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Investigation into the fatigue properties of flax fibre epoxy composites and
hybrid composites based on flax and glass fibres
Antigoni Barouni *, Colin Lupton , Chulin Jiang , Abu Saifullah , Khaled Giasin , Zhongyi Zhang ,
Hom N. Dhakal
Advanced Polymers and Composites (APC) Research Group, School of Mechanical and Design Engineering, University of Portsmouth, Anglesea Road, Anglesea Building,
Portsmouth, Hampshire PO1 3DJ, UK
A R T I C L E I N F O A B S T R A C T
Keywords: Natural fibre reinforced composites (NFRCs) offer a sustainable and environmentally friendly alternative to
Natural fibre reinforced composites composites made from synthetic reinforcements, with their response to dynamic loading phenomena being of
Fatigue behaviour utmost importance for structural applications. Herein, flax fibre reinforced epoxy composites and their glass fibre
X-ray computed tomography
reinforced hybrid counterparts were developed benefiting from synergic effects of hybridisation between flax and
Hybrid composites
glass fibres with the aim of achieving optimised fatigue behaviour. In order to study the fatigue behaviour, three
different types of composite laminates comprised of flax fibres only, and two hybrid flax-glass configurations
were fabricated, with alternating flax/glass reinforced layers. The hybrid effects on the fatigue behaviour of all
the composite laminates were investigated by using constant ratio R under a tension–tension fatigue loading. The
investigated fatigue behaviour showed promising performance in the hybrid laminates, with a great effect of the
hybrid configuration on the fatigue life. The hybrid laminate with alternating layers of flax and glass demon
strated the best performance under fatigue, showing a good damage accumulation indicator; about 7 times
greater, as compared to the other two laminates. The statistical analysis performed indicated that the afore
mentioned laminate has a less probability of failure, i.e. it will fail in a greater number of fatigue cycles, as
compared to the other two laminates. The influence of various parameters such as fabrication induced defects,
fibre matrix interface on the fatigue life has been further characterised using imaging techniques. The findings of
this study significantly contribute towards the exploitation of natural fibre reinforced composites and their
hybrids to understand the damage mechanisms that take place during fatigue loadings and how the fabrication-
related defects have an influence on the overall performance of those structures in load-bearing applications.
* Corresponding author.
E-mail address: antigoni.barouni@port.ac.uk (A. Barouni).
https://doi.org/10.1016/j.compstruct.2021.115046
Received 30 June 2021; Received in revised form 25 November 2021; Accepted 30 November 2021
Available online 4 December 2021
0263-8223/© 2021 Elsevier Ltd. All rights reserved.
A. Barouni et al. Composite Structures 281 (2022) 115046
Fig. 1. Fabricated composite panels, (a) Lam-F; (b) Lam-C; (c) Lam-D.
