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Article M AT E R I A L S
Journal of Composite Materials
2018, Vol. 52(15) 1997–2015
! The Author(s) 2017
The effect of voids on the quasi-static Reprints and permissions:
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tensile properties of carbon fiber/polymer- DOI: 10.1177/0021998317737827
journals.sagepub.com/home/jcm
laminated composites
Abstract
Static longitudinal/transverse tensile tests for unidirectional carbon fiber/polymer (T300/924) laminates and laminates
with lay-ups ½0= 45=0=90s at various void levels were conducted, and degradations in stiffness/strength were observed
with the presence of voids. The void levels were controlled by compression pressure during the compression molding
process. The characterization of voids was achieved by digital microscopy image analysis; the density distributions of
equivalent diameters and aspect ratios were analyzed with respect to compression pressure.
For the purpose of quantifying the effect of voids on the static mechanical properties of composites, a stiffness
prediction method based on the Mori-Tanaka method and void geometric statistical data have been used with the
implementation of a finite element model of the representative volume element for unidirectional composites; the
prediction results show good correlation with experimental data. Finally, a modified continuum damage model for
laminated composites with the presence of voids was proposed, the model is capable of capturing the effect of voids;
and gradual damage analysis for carbon fiber/polymer composite laminates at different void levels was conducted to
evaluate the effect of voids on their tensile properties.
Keywords
Carbon fiber/polymer composites, effect of voids, mechanical properties, voids’ morphological analysis
Figure 2. Image pre-processing and noise elimination: (a) original grayscale image, (b) binary image, and (c) image after noise
elimination.
able to identify the location and geometric characteris- dimensions of 10 mm 10 mm were cut using a
tics of voids; more than one specimen was analyzed to water jet, providing the nonuniform distribution of
reduce the random error and to improve the accuracy voids, from randomly selected positions of plaques.
of measurement in this study. An image analysis soft- Before further observation, the samples were first
ware module based on the image-processing functions embedded into epoxy and cured for 24 h before being
provided by MATLAB has also been proposed to char- polished using abrasive papers and grinding com-
acterize the voids. In detail, the grayscale micro-image, pounds until the surfaces were smooth enough to
as shown in Figure 2(a), was taken from an optical observe. For each single sample, images of three differ-
microscope and then converted to binary images, as ent cross-sectional areas were captured by a PC-based
shown in Figure 2(b). In this process, pixels within CMOS camera using a 200 magnification lens (the
the area of voids would be set to pure black (value selected magnification allows the identification of
‘‘0’’), while the pixels in the rest of the area would be fibers and voids). The resolution of the image is 136
set to pure white (value ‘‘1’’). This process could be pixels per 100 um.
achieved by setting an appropriate threshold in the con- The void content can be obtained through calculat-
verting process, the value of the threshold should be ing the area proportion of all the voids in the micro-
carefully adjusted for each figure until the boundaries images, which has been proven to be one of the efficient
of voids are able to be identified, thus the voids can be and accurate ways for measuring the void level. In this
separated from surrounding fibers and matrix. Note research, some geometric parameters that were
that noticeable noise could be observed after conver- reported as having an impact on the mechanical prop-
sion, which may influence the analysis results. To erties of CFRP composites, including aspect ratio and
enhance measurement accuracy, such noise needs to size of voids, were also analyzed. The measurement of
be eliminated from the processed images before further void size can be achieved by calculation of the equiva-
analysis (Figure 2(c)). lent diameter of the voids (diameter of equivalent cir-
To fully characterize the content and other morpho- cular area), and the aspect ratio is defined as the ratio
logical features of voids, square specimens with of the long to the short axis of the equivalent ellipsoid.
2000 Journal of Composite Materials 52(15)
Figure 3. Geometric schematic of specimens: (a) longitudinal tensile specimen with aluminum tabs, (b) transverse tensile specimen
with aluminum tabs, (c) MD specimen with GFRP composite tabs.
Figure 5. Cross-sectional micrograph of unidirectional laminates: (a) sample prepared for void characterization, (b) cured at 0.5
MPa, (c) cured at 0.3 MPa, (d) cured at 0.1 MPa, and (e) cured at 0.01 MPa.
