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Composites Science and Technology 67 (2007) 1674–1683
www.elsevier.com/locate/compscitech
Received 12 April 2006; received in revised form 22 June 2006; accepted 29 June 2006
Available online 14 September 2006
Abstract
Hemp fibre reinforced unsaturated polyester composites (HFRUPE) were subjected to water immersion tests in order to study the
effects of water absorption on the mechanical properties. HFRUPE composites specimens containing 0, 0.10, 0.15, 0.21 and 0.26 fibre
volume fraction were prepared. Water absorption tests were conducted by immersing specimens in a de-ionised water bath at 25 C and
100 C for different time durations. The tensile and flexural properties of water immersed specimens subjected to both aging conditions
were evaluated and compared alongside dry composite specimens. The percentage of moisture uptake increased as the fibre volume frac-
tion increased due to the high cellulose content. The tensile and flexural properties of HFRUPE specimens were found to decrease with
increase in percentage moisture uptake. Moisture induced degradation of composite samples was significant at elevated temperature. The
water absorption pattern of these composites at room temperature was found to follow Fickian behaviour, whereas at elevated temper-
atures it exhibited non-Fickian.
2006 Elsevier Ltd. All rights reserved.
0266-3538/$ - see front matter 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2006.06.019
H.N. Dhakal et al. / Composites Science and Technology 67 (2007) 1674–1683 1675
absorption of moisture leads to the degradation of fibre– and the structure of hemp fibre are presented in Table 1
matrix interface region creating poor stress transfer effi- [16]. The mechanical and physical properties of the polyes-
ciencies resulting in a reduction of mechanical and dimen- ter, hemp, and glass fibre used in this study are presented in
sional properties [7]. One of the main concerns for the use Table 2 [17].
of natural fibre reinforced composite materials is their sus-
ceptibility to moisture absorption and the effect on physi- 2.2. Processing
cal, mechanical and thermal properties [8]. It is important
therefore that this problem is addressed in order that nat- A combination of hand lay-up and compression mould-
ural fibre may be considered as a viable reinforcement in ing method was used to prepare the HFRUPE composite
composite materials. samples. Non-woven hemp fibre mat was first dried at
Several studies in the use of natural fibre reinforced 100 C to remove storage moisture in a fan-assisted oven.
polymeric composites have shown that the sensitivity of The storage moisture was recorded for hemp mat approx-
certain mechanical and thermal properties to moisture imately 9%. A measured quantity of unsaturated polyester
uptake can be reduced by the use of coupling agents and resin mixed with a catalyst (MEKP) for rapid curing was
fibre surface treatments [9,10]. poured on a pre-weighed amount of non-woven hemp fibre
Moisture diffusion in polymeric composites has shown mat, which was placed in a mould. The mould was coated
to be governed by three different mechanisms [11,12]. The with a semi-permanent, polymer mould release agent,
first involves of diffusion of water molecules inside the Frekote FRP90-NC. After pouring the resin, each layer
micro gaps between polymer chains. The second involves was left for a few minutes to allow the resin to soak into
capillary transport into the gaps and flaws at the interfaces the fibre mat. Trapped air was gently squeezed out using
between fibre and the matrix. This is a result of poor wet- a roller. The hemp fibre and polyester resin were then left
ting and impregnation during the initial manufacturing for about 3 min to allow air bubbles to escape from the sur-
stage. The third involves transport of microcracks in the face of the resin. The mould was closed and the composite
matrix arising from the swelling of fibres (particularly in panel was left to cure in a hydraulic press at a temperature
the case of natural fibre composites). Generally, based on of 22 C and at a compaction pressure of 10 bar for 1.5 h.
these mechanisms, diffusion behaviour of polymeric com- The fabrication route of the HFRUPE composites is
posites can further be classified according to the relative depicted in Fig. 1. The schematic of a hydraulic press used
mobility of the penetrant and of the polymer segments, to consolidate composite panels is shown in Fig. 2. After
which is related to either Fickian, non-Fickian or anoma- being taken out from the hydraulic press, the panel was left
lous, and an intermediate behaviour between Fickian and to cure at a temperature of 22 C for 24 h before being
non-Fickian [13,14]. In general moisture diffusion in a com- removed from the mould. Subsequently, post curing was
posite depends on factors such as volume fraction of fibre, carried out at a temperature of 80 C for 3 h. In addition
voids, viscosity of matrix, humidity and temperature [15]. to this non-woven hemp fibre, a randomly oriented
The objective of this work was to compare the influence chopped strand mat (E-glass fibre 40 w/w%) was used to
of both fibre reinforcement and water uptake on mechani- prepare reference glass fibre composite sample fabricated
cal properties of hemp fibre reinforcement unsaturated using similar procedure for comparison purpose.
