
ultimate shear strength as opposed to 50% in case of
neat foam. On a specific note, for example, at 57% of
τultimate , nanophased sandwich would survive 400,000
cycles more than its neat counterpart.
(3) It is observed that quasi-static shear failure is mostly
governed by a single shear crack diagonally traversing
TCAM 0000 30kV 5μm ×5, 000 through the core. On the other hand in case of shear
fatigue, failure is due to multiple cracks across the
(b)
thickness of the core. In both cases, cracks initially
appear at the coreskin interface, propagate for a short
distance along the interface, and then kink into the
core signaling the final failure event.
(4) Embedded nanoparticles seem to modify the cell
structures, offer resistance to crack propagation, and
delay the kinking of interface cracks into the core.
Acknowledgment
The authors would like to thank the Office of Naval Research
(ONR) (Grant no. N00014-06-1-0696) and the National
TCAM-SB 0000 5kV 100μm ×130
Science Foundation, (NSF) (Grant no. HRD-976871) for
(c) supporting this research.
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