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Investigation into the use of alkali treated screwpine (Pandanus Utilis) fibres
as reinforcement in epoxy matrix
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Jaykumar Chummun
University of Mauritius
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DOI 10.1007/s12588-014-9082-z
R E S E A R C H A RT I C L E
Abstract In this study, epoxy resin vacuum infused in screwpine fibres has been used
to investigate whether it can emerge as a realistic alternative to glass fibre composites.
The screwpine fibres were mercerized and treatment conditions were selected on the
basis of cellulose percentage and fibre surface morphology. Experimental design, based
on Taguchi’s L9 Orthogonal Array showed that mercerization with 5 % NaOH for
45 min at 75 °C offered optimum results. ANOVA illustrated that temperature was in
fact the most influential parameter followed by NaOH concentration and time. ATR-
FTIR was used to analyze the fibre-composition change as a result of mercerization.
Compression testing of composites showed that alkali-treated fibre composites with-
stand more load than untreated fibre composites at 5, 10, and 15 % (weight basis) fibre
loadings. Fatigue test also confirmed that results are significantly better when compos-
ites are made from treated fibre. The outcomes indicate that screwpine fibres may be
used as a potential reinforcing material for low-load bearing composites such as
automobile components.
Introduction
With the growing consciousness of global environmental issues, the concept of sus-
tainability, industrial ecology, eco-efficiency and green engineering are being integrated
into the development of next generation materials, products and processes [1]. For
several decades glass fibre-reinforced composite materials have been a valuable class of
engineering materials but with the availability of a wide range of non-renewable raw
materials coupled with the significant energy consumption for producing glass
fibres composites as well as disposal/ landfill problems, the use of natural-fibre
composite materials has found increasing applications in various industrial sec-
tors. For example, abaca fibres reinforced composites are being used in under-
floor protection of passenger cars by Daimler Chrysler [2]. Studies during recent
years on plant based cellulosic fibres [3] like hemp, flax, kenaf, jute, bamboo,
pineapple, sisal showed that natural fibre reinforced composite enjoy significant
advantages in terms of their environment friendliness, light weight, low cost and
degradability. Most of those natural fibres composites are used for non-structural
parts for the automotive industry, namely, covers, car doors panels and car roofs
[4].
Several methods have been studied to enhance the mechanical, surface prop-
erties as well as the adhesion mechanism of natural fibres, namely, physical
methods (stretching, calendering and thermo-treatment), and chemical methods
such as alkali treatment, acetylation, peroxide treatment, and graft co-
polymerization [5]. Among the numerous chemical treatments, alkali treatment
has been acknowledged as the mostly used, least expensive, effective and
environment friendly method to improve mechanical and interfacial properties
of the fibres [6]. Alkali (sodium hydroxide - NaOH) treatment causes the fibres
to fibrillate [7]; a situation whereby the surface area and surface roughness of the
fibres increase. The former effect encourages greater absorbance1 of resin to the
fibre while the increased surface roughness will engage with the resin better,
known as mechanical interlocking. These effects create a higher fibre aspect ratio
and leads to a better fibre/matrix adhesion.
Note 1 In terms of weight basis - Untreated fibres contain impurities like dirt, wax
etc.., therefore the packing ability (fibre-resin ratio) is less compared to
treated fibres whereby fibres are thinner. Thus if fibres are thinner (fibril-
lation of fibres due to chemical treatment) resin penetrates more into the
test sample (greater absorbance) and bondable area of fibre to resin
increases.
longer fatigue life than polyester matrix composites. Constant life diagrams of epoxy
matrix composite showed the superiority of alkali treated fibre composite especially for
low cycle fatigue [13].