polyester composites and the related kinetics and charac-
teristics of the water absorption. 2.3. Water absorption tests
Table 1
Typical chemical composition and structure parameters of hemp fibre
Cellulose Hemicellulose Lignin Pectins Wax Cell length (mm) Spiral angle (Deg) Moisture content (%)
74.4 17.9 3.7 0.9 0.8 23.0 6.2 10.8
1676 H.N. Dhakal et al. / Composites Science and Technology 67 (2007) 1674–1683
Unsaturated
Catalyst
Resin/catalyst/hemp fibre polyester
(MEKP)
Hemp fibre
Drying
Resin/catalyst mixing/hemp fibre drying Mixing Time: 1 hr
Temp: 100 dc
Post curing
Post curing Time: 3 hrs, temp:80 dc
Composites Composite
laminate
Fig. 1. Process flow chart showing the applied fabrication route of HFRUPE composites.
Mixture of UPE/catalyst/hemp
Top/bottom mould plates in a mould frame
flexural tests containing different fibre volume fractions of weighed regularly at 24, 48, 98, 196, 392 up to 888 h expo-
reinforcement were machined to a size of 150 · 20 · sure. Similarly, the specimens were immersed in water at
3 mm3 and 60 · 15 · 3 mm3, respectively. First all the spec- 100 C to determine water absorption at a higher tempera-
imens were dried in an oven at 50 C and then were allowed ture. For this test, the specimens were placed in a container
them to cool to room temperature in a desiccator before of boiling de-ionised water. After 30 min of immersion, the
weighing them to the nearest 0.1 mg. This process was specimens were removed from the boiling water, cooled in
repeated until the mass of the specimens were reached con- de-ionised water for 15 min at room temperature then
stant. Water absorption tests were conducted by immersing removed and weighed to the nearest 0.1 mg. The weight
the HFRUPE specimens in a de-ionised water bath at 25 C of the samples was measured at different time intervals up
for different time durations. After immersion for 24 h, the to 31 h of exposure until the water content reached satura-
specimens were taken out from the water and all surface tion. The moisture absorption was calculated by the weight
water was removed with a clean dry cloth. The specimens difference. The percentage weight gain of the samples was
were reweighed to the nearest 0.1 mg within 1 min of measured at different time intervals and the moisture con-
removing them from the water. The specimens were tent versus square root of time was plotted.
H.N. Dhakal et al. / Composites Science and Technology 67 (2007) 1674–1683 1677
2.4. Mechanical testing where mi is the initial weight of the moisture in the material
and ms is the weight moisture in the material when the
2.4.1. Tensile testing material is fully saturated, in equilibrium with its environ-
The tensile strength and modulus of the hemp fibre rein- ment. D is the mass diffusivity in the composite. This is an
forced composites before and after water immersion were effective diffusivity since all the heterogeneities of the com-
with a crosshead speed of 10 mm/min in accordance with posites have been neglected. h is thickness of specimen and
BS EN 2747:1998 [19]. Test specimens were individually t is the time and j is the summation index. The diffusion
cut using a diamond wheel into rectangular beams from coefficient is an important parameter in Fick’s law. Solving
the laminate slabs fabricated by a hand lay-up process. The the diffusion equation for the weight of moisture, and rear-
cut edges were then smoothed using 240 Grade SiC paper. ranging in terms of the percent moisture content, the fol-
lowing relationship is obtained:
2.4.2. Flexural testing 4M m t 0:5 0:5
The flexural strength and modulus of the composite M¼ Dx ð3Þ
h p
before and after water immersion were determined using
three-point bending test method following BS EN where Mm is the equilibrium moisture content of the sam-
2746:1998 test method [20]. A span of 48 mm, maintaining ple. Using the weight gain data of the material with respect
a span to depth ratio of 16:1, was used in a 30 kN load cell. to time, a graph of weight gain versus time is plotted. The
The load was placed midway between the supports. The diffusion coefficient can be calculated using the following
crosshead speed applied was 2 mm/min. Each sample was formula:
loaded until the core broke and their average is reported. d2
D¼ ð4Þ
p2 t70
2.4.3. Scanning electron microscopy
In order to understand the effect of water absorption on Where d is sample thickness in mm and t70 is time taken to
the microstructure of composites the surfaces of the water- reach 70% saturation in seconds.
immersed specimens were examined using a scanning elec- The diffusion properties of composites described by
tron microscope (SEM) JSM 6100. Fick’s laws was evaluated by weight gain measurements
of pre-dried specimen immersed in water by considering
3. Results and discussion the slope of the first part of the weight gain curve versus
square root of time by using the following equation [25].
