Characterisation of voids in bre reinforced composite materials

John Eric Little

a
, Xiaowen Yuan
a,n
, Mark Ian Jones
b
a
Department of Mechanical Engineering, The University of Auckland, Auckland, New Zealand
b
Department of Chemical and Materials Engineering, The University of Auckland, Auckland, New Zealand
a r t i c l e i n f o
Article history:
Received 27 July 2011
Received in revised form
29 November 2011
Accepted 30 November 2011
Available online 8 December 2011
Keywords:
Voids
Porosity
Micro-CT
Fibre reinforced composites
a b s t r a c t
Voids and porosity are critical imperfections in bre reinforced composite materials. The aim of this
study is to assess the comparative accuracy and reliability of conventional and novel void character-
isation techniques for analysing voids within carbon bre reinforced composite (CFRC) laminates.
While microscopy and Archimedes density measurements can only give results of limited accuracy and
reliability, micro-computed tomography (micro-CT) analysis was found to have no signicant inherent
errors and is able to characterise the three-dimensional size, shape and distribution of voids in CFRC
laminates. The accuracy of micro-CT was also veried by analysing articial voids of a known size and
shape disbursed throughout a CFRC laminate sample.
& 2011 Elsevier Ltd. All rights reserved.
1. Introduction
Advanced composite materials are becoming increasingly used
in the critical structures of both civilian and military aircraft, as
they often have a higher strength-to-weight ratio compared to
conventional materials, are corrosion resistant and are able to be
tailored to meet specic mechanical criteria [1]. Due to the non-
homogeneous nature of these materials, problems can arise
during their manufacture and handling which result in defects,
some of which can be hidden or uncharacterised [1]. Void
content/porosity, delamination, matrix cracks and impact damage
are just some of the common composite material defects. Identi-
cation and characterisation of these defects are important for
determining the quality of a composite structure, as these
parameters have a signicant effect on the mechanical properties
of the material and can act as failure initiation points [2].
Conventional composite void characterisation techniques provide
results of limited accuracy and/or reliability due to inherent
testing errors.
Conventional void characterisation techniques include:
Archimedes Theoretical versus Actual Density: this method
uses the Archimedes principle to calculate the samples actual
density, and then by using the theoretical density of the sample
with no voids present, the void volume fraction is able to be
calculated [3]. This technique however relies on accurate knowl-
edge of the bre and matrix density and weight fraction values of
the laminate. It is not uncommon for this method to calculate a
negative void fraction, which is theoretically impossible [4].
Matrix burn-off: the Matrix burn-off method utilises a furnace
to degrade and remove the laminates matrix from around the
bres, which allows for the bre weight fraction to be deter-
mined. Fibre degradation and convection currents affect the
accuracy of this technique, as bre mass can be degraded or
removed. This error is especially prevalent for CFRC laminates, as
the temperatures reached when achieving matrix burn are above
carbon bre oxidation [5]. Archimedes density testing is initially
required to measure the samples actual density [3], with accurate
knowledge of the constituent densities still required to calculate
the samples void volume fraction.
Matrix digestion: similar to matrix burn-off, but instead of
using thermal degradation, acid is used to digest and remove the
matrix from around the bres. Toxic fumes are produced during
the chemical break down of the matrix [6], making this process
dangerous.
Microscopy: this is a visual and, if used to characterise the
interior of the samples, a destructive analysis technique, which
allows the void size, shape and distribution to be analysed [7].
Microscopy is widely used in industry due to its visual character-
isation advantage, but also has an inherent section-bias error
associated with analysing two dimensional (2D) cross-sections of
the sample.
The conventional void analysis techniques mentioned are not
only limited in their accuracy and reliability, but also have
limitations with regards to what their data can conclude. The
non-visual techniques (theoretical density vs. actual density,
matrix burn-off and matrix digestion) can only measure total
void fraction, and cannot analyse individual void size, shape and
Contents lists available at SciVerse ScienceDirect
journal homepage: www.elsevier.com/locate/ndteint
NDT&E International
0963-8695/$ - see front matter & 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ndteint.2011.11.011
n
Corresponding author. Tel.: 64 9 923 9535; fax: 64 9 3737479.
