Original article

Journal of Reinforced Plastics and

Composites
Flax fiber and its composites: An 2019, Vol. 38(7) 323–339
! The Author(s) 2018
overview of water and moisture Article reuse guidelines:
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absorption impact on their performance DOI: 10.1177/0731684418818893
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Abdul Moudood1, Anisur Rahman1, Andreas Ochsner 2
,
Mainul Islam3 and Gaston Francucci4

Abstract
Contemporary researchers have specified that natural flax fiber is comparable with synthetic fibers due to its unique
physical and mechanical characteristics which have been recognized for decades. Flax fiber-reinforced composites have
the potential for wide usage in sport and maritime industries, and as automotive accessories. In addition, this composite
is in the development stages for future applications in the aeronautical industry. However, designing the flax composite
parts is a challenging task due to the great variability in fiber properties. This is caused by many factors, including the
plant origin and growth conditions, plant age, location in the stem, fibers extraction method, and the fact that there is
often a non-uniform cross section of the fibers. Furthermore, the water and moisture absorption tendency of the flax
fibers and their composites and the consequent detrimental effects on their mechanical performance are also major
drawbacks. Fibers may soften and swell with absorbed water molecules, which could affect the performance of this bio-
composite. Flax fibers’ moisture absorption propensity may lead to a deterioration of the fiber–matrix interface,
weakening the interfacial strength and ultimately degrading the quality of the composite. This review represents a
brief summary of the main findings of research into flax fiber reinforced composites, focusing on the challenges of its
water and moisture absorption behavior on their performance.

Keywords
Flax fiber composites, moisture absorption, mechanical properties, interfacial strength, water diffusion

Introduction
eco-friendly and sustainable bio-based materials, with
Environmental awareness is a most important concern economic advantages, has resulted in increased
nowadays. Scientists all over the world are enthusiastic attention in developing novel natural fiber rein-
about the research of environment-friendly materials, forced composites.
owing to the increasing rate of greenhouse gas emis-
sions and other related health hazards. The various
products made from plastic and metal have a signifi-
cant impact on the environment. Specifically, for com- 1
Griffith School of Engineering, Gold Coast Campus, Griffith University,
posite materials, global awareness about the Queensland, Australia
2
environmental impact of synthetic fibers throughout Faculty of Mechanical Engineering, Esslingen University of Applied
their manufacturing, usage, and end-life has greatly Sciences, Esslingen, Germany
3
School of Mechanical & Electrical Engineering, University of Southern
increased in recent years. In this context, natural Queensland, Queensland, Australia
fibers and their composites are considered to be one 4
Research Institute of Material Science and Technology (INTEMA-
of the major alternatives and have occupied a substan- CONICET), National University of Mar del Plata, Mar del Plata, Argentina
tial place in the field of material research during the last
few decades. They are lightweight, inexpensive, and Corresponding author:
Gaston Francucci, Research Institute of Material Science and Technology
structurally efficient materials that can replace the com- (INTEMA-CONICET), National University of Mar del Plata, J.B. Justo
monly used conventional synthetic fiber composites in 4302, B7608FDQ, Mar del Plata, Argentina.
some engineering applications. Thus, the production of Email: gastonfrancucci@[Link]
324 Journal of Reinforced Plastics and Composites 38(7)

Plant fibers, a sub-section of natural fibers, are cost- with synthetic fibers, such as carbon or glass fibers, are
effective and offer good specific mechanical properties known as high-performance composites. Several stud-
when compared to glass fibers.1,2 Monteiro et al.3 men- ies11–13 reported about the recycling problems of the
tioned that economic, technical, societal, and environ- synthetic fiber composites and how environmental haz-
mental benefits are achieved by using plant fibers ards were caused by these fibers. On the other hand,
instead of synthetic fibers for reinforcement. researchers11,14–16 indicated that natural fibers, espe-
Summerscales et al.4 also reported that automobile cially plant fibers, are a possible replacement for syn-
accessories manufactured with plant fibers are light in thetic fibers. The extraction and production process of
weight. Due to this weight reduction, vehicles require the plant fibers are almost free of contaminants.
less energy to operate. These fibers are extracted from Furthermore, all residues coming from the leftovers
different parts of the plant such as from the outer part during fiber processing are non-toxic and non-
of the plant stem, i.e. the bast (e.g. jute, kenaf, hemp, hazardous. In a study, Joshi et al.17 stated that compo-
ramie, flax), leaf (e.g. sisal), fruit (e.g. coconut), and sites made with natural fibers are environmentally
seed (e.g. cotton). better than the synthetic fiber composites, in most
According to statistical data, the worldwide produc- cases, in terms of the performance indicators. The cul-
tion rate of bast fibers is higher than the other types, tivation of natural fibers is dependent on solar energy
and they are more popular among current fiber com- and the fiber extraction and production process require
posite researchers.5,6 Further, flax is one of the most only a small amount of fossil fuel energy. However, the
widely used natural fibers of the bast family for com- synthetic fiber production processes require a massive
posite reinforcement.7 However, the chemical compo- amount of fossil fuel, which causes an obvious environ-
sition and microstructure of vegetable fibers permits mental problem. In addition to the environmental
moisture absorption from the environment, which advantages of natural fibers over synthetic fibers,
causes weak bindings between the fiber and the poly- Wambua et al.18 concluded that the mechanical prop-
mer matrix. Like other vegetable fibers, the highly erties of the natural fiber composites are fairly compa-
hydrophilic nature of flax fibers and the moisture sen- rable to those of glass fiber composites. Furthermore,
sitivity of their composites are the main disadvan- few specific properties of the natural fiber composites
tages.8,9 Occasionally, due to the incompatibility have been reported to be superior to the glass fiber
between hydrophilic plant fibers and hydrophobic ther- composites. Nevertheless, natural plant fibers are also
moplastic and thermoset matrices, physical and chem- regarded as the best choice for commercial purposes.19
ical treatments on such fibers and/or matrices are
needed to increase the adhesion between them.2,7,10
In particular, the overall quality of the composites
Classification of natural fiber
depends on the properties of the fibers, the matrix, and According to the origin, natural fibers may be classified
their interface. Water and moisture absorption of plant as plant fibers, mineral fibers, and animal fibers. The
fibers have multiple effects, in terms of their properties, plant or vegetable fibers are often termed as cellulosic
morphology, chemical composition, and dimensional fibers. These fibers can be further sub-divided into non-
stability. The composites made with fibers taken from wood natural fibers and wood natural fibers. Non-
different relative humidity (RH) environments are wood natural fibers can be divided into bast, leaf,
expected to behave differently. On the other hand, seed, straw, and grass fibers. Among all the natural
when the composites are made with dry fibers, these fibers, plant fibers are the ones generally used in the
can also absorb moisture in various conditions of composite industry as reinforcement. A common natu-
humidity. Furthermore, if the composites are immersed ral fiber classification is shown in Figure 1.
under water, their properties are likely to be degraded
by absorbing water. Therefore, the effect of RH and
Flax natural fiber – an important bast fiber
water or moisture absorption on the properties of flax
fibers and their composites are the main points of inter- Flax fiber is considered the most important member of
est of this review paper. the bast family for composite reinforcement due to its
unique properties.7 The bast fibers are collected from
the fibrous bundles situated in the inner bark of a plant
Natural and synthetic fibers stem. The inherent high strength and stiffness of flax
Natural fibers are very popular reinforcements used for fiber and low elongation to failure are the important
manufacturing composites for a wide variety of engi- characteristics of this fiber that make it particularly
neering applications. These fibers are gradually occu- interesting in composite research. Flax (Linum usitatis-
pying the place of synthetic fibers in some applications simum) is typically grown in a moderate climate region.
due to a sustainability viewpoint. The composites made Charlet et al.20 reported that flax plants are cultivated
Moudood et al. 325

