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Composite Laminates
INTRODUCTION
the cure reaction of the polymeric matrix, the use of a high-viscosity resin combined
with closely packed fibers that are not completely wetted by resin, the entrapment of air
in the material system, and fabrication mishaps such as a leaking vacuum bag or a poor
vacuum source [1–10].
Most aircraft composite parts are inspected after fabrication with nondestructive
techniques such as ultrasound either by pulse echo or through transmission. These
techniques are able to detect defects that cause ultrasonic attenuation such as voids,
delaminations, interlaminar cracks, inclusions, foreign object damage, resin-rich regions,
and others [3–5,9].
The behavior of a composite laminate with voids under different types of mechanical
loading has been widely studied. Most works consider the interlaminar shear strength
[3–5,9–15] but the interlaminar fracture toughness [12], bending strength under static and
fatigue loading [9], and compressive strength [3–5] have also been studied. However, there
is no general agreement over the magnitude of the effect of porosity on the mechanical
properties of composites. The difficulty lies in the large number of parameters involved
in the problem.
Different types of prepreg materials used in the manufacture of the laminates affect
the material toughness; the processing parameters (such as temperature and pressure) and
type of reinforcement affect the distribution, location, shape, and size of the voids in the
laminate.
All of these factors, in turn, produce different effects on the laminate strength. The type
of mechanical loading, its nature (static or fatigue), and inspection technique used are also
significant factors.
For example, the use of different frequencies in the ultrasound equipment results
in different values of attenuation. Therefore, only the results obtained from the
characterization of composites produced and tested in a similar way can directly be
compared. The experimental studies mentioned aim at correlating the void content to
the laminate strength for a specific type of loading. In those studies, it is implicitly
assumed that the void content is uniform at least over the critical section of the specimen.
However, in practice, voids are not uniformly distributed but are random in nature.
Note that void content is a measurement associated with a finite volume of material rather
than measurement to a point. The void content measurement by either matrix digestion
or ultrasonic inspection captures some sort of average value over a given volume,
without retaining the information on the shape, size, and distribution of the voids.
However, these features play an important role in determining the effect of voids on the
mechanical behavior of laminate and are primarily controlled by matrix material,
type of reinforcement, and manufacturing problem that originated the defects. The
important issue of the effect of the size of the area of the laminate affected by voids
is not addressed in this work. The voids are assumed to be uniformly distributed over
the laminate.
A fracture criterion that correlates fracture stress with void content or, alternatively,
to ultrasonic attenuation, is needed to establish an acceptance level for the inspection.
Establishing the acceptable level of defects is a critical issue in designing composite
structures. An overly conservative acceptance criterion causes many parts that could
perform satisfactorily to be unnecessarily discarded, increasing the manufacturing cost.
On the other hand, if the deleterious effects of defects are underestimated, in-service failure
of some parts may occur. Both situations are avoided by a judicious choice of acceptable
level of defects in the part. This should be based on reliable fracture criteria supported
Critical Void Content for Thermoset Composite Laminates 1777
EXPERIMENTAL PROCEDURE
The material under research was T700/TDE85 carbon fiber reinforced epoxy prepreg.
The initial fiber volume fraction Vf is 60 2%.
The viscosity was measured on an improved NDJ-7 rheometer. The viscosity was
measured at the manufacturer’s temperature cure cycle. The temperature was increased
up to 120 C at a rate of 2 C/min and was held for 2 h. Then it was increased to 160 C
at the same rate and was held for 4 h . Finally, it was cooled down to room temperature.
Polymer composites with high void content were manufactured using a procedure based
on the rheological analyses of the wet prepregs [3–5]. Laminates presenting intentionally
high porosity levels were produced, combining the technique proposed by Almeida
and Neto [9] and Olivier et al. [16]. This procedure involved the control of effective
pressure on liquid resin during cure with the simultaneous introduction of moisture
between layers during layup, as suggested by Gurdal et al. [17]. Moisture was introduced
by spraying water finely and uniformly to produce laminate plates with homogeneous
porosity. The effective pressure on the liquid resin and the amount of moisture dispersed
into the laminate were used to control the void content [5]. All specimens were cured in an
autoclave at 160 C with different pressures.