ultimate tensile strength [8]. mechanical properties of its constituents. Their results showed that flax
In recent years, to minimise some of the drawbacks of natural fibre fibre in a hybrid flax/basal composite played a significant role in
reinforcement in composites, a hybrid approach has been considered. In deflecting cracks and improving the fatigue resistance compared to
this approach, the synergic benefits of each constituent are utilised [9]. basalt laminates. Similar hybridisation strategies were the focus of many
Dhakal et al. [10] investigated the effects of carbon fibre hybridisation studies which aimed to study the performance of a certain NFC when
on flax composites. They reported a significant improvement towards combined with another NFC or with synthetic composites [21–23]. Das
moisture repellence behaviour of flax composites without hybridisation. et al. [24] reported that the amount and location of glass layers within
Cyclic fatigue behaviour of flax fibre reinforced composites comprised of hybrid glass/flax laminates have a significant influence on their me
six different textile architectures were reported by Bensadoun et al. [11]. chanical properties (Tensile strength, flexural strength, bending
Their work suggested that fibre architecture played a significant role in strength). Panciroli et al. [25] investigated flax- and glass-based lami
the fatigue life of flax fibre composites. It was highlighted that the nates having similar weight, flexural modulus and quasi-isotropic
stiffness and static strength combinations provided the optimal fatigue lamination. The aim was to perform a direct comparison of the perfor
endurance limit. Another study on date palm petiole wood [12] inves mance of the flax- and glass-based laminates when subjected to low-
tigated the morphology of their fibre form as well as their fatigue velocity impacts. Their results showed that the main failure mode in
behaviour, showing promising results on the fatigue life of these com glass-based laminates was delamination, while fibre breakage was found
posites. Further fatigue studies on composite laminates made from the to be the main damage mechanisms in flax-based laminates. Blanchard
bark of Lata’s Palm “Bactris Guineensis” have been conducted by Pertuz et al. [26] indicated that since both flax and E-glass fibres have similar
et al. [13], to identify their potential for the development of new engi properties, then the later can be used in structural applications. Never
neering materials. The study carried out by Barouni and Dhakal inves theless, their review also indicated that when the two are incorporated
tigated the effects of glass fibre hybridisation on flax fibre reinforced to form a hybrid laminate then the strength properties of flax are lower
composites [14]. They reported that the hybrid system offered an than E-glass. Finally, Zuo et al. [27] investigated the benefits of
improved impact damage behaviour of flax fibre reinforced vinyl ester hybridisation of natural fibre reinforced laminates as well as fibre metal
composite. The hybridisation technique offers promises to improve the laminates, emphasizing on the dynamic response of the structures. From
water repellence behaviour of NFRCs. In another study, hybrid glass-flax this work it is evident that the behaviour of hybrid natural fibre com
hybrid composites exhibited improved water repellence and impact posites is not well understood yet, due to various factors, such as the
toughness properties at room and high temperatures [15]. Jeannin et al. batch-to-batch variability or adhesion issues with certain matrices.
[16] studied the behaviour of a flax-epoxy composite under high-cycle In this work, a hybrid approach has been employed to investigate the
fatigue loadings. Their results showed that unidirectional flax-epoxy effect of glass fibre hybridisation on the fatigue performance of flax fibre
composites exhibited high fatigue resistance of up to 55% of the reinforced epoxy composite and its hybrids. Three different types of
quasi-static strength. Panzera et al. [17] performed thermogravimetric composite laminates were designed and fabricated to examine their fa
analysis on autoclaved flax composites and found that they have good tigue life. This study aims to establish key influencing factors to the
thermal stability up to 300 ◦ C. Ben Ameur et al. [18] found that flax fatigue life and damage mechanisms of flax fibre composites to use these
fibre-based composites had better damping properties than carbon fibre bio-based composites for semi-structural and structural applications.
composites under bending fatigue loading. Zahirul Islam et al. [19] Fatigue tests of the fabricated composites were performed, and thermo-
found that the fatigue life of flax fibre reinforced composites decreased mechanical properties were extracted and analysed. The morphology of
with increasing fatigue loading frequency. Seghini et al. [20] showed the fractured surface of all specimens was further studied using Scanning
that combining different NFCs (hybridisation) can improve certain me Electron Microscopy (SEM) technique. Finally, X-Ray mCT in-situ
chanical characteristics of the hybrid material in comparison with the testing was used to monitor the behaviour of the composite samples
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A. Barouni et al. Composite Structures 281 (2022) 115046
Fig. 2. Experimental testing configuration for (a) tensile tests according to ASTM D3039 using extensometer and strain gauges and, (b) DCB tests according to BS
ISO 15024.
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A. Barouni et al. Composite Structures 281 (2022) 115046
Table 2
Applied stress levels for fatigue testing.