Figure 1. Classification of natural fiber.

widely in Western Europe where the daily temperature primary (outer) and a secondary cell wall. These are
is below 30
C generally. However, flax is also grown concentric cylinders with a small open channel in the
in Southern Europe, Argentina, India, China, and middle called a lumen. The primary cell wall can be up
Canada. Flax fibers are not continuous fibers as com- to 0.2 mm thick and the lumen can be as small as 1.5%
pared to the synthetic fibers, but they have a structure of the fiber cross section. The secondary cell wall con-
similar to that of composites and are hierarchically tains three sub-layers S1, S2, S3.26,27 The single flax
organized. Their macroscopic properties arise from fibers have been shown to possess different shapes
their micro and nano-structural level. Flax is an impor- within cross sections along the fiber axis, which some
tant industrial fiber that has been used since ancient researchers approximated to hexagonal or pentagonal
time. More than 30,000 years ago, prehistoric hunters cross sections.28 However, the fibers vary in their non-
were using twisted wild flax fibers for making cords uniform geometrical shapes along the axis. Owing to
for hafting stone tools, weaving baskets, or these irregularities in the thickness of the cell walls, the
sewing garments.21 fibers vary greatly in strength.27
The main constituents of flax fibers are cellulose,
Structure and composition of flax fiber hemicellulose, lignin, and pectin. A small percentage
of wax, oil, and structural water are also found.9,29
A flax stem has the constituents of bark, phloem, Both primary and secondary cell walls are composed
xylem, and a void at the center. The fibers are located of cellulosic materials. Cellulose fibrils (diameter
as fiber bundles in the outer surface of the plant stem as between 0.1 lm and 0.3 lm) are surrounded by con-
shown in Figure 2. The flax plants can grow to heights centric lamella, composed of about 2% pectin and 15%
of 80 to 150 cm in less than 110 days since the plants hemicellulose, which contribute to the thermal degra-
are fast-growing by nature. The bundles (technical dation and water uptake behavior of the fibers.30 The
fibers) are between 60 and 140 cm long and their diam- secondary cell wall is the major part of the fiber diam-
eter ranges from 40 to 80 lm. A flax stem contains eter and S2 layer is its dominating constituent. This
20–50 bundles in its cross section. Each bundle consists layer consists of highly crystalline cellulose microfibrils
of 10–40 spindle-shaped single (elementary) fibers bounded by lignin and hemicellulose. The microfibrils
1–12 cm long and 15–30 lm in diameter.23 Charlet in the S2 layer follow a spiral pattern at an angle of 5–
et al.24 reported that the elementary fiber diameters 10
along the fiber axis, which explains the stiffness and
are different if taken from the bottom, the middle, strength of the fiber in the axial direction. The middle
and the top part of the flax stems. The mean fiber diam- lamella is considered to be the matrix which bonds the
eter was found to decrease from the bottom to the top cell together.27 Bos et al.27 described the technical
of the stems. fibers, which are extracted by partially separating the
The elementary fiber (Figure 3) denotes a single cell fiber bundles in the flax plant and can be as long as the
in the flax plant. Each elementary fiber is composed of stem length (approximately 1 m). The technical fibers
concentric cell walls that are different from each other (i.e. the bundles of elementary fibers) consist of 10–40
in terms of thickness and the arrangement of their con- elementary fibers in the cross section. The elementary
stituents. Each cell wall consists of what is known as a fibers overlap for a considerable length and are glued
326 Journal of Reinforced Plastics and Composites 38(7)

Figure 2. Structure of the flax fiber: (a) cross section of flax plant stem and position of the bundles of elementary fibers and technical
fibers after extraction, (b) SEM image of a technical fiber with its constituting elementary fibers.
Source: reproduced with permission from Bensadoun et al.22

together by an interphase known as a middle lamella, properties (tensile strength and modulus of elasticity,
consisting mainly of pectin and hemicellulose, which is among others) is a consequence of many factors,
a mixture of lower molecular weight branched polysac- including plant origin and growth conditions, plant
charides. Table 1 illustrates the composition and age, location in the stem, and a non-uniform cross sec-
mechanical properties of flax and other bast fibers. tion of all the fibers. Due to this inherent variability, a
Weibull distribution function was used to describe the
tensile strength of the flax fibers.34–37
Factors affecting the properties of
Charlet et al.24 found that mechanical properties of
flax fibers flax fibers were influenced by the location in the stem.
Flax is investigated at the elementary and technical Flax fibers located at the bottom of the stem display the
fiber level. The great variability reported for flax fiber poorest mechanical properties, while the fibers located
Moudood et al. 327