Two groups of cure pressure cycles were selected to assess the influence of voids on the
mechanical properties. One group kept the first isothermal time as 120 min and changed
1778 Z.-S. GUO ET AL.
the autoclave pressures as 0.0, 0.1, 0.2, 0.4, and 0.6 MPa. The other group selected the
temperature held at 120 C for 0, 30, 90, and 120 min. The autoclave pressure was set
as 0.2 MPa. The time for which the pressure was applied was chosen with respect to the
minimum viscosity and gelation points. The pressure inside the vacuum bag is 0.1 MPa and
remains so throughout the entire cycle for all experiments. A reference specimen
was produced to represent the behavior of low void content laminates. All laminates
with 12 plies, [0/90]3S, were manufactured as described above for each of the cure routes
considered respectively. The size of each plate was about 300 300 2 mm.
All plates were ultrasonically inspected to assess the resulting distribution of porosities.
Areas of uniform porosity within each plate were identified, and different levels of void
and fiber content specimens and at least 10 interlaminar shear and flexure specimens
were cut from each of those areas.
At
¼ ð1Þ
t
where is measured in decibels per millimeter and depends on the internal condition of
the laminate, particularly on void content, and where transmission loss At (measured
in decibels) is assumed to increase linearly with plate thickness t.
Three independent scans of each plate were performed to measure the absorption
coefficient of selected areas with approximately uniform porosity level.
After the C-scan inspection, specimens were cut and their densities were determined
in order to estimate void content. The density of each composite sample was determined
using the water displacement method by measuring its weight in air and in water. The void
content and volume fiber content of each specimen were measured by matrix digestion
according to ASTM D3171. The void content measurement was made with five specimens
on each plate and the average was taken as the normal void content associated with
each porosity level. Specimens with different porosity levels ranging from 0 to 3.5%
were obtained for these carbon/epoxy laminates. The fiber and resin density used for
computations were provided by the manufacturer.
Microstructural Analysis
Microscopic image analysis is reported as one of the best methods to measure void
contents [1]. In addition, this technique provides detailed information on other vital
parameters such as void location, shape, and size that cannot be assessed by other
methods. The void morphology in composite laminates is usually assessed by microscopic
image analysis. A ZEISS MC80DX Microscope equipped with a camera and an image
processing system was used for all analyses. Void features are obtained from images
acquired at 200 magnification using a PC-based CCD camera mounted on a MEIJI
optical microscope. The selected magnification of 200 enables the assessment of voids as
small as the radius of a single fiber of 7 mm. Consequently, all identifiable voids
throughout the entire composite samples were included in the analysis of void content
and morphology.
Mechanical Tests
Rheological tests provide important information used to determine the time during
which the pressure must be applied. The results of viscosity are plotted against time
and temperature in Figure 2. It shows that there exists one minimum viscosity plateau
(from Point A to B) in the viscosity versus time curve. At the end of the plateau, the
viscosity increases quickly with time or temperature owing to the initiation of cure
reaction. In those cure temperature cycles, a—b—c—d is the cure cycle recommended
by the prepreg’s manufacturer.
200
12 Viscosity
-------- Temperature
d
10 160
g
Temperature (°C)
f e c
Viscosity (Pa s)
8 b
120
6 a
80
4
40
2
A B
0
0 30 60 90 120 150 180 210
Time (min)
attenuation level, denoted as the echo amplitude. The area porosity corresponding to echo
amplitude is also shown. It was calculated from the results of ultrasonic attenuation and
void contents through experimental method. Hence, area porosity levels are affected
by frequency and echo amplitude of ultrasonic inspection, material type such as the fiber
and the matrix, and the thickness of composite laminates, and so on. This method
is a quantitative grading evaluation criterion that will be very useful in engineering
application.
Figure 4 correlates the void content determined by acid digestion (ASTM D3171) to the
measured absorption coefficients for all laminates studied. As expected, the smallest
Figure 3. C-scan showing areas with different void contents: (a) cure pressure is 0.0 MPa; (b) cure pressure
is 0.6 MPa; and (c) presentation of grey level and its porosity.
absorption coefficient corresponds to the low porosity laminates. This suggested that
greater void content causes increased attenuation and a linear correlation between the
porosity and the absorption coefficient can be observed for laminates with a porosity
range from 0 to 3.5%. Few measurements could be made of very high void content
laminates because of the difficulty in consistently obtaining laminates with a uniform
distribution of voids for high void contents. However, the results of this work demonstrate
that the range of void content obtained for all specimen types sufficed to determine the
maximum allowable void content.