E-mail address: xw.yuan@auckland.ac.nz (X.W. Yuan).
NDT&E International 46 (2012) 122127
distribution. It has been proven that two laminates that show the
same void content can have a varying mechanical response [8],
which highlights the important of visual analysis. Whilst micro-
scopy can detect this important visual information, it is however
limited by the information being 2D and non-representative of
the whole sample. Unless multiple images are obtained on very
thin slices, it also has potential for missing any pore intercon-
nectvity between adjacent slices.
X-ray computed tomography is a novel non-destructive and
visual technique that can be used for three dimensional (3D)
analysis of internal structures [1,9]. Computed tomography was
conceived in the early 1960s and has been predominately used for
medical diagnosis [1]. Over the past 20 years, however, micro-
computed tomography (micro-CT) has been developed and allows
for wider application, including the qualitative and quantitative
non-destructive evaluation of composite materials [1].
Micro-CT imaging works by recording the change in attenua-
tion along the path of an X-ray beam red through a sample [10].
A cross-sectional image is then mathematically reconstructed
from attenuation measurements made at different angles by the
detectors [10]. Each 2D slice is of a known thickness, which allows
the images to be virtually stacked to create a 3D model. The image
stack can then be converted to binary (black and white), allowing
for the voids to be separated from the bre and matrix which
make up the laminate.
This research paper compares the aforementioned conven-
tional techniques to micro-CT analysis for analysing voids in CFRC
materials. Matrix digestion and matrix burn-off were not tested,
as they have signicant errors and/or difculties when dealing
with carbon bre reinforced plastic laminates.
2. Experimental procedures
To compare the various composite characterisation techniques,
two 24-ply oven cured carbon bre reinforced composite (CFRC)
laminates were manufactured. One panel was made from unidirec-
tional (UD) preimpregnated (prepreg) carbon bre, while the other
was a twill weave carbon bre prepreg. The laminates were oven
cured under vacuum to ensure that voids were present within the
laminates for analysis. Samples measuring 15 by 7 by 5 mm were
cut from the middle of the panels for testing. The size of the
specimens was a compromise between the different techniques
requirements, with micro-CT requiring small samples to reduce data
le size. Carbon bre epoxy laminates were used for the samples as
characterisation interest primarily lies with this material.
The determination of the void volume fraction using the
Archimedes Theoretical versus Actual Density technique was
carried out in accordance with ASTM D3171. Due to size restric-
tions of the micro-CT technique, the samples were smaller than
the recommended testing standard sample volume of 1 cm
3
. This
variation is necessary and is assumed to have negligible impact
on the accuracy of the Archimedes results.
The testing procedure requires the density of the sample to be
measure using Archimedess Principle, where the specimen is
weighed in air (W
specimen
) and then weighed while submerged
(W
submerged
). It is critical that no air bubbles are present on the
coupon while submerged, as this will decrease the measured
mass and thus inaccurately increase the measured void volume
[11]. The coupon volume (V
coupon
) can be calculated in conjunc-
tion with the submerging liquid density (Eq. (1)), which in this
case is distilled water (r
water
). The actual density of the sample
specimen is then calculated using Eq. (2).
V
coupon

W
coupon
W
submerged
r
water
1
r
coupon

W
coupon
V
coupon
2
The void volume fraction (V
V
) is able to be calculated using
Eq. (3), with the mass fraction (%
m
) and density (r) of the primary
constituents required. It is critical that the material properties are
accurately known, as minor variations can signicantly affect the
accuracy of the calculated void volume fraction.
V
v
100r
coupon
%
mmatrix
r
matrix

%
mf ibre
r
f ibre
!
3
In order to gain this visual information a sample cross-section
is required, making this technique destructive. The testing pre-
paration required for microscopy analysis of composite materials
is a time consuming and sometimes difcult process due to the
non-homogenous composition of composites. Microscopy pre-
paration requires the sample to be set in resin and then a at
cross-section prepared to a mirror like nish, with no visible
preparation damage, such as scratches and void distortion. The
high quality surface nish is achieved by sequentially grinding
the surface with smaller sized particle paper, from 35 to 2.5 mm.