in the middle are the ones that show the best mechan- constituents, which happens especially in the
ical performance. The biochemical analysis confirmed secondary cell wall region. As a result, less-efficient
that both cellulose and non-cellulosic polymers are to stress transfer was found in the tensile tests, producing
be found prolifically in most extensive contents of the reduced strength as compared to elementary fibers.
middle fibers. Cellulose is considered as the equivalent These results are quite consistent with that of
reinforcing material of a composite structure, whereas Bensadoun et al.22
non-cellulosic materials are the matrix constituent that Fiber extraction methods also influence the mechan-
supports the exchange of load from one microfibril to ical properties of the flax fibers. Bos et al.27 revealed
another. Bos et al.27 reported that the technical fiber that the tensile strength of the fibers is dependent on
strength decreases when the clamping length increases the isolation procedure, with manually isolated fibers
because of the similar composite-like structure of this being stronger than mechanically isolated ones. The
fiber. They performed tensile tests to determine the mechanical processes of fiber extraction were found
strength of elementary and technical flax fibers and to induce kink bands in the fibers, thus reducing their
found that elementary flax fibers showed a consider- tensile strength. However, they noted that the scatter in
ably higher strength than technical fibers of the same strength is much larger for the elementary fibers isolat-
length due to a bundling effect. During testing of the ed by hand than for the standard mechanically isolated
technical fiber bundle, it was found that all elementary ones. They claimed that the mechanical fiber processing
fibers are not firmly bonded with the matrix methods generate a number of large defects, which
reduces the scatter in the fiber strength, although the
fibers show a lower mean strength. In a different
study38 of elementary flax fiber tensile tests, it was
found that fibers separated by enzyme treatment may
receive less damage than those by mechanical process-
es. Zeng et al.39 introduced a new method of fiber
extraction from 35% aqueous ammonia pre-treated
flax stems, comparing this with a standard extraction
process. They found both tensile and flexural properties
of flax fibers were increased due to the ammonia treat-
ment. The average tensile strength of ammonia-treated
fibers was almost 50% higher than the one obtained
with the commercial extraction processes. In addition,
higher flexural toughness was also evident for the
ammonia-treated fibers.
The tensile strength of the elementary flax fibers was
tested by Baley,40 who found that fiber kink bands and
micro-compression defects were the main cause of
strength reduction. These two defects act as points of
fracture initiation during fiber failure. Both the tensile
Figure 3. An elementary fiber structure. strength and Young’s modulus decreased when the
Source: reproduced with permission from Stamboulis et al.25 fiber diameter was increased, with associated fiber

Table 1. Bast fibers: compositions, physical and mechanical properties.1,31–33

(%)

Young’s Tensile
Density modulus strength Elongation
Bast fibers Cellulose Hemicellulose Lignin Pectin Wax (gm/cc) (GPa) (MPa) at break (%)

Flax 60–81 14–20.6 2–3 1.8–5 1.7 1.5 27.6 345–1500 2.7–3.2
Hemp 70–92 17.9–22.4 3–5.7 0.9 0.8 1.4–1.5 17–70 368–800 1.6–4
Jute 51–84 12–20.4 5–13 0.2 0.5 1.3–1.4 10–30 393–773 1.2–1.5
Kenaf 31–57 13.6–21 5.9–19 2 – 1.2 14–53 240–930 1.6
Ramie 68.6–76.2 13–16.7 0.6–1 1.9–2 – 1.5–1.56 27–128 400–1000 1.2–3.8
Banana 60–65 6–19 5–10 3–5 – 1.3–1.35 27–32 529–914 1–3
328 Journal of Reinforced Plastics and Composites 38(7)

Figure 5. Equilibrium moisture absorption of flax sliver at

different RH.
Source: reproduced with permission from Zhang et al.43

Figure 4. Effect of fiber diameter on fiber strength.

Source: reproduced with permission from Baley.40 been considered the sum of two components: flow
into the capillaries (pore absorption) and penetration
into the fibers (fiber absorption). The fiber absorption
defects. The effect of fiber diameters on fiber strength is accounts for an increase in fiber thickness during
shown in Figure 4. However, there was no clear rela- penetration.
tion between the tensile strength and the number and Zhang et al.43 studied the moisture absorption
shapes of the kink bands. In a different study, Baley mechanism of flax fibers exposed to different humid
et al.41 analyzed the effect of a drying stage on the environments. They found a linear relationship
tensile strength of the elementary flax fibers and between the equilibrium moisture content and the sur-
found it to decrease after drying. rounding RH until it reaches 70% RH and, after that
Among the different factors affecting the fiber prop- value, moisture absorption was found to increase
erties, moisture absorption and its effects on the fiber sharply (Figure 5). More than 10% of the air’s mois-
properties have been investigated by many authors and ture content can be absorbed by flax fibers within 1 h at
the main findings are presented in the following 90% RH. These results are quite consistent with that of
sub-sections. a recent study,44 where researchers found equilibrium
moisture absorption is almost double (14.3%) at 95%
Moisture absorption of flax fibers RH than that at 70% RH. Interestingly, all the fibers
reached the equilibrium moisture content at ambient
Most of the bast fibers have almost similar structures temperature within 60 min regardless of the RH value
and constituents. Moisture susceptibility is treated as (Figure 6).
one of the main problems in the usage of these fibers. A detailed investigation of such environmental
As cellulose and hemicellulose are the dominant con- effects on duralin (treated) and green (raw) flax fibers
stituents of the plant fibers, so hydrogen bonds exist was carried out by Stamboulis et al.25,45 They found
between the molecules of the fiber cell wall. Cellulose 3%, 15%, and 24% moisture contents in the flax fibers
and hemicellulose consist of a large hydroxyl (OH)-to- when exposed to 20%, 66%, and 93% RH environ-
carbon (C) ratio. Cellulose also consists of a highly ments, respectively, and the absorption curves followed
crystalline region and it may not be possible for typical Fickian behavior. However, when the fibers
water molecules to enter. However, water molecules were exposed to 100% RH, the absorption mechanism
diffuse into the amorphous regions of the cellulose changed, and did not behave according to Fick’s law.
and hemicellulose and break inter-molecular hydrogen Basically, they observed an absorption curve that
bonds. This allows an increase in the inter-molecular increased in a stepped manner, reaching different equi-
distance of the cellulose chains, which causes fiber librium levels (showing a maximum of 42% moisture
swelling. Either a nanolayer can be formed in between content). They attributed this behavior to swelling
the fibers where a close association was seen with the stresses that develop during moisture absorption and
OH groups or a multilayer can be generated where all relax after a certain time once the first equilibrium is
the water molecules might not intimately relate with the reached, changing the equilibrium moisture condition.
OH groups.42 It is known that the water-holding capac- In a different study,46 the absorption-desorption equi-
ity correlates strongly with the volume and structure of librium for flax fibers at 21
C and 40% RH was
the pores in the fiber wall. The uptake of water has reached in 40 min and in 40–45 min for hemp fibers
Moudood et al. 329