The composite characteristics especially mechanical depend not only on the prop-
erties of the treated or untreated fibres but also on the extent to which an applied load is
being transmitted to the fibres by the matrix (resin). The extent of this load transmit-
tance is a function of the fibre length commonly known as the critical fibre length, Lc
[14]. According to Kelly-Tyson model [14], this critical fibre length Lc is dependent on
the fibre diameter d, it’s ultimate strength σf, and on the matrix shear strength τc,
according to the
Lc ¼ ð f dÞ=2 c ð1Þ
There are several native plants in different countries which have been in use for
decades in the textile and composite industries [15]. In Mauritius, there are many
local plants where fibres can be extracted, namely, filao, bagasse (from sugar
cane), banana, screwpine, coconut. Screwpine plant also known as Pandanus
Utilis belongs to the Pandanaceae 2 family, and this plant grows along the
mangroves and in local forests. Its leaves can yield strong fibres which may be
used, not only for weaving mats, baskets or rope making but also fibre
composites. So far there does not seem to be any report in the available
literature about the potential of using Pandanus utilis fibres as a reinforcing
material in a polymer matrix.
Note 2 There are about 600 known species of the pandanaceae and each one
possesses its own specificities. Some species vary in size from small shrubs
less than 1 m tall, to medium-sized trees 20 m tall, typically with a broad
canopy. The Pandanus Utilis plant has large and long leaves which can
provide fibres up to 1 m long.
Fibre preparation
Dried screwpine leaves (Fig. 1a) were collected at the Mauritian Natural Forestry
Division. The spiny and midribs of the leaves were removed and hand washed with
running water. Leaves were then chopped into 50×5 cm pieces and immersed in
boiling water for 15–20 min. The leaves were allowed to cool and fed into a fibre
extractor (Fig. 1b) whereby the cuticle and epidermal layer were removed. Fibres
obtained (Fig. 1c) were then dried at room temperature for 3 days.
Taguchi’s Design of Experiment (DOE) was used to determine a proper alkali treatment
which would yield maximum cellulose percentage through removal of hemicelluloses,
lignin and other surface impurities without damaging the fibre. Based on existing
literature, three main variables have been selected for the alkali treatment, namely,
the concentration of NaOH, the temperature and the duration of the process. Three
levels of each of the three factors were chosen3 in order to run an L9 Orthogonal Array
(OA). Table 1 summarises the levels for the three controllable factors.
Note 3 Preliminary test were conducted on extracted fibres and treatment conditions
exceeding 5 % NaOH concentration for more than 45 min at 75 °C led to fibre
disintegration.
After NaOH treatment the fibres were washed with distilled water for 2–3 min to
remove residual alkali solution. The fibres were left to dry at room temperature for 24 h
and oven dried at 60 °C for 24 h [18, 19].
Since increasing cellulose content is a key factor for improved natural fibre com-
posites, the cellulose percentage of the treated fibres was considered as the quality
characteristic. The Signal to Noise (SN) ratio based on the “Larger-the-better” method
(Eq. 2) was computed for each experimental run, and an analysis of mean (ANOM) as
well as an analysis of variance (ANOVA) were done in order to determine the optimum
process conditions which would yield maximum cellulose percentage (Ross, 1988).
a b c
Fig 1 a: Screwpine leaves. b: Fibre production using a fibre extractor machine in textile laboratory at
University of Mauritius. c: Screwpine fibres after extraction
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1 2 3
1 NaOH Concentration % A 1 3 5
2 Temperature °C B 25 50 75
3 Time min C 15 30 45
1 1
SN ¼ −10log10 Σ ð2Þ
n y2
Where n: the number of measurement in a trial/row.
y: the measured value in a run/row
The cellulose percentage was determined by using two tests namely Acid Detergent
Fibre (ADF) and Acid Detergent Lignin (ADL) test; methods set by Van Soest P.J
(1963) in the analysis of fibrous feeds. The FibreTec 1020 (Tecator) hot and cold
extraction machine was used. In ADF test sample was boiled in the Tecator hot
extraction unit for 1 h with sulphuric acid (1N) together with Cetyl-Trimethyl Ammo-
nium Bromide (CTAB) (pH=4) and insoluble matter was separated by filtration. The
residue after the test consisted of Cellulose + Lignin + Mineral ash. In the ADL test, the
sample after the ADF test was treated in the Tecator cold extraction unit with 72 %
H2SO4 for 3 h. The process dissolved cellulose and the remaining residue consisted of
Lignin + Mineral ash. Cellulose content was therefore obtained by subtracting values
obtained from the ADF and ADL test [20–24]. For each experimental run, two replicate
tests of ADF and ADL were done, and a mean was calculated.
