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Creep and Interfacial Behavior of Carbon Fiber

Reinforced Epoxy Filament Wound Laminates

Jose Humberto S. Almeida Jr. ,1,2 Heitor L. Ornaghi Jr. ,3 Nata  lia P. Lorandi,3 Bernardo P. Bregolin,3
1
Sandro C. Amico
1
PPGE3M, Federal University of Rio Grande do Sul, Av. Bento Gonçalves, 9500, Porto Alegre, RS 91501-970,
Brazil

2
Department of Composite Materials, Leibniz-Institut fu€r Polymerforschung Dresden e.V., Hohestraße 6,
Dresden 01067, Germany

3
PGMAT, Caxias do Sul University, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, RS 95070-560, Brazil

This article focuses on the investigation of the interfacial marine, aerospace and aeronautic areas are continuously
and creep characteristics of carbon fiber-reinforced replacing metallic structural counterparts by composite
epoxy laminates at different fiber orientations. Flat unidi-
rectional 12-layer laminates were manufactured by dry-
ones, to increase payload [1, 2]. Nevertheless, the use of
filament winding and cured under hot compression. The advanced composites in structural counterparts is still lim-
following winding sequences were studied: [0]12, [30]12, ited. One of the reasons is that their mechanical proper-
[45]12, [60]12, and [90]12. Short-beam testing aided by ties, including interfacial and interlaminar properties are
microscopy and dynamic mechanical analysis were significantly dependent on time, temperature, and fiber
used to assess interfacial characteristics and creep
behavior of the laminates. Short beam strength and
orientation. For instance, laminas are not prone to creep
creep behavior were strongly influenced by fiber orienta- when loaded in the fiber direction, but this does not occur
tion. Short beam strength decreased 270%, and only the when there is a mismatch between them, which can lead
laminates wound at 08 presented delamination purely at to excessive strain and premature failure [3].
the mid-plane. Fiber/matrix stress transfer is more effi- The mechanical performance of a composite with
cient for laminates wound at 08, providing better creep
behavior. Dynamic mechanical analysis results indicated fibers embedded into a polymeric matrix strongly depends
the storage modulus to be dependent on the ply angle. on its fiber/matrix interface and on suitable interfacial
Findley’s and Burger’s fitting were used to analyze creep fiber/matrix bonding. There are some micromechanical
data from the DMA and correlate structure and property methods to evaluate interfacial strength, such as push-out
of the composites. The creep strain increases from lon- [4] and pull-out [5] tests. However, apart from their com-
gitudinal to transversal fiber orientation and by increas-
ing the temperature. At higher temperatures, samples plexity, they are mostly unable to evaluate the effect of
longitudinally oriented exhibited an elastic behavior, with fiber orientation on the interfacial strength as a single
good agreement with the Findley’s model. POLYM. COM- fiber is embedded in a matrix. In this way, a more macro-
POS., 00:000–000, 2017. V
C 2017 Society of Plastics Engineers
scopic method to assess fiber/matrix interface is more
appropriate. The short beam test is suitable to correlate
fiber orientation and interfacial stress transfer capability,
easily enabling direct evaluation of interlaminar strength
INTRODUCTION
or indirect evaluation of interfacial strength [6, 7].
Carbon fiber reinforced polymer (CFRP) composites In addition, study of the influence of fiber orientation
are well known to possess high stiffness- and strength-to- on long-term characteristics of these laminates is essential
weight ratio, as well as lack of corrosion. Among others, for safe design. Creep refers to a time-dependent defor-
mation under a constant load at a specified temperature.
Correspondence to: J.H.S. Almeida; e-mail: jhsajunior@globomail.com Creep is considered a crucial material property at a long-
and humberto@ipfdd.de term point of view [8]. For composites, creep resistance
Contract grant sponsor: AEB (Brazilian Space Agency), CAPES, and is directly associated with viscoelastic strain and fiber/
CNPq.
DOI 10.1002/pc.24537
matrix interfacial behavior. As temperature, stress, and
Published online in Wiley Online Library (wileyonlinelibrary.com). time are crucial parameters to describe viscoelastic behav-
C 2017 Society of Plastics Engineers
V ior, especially when the fiber/matrix coupling needs to be