Figure 6. Moisture absorption kinetics of flax fibers at different RH.

Source: reproduced with permission from Moudood et al.44

with the same conditions. Similar findings were found tensile tests on ‘as received’ raw fibers, dried fibers, and
in a previous study,47 where flax fibers reached the dried fibers in contact with ambient air where moisture
moisture equilibrium after 28.5, 34, and 37 min was absorbed. The experimental analysis confirmed
during a drying stage at 80
C, 60
C, and 40
C, that in each case, fibers were damaged, which reduced
respectively. their mechanical properties. Surprisingly, moisture-
absorbed raw flax fibers presented higher tensile
Effect of moisture absorption on properties strength than the fibers subjected to drying stages.
of flax fibers They concluded that the cohesion between the matrix
and the microfibrils is lost after drying, potentially
Moisture absorption and its effects on flax fibers have leading to a decrease in tensile strength. Mustata and
been investigated in detail due to their excellent Mustata46 studied the moisture equilibrium in yarns of
mechanical properties and extensive use in the compos- flax and hemp fibers finding a higher tensile strength in
ite manufacturing process. Nilsson48 reported that the the wet yarns than the dry ones for both fibers. Joffe
moisture content in natural fibers has a great influence et al.38 revealed that strain at failure increased with
on their stiffness. Davies and Bruce34 found that the moisture penetration at the fiber cell wall and is the
tensile modulus of flax fibers is strongly dependent on outcome of the plasticizing effect of absorbed water
the environmental RH, both static and dynamic moduli on a flax fiber. Netravali and Chabba49 also found
of flax fibers decreasing remarkably with an increase in that fiber strength can be significantly decreased with
RH. Specifically, they considered four different RH continuous moisture absorption and desorption cycles.
(between 30% and 70%) during their experiments Stamboulis et al.25 observed the changes in the struc-
and found that the static modulus showed a decreasing ture of the fibers as they were exposed to high humidity
trend with increasing RH at a rate of 0.39 GPa/%RH levels. The surface of dry fibers was smooth, and the
for a single flax fiber. Fiber strain was independent of fibrils were well connected by the organic matrix form-
static modulus, but dynamic modulus displayed an ing a bundle, while the 100% RH-conditioned fibers
increasing rate with an increasing strain at a rate of were swollen, and their surface was rougher than that
13% GPa/% strain. This phenomenon was confirmed of the dry ones. In addition, the individual fibrils were
by Baley.28 In another study, Baley et al.41 also inves- more separated and some damage in the form of kink
tigated the effects of absorbed water on the tensile bands were observed. These observations strongly sug-
properties of elementary flax fibers. They carried out gest that properties of composites manufactured with
330 Journal of Reinforced Plastics and Composites 38(7)

natural fiber fabrics having different moisture contents properties and is easy to cure and use. No volatile
could vary significantly. agents are formed during the curing process, which is
a major advantage as compared to phenolic, polyester,
and vinyl ester resins.
Flax fiber reinforced composites
Elementary flax fibers are processed into the form of Manufacturing aspects of the flax fiber
mats, rovings, fabrics, and yarns to use in the reinforced composite
manufacturing of composites. After selecting a suitable
manufacturing technique, these are combined into sev- A number of factors require consideration before proc-
eral layers with the matrix material of some form of a essing the flax fiber composite: fiber type, fiber content,
resin to manufacture composites. The hydrophilic fiber orientation, and the moisture content of the fibers.
behavior of these fibers and hydrophobic matrix mate- Engineers would mainly focus on criteria that include
rial often affect the adhesion between them. To address the desired properties, size, and shape of the resultant
this issue, chemical and physical treatment of the fibers composites, the processing characteristics of raw mate-
is used, e.g. acetylation, alkali treatment, bleaching, rials (both fibers and polymers: bio-based or
peroxide treatment, isocyanate treatment, vinyl graft- petroleum-based). In addition, the production speed
ing, coupling agents, etc. The details of the different and the manufacturing cost required also affect the
treatment processes are out of the scope of this selection of a proper process to fabricate natural fiber
review and can be found in various studies.50–53 composites. Furthermore, based on the processing
techniques, semi-finished product manufacturing, mat
Suitable matrix selection for flax composites production, slivers, fiber yarns, fiber preparation
(opening, mixing, and carding), and granule produc-
Fibers are held together by the matrix in a fiber rein- tion are the important steps to be taken into account
forced composite which is an essential and key consum- for the production of natural flax fiber composites.56,57
able for the manufacturing of composites. Temperature The fiber length, aspect ratio (length/diameter of
is an important factor in resin selection for the flax fiber fibers), and the chemical composition of the fibers
composites. Summerscales et al.54 reported that tem- can also influence their processing.
perature limits the matrix selection as natural fiber Several methods are available for manufacturing
degrades at a higher temperature. In most cases, vege- natural fiber reinforced composites. According to the
table fibers start to degrade at 200
C or above over resin used for these composites, it is suitable to divide
time. Therefore, matrix selection for the composite the bio-composites into thermoplastic and thermoset
materials is restricted to thermosetting polymers of matrix-based composites. Usually, traditional
thermoplastics with a low melting temperature. manufacturing techniques can be used to manufacture
Although composites manufactured with thermo- natural fiber thermoplastic composites: compounding,
plastic matrices are less expensive and recyclable, they mixing, extrusion, injection molding, and compression
possess limited mechanical properties and a higher molding (CM). On the other hand, natural fiber rein-
tooling cost is required. In addition, the directional forced thermoset composites are usually manufactured
properties of flax fibers cannot be used completely by liquid composite molding (LCM) processes. Resin
when randomly oriented short fibers are used with ther- transfer molding (RTM), vacuum infusion (VI), injec-
moplastics.55 Thermosetting matrices offer many tion compression molding (ICM), sheet molding, pul-
advantages like being easy to process (low viscosity), trusion, reaction injection molding, and bulk molding
requiring less processing temperature, and being less compound are some examples of LCM. Francucci and
expensive. Furthermore, as the impregnation of the Rodriguez58 presented a comprehensive review on the
fibers is easier, the manufacturing process requires a manufacturing of vegetable fiber composites by LCM
lower pressure and facilitates a higher loading techniques. Some LCM methods are illustrated in
of fibers.33 Table 2.
Undoubtedly, epoxy is the most widely used resin Oksman et al.59 studied the influence of fiber micro-
in the flax fiber composite manufacturing processes. structure on the mechanical properties of extruded
A variety of benefits can be found in the epoxy-based composite materials. They used jute and enzyme-
resins during the manufacturing process. Epoxy pos- treated flax fibers to reinforce polypropylene (PP).
sesses excellent mechanical and chemical properties. It The composite materials were manufactured via a
also has a high-hardness with good heat- and water- long fiber thermoplastic (LFT) processing method
resistant properties. The shrinkage associated with whereby rovings were continuously fed into an extrud-
epoxy resins is extremely low as compared to vinyl er. A twin-screw extruder was utilized to compound
esters and polyesters. It also contains excellent adhesive the samples and PP plastic. A temperature profile of
Moudood et al. 331