Figure 6(a) demonstrates the void contents of 15 have an average void number below 100, while samples
samples from the three groups of materials cured at with void content of 9.3% have approximately
various pressures. The obvious trend can be seen that 630 voids in the same size of analyzed area. The num-
the samples cured at higher compression pressure have bers of interlaminar voids, on the contrary, seem to be
lower void content; scatter in the void contents of dif- less sensitive to the void content, as shown in
ferent samples as well as different positions can also be Figure 6(c), even if a similar trend can be observed
observed as a result of the nonuniform distribution of for the relationship between void number and compres-
the intralaminar and interlaminar voids. The void sion pressure.
content of each group was determined by statistical Figure 7 shows the distributions of equivalent diam-
averaging of all the values obtained from each image; eters and aspect ratios of voids in composites at differ-
the void content of the four batches of unidirectional ent void levels. As can be seen in the figure, the
laminates can be determined as 0.8%, 2.2%, 4%, and distributions of both equivalent diameters and aspect
9.3%, respectively. ratios are close to normal distribution. As for the
The formation mechanisms of voids in composites equivalent diameter, the peak values of the equivalent
have been studied in much research,22,23 and the voids diameter distribution curves of samples from the four
can usually be divided into two categories: The first groups are all between 5 um and 10 um. However, the
comprises interlaminar voids existing in resin-rich scatter of data for samples with higher void content is
areas, which may derive from the entrapped air higher than that of samples with lower void content,
during autoclaving; this kind of void is usually bigger which demonstrates a little higher average void size.
in size and is detrimental to the ILSS of the material. According to Figure 7(e) to (h), samples with 0.8%,
The other kind of voids are intralaminar voids, which 2.2%, 4%, and 9.3% voids do not show marked differ-
may come from the volatiles embedded in the matrix ences in the aspect ratio of the voids; most of the voids
that derive from the chemical reaction during the man- have an aspect ratio between 1 and 3.
ufacturing process; the intralaminar voids are usually
small in size and distributed uniformly within fiber
tows. In this study, the numbers of both kinds of
Quasi-static tensile testing
voids in the analyzed area for each sample have also Longitudinal quasi-static tensile test for UD CFRP
been recorded, as detailed in Figure 6(b) and (c). The laminates. The results of the longitudinal quasi-static
number of intralaminar voids is found to be sensitive to tensile test are listed in Table 2, and the stress–strain
the void content; samples with void content of 0.8% curves are depicted in Figure 8. The tensile failure of
2002 Journal of Composite Materials 52(15)
Figure 6. Void content of specimens cured at various compression pressures: (a) void content of samples, (b) number of intrala-
minar voids, and (c) number of inter-laminar voids in the analyzed area.
the samples shows a brittle fracture, with slight reduc- failure (Figure 9(c)). Some defective fibers may break
tion in the tensile modulus occurring only at the final successively as the axial loading increases before final
stage of the test. In this stage, some small ‘‘teeth’’ can fracture; the breakage of defective fibers can initiate
be observed on the stress–strain curves; the reason for transverse micro-cracks in the epoxy matrix that will
this is the breakage of some defective fibers in random continue propagating as the loading increases to form
positions during the loading process. The fiber defects a macro-crack or a crack with fiber bridging until stop-
can be voids either at the surface or within the fibers, ping at the fiber/matrix interface or deflecting to the
inclusions as a result of incomplete carbonization, or longitudinal direction to form interfacial de-bonding.
cracks initiated during the cooling process in manufac- The propagating interfacial de-bonding can cause fur-
ture as a result of the different thermal expansion coef- ther fiber breakage and be able to connect the trans-
ficients in the longitudinal/transverse directions.24 By verse cracks at various positions; the final fracture of
comparing the stress–strain curves for samples at dif- the sample will occur once there exists a cross section
ferent void levels, it can be seen that the samples with where the stress is high enough to break the remaining
higher void content are more likely to experience an fibers. It should be noted that the transverse/longitu-
earlier initial filament breakage than those with lower dinal cracks may also initiate from the voids in the
void content. For the samples with 0.8% voids, fiber matrix, which can act as local concentrators; this will
breakage can be seen only at the very final stage of the lead to an earlier random fiber breakage and thus accel-
test. erate the failure process. Aside from broken fibers, in
Figure 9 shows the scanning electron microscope Figure 9(c), large quantities of fiber imprints as a result
(SEM) images for the fracture surface of the UD spe- of fiber/matrix interfacial de-bonding can be seen; in
cimen in the longitudinal tensile test. As expected, the addition, cusps between adjacent fibers, which is an
crucial failure mechanisms are fiber breakage indicator of shear failure of the matrix, can also be
(Figure 9(a), (b), and (d)) and fiber/matrix interfacial observed.
Liu et al. 2003
Figure 7. Geometrical parameter distribution of voids for laminates cured at various compression pressures.