Lam-F Δσmin = 32.5MPa Δσmax = 47.3MPa
(3)
α
Pf (x) = 1 − e
previously in section 2. The size and geometry of the specimens were
according to ASTM D3479 testing standard. The number of specimens Taking the natural logarithm of both sides of Eq. (3), the distribution
used for the fatigue testing of each laminate varies, with 21 specimens parameters, α and β, can be implemented as:
being tested for Lam-F, 13 specimens for Lam-C and 12 specimens for ( ( ))
1
Lam-D. This quantity provided a robust and well-fit group of results ln ln = βln(x) − βln(α) (4)
1 − Pf (x)
which was adequate to drive conclusions for their fatigue behaviour.
Two machines were used for this testing: an Instron 8000 series frame Eq. (4) is considered as a linear function (y = mx + b) which means
and actuator fitted with a 100 kN load cell coupled to an MTS control that the relationship between the double natural logarithm in the left-
system and an MTS 15 kN frame with a 15 kN load cell. Both units were hand side of the Eq. (4) and the ln(x) is linear. Hence y =
( ( ))
set with the same testing parameters which were maintained through
ln ln 1− P1f (x) , where m = β which is called the Weibull modulus and
the testing cycle. The testing was conducted with a targeted R ratio of
0.1, sine wave and a test frequency of 5 Hz in all cases. Prior to fatigue
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A. Barouni et al. Composite Structures 281 (2022) 115046
Fig. 4. 3D reconstructed images from µ-CT scanning of Lam-F specimen. (a) 3D volume; (b) detail with surface features; (c) porosity on part of the specimen.
Fig. 5. Failure of specimens near the gripping area at the end of the fatigue cycle for (a) Lam-F, (b) Lam-C and (c) Lam-D specimens.
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Fig. 6. Fractured area after fatigue loading at 47 MPa. Side view of (a) Lam-F failing at 18,278 cycles, (b) Lam-C failing at 79,678 cycles and (c) Lam-D specimen
series failing at 194,499 cycles; Top view of (a) Lam-F, (b) Lam-C and (c) Lam-D specimen series.
Fig. 7. μ-CT images for the Lam-F specimen; (a) whole 3D volume, (b) cut along the yz plane.
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Fig. 8. μ-CT images for the Lam-C specimen; (a) whole 3D volume, (b) side view of delamination, (c) cut along the yz plane.
3.2. Damage mechanisms during fatigue present on the top surface of the specimen, however, several pores can
be found in the internal of the specimen, as shown in Fig. 7(b), where a
During the fatigue loading, most of the specimens failed in the area clipping plane has been applied to the volume on the yz plane and at the
around the grips, as demonstrated in Fig. 5 for Lam-F, Lam-C and Lam-D distance of 9mm from the side. The damage mechanisms that occur for
specimens. As mentioned above, because of the nature of the failure, the the hybrid Lam-C and Lam-D specimens are very different to Lam-F, due
accurate measurement of the failure cross-sectional area (CSA) at the to the presence of the glass layers.
failure position was impossible. Hence, some further µCT scans were In Fig. 8(a) the different colours in the selected colourmap indicate
performed at selected failed specimens to investigate the damaged area. the different material density, hence the glass fibre and flax fibre rein
One specimen from each series which was loaded at ~ 47 MPa and all forced layers are easily distinguished. Due to the manufacturing process
failed near the lower grip area was scanned around the failure area. and the stitching of the biaxial glass fibres prepregs, the surface features
Fig. 6 shows pictures from the fractured area for Lam-F, Lam-C and created during manufacturing tend to open during the cyclic loading and
Lam-D series from two different viewpoints. The high stress concentra produce high stress concentration points. After the matrix cracking on
tion and local delamination along the stitching horizontal lines, as they the outer glass layers, the stitching horizontal lines appear to be the
appear for Lam-C and Lam-D specimens (Fig. 6(b) & (c)) indicates part of main crack propagation direction (Fig. 8(a)) with the biaxial fibres
the damage mechanisms that take place during fatigue. Also, various receiving all the load at the end and leading to the complete rupture of
elongation areas are present, which are obvious from the images as the specimen at the ± 45◦ direction for the glass layers. The middle flax
white lines, on the ± 45◦ directions. fibre layers demonstrate a similar behaviour to the Lam-F specimen,
For a better understanding of the damage mechanisms in each ma with several fibre breakages appearing. From the side view of the
terial, μ-CT scans were performed around the fractured areas and the 3D specimen (Fig. 8(b)), clear delamination between the glass and flax
reconstructed volumes for each specimen are shown in Figs. 7-9. layers is present, as well as cracks within the flax layers. Finally, in Fig. 8
Extensive fibre breakage appears to be present in the fractured area of (c) a clipping plane has segmented the volume along the yz plane at the
the flax fibre laminate (Lam-F) which led to the complete rupture of the mid-plane, where the penetration of the openings has passed almost
specimen (Fig. 7(a)). Some surface features (such as pores) are also through the whole thickness of the glass layer, indicating the critical role
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Fig. 9. μ-CT images for the Lam-D specimen; (a) whole 3D volume, (b) cut along the yz plane.