Table 2. Liquid composite molding processes.58

Volume of Part
Methods Type of mold used production complexity Part size

Resin transfer molding (RTM) Rigid mold (steel or aluminium) High High Small-medium
Light resin transfer molding Rigid mold (glass fibre reinforced composites) Low-Medium Medium Small-medium
(LRTM)
Vacuum infusion (VI) Rigid lower mold-flexible sheet (vacuum bag, Low Medium Medium-large
plastic sheet, silicone or rubber membrane)
Injection compression Rigid mold (steel or aluminium) Medium-high Medium Small-medium
molding (ICM)

180–200
C between the feeding zone and the die was obtained mechanical properties of the materials
maintained to ensure complete and homogenous showed that the composite with 50% arctic flax has
mixing. As expected, the authors observed an increased significantly more stiffness (40 GPa) compared to
flexural stiffness when the fiber loading was increased. that of pure epoxy (3.2 GPa). A similar pattern was
It was noted that the use of 2% maleated PP signifi- observed in the tensile strength of composites com-
cantly improved the composite properties because of pared to the neat epoxy. This study verifies that
the better compatibility in the mixing process. RTM is a suitable processing method for natural
In a different study, Oksman et al.60 studied flax fiber composites based on epoxy resins.
fiber reinforced polylactic acid (PLA) composites man-
ufactured by CM. They found the PLA-based compos-
ite has 50% better strength than the conventional flax/ Effect of RH, moisture, and water on flax
PP composites. In contrast, a microscopy study of the fiber composites
microstructure confirmed the poor adhesion between the
Since flax fibers are highly hydrophilic, the RH has a
fibers and the PLA matrix. The researchers found no
vital role on the fiber reinforced composites. Generally,
difficulty in processing flax/PLA composites with a tra-
moisture absorption of the flax fibers increases with
ditional manufacturing process and this composite can
increasing RH. Immersion of the composites under
be processed in a similar way as flax/PP composites.
water boosts water absorption and the water molecules
Pultrusion and RTM are two of the most common
processes used to make thermosetting composite mate- diffuse within the composite materials and affect them
rials. Pultrusion can be assumed as a continuous pro- by swelling.
cess for producing long profiles made of composite
materials. Reinforcing fibers are saturated with the Moisture present in the fibers prior to manufacturing
liquid resin, and then pulled through a heated die to the composites
form a composite with a specific shape and dimension.
In general, moisture in fibers is considered to be detri-
Angelov et al.61 were one of the first to pultrude flax
mental to composite performance. The flax fiber fabrics
fibers into a fixed shape. They varied the preheating
are usually dried before the manufacturing stage, which
and die temperatures while pulling the flax fibers and
PP yarns. After passing through the preheating zone would likely be beneficial for the quality of the
(approximately 600 mm at temperatures of 155– obtained composites.61 However, Baley et al.63
166
C), the profile was pulled through the die. The proved that drying the fibers (for 14 h at 105
C) results
temperature of the hot die was tested at 200
C and in a significant loss of strength (44% on average) and
210
C. After the hot die, the polymer passed into the failure strain (39%). They also performed tensile tests
cold die that was maintained at room temperature. on unidirectional (UD) flax/epoxy composites, where
The pulling speed was varied from 8 to 38 cm/min. reinforcement was dried and ‘as-received’ flax fibers.
The authors concluded that similar mechanical perfor- It was found that drying did not affect the axial stiff-
mance can be obtained in the pultrusion process as ness but caused a large drop (36%) in composite
compared to the composites manufactured by CM. strength, in a similar way to the drop found in fiber
In addition, RTM is also a processing technique strength. Furthermore, they postulated that the remov-
suitable for manufacturing high-quality natural fiber al of moisture would also influence the properties of the
reinforced composites. In a related study,62 arctic flax fiber surfaces and, hence, the interfacial bonding.
fibers and epoxy resin were used as reinforcement and Therefore, they suggested that a more detailed study
matrix, respectively. A comparison between the was necessary to optimize the conditioning of plant
332 Journal of Reinforced Plastics and Composites 38(7)