In order to verify the results of the ADF and ADL testing methods with respect to the
effect of the alkali treatment on the cellulose content, an FTIR analysis was conducted
on the fibres obtained from the Taguchi experimental run which yielded the best result,
and from fibres treated under the optimum alkali conditions obtained through the
ANOVA and ANOM analysis. The infra-red measurements were performed using a
Bruker platinum ATR-FTIR spectrometer in the range of 400–4,000 cm−1 to investigate
possible change in functional groups of fibres after the chemical treatment.
For effective strengthening and stiffening of composite the critical fibre length was
computed using the Kelly-Tyson model (Eq. 1). The ultimate fibre strength, f =(fibre
load carrying capacity/cross sectional area), fibre load carrying capacity=78.5 N [25],
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matrix strength c = 70 MPa [26] and mean fibre diameter4 d=0.271 mm (Standard
deviation=0.018 mm).
Note 4 diameter measured using a digital thickness micrometer gauge. Three replicate
were done on three different sample sets and the mean fibre diameter was
calculated.
Compression test
The test was carried out in conformity with ASTM D 695 and the size of specimen was
12.7×12.7×25.4 mm. Samples were tested on a Contro-Lab Compression machine
consisting of a hydraulic press which axially compresses the specimen at a rate of
1.27 mm/min until the composite fractures. The reading was obtained on the data
screen and the value remained fixed when the maximum load taken by the composite
was reached. The test was carried out at room temperature, and three replicate tests
were done for each specimen and the mean value was computed.
a b
Vacuum tubes
Fatigue testing
The fatigue performance was characterized using a Denison Meyes fatigue tester with
fatigue specimen as shown in Fig. 3. A stress range of 69, 46 and 32 MPa representing
approximately 75, 50 and 35 % of the static strength of treated (10 % fibre: resin ratio)
screwpine/Epoxy composite in a tension-compression mode was applied on the spec-
imen. The stress load was imposed at one end of the latter by an oscillating spindle
driven by means of a connecting rod, crank and eccentricity adjusted as shown in
Table 2 to give necessary range of bending angle. The stress load was measured at the
opposite end of the specimen by means of a torsion dynamometer, the angle of twist of
which is registered on dial gauges. Furthermore, the failure mode was investigated and
the fatigue life was compared to that of unreinforced epoxy, untreated screwpine/Epoxy
and glass fibre composite.
Alkali treatment affects the chemical composition of fibres. This treatment is supposed
to remove and hydrolyze the hemicellulose, soluble minerals, silica and ash [27, 28].
The morphology of fibres at some different stages of NaOH treatment is shown in
Fig. 4. Fibres after the extraction process are in fact the vascular bundles consisting
mainly of xylem and phloem which provide mechanical support to the plant leaves
[29]. Impurities observed on the fibre surface (Fig. 4a) are detrimental to good fibre
matrix adhesion; but with the different chemical treatment conditions (Fig. 4b–d) the
impurities were significantly reduced. The decrease in impurities together with hemi-
cellulose and lignin accounts to why the cellulose percentage has increased as observed
in Table 3. Figure 4c indicate that fibres initially in leaves were bonded together by
cement like components which were partially diminished after the mercerization
process. With treatment condition 5 % NaOH for 45 min at 50 and 75 °C (Fig. 4d),
fibre surface were smooth, free from impurities and no fibre deterioration were
observed.