Ultrasonic attenuation depends on a number of factors [3–5,9]: laminate
thickness, type of reinforcement, matrix material, fiber content, and the internal condition
of the material, which includes the void content. Moreover, the shape, size, and
distribution of voids in the laminate and parameters such as the ultrasound frequency,
size of the probe, and calibration procedure also affect the absorption coefficient
measurements. Therefore, it is difficult to compare ultrasonic attenuation results
obtained by other researchers without full knowledge of all the factors that affect the
measurements.
As illustrated in Figure 5, voids are seen at two different locations within the laminates.
The first location is defined as areas rich in matrix away from fibers. Voids encountered
in this location are completely surrounded by the epoxy matrix. The shapes of voids are
mostly circular (Figure 5(a)). The second location is defined as areas rich in interface,
where the area is primarily composed of reinforcing fibers. The shapes of voids are more
elliptical or of different irregular geometry (Figure 5(b)). A photomicrograph of the
sample of low porosity laminate is shown in Figure 5(a), which has a void content of 0.6%
with a curing pressure of 0.6 MPa. In this view, the voids occur mostly at the resin-rich
region. Figure 5(b) shows the occurrence of much larger, flattened, and elongated voids
distributed in the samples with a cure pressure of 0.0 MPa. As can be seen, the voids occur
Figure 5. Photomicrograph of voids with different cure pressures: (a) 0.6 MPa and (b) 0.0 MPa.
Critical Void Content for Thermoset Composite Laminates 1783
mostly at the ply interface. The differences in the morphology of the voids are determined
by the process parameters and physical properties of the resin.
3.0
2.5
1.5
1.0
0.5
0.0
0 30 60 90 120 150
Dwell time (min)
1.2% 0.9%
100
(Void content) 2.0%
2.2%
Strength fraction (%)
95
90
85
Shear strength
80 Flexural strength
Tensile strength
75
0 30 60 90 120
Dwell time (min)
time span from 50 to 90 min. An improved cure cycle is obtained as a—b—e—d (Figure 2).
The time was shortened to 30 min.
Fracture Criterion
A fracture criterion that correlates fracture stress with void content or, alternatively,
to ultrasonic attenuation, is needed to establish an acceptance level for the inspection.
Criteria to predict the laminate strength under certain loading conditions in the presence
of voids are scarce in the literature. Almeida and Neto [9] proposed a fracture criterion
that presented good correlation with experimental data on the bending strength of
composite laminates with voids. The same idea was successfully applied to predict the
interlaminar shear strength by Costa et al. [3–5], Jeong [7], and Almeida and Santacreu [8].
Critical Void Content for Thermoset Composite Laminates 1785
Almeida and Neto [9] also took advantage of the form of the equation to estimate the
critical void content defined as the void content below which the strength of the laminate is
not significantly affected by the presence of the voids. A similar approach was used by
Soriano and Almeida [19] to analyze the fracture strength data of composite laminates
with circular notches.
The considered fracture criterion for the strength of composite laminates containing
voids is given by
f ¼ HðÞm ð2Þ
where f is the fracture stress, H is the laminate toughness, is the ultrasonic absorption
coefficient in decibels per millimeter, and m is the slope parameter.
Equation (2) provides a good fit to experimental results for specimens with voids
[3–5,7–9,20]. However, it predicts infinite fracture stress for void-free laminates. To avoid
this inconsistency, the fracture criterion assumes that, for low void content, fracture
occurs according to classical fracture mechanisms with no influence of void content
(fiber microbuckling for compression and shear failure for ILSS tests). Therefore, for low
void content, fracture stress f is assumed to be given by
f ¼ f0 ð3Þ
1
f0
logðcr Þ ¼ log ð4Þ
m H
where cr is the critical value of the ultrasonic absorption coefficient. Note that the
definition of the critical ultrasonic absorption coefficient provides a systematic approach
to establish a maximum allowable value for void content. The approach is derived from
the mathematical form of the fracture criterion, which, in turn, is a consequence of the
basic assumptions described earlier. Therefore, the critical ultrasonic absorption
coefficient cr should be interpreted as a reference value for the minimum value of void
content that affects laminate strength rather than as a physical characteristic of the
laminate.