Fig. 10. Specimens set up for SEM imaging in the Zeiss lab.
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Fig. 11. SEM images for Lam-F specimens. Image of the right end of the specimen (a) at minimum load (Lam-F-1) and (b) at maximum load (Lam-F-2). (c) Detailed
view, as circled in (a). (d) Detailed view as circled in (b).
The morphology of the fractured area after fatigue was also studied adjacent flax layers of the Lam-C-2 samples from an SEM picture taken at
using scanning electron microscopy (SEM) on a Zeiss system. A selection the left end of the sample, as shown in Fig. 12(d). The glass and flax
of specimens from each laminate that failed at the lowest and highest layers have debonded with a gab measured at approx. 278 μm, whereas
fatigue load was made, as shown in Table 3. The samples were cut, the subsequent flax layer demonstrates fibre pull-outs, as shown in the
coated and loaded on the Zeiss system, as shown in Fig. 10. detailed images. An SEM image from the through-the-thickness area of
From the images of the fractured areas of the Lam-F-1 (Fig. 11(a)) the specimens is also shown in Fig. 12(e) and 12(f) for the Lam-C-1 and
and Lam-F-2 (Fig. 11(b)) specimens, a more intense event occurs when Lam-C-2 respectively. Two dominant delamination cracks are developed
the maximum load is applied at the Lam-F-2 specimen with more fibre around the fractured area, with several cracks propagating further down
pull-outs. The more loaded specimen Lam-F-2 shows deeper hollow the specimen’s length for Lam-C-1, as shown in the detailed image in
areas, where the flax layers have been completely cut off. The breakage Fig. 12(e) with the crack’s length being approx. 1.76 mm. This crack’s
of the bundle of fibres is evident at various points of the fractured areas, direction is propagating inside the less stiff flax fibre layers and the glass
as shown in Fig. 11(c) and 11(d). The fibre breakage appears to be the fibre layers are increasing the fatigue lifetime of the laminate, by pro
dominant cause of failure for this laminate. tecting it from the crack propagation. For Lam-C-2 in Fig. 12(f), the
The surface morphology becomes more distinct between the layers of delamination cracks between the hybrid glass and flax layers are
different materials for the Lam-C and Lam-D specimens. From the im dominant, as expected.