The data collected for each of the nine experiments as well as the calculation of the
respective SN ratio are shown in Table 3. The relative significance of individual factors
was determined by the ANOVA analysis and summarized in Table 4. Based on the
results obtained from the ANOVA, factor B (temperature) is the most dominant factor
Stress level Stress applied Bending moment Dial gauge Degree of Dial gauge
(%) MPa (lb.inch) range eccentricity reading (±)
influencing the cellulose percentage since its F value is well above 4, followed by the
percentage concentration of NaOH and the heating time. However, given that the F
value of the three factors is above 2, it can be concluded that all the three factors do
influence the percentage of cellulose. Given that the values of y1 and y2 for each
experiment (Table 3) show very low variation, this explains the low value of the
variance due to the error. Moreover, given that only three factors were tested, and that
b c
Impurities/Sponge-like layer on
fibre surface slowly being removed
Table 3 Taguchi table (L9 OA for cellulose percentage in fibre after alkali treatment)
A B AB C y1 y2 Mean
the third column was not assigned to any factor, then it is believed that the interactive
effect (A×B) of the factors is minimal.
The results of the analysis of the mean (ANOM) of the signal to noise (SN) ratios for
the three controllable factors are shown in Fig. 5a–c. Based on these results, it can be
deduced that the optimum combination (within the tested range of values) of the
process factors would be A3B3C3, that is, 5 % NaOH (A3), 75 °C (B3) and 45 min
(C3). However, based on the results of the L9 OA, the best result for % cellulose was
obtained for A3B2C3 for experiment 8.
Confirmatory test
A confirmatory test was run in order to check whether a better percentage cellulose
content was obtained with the A3B3C3 combination. Table 5 shows the result of
cellulose percentage of the three replicates for the confirmatory test. The results show
a
% NaOH Concentration
36.00
35.00
33.00 33.27
32.00
A1 A2 A3
b
Temperature
36.00
35.00
35.02
34.00
33.88
33.00 32.25
32.00
B1 B2 B3
c Time
36.00
35.00
33.85
34.00
32.99 34.32
33.00
32.00
C1 C2 C3
Fig 5 a: Main effect plot of SN values for % NaOH concentration. b: Main effect plot of SN values for
temperature. c: Main effect plot of SN values for Time
an increase in cellulose up to 67.1 % representing 4.2 % more than fibres treated with
5%NaOH, 50 °C, for 45 min, experiment 8 of the L9 OA.
The composition change of untreated and treated screwpine fibres were investigated
using the Fourier Transform Infra-red spectra. The three main components namely
cellulose, hemicellulose and lignin having characteristic bands at about 3,300, 1,730
and 1,200 cm−1 respectively were observed. The peak at about 3,300 cm−1 is due to
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1 66.82
2 67.44
3 67.16
Mean 67.10
hydrogen bonded O-H stretching. Abraham et al. [30] claimed that alkali treatment
reduced hydrogen bonding due to removal of the hydroxyl groups by reacting with
sodium hydroxide and this resulted in the increase of the –OH concentration. This
phenomenon is clearly evident from the increased intensity of the peak between 3,200
and 3,500 cm−1 bands on Fig. 6 when compared to the untreated fibre. This stretching
peak also corresponds to the aliphatic moieties in cellulose.
The decrease in transmittance of functional groups associated with untreated and
treated fibres at optimum conditions was also observed Fig. 7. Hemicellulose
representing characteristic peaks in the range of 1,730–1,740 cm−1 corresponds to the
C=O stretching in acetyl and uronic ester groups or in carboxylic group of ferulic and
coumaric acids have subsequently decreased after the NaOH treatment. The significant
decrease of band at 1,200–1,300 cm−1 could have been caused by the removal of lignin.
The peak at 1,030 cm−1 was assigned to the C=O deformation in secondary alcohol
and aliphatic ether or aromatic region [31]. It could be noted from Fig. 6 that the
content of both treated fibres more or less similar in chemical constituents; which
explains why the values in Table 6 was very close.