The proposed criterion in logarithmic form becomes
logðf0 Þ cr
logðf Þ ¼ ð5Þ
logðH Þ m logðÞ > cr
Therefore, this criterion implies that the logarithmic plot of fracture stress f,
as a function of ultrasonic absorption coefficient , should be approximately linear
for >cr and constant for cr. Logarithmic plots of experimental results are presented
to assess the validity of this hypothesis for all cases considered in the present work (Figures
9–11). A straight line obtained from a best-fit procedure is included in all plots. Note that,
1786 Z.-S. GUO ET AL.
44
σf = 47.3(α)−0.364
42
38
36
34
32
0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6
Absorption coefficient (dB/mm)
560 σ = 609(α)−0.365
540
Flexural strength (MPa)
520
500
480
460
440
420
0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6
Absorption coefficient (dB/mm)
to be consistent with Equation (5), the best-fit procedure must not include the reference
laminate that corresponds to the fracture stress of a laminate with low void content, f 0.
To verify the robustness of the fracture criterion, it was also applied to experimental
data obtained independently. Figure 12 shows the application of the proposed fracture
criterion to results obtained by Costa et al. [3–5] for the interlaminar shear strength of
carbon tape/epoxy laminates with voids. Figure 13 shows the application of the proposed
fracture criterion to the results obtained by Stone and Clarke [18] for the interlaminar
shear strength of carbon tape/epoxy laminates with voids.
Critical Void Content for Thermoset Composite Laminates 1787
1450
σ =1536(α)−0.310
1400
1300
1250
1200
1150
1100
0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6
Absorption coefficient (dB/mm)
Figure 12. Logarithmic plot of interlaminar shear strength as a function of ultrasonic absorption coefficient for
carbon tape/epoxy laminates by Costa et al. [3–5].
The results shown in Figures 9–13 demonstrate that a good agreement with
the experimental results was obtained from the application of the fracture criterion to
fit the fracture stress as a function of the absorption coefficient for all the
cases considered. Note that the experimental data include the effect of load type
(flexure and interlaminar shear) and experimental data from other researchers. Therefore,
the proposed fracture criterion yields good estimates of laminate fracture stress for a wide
1788 Z.-S. GUO ET AL.
Figure 13. Logarithmic plot of interlaminar shear strength as a function of ultrasonic absorption coefficient for
carbon tape/epoxy laminates by Stone and Clarke [18].
range of situations, provided that adequate values for fracture parameters are used in each
case. The fracture parameters are the laminate toughness H, slope parameter m, and
critical void content, either in terms of the absorption coefficient cr (decibels per
millimeter), or in terms of volume fraction Vcr (percent).
The values of the fracture parameters which are listed in Table 1 are obtained from the
linear regression procedure based on Equation (5). The value of m is about 0.365 either
under flexure or interlaminar shear loading, 0.310 under tensile loading for all specimens.
It seems that the slope parameter m depends on the loading type. The laminate toughness
H depends on the loading type as demonstrated by the results in Table 1.
An important fracture parameter is the critical void content, which establishes
an acceptance criterion for the nondestructive inspection of composite laminates.
When expressed in terms of the critical absorption coefficient, it depends on the type of
loading. For laminates under ILSS and tensile loading, the critical absorption coefficient
is 1.45 dB/mm; for flexure strength measurements, the critical absorption coefficient
is 1.38 dB/mm. These results indicate that the type of loading has a significant effect on
the critical absorption coefficient.
When the critical void content is expressed in terms of critical volume fraction Vcr, the
load type has little influence on the critical void content. Note, however, that from
Critical Void Content for Thermoset Composite Laminates 1789
the point of view of nondestructive inspection, the critical void content must be established
in terms of the parameters of ultrasonic inspection, that is, the critical absorption
coefficient cr.
CONCLUSIONS
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