ages of the right end of the Lam-C-1 and Lam-C-2 samples (Fig. 12(a) and Finally, the SEM images from the Lam-D specimens have some
12(b)), it is evident that the fibre breakage is more dominant on the flax interesting findings on the failure mode of the glass and flax fibres as
layers as compared to the outer glass layers. The deformation of the flax well as their interphase. From the SEM images taken at the left end of the
fibres is greater whereas the glass fibres have broken in a more brittle samples Lam-D-1 and Lam-D-2 (Fig. 13(a) and (b) respectively), the total
way, as shown in Fig. 12(c) for Lam-C-1. This indicates that the material rapture of the flax fibres is very clear, whereas the glass fibre layers
has failed mainly due to the complete rapture of the flax fibre layers. It is demonstrate a more brittle and smooth failure. The same pattern is
also interesting to see the detailed view between the outer glass and observed in all four glass layers, with the glass fibres being broken in a
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A. Barouni et al. Composite Structures 281 (2022) 115046
Fig. 12. SEM images for Lam-C specimens. Image of the right end of the specimen (a) at minimum load (Lam-C-1) and (b) at maximum load (Lam-C-2). (c) Image of
the middle section of the fractured area of Lam-C-1 and detailed view. (d) Image of the left end of Lam-C-2 and detailed views. (e) Through-the thickness image of
Lam-C-1; (f) through the thickness image of Lam-C-2.
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A. Barouni et al. Composite Structures 281 (2022) 115046
Fig. 13. SEM images for Lam-D specimens. Image of the left end of the specimen (a) at minimum load (Lam-D-1) and (b) at maximum load (Lam-D-2). (c) Image of
the right end of the fractured area of Lam-D-2 with fibre pull-out. (d) Through-the thickness image of Lam-D-1; (e) through the thickness image of Lam-D-2.
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A. Barouni et al. Composite Structures 281 (2022) 115046
Table 4
The average fatigue life of Lam-F, Lam-C and Lam-D specimens.
0.7 UTS 0.6 UTS 0.5 UTS 0.45 UTS
Fig. 15. Weibull lines for Lam-F, Lam-C and Lam-D composite samples.
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Fig. 17. Displacement of specimens (a) Lam-F, (b) Lam-C and (c) Lam-D for fatigue loading from 0.5 to 0.7 UTS.
Fig. 18. Displacement evolution for Lam-C and Lam-D specimens at 0.6 and 0.7 Fig. 19. Damage accumulation for all specimens with respect to the applied
UTS loading conditions. fatigue stress.
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Fig. 20. (a) The internal scanning area of the Nikon CT system; (b) the 3 kN in-situ test rig for tension or compression; (c) geometry of the testing samples.
Fig. 21. In-situ porosity measurement for the Lam-F material at (a) preload stage, where no load is applied on the specimen, (b) 1 kN of tensile load and, (c) 2.5 kN of
tensile load applied on the flax fibre reinforced specimen.
interfacial properties at a wide range of temperatures and any possible molecular chains above the glass transition temperature (Tg). Lam-F
relations between them and measured fatigue properties of tested composite provided the lowest storage modulus while the highest
composites. Fig. 22 shows the changes in storage modulus (E’) and tan δ values were measured for the Lam-D composite. Lam-C and Lam-D
(damping factor) values of Lam-F, Lam-C and Lam-D composites as a composites exhibited a higher modulus compared to Lam-F composites
function of temperatures at 1 Hz oscillation frequency. The stiffness, and it becomes clear that the hybrid ply arrangements (glass and flax) in
degree of crosslinking and fibre–matrix interfacial bonding behaviours Lam-C and Lam-D composites can increase the storage modulus
of composites can be described based on the data provided in a storage compared to only flax fibre-based Lam-F composite. Although Lam-C
modulus (E’) versus temperature curve and the storage modulus is and Lam-D curves started from similar storage modulus values, Lam-D
proportional to the energy stored during a cycle in a DMA test [34]. composite showed a slower change and a better resistance of storage
From the storage modulus curves in Fig. 22(a) all types of tested com modulus reduction compared to Lam-C composite in the tested tem
posites showed a slow reduction of the E’ values at the beginning with perature range. This result could be associated with the improved
the increase of temperatures as polymer matrix chains become flexible interfacial adhesion and properties at the fibre–matrix interface devel
at higher temperatures with a subsequent sharp decline of the E’ values oped through the alternate glass and flax fibre ply arrangements in the
in the glass transition region due to the mobility of the polymer hybrid Lam-D composite which enabled the Lam-D composite to carry,
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4. Conclusions
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