POLYMER COMPOSITES—2017
assessed, several models have been proposed to predict D3171) and overall mean thickness of the 12-layer lami-
long-term creep behavior of composites [9–11]. nate was 4.2 mm. Unidirectional laminates were produced
Among the proposed models, Findley et al. [12] used and the specimens were cut using a CNC machine at dif-
an empirical power equation to describe creep behavior ferent off-axis angles, producing the following laminates:
of several polymers with good accuracy over a wide [0]12, [30]12, [45]12, [60]12, and [90]12.
time-scale. According to Yang et al. [13], this power law
is suitable for materials that do not exhibit a pronounced
Characterization
second creep stage, especially under low stress, which is
the case of the current study. However, it is difficult to The dynamic mechanical and creep behavior was
interpret the results due to numerous variables involved assessed using a dynamic mechanical analyzer DMA Q-
in this model, including degree of crosslinking of the 800 equipment from TA instruments. Three samples hav-
matrix, which may vary between bulk and close to the ing dimensions of 50 3 10 3 4 mm3 were used for DMA
fiber interface, physical aging, temperature and moisture tests under three-point mode with a span-to-thickness ratio
effects, matrix shrinkage under isothermal curing, and of 12:1. General dynamic mechanical analysis was per-
thermal expansion of both resin and fiber [14]. Another formed first aiming to detect mobility regions. Two runs
important model is the Burger’s creep model [8], also were carried out under the following conditions: 258C–
known as the four-parameter model, which includes the 1508C temperature range, heating rate of 38C/min (in the
essential Maxwell and Kelvin-Voigt elements and can sat- first run 108C/min), constant frequency of 1 Hz, pre-load
isfactorily model the practical behavior of viscoelastic of 0.1 N, amplitude of 15 lm, and force track of 125%.
materials [13]. The second run was performed seeking to avoid interface
Goertzen and Kessler [15] evaluated creep behavior of concerns [18, 19].
carbon/epoxy composites under tensile and flexural load- Creep tests were carried out using the same three-point
ings and concluded by extrapolating creep results that the bending setup, sample dimensions, and DMA equipment.
material would not fail below 65% of the tensile strength A static stress value of 2 MPa was applied at the center
for 1,600 h. Melo and Medeiros [16] determined creep- point along the length of the sample for 10 min after con-
rupture failure of epoxy coupons based on tensile, ditioning at 308C, and creep strain was measured as a
compressive and dynamic-mechanical tests at different function of time (30 min) at constant temperature (308C)
temperatures, and produced master curves and failure [9, 12].
envelopes based on the Tsai-Wu criterion. In addition, Ha Findley’s and Burger’s models were applied to predict
et al. [17] concluded that, to obtain standard master creep behavior of the laminates. Findley’s power law is
curves to describe creep-rupture of polymer and/or com- given by:
posites, suitable properties, such as constituent strengths,
should be directly measured. EðtÞ5E0 1Atn (1)
In this context, the scope of this work is to apply both
Findley’s and Burger’s models to predict creep behavior of where EðtÞ is the creep strain at time t, E0 is the instanta-
carbon fiber reinforced epoxy filament wound flat laminates neous elastic strain or time-independent, A is the ampli-
and validate the analytical results with experimental ones. tude of transient creep (time-dependent) and n is a
In addition, short beam strength (SBS) is used to indirectly constant independent of the stress and generally less than
assess the interfacial characteristics of the laminates. one [12, 20].
Burger’s model (Eq. 2) is shown in Eq. 2:
EXPERIMENTAL
r0 r0 r0
EðtÞ5 1 2E t=g
1 (2)
Materials and Manufacturing EM eK ð12e K K Þ gM

Carbon fiber reinforced epoxy prepreg tow (usually where r0 is the stress, EM is the elastic modulus of the
known as towpreg) from TCR Composites, which is com- Maxwell model (spring), EK is the elastic modulus of the
posed of Toray T700–12K-50C carbon fibers and UF3369 Kelvin model, hM and hK are the viscosities of Maxwell
epoxy as resin system, was used. The flat laminates were and Kelvin dashpots, respectively. The first term is a con-
produced using a rectangular stainless steel mandrel (327 stant related to the deformation of the Maxwell model,
3 228 3 12 mm3) in a filament winding system from the second represents the early creep stage, and the third
MFTech coupled with a KUKA robot KR 140 L100. The the creep trend at a sufficiently long time [9].
towpregs were wound onto the mandrel and then a shrink The interfacial behavior was investigated using short-
tape was used to help consolidating the laminate through- beam test, following ASTM D2344–13 using a span-to-
out the curing process that followed. thickness ratio of 4:1. Length and width of the specimens
The laminates were cured by hot compression under 6 are 24 mm ð63tÞ and 8 mm ð23tÞ, respectively. The
ton for 4 h at 1308C. The final fiber volume fraction was SBS was calculated by Eq. 3. Ten specimens were tested
72% (measured by acid digestion following ASTM in each case and fractographic studies of failed specimens

2 POLYMER COMPOSITES—2017 DOI 10.1002/pc


P
SBS50:75 (3)
wt
where P, w, and t are the ultimate load, width, and thick-
ness of the specimen, respectively.