2004 Journal of Composite Materials 52(15)
Figure 8. Longitudinal tensile stress–strain curves for UD laminates at different void levels.
Liu et al. 2005
Figure 9. Fractography of longitudinal quasi-static tensile failure using scanning electron microscope.
Figure 10 depicts the degradation of the longitudinal As can be expected, both the stiffness and strength seem
tensile modulus and strength of UD laminates with the to be affected by the presence of voids. Marked differ-
presence of voids. According to the figure, the tensile ences in transverse tensile modulus/strength can be
modulus of the samples is not affected by the presence found among laminates with void contents ranging
of voids; however, the ultimate tensile strength shows a from 0.8% to 9.3%; the effect of voids on the transverse
marked decrease as the void content increases from stiffness and tensile strength is non-negligible. Linear
0.8% to 9.3%, which shows that high void content is fitting was employed to describe the relationships
detrimental to the longitudinal tensile properties of UD between the transverse tensile modulus/strength and
laminates by reducing the ultimate tensile strength. the void content (see Figure 12(a) and (b)). Moreover,
Transverse quasi-static tensile test for UD CFRP since the transverse properties and failure mechanisms
laminates. Figure 11 presents the stress–strain curves of UD laminates are matrix-dominated, the residual
of the transverse tensile test for 12-ply UD laminates, stiffness of the material is closely related to the
and the experimental results are presented in Table 3. transverse crack density in the matrix. According to
2006 Journal of Composite Materials 52(15)
Figure 11. Transverse tensile stress–strain curves of UD laminates at different void levels.
Figure 11, the samples with 9.3% voids, in particular, as the void content increases from 0.6% to 8.9%), while
yield at a relatively lower axial stress compared with the influence of voids on the tensile modulus is limited.
those with void content of 0.8%, 2.2%, and 4%,
which demonstrates that the high void level promotes
crack nucleation, and thus the yield strength decrease in Mechanical models
the transverse direction can be observed. Stiffness prediction method for CFRP-laminated
Figure 13 shows an SEM photo of the fracture sur-
face of samples in the transverse tensile test. Different
composites with the presence of voids
from that of the longitudinal tensile test, the fracture As has been revealed by the preceding tests, neglect of
surface is relatively smooth. The final fracture of trans- the presence of voids may lead to the overestimation of
verse UD laminates comes from the propagation and the stiffness or strength of the material in some cases,
merging of cracks in the matrix or interfacial failure thus resulting in unexpected component failure in
perpendicular to the loading direction; the transverse real-world applications. In the interest of safety, quan-
cracks may initiate from voids or other defects such titative evaluation of the effect of voids on the static
as fiber waviness. As shown in Figure 13, exposed mechanical properties of CFRP laminates needs to be
fibers, fiber imprints, and scarps can be observed on done by a proven method, which is essential in real-
the fracture surface, which are typical indicators for world applications. In this study, the modulus of the
Mode I failure of transverse UD laminates. CFRP laminate was predicted by a stiffness prediction
Quasi-static tensile test for laminates with lay-ups approach based on the Mori-Tanaka method, void geo-
½0= 45=0=90s . The post-failure mode for laminates metric statistical data, and finite element (FE) analysis
with lay-ups ½0= 45=0=90s is shown in Figure 14. As for a fiber randomly distributed RVE model of an UD
expected, plies with different fiber orientations have dif- composite.
ferent failure modes. For 0 plies, fiber breakage and The equivalent stiffness of a pure matrix with differ-
interfacial de-bonding are the dominant failure modes, ent void levels was first evaluated by the modified
whereas for 45 and 90 plies, cracks propagate along Mori-Tanaka method with the use of the morpho-
fiber tows, and enormous amounts of delamination and logical parameters of the void. In this paper, the inter-
fiber/matrix interfacial de-bonding can be observed. actions between voids are ignored since the average size
Moreover, delamination can also be seen between adja- of the voids is much smaller than the average distance
cent plies. According to the test data shown in Table 4, between adjacent voids. If a single void is treated as an
the presence of voids greatly reduces the tensile strength inclusion with zero mechanical properties in the infinite
of the samples (decreasing from 523 MPa to 415 MPa matrix, the strain of the inclusion "i can be expressed as
Liu et al. 2007
Stiffness/GPa UTS/MPa
the following function of the remote strain "0 according average strain; the strain of the inclusion in the Mori-
to inclusion theory25 Tanaka method is defined in equation (2)25
1
"i ¼ ½I þ Pi ðCi Cm Þ1 "0 ð1Þ "i ¼ ½I þ Pi ðCi Cm Þ1 cm I þ ci ½I þ Pi ðCi Cm Þ1
ð2Þ
where I is unit tensor; Ci and Cm are the stiffness ten-
sors of the inclusion and matrix, respectively; tensor Pi where cm and ci are the volume fractions of the matrix
is related to the shape of the inclusion. and the inclusion, respectively.