fiber fabrics in order to obtain the highest quali- 90% RH. Therefore, this study concluded that RH
ty composites. should be less than 70% to manufacture a composite
Recently, Fuentes et al.64 studied the influence of with consistently better quality.
moisture present in the environment during the
manufacturing of flax fiber-unsaturated polyester Water and moisture absorption mechanisms
(UP) composites on their performance. They compared
Newman65 studied the water-absorption process of
the performance of the composites which were manu-
flax-epoxy composites after being immersed under
factured under dry and 100% RH conditions. Results
water. Fiber swelling occurs and the matrix material
were an 18% and 25% reduction in tensile strength and
around the fibers is stressed due to water absorption.
modulus in dry conditions and 11% and 8% reduction
Next, the matrix molecules’ relaxation processes release
in flexural strength and modulus when the composites
were manufactured at 100% RH. This fact was related a few of these stresses. Drying of natural fiber compos-
to the decrease of the fibers’ mechanical properties due ite materials that have absorbed water results in fiber
to the softening and possible dissolution of the inter- shrinkage, causing the matrix material to lose contact
face between the elementary fibers. with the fibers. As a result, a gap is generated between
Moudood et al.44 reported the effects of moisture the fibers and the matrix, having a detrimental effect on
present in the fibers prior to manufacturing flax fiber the interfacial properties. The author explained this
reinforced epoxy (FFRE) composites by a vacuum phenomenon as an auto accelerative process where
infusion process. Composite panels manufactured the drying cycle enhances the water damage which
with flax fibers taken from 70% RH and 95% RH increases the rate of fiber shrinkage. In contrast, the
environments showed severe warpage. They suggested shrinking process of the matrix material is relatively
that as the fibrous preform was in a swollen state when slow and, therefore, stress is released by the generated
compacted by the vacuum bag and some of the mois- microcracks within the fibers and at the fiber–matrix
ture was gradually extracted during the infusion pro- interfaces. This water-absorption mechanism with
cess (drawn away by the vacuum and dissolved in the debonding is shown schematically in Figure 7.
resin), fiber shrinkage was caused. Thus, residual com- The water and moisture absorption behavior of flax
pressive stresses developed during the curing process, fiber reinforced composites depend on the surrounding
which ultimately led to part warpage after demolding. temperature, the humidity present in the environment,
The fiber–matrix interface became weaker due to high and also on the nature of the composite. The water
moisture content in the fibers and porosity was molecules spread in the composite by a diffusion mech-
increased in the microstructure of the composites. anism inside the matrix. Sometimes micro-pores and
Although the fiber–matrix interface was affected, the cracks that are generated within the matrix or even
optimum tensile strength was found at composites the capillarity transport along the fiber–matrix inter-
made with 50% RH conditioned fabrics and, below face can enhance the diffusion rate. The diffusion
and above that value, the tensile strength of the com- behavior of the polymeric composites can be divided
posites was decreased. This was explained by water as Fickian, non-Fickian, and intermediate. Assarar
molecules increasing the tensile strength of the fibers et al.67 studied the water uptake behavior of FFRE
but at the same time negatively affecting the fiber– composites, reporting that it is Fickian at room tem-
matrix interface and overall microstructural condition. perature. The water-absorption behavior of flax-epoxy
The researchers also indicated that the plasticizing composites is shown in Figure 8, which is linear initially
effect of water molecules on flax fibers significantly (Fickian diffusion) but slows down as the moisture
increased the strain at break and decreased Young’s content approaches its saturation level. The saturated
modulus. On the other hand, the flexural strength water-absorption at equilibrium is almost 13.5% for
and modulus decreased continuously with increasing each unit thickness of the composite.
RH. Furthermore, composites made with fibers condi- Cheour et al.68 studied the flax-epoxy composites
tioned at 95% RH showed a sharp drop in mechanical with different fiber orientations to measure the effects
properties (Young’s modulus, flexural strength, of moisture absorption on composite performance.
and modulus). They used water immersion test of composites for
The effect of RH in the fabrication of flax/UP com- three different fiber orientations (0
, 45
, and 90
)
posites on interfacial shear strength (IFSS) and flexural and found that fiber orientation has a significant
properties was investigated by Zhang et al.43 The IFSS impact on the moisture uptake of flax composites.
of the composites started to drop sharply at 70% RH The UD FFRE composites with fibers at 45
absorbed
and ended up with a more than six-fold reduction at the highest amount of water among the different
Moudood et al. 333

Figure 7. Debonding process in fiber/matrix interface with water.

Source: reproduced with permission from Azwa et al.66

Figure 8. Water absorption pattern of flax-epoxy composites.

Source: reproduced with permission from Assarar et al.67

orientations. The FFRE 45
and FFRE 90
absorbed

25.1% and 5.2% more water, respectively, than the Figure 9. Moisture absorption of flax composites with different
FFRE 0
laminate (Figure 9). They explained this fiber orientation.
fact by stating that water diffusion occurred Source: reproduced with permission from Cheour et al.68
334 Journal of Reinforced Plastics and Composites 38(7)

Figure 10. Water diffusion of flax composites in different fiber orientation (a ¼ 0
, b ¼ 90
, c ¼ 45
).
Source: reproduced with permission from Cheour et al.68