This process is difcult, as the brittle bres regularly break free
and gouge large scratches in the specimen surface. It is very
important that the nished surface has little or no scratches,
as these will be counted as a void when using image analysis
software.
The numerical analysis of microscopy images is carried out
using image analysis software, which works by analysing the
individual pixels that make up the image cross-section. The image
analysis process requires the microscopy cross-section image to
be converted to binary, with the voids remaining black and the
matter (bre and matrix) converted to white. The image is then
cleaned, to remove unwanted noise and outliers [12]. This
conversion and cleaning process is susceptible to error only if
care and common sense are not applied. The image is then able to
be analysed using built in analysis tools within the software,
which is able to calculate the total number of voids, their overall
area fraction, plus analyse individual void size, shape and two
dimensional location.
The micro-CT scanning and image reconstruction was conducted
at the Auckland Bioengineering Institute. The micro-CT scanning
reconstruction parameters were kept constant for all samples, while
the alignment parameter was tailored for increased accuracy. Micro-
CT scanning requires little specimen preparation, as this technique is
non-destructive with respect to the sample specimen. The scanning,
image reconstruction and the data acquisition processes can be time
consuming steps and vary with respect to the sample size and the
micro-CT scan settings, most notably the scanning resolution. A
constant scanning resolution of 7 mm was used for each sample and
represents the physical dimension of the voxels (3D pixel) making
up the image slices.
The micro-CT data acquisition process was completed using
software provided by Skyscan, the micro-CT scanners manufac-
turer. This software has the ability to be able to calculate overall
void fraction and the individual void size, shape and distribution
in three dimensions (3D), while also being able to produce 3D
rendered models of the voids.
3. Results and discussion
The following sections concentrate on the characterisation
techniques themselves, while using the sample laminates as an
example of the capabilities and comparative accuracy of each
technique. The overall void volume fraction calculated for each
technique is compared in a later section.
J.E. Little et al. / NDT&E International 46 (2012) 122127 123
3.1. Archimedes Theoretical versus Actual Density
The Archimedes Theoretical versus Actual Density testing
technique is a non-destructive and non-visual technique that
is able to calculate the overall void volume fraction within a
specimen, providing accurate material properties and mass frac-
tion values are known and the testing procedure is accurately
performed. Since this technique is non-visual, the only quantita-
tive data ascertained is the total void volume fraction of the
sample.
This Archimedes based characterisation technique requires
accurate knowledge of the materials physical properties, includ-
ing both constituents densities and mass fractions. The necessity
of having to know physical properties and make-up of the
laminate is a considerable weakness of the Archimedes based
testing procedures, and limits it to samples of known material
properties. Small variations in densities or the mass fractions can
lead to noticeable variations in the overall result, which can lead
to calculating the impossibility of a negative void fraction.
The material properties, bre and matrix density, of both
laminates were acquired from the carbon bre prepreg manufac-
turer. Due to cure variables the exact matrix density is unknown,
with a provided range between 1.15 and 1.18 g/cm
3
. Due to this
variation only a range of the samples void volume fraction could
be calculated (Eq. (3)), with the exact value remaining unknown.
The pre-cure weight fractions were acquired from the material
data sheets that are produced for each batch of prepreg material
by the manufacturer, with the nal values taking into considera-
tion the resin bleed during cure. The complications of having to
accurately know the material properties is an inherent error of
Archimedes based characterisation techniques (including matrix
digestion and burn-off), which limit their effectiveness and use to
known materials.
In some cases, however, the Archimedes Theoretical versus
Actual Density technique is more suitable than others, as visual
information is not always, at least initially, required. This techni-
que is suited for quality control purposes, as it is able to handle
relatively large samples and is less time consuming than other
techniques. An example application of this technique is the
inspection of autoclaved cure products for manufacturing defects,
such as bag rupture and corner bridging. These particular man-
ufacturing defects generally cause signicant increases in the
overall void volume fraction, so providing the material properties
and constituent volume fractions are within reasonable accuracy
these faults are able to be identied using this technique. If a fault
is found the cause of the increased void volume fraction is then
able to be investigated further, using more time consuming and
destructive visual techniques, or simply, the specimen can be
discarded.