Mori-Tanaka improved the traditional inclusion To take the size effect of voids into account, the
method by replacing the remote strain with matrix voids are divided into several groups judged by the
2008 Journal of Composite Materials 52(15)
Stiffness/GPa UTS/MPa
Table 5. Equivalent strain and critical strain for different failure modes.
Critical equivalent
Failure mode Equivalent strain "I Constants AI , BI strain ½"I
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
2 ffi 2
G X Xt
FT "FT ¼ h"21 i þ AFT 12 þ 13 2 AFT ¼ FT E121 S t E1
12
ð1 4 0Þ
Xc
FC "FC ¼ jh"1 ij —— E1
ð1 5 0Þ
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi 2
G12 Yt Yt
MT "MT ¼ h"22 i þ AMT 12 2 þB
MT 23
2 AMT ¼ MT E2 S 12 E2
2
G23 Yt
ð2 4 0Þ BMT ¼ E2 S 23
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi 2
G12 Yc Yc
MC "MC ¼ h"22 i þ AMC 12 2 þB
MC 23
2 AMC ¼ MC E2 S 12 E2
2
ð2 5 0Þ G Y
BMC ¼ E232 S c
23 Yt
IS qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
2 ffi 2 E2
G12 Yt
"IS ¼ h"22 i þ AIS 12 þ 13 2 AIS ¼ E2 S
12
ð2 4 0Þ
FT: fiber tension breakage; FC: fiber compression failure; MT: matrix tension failure; MC: matrix compression failure; IS: fiber/matrix interfacial shear
failure.
Table 6. Numerical prediction results of transverse modulus of UD laminates at different void levels.
(FC), matrix tension failure (MT), matrix compression matrix and the fibers, it is reasonable to assume that
failure (MC), and fiber/matrix interfacial shear failure the shear stress factors are functions of fiber content. In
(IS), are taken into account. The equivalent strain "I this paper, gradual damage FE analysis based on a typ-
and critical equivalent strain ½"I for each failure mode ical RVE model with uniformly distributed fibers at
(I2FT, FC, MT, MC, IS) have been defined (see different fiber content levels has been conducted to
Table 5). When "I exceeds ½"I , the damage begins to determine the shear stress factors. The characteristic
initiate. In Table 5, "1 and "2 indicate the strain com- distance between adjacent fibers was changed by setting
ponents caused by stress components 1 and 2 , different fiber volume fractions. Mises criteria were
respectively; X k , Y k (k 2 t, c), S 12 , and S 23 stand for used in the simulation to identify the failure of fibers/
the longitudinal strength, transverse yield strength, matrix; a simple abrupt degradation rule was applied to
and longitudinal/transverse shear strength, respectively, characterize the local damage, in which the correspond-
of the material considering the effect of voids. I (I2FT, ing modulus of the failed element was multiplied by a
MT, MC) are the shear stress factors. very small value (0.1) rather than 0 to avoid a singular
In previous research, the shear stress factors stiffness matrix. The stiffness and strengths of fiber and
I (I2FT, MT, MC) in modified Hashin criteria are usu- matrix used in this study are presented in Tables 6 and
ally empirically set as constants, which might not work 7. As for load condition, a pure incremental longitu-
very well in some cases. Since fiber content could influ- dinal or transverse shear stress was applied to the RVE
ence characteristic distances between adjacent fibers, model; the applied shear stresses at initial failure of
which may have an impact on the stress field in the certain failure modes were recorded to determine the
Liu et al. 2011
Table 7. Static strength of fiber/matrix.16,32 The stiffness degradation in this paper is character-
ized by defining a failure index tensor Mð fI Þ, the com-
Components Xt Xc
pliance matrix with damage Sf can be calculated from
Toray T300 3530 MPa 2070 MPa the initial compliance matrix S0 through equation (8).
Hexply 924 65 MPa 175 MPa The expression of Mð fI Þ can be seen in equation (9).