The results obtained from this experimental study can The coefficient of diffusion (D) defined
p as the slope of the
be divided into two parts. The first part considers the nat- normalised mass uptake against t and has the form:
ure of the diffusion into the hemp reinforced composites 2
kh
and the second evaluates the effects of water absorption D¼p ð5Þ
4M m
at room temperature and at 100 C exposure on the
mechanical properties. where, k is the initial slope of a plot of M(t) versus t1/2, Mm
is the maximum weight gain and h is the thickness of the
3.1. Sorption behaviour composites.
Fig. 3 shows percentage of weight gain as a function of
The percentage of water absorption in the composites square root of time for UPE and various loading levels of
was calculated by weight difference between the samples
immersed in water and the dry samples using the following UPE only UPE/2 Layer hemp UPE/ 3 Layer hemp
equation: UPE/4 Layer hemp UPE/5 Layer hmep UPE/CSM
mt mo 12
DMðtÞ ¼ 100 ð1Þ
mo
10
where DM(t) is moisture uptake, Mo and Mt are the mass
Weight gain (%)
8
of the specimen before and during aging, respectively.
Different models have been developed in order to describe 6
the moisture absorption behaviour of the materials [21,22].
For one-dimensional moisture absorption each sample is 4
exposed, on both sides, to the same environment, the total
2
moisture content G can be expressed as follows [23,24]:
" # 0
8 X 1 2
m mi 1 ð2j þ 1Þ p2 Dx t 0 10 20 30 40
G ¼1 2 exp
ms mi p j¼0 ð2j þ 1Þ2 h2 Time (Hours) 1/2
UPE/hemp reinforced samples immersed in de-ionised UPE only UPE/3 Layer hemp
water at room temperature (23 C). The maximum percent- 16 UPE/4 Layer hemp UPE/5 Layer hemp
age weight gain for UPE, 3, 4 and 5 layers of hemp fibre
14
reinforced specimens, corresponding to 0, 0.15, 0.21 and
0.26 fibre volume fractions, respectively, immersed at room 12
temperature for 888 h is 0.879, 5.63, 8.16 and 10.97%,
Fig. 4. Failure showing (a) matrix cracking, (b) fracture running along the interface and (c) fibre–matrix debonding due to attack by water molecules.
H.N. Dhakal et al. / Composites Science and Technology 67 (2007) 1674–1683 1679
by 28% and after 72 h of water immersion, and flexural composite was calculated using the following standard
strength was increased by 45% [35]. formula:
The failure tensile strain value for all water-immersed
wf wm
specimens was found to increase compared to dry speci- V v ¼ 1 qc þ ð6Þ
qf qm
mens. The increase in failure strain upon exposure of the
samples to a wet environment can be attributed to the plas- where Vv is the volume fraction of voids, qc the density of
ticisation of hemp samples caused by moisture absorption. composite, wf the weight percent of fibre (%), wm the weight
Fig. 9a shows a SEM picture of hemp fibre. At regular percent of matrix (%), qf the density of fibre g/cm3 and qm
intervals along the fibre surface, kinks or nodes can be is the density of matrix g/cm3.
clearly seen. Fig. 9b shows a HFRUPE composite where As far as voids content in natural fibre composites is
the effect of kinks or nodes on the surface of the compos- concern, the fabrication techniques are not yet fully devel-
ite laminate reflect the misalignment of fibres. When these oped and the natural origin of the fibre component neces-
irregularly shaped fibres are placed in composites they do sarily induces an element of variation in to the
not seem aligned properly leading to fibre entanglement. composites; both factors contribute in creation of voids
Fibre alignment factors play a crucial role in the overall which affects to the overall composite properties. It is evi-
properties of composites. There is always a chance of fibre dent in this study that as the fibre volume fraction of hemp
entanglement with randomly oriented fibre reinforced reinforced composite sample increases the void content
composites. The random orientation of fibres produces also increases.
lower mechanical properties compared to long unidirec-
tionally orientated fibres. This fibre entanglement can cre- 3.2.2. Flexural properties
ate resin rich areas, which can contribute to the formation The flexural stress–strain versus fibre volume fraction
of voids and porosity (Fig. 10). Voids and porosity can results for dry and water immersed (exposure time 888 h
act as stress concentrators leading to failure of composite at RT) HFRUPE composites are shown in Figs. 11 and
samples. Hence, the void content for 2, 3, 4 and 5 layers 12. The observations made earlier for the effect of water
of hemp fibre composites specimen was found to be 12.56, absorption on tensile stress/strain properties are also rele-
14.46, 16.60 and 18.64%, respectively. The void content of vant here. The flexural stress drops incrementally as the
fibre volume fraction increases hence increased moisture
uptake percentage. The decrease in flexural properties after
water immersion can be related to the weak fibre–matrix
interface due to water absorption.