3.2. Microscopy
There are various kinds of microscopes that can be used for
imaging material cross-sections, with optical and environmental
scanning electron microscopy (ESEM) the most common for void
analysis [13].
Fig. 1 shows the same area of a twill weave laminate cross-
section under both optical and ESEM microscopy. The optical image
(Fig. 1a) shows the bres as an illuminated white, the matrix as grey
and the voids black. While the ESEMimage (Fig. 1b) shows the bres
as a light grey, the matrix as a slightly darker grey and the voids
black. The most notable and critical difference between the two
microscopy images is the superior contrast between void and matter
(bre and matrix) of the ESEM image in comparison with the optical
image. When utilising image analysis software, it is important that
the contrast between void and matter is distinguishable so that an
accurate binary conversion can occur for image analysis purposes.
An example of this contrast difference can be seen around the large
circular void in Fig. 1, where the optical image shows a dark and less
well dened area to the right of the void. Optical microscopy,
however, has a greater contrast between bre and matrix, which
is benecial if the primary constituents are being examined. Another
benet of optical microscopy is the nancial investment required, as
optical microscopes are generally much cheaper to own, operate or
lease. In this study, an ESEM microscope was solely used for the
cross-sectional analysis, since it is the preeminent microscopy
technique for the imaging of voids in CFRC laminates.
An advantage of ESEM is the capability to easily and relatively
efciently image the entire specimen cross-section. Since an ESEM
detector is computerized, it is able to incrementally change location
during imaging, which allows the whole cross-sectional surface to
be systematically imaged. The sequential images are able to be
meshed together to create a complete image of the specimen cross-
section (Fig. 2). The cross-sections for this study, 15 by 5 mm,
required twenty one images (Fig. 2) at 100 magnication.
Fig. 3 is an example of the numerical analysis that is able to be
performed using image analysis software. This graph shows the
Fig. 1. (a) Optical image and (b) SEM image of the same area of a twill weave CFRC laminate cross-section.
Fig. 2. An example of ESEM microscopy cross-section.
J.E. Little et al. / NDT&E International 46 (2012) 122127 124
cumulative number of voids and their cumulative area fraction
plotted against void projected area diameter for the unidirec-
tional laminate cross-section shown (Fig. 2).
To limit the effects of section-bias three cross-sections were
analysed per sample, making a total of fteen cross-sections per
laminate. This large number makes the analysis process very time
consuming, with each surface requiring careful preparation to a
mirror like nish.
Microscopy analysis allows important individual void charac-
teristics to be assessed. Fig. 3 for example shows that E45% of
the total number of voids with a projected area diameter between
15 and 200 mm have a projected area diameter of less than 50 mm,
while only accounting for E6% of the total void area fraction. On
the other hand, this graph shows that voids with a projected area
diameter greater than or equal to 200 mm account for only 1.5% of
the total number of voids greater than 15 mm, but contribute to
E24% of the overall void area fraction. This example highlights
the benets of visual analysis, where the individual character-
istics of the voids are able to be evaluated against each other.
As can be seen in Fig. 2, the voids observed within a single
cross section of a laminate are not consistent, but have variable
shape and distribution due to the section cutting through pores at
different orientations. Due to this fact, microscopic characterisa-
tion of composite laminates has an inherent section bias, where
one cross-section is not necessarily an accurate representation of
the complete sample. In order to limit the effects of section bias, it
is important that multiple cross-sections are analysed, which is a
time consuming and costly process. It is also difcult when
obtaining multiple sections of the same sample to know exactly
where those sections are being taken from within the sample.
3.3. Micro-CT
The limitation of current micro-CT technology means that only
small samples are able to be scanned. Small increases in the
Fig. 3. The void number and voidarea cumulative distribution curves from the
ESEM cross-section in Fig. 2.