RESULTS AND DISCUSSION

Interfacial Characteristics
The interfacial behavior is herein indirectly evaluated
through short-beam testing, formerly known as interlami-
nar shear strength. Figure 1 depicts the typical short beam
stress versus displacement for the on- and off-axis lami-
nates studied. The strong influence of fiber orientation on
interlaminar behavior of the specimens is clear. The [0]12
specimens presents the most non-linear behavior, where
FIG. 1. Representative stress versus displacement curves for the speci-
mens. [Color figure can be viewed at wileyonlinelibrary.com]
several load drops can be seen after the maximum load is
achieved, which is caused by multiple horizontal cracks
on the specimens. A large delamination at the mid-plane
were carried out using optical microscopy, in a Carl Zeiss of the specimen is reported, which is observed at the final
Axioscope, and scanning electron microscopy (SEM), in a load drop [21] and clearly corroborates the SEM images
Phenom ProX equipment. of the [0]12 fractured specimen (Fig. 2a and b).

FIG. 2. SEM micrographs of the [0]12 (a-b) and [90]12 coupons (c-d).

DOI 10.1002/pc POLYMER COMPOSITES—2017 3


FIG. 3. Optical micrographs for [0]12 (a), [30]12 (b), [45]12 (c), [60]12 (d), and [90]12 (e) post-mortem SBS
coupons.

The stress supported by the specimens wound at higher The [30]12 and [45]12 samples had homogeneous shear
angles is lower than the [0]12 sample, as would be failure, which is characterized by a clear final load drop
expected for unidirectional composites subjected to 3- and small cracks distributed along the specimen. Failure
point bending. The [30]12 and [45]12 coupons present less in the [60]12 and [90]12 coupons were dominated by ten-
non-linearity in their curves, with less evidences of shear sile forces, with a vertical opening of the major crack
failure. Furthermore, specimens oriented at [60]12 and centrally located at the bottom surface and a brittle
[90]12 support almost the same stress, with similar stress failure.
versus displacement profile. The abrupt drop noticed in Figure 2 presents the post-mortem analysis of the SBS
some of the specimens is an indication that bending and fractured [0]12 (a-b) and [90]12 specimens (c-d). Failure
compressive loads are more important in this case, and in [0]12 specimens occurred as expected for this type of
the lack of fibers along the longitudinal direction pro- loading, as a large delamination at the mid-plane of the
motes sudden failure. Thus, short-beam strength, similarly specimen thickness and multiple minor horizontal cracks
to other composites properties, increases when the rein- were found, characterizing interlaminar shear failure. That
forcement is oriented along the loading direction [22]. is, a simple shear state was generated on the test as
Daniels et al. [23] listed all possible failure modes parallel regions slide in opposite directions, generating
involved in short-beam testing. The [0]12 coupon had dis- horizontal cracks and delamination. Conversely, [90]12
crete shear failure characterized by a large single horizon- specimens have a matrix-dominated failure with no evi-
tal crack, and the final load drop represents delamination. dence of shear as a vertical crack initiated at the specimen