Sf ¼ Mð fI ÞS0 ð8Þ
2 1 3
1f1 0 0 0 0 0
6 1 7
6 1f2 0 0 0 0 7
6 7
6 1
0 0 0 7
6 1f3 7
Mðfi Þ ¼ 6
6
7 ð9Þ
6
1
1f23 0 0 7
7
6 7
6 syn 1
0 7
4 1f13 5
1
1f12
8 2 2
> 2
> g2,I l g12,I l
>
> k þ G12c þ gG23,I23cl ¼ 1
< G2c
ðI 2 MT, MC; k 2 t, cÞ ð12Þ
>
> 2 2
>
>
: gG2,I l þ l 2 g212,I þ g213,I ¼ 1 ðI 2 ISÞ
2c G 12c
Z ½"fI
1 1
gj,I ¼ j,I d"j,I ½ j,I ½"fj,I ¼ j,I ½ j,I ½"fI ð13Þ
0 2 2
element C3D8R and the adjacent plies were bonded The simulated stress–strain curves of samples at dif-
together by applying tie constraints to the nodes on ferent void levels as well as test results are shown in
interfaces. In gradual damage analysis, the preceding Figure 19. It can be found that the predicted stress–
CDM was implemented to define the intralaminar strain curves demonstrate a good agreement with the
material softening process. Incremental displacement test results, except that a little higher predicted ultimate
loadings were applied to the tabs at both ends to simu- tensile strength can be seen. This may be due to the
late the real loading conditions. transverse cracks initiated in the 90 /45 ply propagat-
ing into the adjacent 0 ply as the loading increases and
accelerating the failure process, which has not been
Table 8. Stiffness data of material components.16,32 taken into account in the present model. Figure 20
depicts the number of damaged elements of each failure
Components E1 E2 ,E3 G12 ,G13 G23 u12 ,u13 u23
mode in the FE model with incremental axial loading.
Toray T300 230 GPa 35 GPa 17 GPa 4.8 GPa 0.3 0.42 The dominant damage modes are matrix tensile
Hexply 924 3.8 GPa 1.34 GPa z0.41 damage and interfacial damage at the early stage, and
these two failure modes are the main driving force of
Figure 20. Number of degraded elements versus applied strain for laminates with lay-ups ½0= 45=0=90s with void content of 0.6%,
3.8%, and 8.9%.
the stiffness degradation; as the load increases, fiber ½0= 45=0=90s were conducted. The results suggest
breakage can be observed, which leads to the final frac- that both longitudinal and transverse tensile
ture of the samples. As for the influence of void con- strength of UD laminates show an obvious reduc-
tent, samples with an average of 8.9% voids show tion as the void content increases from 0.8% to
matrix/interface damage at a slightly lower loading 9.3%. In addition, the transverse tensile modulus
level compared with those with 0.6%/3.8% voids, shows a decline with the increasing void content,
which reveal the detrimental effect of voids on the ten- while the longitudinal tensile modulus is not
sile properties of CFRP laminates. affected by the voids. Finally, the tensile strength
of laminates with lay-ups ½0= 45=0=90s is also
influenced by the presence of voids; earlier delam-
Conclusion ination can be observed for the laminates with
higher void content as a result of the lower inter-
1. A void morphological study for T300/924 laminates laminar strength.
at different void levels fabricated by controlling com- 3. The effects of voids on the stiffness of CFRP
pression pressure in compression molding was con- composites were quantitatively evaluated through a
ducted with the implementation of a DM analysis prediction method based on the Mori-Tanaka
method. Three parameters, namely, void content, method and a fiber randomly distributed RVE
equivalent diameter, and aspect ratio of voids, model. Additionally, gradual damage analysis
were analyzed. The results indicate that low curing method based on the modified CDM for CFRP-
pressure can greatly enhance the resulting void con- laminated composites with the presence of voids
tent. As for the morphological parameters, the inter- was used to predict the quasi-static failure process
laminar voids have an average larger size than the of laminates with given stacking sequence and void
intralaminar voids; moreover, the average equivalent content. The present method is able to capture the
diameter of voids increases with increasing void con- effect of voids by the introduction of void content
tent, whereas the average aspect ratio of voids into the conventional model. By comparing the pre-
remains relatively stable as the void content dicted stress–strain curves and experimental results
increases from 0.8% to 9.3%. of samples with lay-ups ½0= 45=0=90s and void
2. Longitudinal/transverse quasi-static tensile tests for content of 0.6%, 3.8%, and 8.9%, a good correl-
T300/924 UD laminates as well as tensile tests for ation can be found between the simulation results
laminates with a stacking sequence of and the test data.
Liu et al. 2015