preferentially both in the fiber direction and thickness

directions of the composites. The water diffusion in
fiber orientation for FFRE 0
is negligible as compared
to the diffusion in thickness direction due to the fiber
length in the composites. However, the fibers are
shorter in width for FFRE 45
and FFRE 90
samples,
which makes water diffusion easier in the fiber direc-
tion for these composites. This diffusion of water into
flax composites with different fiber orientation is illus-
trated in Figure 10.
Recently, Chilali et al.69 compared the water uptake
behavior of flax fiber reinforced thermoplastic and
thermosetting composites. The water-absorption
behavior was found to be the same as reported for
different conditions of the flax composites.
The amount of absorbed water increases linearly at
the beginning, but the absorption slows down as the
saturation level is reached. In addition, flax composites
with a thermosetting resin (epoxy) absorb more water
Figure 11. Water absorption of flax/epoxy and flax/acrylic
than the composites with the thermoplastic resin (acryl- composites.
ic) (Figure 11). Dhakal et al.70 compared the water- Source: reproduced with permission from Chilali et al.69).
absorption behavior of two natural fiber composites:
flax and jute. In order to measure the influence of mois- Different diffusion coefficients for flax fiber rein-
ture they conducted water immersion tests for 40 days forced composites are found in different literature as
at room temperature and found that saturated mois- shown in Table 3.
ture contents were 9.61% and 14.41% for flax and jute
composites, respectively. Berges et al.71 studied the
Moisture and water absorption of composites - effect
moisture uptake behavior of UD FFRE laminates,
finding their diffusion kinetics follow a one- on the performance
dimensional Fickian behavior when exposed to hygro- The moisture content at a given RH has a substantial
thermal conditioning at 70
C and 85% RH. These effect on flax fiber reinforced composites. Generally,
results were also supported by Scida et al.,72 who con- plant fiber reinforced composites have a tendency to
firmed that flax fiber composites follow a Fickian dif- significantly decrease their tensile and flexural proper-
fusion mode at similar conditions. The tensile ties and interfacial strength in wet conditions.2,77
mechanical behavior is clearly affected by the hygro- The effect of water absorption on the mechanical
thermal aging which was confirmed by the shape of the properties of the flax fiber/bio-epoxy composites has
stress–strain curves. At 90% RH and 20
C, Young’s been evaluated by Munoz and Garcia.75 This study
modulus decreased by 33% for the first 3 days and a was done by immersing the samples into water at
55% reduction was found after 38 days. room temperature. The authors found that fiber
Moudood et al. 335

Table 3. Diffusion coefficients of flax fiber composites according to literature.

Diffusion coefficient, Manufacturing methods and

Fiber conditions and humidity Matrix used D (cm2/s) other conditions Reference
3
UD and twill fibers at 55
C and UP 0.00104  10  0.02 Hand lay-up, 8.89% water uptake 73

75% RH for UD flax composites and

0.00287  103  0.08 10.24% uptake for twill
flax composites
Green flax PP 1.3  102 Moisture uptake reduced by 30% 45

Treated flax PP 7.8  103 in treated flax composites

Treated flax MAPP 5.0  103 (duration 14 days)
Flax at 23
C, 80% RH 0.002  103 Extrusion 74

Flax at 25
C, maximum immer- Bio epoxy 37.1 Hand lay-up, Equilibrium mois- 70

sion 40 days ture content, 9.61%

Flax at three orientations Epoxy 6.67  109 for 0
Press platen process, maximum 68

(0
, 45
, 90
), immersion at 12.45  109 for 45
moisture uptake 13.70% by
room temperature 14.19  109 for 90
45
fiber orientation
0
/90
flax at 40 and 55 wt%, Bio-epoxy 1.63  108 for 40% RTM, Saturation water absorp- 75

immersion at room tempera- 2.32  108 for 55% tion 8.71% and 6.23% by 55%
ture, 32 days immersion test and 40% fiber volume,
respectively
Twill flax, immersion at room Acrylic 7.7  109  0.03 Vacuum infusion, moisture at 69

temperature Epoxy 8.1  109  0.04 equilibrium, 6.6% for flax-

acrylic and 7.31% for flax-
epoxy composites
Flax fiber bundles, immersion PP 2.23  109 Compounding, saturated mois- 76

test at room temperature MAPP 0.92  109 ture content, 9.09% for flax-PP
(212 days), 40% fiber volume and 8.53% for flax-
MAPP composites
UD: unidirectional; UP: unsaturated polyester; PP: polypropylene; MAPP: Maleic Anhydride-grafted PP.

content influences the moisture absorption behavior of Different matrix materials were used in both studies
the composites, which have a tendency to absorb more which might be a reason of this discrepancy.
water as the fiber content was increased. They further In many cases, the interfacial strength between the
found that water-absorbed composites have a higher fiber–matrix bonding becomes weaker with increasing
tensile strength and strain than the dry composite sam- moisture content. However, Le Duigou et al.79 studied
ples. The water-absorbed fiber swelling filled the gaps the fiber–matrix interface with water-treated flax/PLA
between the fiber–matrix interfaces and the tensile and untreated flax/PLA composites. They found both
strength was increased up to 35%. The tensile strain IFSS and frictional stress were increased by 13% and
also increased due to the plasticization effects of the 30%, respectively, for water-treated flax fiber rein-
wet composite samples. In contrast, the flexural forced Poly-L-lactic Acid (PLLA) composites. In gen-
strength decreased by 20% when compared to the dry eral, the fiber roughness properties, chemistry, and the
composites. The researchers concluded that, a higher surface energy mainly influence the interfacial strength
percentage of water absorption might cause more between the fiber and the matrix material.79,80
micro-cracking due to the swelling of the flax fibers However, in a different study Fuentes et al.64
which generated a poor fiber–matrix interface during reported that the flax fiber surface is susceptible to
bending loading. However, they observed that the flex- water absorption due to its amorphous polymer con-
ural and tensile moduli of the composites decreased stituents, but the surface energy and IFSS of the flax
with increasing water absorption since these properties fiber were both found to be relatively constant at dif-
depend on fiber properties not on fiber–matrix inter- ferent RH. Nevertheless, they found a reduction in
face. The findings of this study are opposite to those of strength of the flax composites at different RH as the
Le Duigou et al.78 who found that flax/PLA compo- fibers turn soft, thus a dissolution of the interface might
sites degrade both in terms of tensile strength and stiff- occur between the elementary fibers. Scida et al.72
ness when the composite absorbs water molecules. pointed out that the matrix material was mainly
336 Journal of Reinforced Plastics and Composites 38(7)