4 POLYMER COMPOSITES—2017 DOI 10.1002/pc


Dynamic Mechanical Behavior
Dynamic mechanical analysis of the composites was
carried out aiming to observe initial regions where molec-
ular mobility takes place. Figure 4 presents storage and
loss moduli, and tan delta of the composites. Large differ-
ences are noticed among the laminates in the glassy
region from 08 to 908 loading direction. This is due to
distinct stress transfer efficiency, where for composites
transversally oriented, adhesion forces play a major role.
For the [0]12 specimen, the fibers carry nearly all applied
load, thus greater modulus is expected.
Loss modulus refers to dissipated energy in the senoi-
dal deformation cycle and it was used here to select the
temperatures for the creep tests, that is, 308C and 608C,
being both in the glassy region. It is noted that peak
height varies in accordance to the storage modulus, and
the higher the drop in storage modulus above the glassy
region, the higher the loss modulus peak. This results in
similar tan delta curve shapes [24].
According to Akay [25], E00 gives a better indication
of the molecular mobility in composites materials com-
pared to tan delta. However, Qin and McKenna [26]
showed that the activation energy is more useful for clas-
sifying the temperature dependency of the dynamic prop-
erties than the glass transition temperature (Tg). In the
current study, Tg values were collected from the loss
and tan delta curves aiming to further investigate this
(Table 1).
Tan delta curves indicate that Tg is similar for all ori-
entations, considering the errors involved (6 58C) and
that fiber and matrix systems are the same in all samples
[27]. Tg values remain almost the same because thermal
conductivity distribution is more uniform, and (as the
resin is the same) sensitivity to variations experienced by
the resin is not so pronounced. It is important to mention
that Tg is not the best way to evaluate molecular mobility
and does not represent the reinforcement effect, as men-
tioned earlier. The tan delta peak height also indicates
energy dissipation in the composite and higher peak
height suggests poorer interface, which can be a conse-
quence of the variable stress transferring efficiency.
According to Table 1, no significant differences among
FIG. 4. Storage (a) and loss moduli (b), and tan delta (c) for the stud- the results are seen. In Akay’s study [24], a more
ied composites. [Color figure can be viewed at wileyonlinelibrary.com]
pronounced variation (DT) was achieved, and the loss
modulus peak was a more consistent indicator of the
upper surface between the supporting cylinders, character- mechanical behavior of the composite. The divergence
izing failure by flexure and primarily transverse tensile, could be justified by a combination of factors such as the
corroborated by the brittle behavior of the epoxy resin.
The other failed short-beam specimens are presented in TABLE 1. Tg values obtained in the DMA analysis of the laminates.
Fig. 3. Optical microscopies corroborate delamination and
Laminate Tg from (E00 )max (8C) Tg from (tan d)max (8C) DT (8C)
horizontal minor cracks at the thickness mid-plane for
[0]12 specimens, confirming interlaminar shear failure. On [0]12 86 95 9
the off-axis specimens, multiple cracks can be found in [30]12 85 97 12
the fiber direction. A combination of shear and tensile [45]12 78 91 13
[60]12 78 91 13
loads acting on the specimen are found, confirmed by a
[90]12 83 95 12
slight influence of bending during the test.

DOI 10.1002/pc POLYMER COMPOSITES—2017 5


FIG. 5. Creep behavior of the CFRP laminates: experimental data and curve fitting according to Findley’s
and Burger’s models at 308C (a) and 608C (b) under a stress of 2 MPa. [Color figure can be viewed at
wileyonlinelibrary.com]

non-uniform compliance in the matrix due to fiber-matrix Findley’s parameter A was found to increase from
interactions (which considerably changes with fiber orien- [0]12 to [90]12, as expected. This means that instantaneous
tation). In the current study, deformation from thermal deformation is higher due to poorer stress transfer for
effects is not so pronounced due to the processing method transversely oriented specimens. Furthermore, as fiber/
used, which gives a more uniform structural composite, matrix interactions are of the frictional type, transverse
with very different storage modulus range. For the sample load is more prone to creep as it relies purely on tensile
longitudinally oriented, this difference was lower in com- decoupling of the fiber/matrix interface. The n parameter
parison to the other specimens due to a more efficient was found to decrease with the angle but this is not
thermal conductivity resulting in a more uniform tempera- necessarily related to any particular characteristic of the
ture distribution, which narrows the difference between material [9, 10, 20].
moduli. Higher difference is achieved for transversely ori- By increasing the temperature, a similar trend is
ented coupons (which show similar DT due to similar observed in relation to fiber orientation. However, greater
thermal conductivity). deformation is noted due to higher molecular mobility
promoted by thermal effects. Overall, the systems are in a
more relaxed state, so even small perturbations (which
Creep Behavior
are dependent on volume, for example) are sufficient to
Creep curves for all laminates at a stress level of 2 promote conformational relaxation, which affects the
MPa at 308C and 608C are shown in Fig. 5a and b, along change in volume. The structural change in response of
with the fitting obtained using both Findley’s and temperature variation is then more pronounced. However,
Burger’s models. It can be clearly noted that creep behav- as the ply angle increases, the Burger’s model fitting
ior changes with the orientation angle, especially instanta- becomes unsuitable, which can be associated with higher
neous deformation (initial deformation). All curves follow mobility degree due to thermal effects [9].
the classical creep curve trend, as reported by Findley All Burger’s parameters (Table 3) were discussed con-
[12]. From these curves, Findley’s and Burger’s model sidering the present system, which differs from a semi
parameters were calculated and are presented in Table 2 crystalline matrix, for instance. In this study, EM can be
and Table 3, respectively. associated with the instantaneous modulus and represents

TABLE 2. Findley’s parameters A and n, and the coefficient of determination R2 for the CFRP laminates with different fiber orientations, at 308C
and 608C.