Fig. 4. Orthographic snapshots of a 3D unidirectional model from micro-CT analysis, with (a) top, (b) 3D model and (c) front and (d) side.
J.E. Little et al. / NDT&E International 46 (2012) 122127 125
sample size or scanning resolution signicantly increases the
required scanning time, data le size and the required data
acquisition computer power. The samples for this study required
a scanning time of 1 h at a scanning resolution of 7 mm, which
produced a le size of 10 gigabytes.
An advantage of micro-CT analysis is the ability to view 3D
rendered models of the internal structure of a sample. Fig. 4(acd)
shows an orthographic projection of the 3D unidirectional lami-
nate model (Fig. 4b). Three dimensional visual analysis of the
internal laminate structure provides the user with a basic under-
standing of what is present within the laminate. In these images,
it is possible to see large elongated voids, while the small rounder
voids are scatted throughout the volume. This non-analytical
understanding of the voids present within the sample can then
be used to help direct the analytical analysis.
Three dimensional analytical analysis of micro-CT scans can
also be carried out using the supplied software. This software
works in a similar manner to the image analysis software used
during microscopy, but takes into account the through slice
thickness of the pixels and the interconnectivity of the voids
between cross-sectional images.
A scanning resolution of 7 mm was deemed to suitable for the
analysis of voids in CFRC laminates. Although there is likely to be
a very large number of voids within the laminate that have a
projected area smaller than 7 mm, microscopy (Fig. 3), however,
has shown that their combined area fraction and inuence on the
quality of the laminate is negligible, whereby around 20% of the
voids had a projected area diameter below 20 mm but the area of
all of these pores contributed less than 0.5% to the total pore area.
Fig. 5 shows the average sphericity of individual voids with
respect to their projected area diameter for the unidirectional
laminate sample from analytical micro-CT analysis. This graph
shows a linear decrease in sphericity as the projected area
diameter increases, which indicates that a void becomes more
elongated as its volume increases. This analytical trend matches
the non-analytical visual observations made from the 3D ren-
dered images in Fig. 4, highlighting the effectiveness of non-
analytical visual analysis. Analytical micro-CT analysis is also able
to analyse the overall volumetric void fraction and the total
number of voids within a sample, while also calculating indivi-
dual voids 3D size and location. The individual 3D void analysis
capabilities of micro-CT which allows for individual voids to be
analysed in a similar manner to microscopy (Fig. 3), however
fundamentally micro-CT has no inherent section bias that affects
accuracy.
Determining the accuracy of the micro-CT analysis using
naturally occurring voids is difcult since their size and shape is
uncontrollable and independently unknown. In order to validate
the accuracy of the micro-CT analysis of voids in CFRC laminates a
verication laminate was manufactured with articial voids of a
known size and shape. The articial voids were manufactured
into a 12-ply CFRC twill weave laminate using hollow glass micro-
spheres manufactured by 3 M. These micro-spheres were classi-
ed using sieves into a size range 7580 mm. Under microscopic
analysis the spheres were observed to have an average outer
diameter of 68.583 mm (Fig. 6a), which includes a 6% sieve error
and takes into consideration an average shell thickness of 1 mm.
The micro-CT verication laminate was scanned and recon-
structed with the same settings used for the sample laminates.
Fig. 6b shows a 3D rendered model of a glass micro-sphere, which
is shown to be approximately spherical in shape. The volume and
surface area of fty micro-spheres were individually calculated
using micro-CT analysis software. This analysis calculated an
average projected area diameter for the fty micro-spheres to
be 70 and 75 mm with respect to the measured volume and
surface area, respectively , with both having a standard deviation
of E5 mm. These results are within the known inner glass-bubble
diameter range 68.583 mm, while the standard deviation is less
than the 7 mm voxel size. Micro-CT accuracy verication testing
has shown that analytical micro-CT analysis is accurate to within
one voxel, which infers accuracy is dependent on scanning
resolution.