damaged when the flax fiber composites are aged with Summary and concluding remarks
90% RH across different time durations. This damage
The growing trend of flax fiber usage in the composite
affects the fiber–matrix interfacial bonding and fiber
industry has proved it to be a potential candidate to
breakage occurs.
draw more interest among researchers. Due to its wide
Le Duigou et al.8 tested the interfacial strength of a
range of applicability in various industries, it is impor-
single flax fiber/epoxy micro-composite by immersing
tant to understand what factors affect the properties of
samples in water for different time durations and found
flax fiber reinforced composites. Flax fibers have an
a 60% reduction of shear strength from their initial
intrinsic variability in their physical and mechanical
value after 135 h. In an earlier study78 of wet (sea
water) aging of flax/PLLA composites, they also properties, which must be considered when designing
found the fiber–matrix interfacial strength was dam- structural parts. Moisture and water absorption are
aged due to swelling of the fibers at the interface. The two key factors responsible for the deterioration of
absorbed water can form hydrogen bonding with the the composite. Some key points of the effects of mois-
fibers, which eventually reduce the interfacial bonding. ture and water content on the properties of the flax
Assarar et al.67 also reported the weak fiber–matrix fibers and their composites can be summarized
interface of water-absorbed flax/epoxy composites as follows:
when tested with acoustic emission.
1. Moisture present in flax fiber fabrics before
manufacturing the composites affects the final
Present and future scope of flax microstructure and properties of the obtained mate-
fiber composites rial. The microstructure of the composite materials
Several unique properties and strength of natural fibers is negatively affected by moisture in the fabrics,
have prompted researchers to become interested in leading to pores and fiber debonding from the
these composites. The renewable resources of plant matrix. Flexural strength continuously decreases as
fibers are experiencing an increasing uptake in different the moisture in the fabrics is increased, but the ten-
industrial usage. For example, Saheb and Jog81 sile strength is shown to have an optimum value due
reported that natural fibers can be used in composites to two opposite effects: the positive effect of water
which have various applications from normal applian- molecules on the tensile properties of the fibers and
ces to space-craft. Specifically, the flax fiber industrial the deterioration of the overall composite micro-
supply is increasingly being used for manufacturing structure (pores, poor interface, etc.). When the
composite materials. moisture content in the fibers is higher, both
Suddell and Evans82 reported that flax fiber compo- Young’s modulus and the flexural modulus decrease,
sites are widely used in the automotive and other trans- while the strain at break increases because of plasti-
port industries. For instance, several automotive cization effects.
components previously manufactured with glass fibers 2. Due to the preferential water transport paths along-
are being replaced by these fibers and flax fibers can side the fiber direction, fiber orientation with respect
also be used in car disk brakes to replace asbestos. to the thickness direction of samples has a significant
George et al.83 stated that the advantage of these effect on the water-absorption behavior of the com-
fibers over synthetic ones in automotive interior com- posites. Composites having the fibers oriented per-
ponents is that the natural fiber composite automotive pendicular to the thickness direction show the least
parts can be ruptured instead of splintering during fail- water uptake, while using fibers oriented at 45

ure of the structures if an accident occurs. In addition, causes the most water absorption.
these fibers lead to lighter parts and a consequent 3. In some cases, superior mechanical properties were
reduction in fuel consumption, which has economic observed in composites having moisture-absorbed
and environmental advantages. flax fibers than dried fibers. Swelling of flax fibers
Flax fiber reinforced composites are widely used in in the composites can improve their tensile strength
sports industries (bicycle frames, stand-up paddle as this could fill the gap in the interface, increasing
boards, most kind of boards, etc.) and the maritime friction and thus the interfacial strength. However,
industry (small to medium sized boats). In addition, the flexural strength was found to decrease as the
flax prepregs with heavy areal weight (300 to 550 gm/ moisture content of the fibers increases.
m2) are in developmental phases for future application 4. Both the fibers and the composites follow a one-
in the aeronautical industry.82 Flax fiber composites dimensional Fickian diffusion behavior during the
are also used with concrete structures for building con- absorption of water molecules at high humidity
struction materials to enhance the structural strength.84 and temperature, except at 100% RH.
Moudood et al. 337

5. If the composites have been immersed under water 7. Yan L, Chouw N and Jayaraman K. Flax fibre and its
or exposed to high RH for a long time, fiber swelling composites – a review. Compos Part B-Eng 2014;
at the interface can damage the fiber–matrix interfa- 56: 296–317.
8. Le Duigou A, Davies P and Baley C. Exploring durabil-
cial strength, by letting water remove water-soluble
ity of interfaces in flax fibre/epoxy micro-composites.
substances from the fibers and also by establishing
Compos Part A-Appl S 2013; 48: 121–128.
hydrogen bonds between the water molecules and 9. Celino A, Freour S, Jacquemin F, et al. The hygroscopic
the OH present in the fibers. behavior of plant fibers: a review. Front Chem 2014;
6. It is well established that physical and chemical 1: 1–12.
treatments improve the moisture absorption proper- 10. Kalia S, Kaith BS and Kaur I. Pretreatments of natural
ty of flax fibers, which will increase the quality of the fibers and their application as reinforcing material in
composites. However, further study is still needed to polymer composites-a review. Polym Eng Sci 2009;
reduce the moisture absorption behavior of the 49: 1253–1272.
11. Venkateshwaran N and Elayaperumal A. Banana fiber
fibers and their composites. Furthermore, the influ-
reinforced polymer composites – a review. J Reinf Plast
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Comp 2010; 29: 2387–2396.
strength still needs some attention. This will extend 12. Alves C, Ferrao PMC, Silva AJ, et al. Ecodesign of auto-
the usage of flax fiber reinforced composites in pre- motive components making use of natural jute fiber com-
cise engineering applications such as aeronautical posites. J Clean Prod 2010; 18: 313–327.
and automotive parts. 13. Pickering SJ. Recycling technologies for thermoset com-
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Declaration of conflicting interests 14. Yang YX, Boom R, Irion B, et al. Recycling of composite
The author(s) declared no potential conflicts of interest with materials. Chem Eng Process 2012; 51: 53–68.
respect to the research, authorship, and/or publication of 15. Biagiotti J, Puglia D and Kenny JM. A review on natural
this article. fibre-based composites-part I: structure, processing and
properties of vegetable fibres. J Nat Fibers 2004; 1: 37–68.
16. Suddell BC, Evans W, Isaac D, et al. A survey into the
Funding application of natural fiber composites in the automotive
industry. In: Proceedings of fourth international sympo-
The author(s) received no financial support for the research,
sium on natural polymers and composites, S~ao Pedro,
authorship, and/or publication of this article. Brazil, 2002; pp.455-460.
17. Joshi SV, Drzal L, Mohanty A, et al. Are natural fiber
ORCID iD composites environmentally superior to glass fiber rein-
Gaston Francucci [Link] forced composites? Compos Part A-Appl S 2004;
35: 371–376.
18. Wambua P, Ivens J and Verpoest I. Natural fibres: can
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