T (8C) Findley’s parameter [0]12 [30]12 [45]12 [60]12 [90]12

30 A (mm mm21 s21) 5.14 3 1023 1.39 3 1022 2.44 3 1022 3.68 3 1022 5.43 3 1022
n 0.0471 0.0359 0.0195 0.0303 0.0177
R2 0.9924 0.9998 0.9998 0.9998 0.9998
60 A (mm mm21 s21) 8.37 3 1023 1.38 3 1022 2.93 3 1022 3.90 3 1022 4.36 3 1022
n 0.0738 0.0957 0.0844 0.0890 0.0927
R2 0.9960 0.9962 0.9997 0.9998 0.9998

6 POLYMER COMPOSITES—2017 DOI 10.1002/pc


TABLE 3. Burgers parameters EM, gM, EK, and gK, and the coefficient of determination R2 for the CFRP laminates with different fiber orientations,
at 308C and 608C.

T (8C) Burgers parameter [0]12 [30]12 [45]12 [60]12 [90]12

30 EM (Pa) 1.69 3 108 9.54 3 107 9.66 3 107 4.04 3 107 6.75 3 107
gM (Pa s) 1.03 3 107 5.42 3 106 7.58 3 106 2.56 3 106 3.60 3 106
EK (Pa) 1636.76 630.90 379.22 242.51 171.76
gK (Pa s) 1879.26 682.69 397.05 263.11 170.73
R2 0.9986 0.9992 0.9997 0.9995 0.9998
60 EM (Pa) 2.19 3 105 4.10 3 103 3.45 3 103 1.65 3 103 1.051 3 103
gM (Pa s) 7.35 3 105 3.10 3 105 1.73 3 105 1.23 3 105 1.06 3 105
EK (Pa) 182.65 102.45 50.53 37.36 33.08
gK (Pa s) 270.21 212.23 88.96 75.66 75.16
R2 0.9256 0.9236 0.9328 0.9306 0.9232

the composite stiffness regarding stress application. In our mid-plane was found. For the other specimens, the main
study, similar results were found. It is expected that 08 failure occurred at the bottom surface, indicating bend-
angle yields higher values in comparison to 908, consider- ing effects.
ing the previous storage modulus results. As a low stress The viscoelastic behavior is also dependent on fiber
level was applied in the creep tests, this behavior remains orientation, as well as the creep performance. Storage and
nearly unaltered. loss moduli showed great dependency with fiber orienta-
The hM parameter corresponds to the irreversible tion, and the overall curves were used to determine
deformation in the amorphous regions, or the irrecover- parameters of the creep analytical models. Both Burger’s
able creep. A decreasing trend is observed for this param- and Findley’s models were suitable to predict creep
eter, which can be associated with the polymer chains behavior of the unidirectional specimens herein analyzed,
restrained due to a more efficient stress transfer. The hK showing good fitting of the experimental data. A larger
parameter is related to the viscosity of the amorphous difference in fitting is observed at higher temperature. As
regions and a decreasing trend is observed, associated to the angle ply increases, Burger’s seems not to adjust to
the increase in mobility of molecular chains of the matrix. the experimental data as well as Findley’s.
In the studied composites, this decrease is perhaps justified Findley’s power law is simpler and can satisfactory
by a more equally distributed stress between matrix and express long-term creep properties, whereas Burger’s pro-
fibers, as the orientation changes from 08 to 908. Thus, vides a more constitutive model, and allows a more detailed
greater mobility is obtained for the composites in which structure-to-property relationship analysis. A larger difference
the matrix carries relatively more stress and short-term vis- was noticed at higher temperatures being only satisfactorily
cosity of the amorphous polymer chains increases. adjusted using a three-parameter model (Findley’s).
Finally, EK is associated to the short-term stiffness of
the amorphous polymer chains. In this study, higher val- REFERENCES
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8 POLYMER COMPOSITES—2017 DOI 10.1002/pc

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