3.4. Comparison of characterisation techniques
This section compares the accuracy and reliability of the void
characterisation techniques discussed and tested within this
study. It is not possible to comment on the accuracy of each
method, as the actual void content is unknown, but the compara-
tive variation is able to be assessed. The void volume fraction
results are obtained from testing ve samples per technique. Due
to section-bias errors, three cross-sections per sample were
analysed using microscopy, making a total of fteen measure-
ments for this technique.
Fig. 7 shows the average calculated void volume fraction and
standard deviation of the ve unidirectional laminate samples
tested using each of the analysed techniques. The average void
volume fraction between the three techniques is between 1% and
2%, which can be considered small when taking into account the
whole specimen volume and the inherent errors of each techni-
que. The small discrepancy between the void characterisation
techniques is signicant if dealing with high quality, high perfor-
mance products, such as in the aerospace industry. A notable
difference between the techniques is the larger standard devia-
tion of the Archimedes void fraction. This standard deviation
(0.74%) is nearly twice as large as that of microscopy (0.41%) and
over three times that of micro-CT (0.23%).
Fig. 5. Unidirectional laminate sphericity distribution with respect to projected
area diameter from micro-CT analysis.
Fig. 6. (a) Micro-spheres under optical microscopy and (b) 3D micro-CT render of
scanned microsphere.
J.E. Little et al. / NDT&E International 46 (2012) 122127 126
Fig. 8 shows the void volume fraction calculated by the three
characterisation techniques for the twill weave laminate samples.
The void fraction calculated by the Archimedes based technique
averaged 0.22%, with a standard deviation of 0.81. The Archi-
medes standard deviation for the twill weave samples was
signicantly higher than that of the visual techniques (0.07
0.08), which were similar to the values obtained for the unidirec-
tional laminate, and highlights the inaccuracy of the Archimedes
method when the material properties are not accurately known.
The negative portion of this result is not shown in Fig. 8 as this is a
physically impossible result.
There is a good comparison between microscopy (0.1270.07%)
and micro-CT (0.2670.08%) in Fig. 8, with the upper range of the
microscopy void fraction over lapping with the lower end of the
micro-CT results. The variation in the average void fraction between
the two visual techniques is also minimal, with a difference of 0.14%.
The individual void characterisation carried out by microscopy
and micro-CT showed comparatively similar trends. Both techni-
ques showed that the majority of voids account for a small
minority of the total void fraction, while as a voids volume
increases it becomes increasingly elongated. Although the trends
were similar, microscopy had a predominately higher standard
deviation, which can be attributed to the inherent section-bias
and highlights the variability and potential inaccuracy when
using microscopy. It is noted that Figs. 2 and 3 are examples of
the individual void analysis capabilities of both visual techniques,
with both able to assess void size, shape and distribution.
The characterisation techniques analysed have all shown
limitations and accuracy constraints. Microscopy for example is
a destructive technique and micro-CT currently requires a small
sample size, whilst Archimedes Density requires accurate knowl-
edge of the materials physical properties and constituent mass
fractions. Due to the inherent error with the Archimedes method
it has been proven to have a relatively large standard deviation,
whilst also lacking in ability to obtain characteristic data about
the individual voids. Although microscopy is able to measure this
critical information, its accuracy and reliability is limited due to
the errors of section-bias. The use of micro-CT has shown good
reliability, a low standard deviation and adequate void character-
isation tools. The current limitations of micro-CT analysis, most
notably the small sample size, are due to limitations of technol-
ogy and are not inherent within the technique.
4. Conclusion
This work researched and tested void characterisation techni-
ques for composite materials to assess their accuracy and relia-
bility. The study has proven that each technique has its own
strengths and weaknesses, with Archimedes and microscopy
having critical inherent limitations. Taking into consideration
the required preparation and testing processes, the characterisa-
tion information available, cost and the overall accuracy and
reliability, it is concluded that micro-CT analysis is the most
accurate and reliable technique for characterising voids in com-
posite materials.
Acknowledgement
This research was supported by the New Zealand Foundation
for Research Science and Technology (FRST) for Advanced Com-
posites Structures.
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J.E. Little et al. / NDT&E International 46 (2012) 122127 127