Flexural strain for water-immersed samples has
increases dramatically compared to dry samples. Flexural
strain for 5 layer hemp reinforced dry samples is 8%
whereas after 888 h of water immersion the strain is
almost doubled. HFRUPE composites become more rigid
due to the lower flexibility of the unsaturated polyester
chain. After water aging for 888 h, strain is almost dou-
bled compared to dry specimens since natural fibre rein-
forced composites tend to be ductile once the loss of
cellulose and integrity has taken place [36]. It has been
Fig. 9. SEM micrograph of hemp fibre (a) showing kinks or nodes (b) reported that water molecules act as a plasticiser agent
showing fibre misalignment and entanglement.
in the composite material, which normally leads to an
Fig. 10. Micrograph of water immersed hemp/UPE samples showing effects of voids (a) voids, (b) voids acting as reservoirs and (c) matrix cracking and
delamination after 888 h of immersion.
H.N. Dhakal et al. / Composites Science and Technology 67 (2007) 1674–1683 1681
140 Dry sample Water immersed sample acteristics of water immersed specimens are influenced not
only by the nature of the fibre and matrix materials but
120 also by the relative humidity and manufacturing technique,
which determines factors such as porosity and volume frac-
Flexural stress (MPa)
100
tion of fibres. Water uptake can be advantageous for some
80 natural fibres (such as Duralin fibre) at 66% relative humid-
ity as can fibre plasticising effect as a result of from the
60 presence of free water [41]. Excessive water absorption,
however, leads to an increase in the absorbed bound water
40 and a decrease in free water. In this situation, water can
penetrate into the cellulose network of the fibre and into
20
the capillaries and spaces between the fibrils and less bound
0 areas of the fibrils. Water may attach itself by chemical
UPE 0.1 0.15 0.21 0.26 links to groups in the cellulose molecules. The rigidity of
Fibre volume fraction the cellulose structure is destroyed by the water molecules
in the cellulose network structure in which water acts as
Fig. 11. Flexural stress versus fibre volume fraction.
a plasticiser and it permits cellulose molecules to move
freely. Consequently the mass of the cellulose is softened
and can change the dimensions of the fibre easily with
30 Dry sample water immersed sample
the application of forces. Observation of the fracture sur-
25
face from the flexural test sample further emphasises the
importance of fibre–matrix adhesion on flexural strength.
Flexural strain (%)
20
3.2.3. Influence of moisture on the modulus
15 Table 4 represents the results of tensile modulus and
flexural modulus for both dry and water-immersed speci-
10 mens at RT. It can be seen that moisture absorption causes
change in the modulus as determined by tensile and flexural
5 tests. The tensile modulus decreases for all hemp reinforced
samples. The reduction in tensile modulus for 3, 4 and 5
0 layer hemp reinforced specimens compared to dry speci-
UPE 0.1 0.15 0.21 0.26 mens is 61, 97 and 87%, respectively. A plausible explana-
Fibre volume fraction tion for this would be that, the elastic modulus is a fibre-
Fig. 12. Flexural strain versus fibre volume fraction.
sensitive property in composites and is affected as a result
of moisture absorption. This effect is particularly greater
for the composites with higher fibre content, in which stress
increase of the maximum strain for the composites after transfer capability between fibre and matrix interface gets
water absorption [37]. sharply reduced due to moisture content.
The decrease in mechanical properties with increase in The flexural modulus, however, is not adversely affected
moisture content is may be caused by the formation of by moisture absorption. The increase in flexural modulus is
hydrogen bonding between the water molecules and cellu- more pronounced with higher fibre content specimens,
lose fibre. Natural fibres are hydrophilic with many hydro- hence higher moisture content. It would be intuitive to
xyl groups (–OH) in the fibre structure forming a large assume that the effect of fibre reinforcement to be less crit-
number of hydrogen bonds between the macromolecules ical for the flexural failure stress than in tensile failure
of the cellulose and polymer [38]. With the presence of a
high –OH group percentage, natural fibres such as hemp
Table 4
tend to show low moisture resistance. This leads to dimen-
Tensile and flexural modulus for dry and wet samples
sional variation of composites products and poor interfa-
Specimens Fibre Tensile Flexural
cial bonding between the fibre and matrix, causes a
volume modulus (GPa) modulus (GPa)
decrease in the mechanical properties [39]. (%) Dry Wet Dry Wet
Water absorbed in polymers is generally divided into
free water and bound water. Water molecules (which are UPE only 0 0.56 0.60 5.51 5.81
2 Layer hemp 10 0.72 0.64 4.20 5.76
contained in the free volume of polymer and are relatively
3 Layer hemp 15 1.0 0.62 5.34 6.08
free to travel through the micro voids and holes) are iden- 4 Layer hemp 21 1.22 0.62 7.30 6.06
tified as free water. Water molecules that are dispersed in 5 Layer hemp 26 1.27 0.68 6.49 8.05
the polymer–matrix and attached to the polar groups of Data in table are means with a sample size of 5 for dry and 3 for wet for
the polymer are designated as bound water [40]. The char- each specimen group.
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