Given that there is only 4.2 % increase in the cellulose content between the optimum
condition, that is, A3B3C3, and the result of experiment 8 (A3B2C3) of the orthogonal
array but that there is a significant increase in terms of energy requirement to apply the
optimum condition, it is important to evaluate the mechanical properties for the two sets
of process conditions. Thus compression and fatigue tests were performed in order to
compare the performance of unreinforced polymer, untreated fibre reinforced
Untreated Fibre
Untreated Fibre
composite, treated fibre reinforced composite at 50 and at 75 °C, and for fibre glass
reinforced composite.
Based on Kelly-Tyson model (Eq. 1), the critical fibre length (Lc) of screwpine
fibre is found to be 2.64 mm. This eventually means that for the composite to be
effective (good load transmittance from fibre to resin) the minimum length of the
fibre should be 2.64 mm. However according to Vas et al. [32] and Oksman et al.
[33], if the fibre length L is longer than the critical fibre length (L ≥ Lc), the fibre
reinforcement in the matrix phase (resin) becomes more effective as the fibre
aspect ratio L/d, and the interfacial shear strength of the composite increases. This
explains why long continuous fibres and woven fibre composite have more
mechanical strength when compared to chopped, random and discontinuous fibres.
Based on the model of Kelly-Tyson, it is recommended that the actual fibre length
(L) should be long (L > 15Lc) and continuous. The fibres that were used for the
experiments were long, continuous, and for the fatigure testing, the fibres were
chopped to 75 mm length.
Compression test
Note 5 Optimum spacing refers to the minimum allowable spacing between fibres,
below which the structure shall start to disintegrate under loading before
tensile or compressive failure [35, 36].
120
UTR/ EPOXY TR (75)/ EPOXY TR (50)/ EPOXY GL/EPOXY
110
Compressive Strength (MPa)
100
90
80
70
60
50
40
0% 5% 10% 15%
Fibre-Resin Percentage
Fig. 8 Compressive strength of different composites with different fibre volume fractions
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75 °C. The maximum compressive strength for the glass fibre (16.9 kN/104.8 MPa)
was obtained at 15 % fibre-resin ratio whereas that for the alkali treatment at 75 °C
(15.8 kN/ 97.9 MPa) was obtained at 10 % fibre-resin fraction, which yields a
maximum difference of only 6.5 % in the compressive strength. It was also noted that
due to the higher fibre content in screwpine fibre composite, the amount of base
polymer utilized was significantly reduced; this means saving in terms of cost and
composite weight as well as green and sustainable approach to composite materials
when compared to glass fibre composites.
The higher compressive strength (6.3 % higher) due to the 75 °C alkali treatment as
compared to the 50 °C treatment seems to indicate that there has not been any fibre
deterioration at the higher temperature. On the contrary, the increase of 4.2 % of the
cellulose content at 75 °C alkali treatment as compared to the 50 °C alkali treatment has
lead to this 6.3 % increase in compressive strength. The results also give a clear
indication that the alkali treatment has enhanced the fibre/matrix interfacial adhesion;
the reduction in hydrogen bonding capacity due to mercerization and drying has
eliminated the open hydroxyl groups that tend to bond with water molecules and forms
voids.
The above finding is comparable to that of Venkatesha Prasanna et al. [37], who
mentioned that alkali treatment leads fibrillation i.e., breaking of composite fibre
bundles into smaller fibres. This could have lead to a significant increased in the
effective surface area available for wetting by the matrix material and a reduction in
the fibre diameter. This would have resulted in a better fibre-matrix interface adhesion
property. With the removal of surface impurities, decrease in hemicellulose and lignin,
and fibrillation, the area and surface roughness of fibres have increased. This resulted in
a higher fibre aspect ratio which in turn promoted fibre mechanical interlocking and
wetting.
The untreated screwpine fibre composite has shown lower compressive
strengths for all the three fibre-resin fractions as compared to the treated compos-
ites. In fact there is a clear degradation of the compressive strength with increasing
fibre-resin fraction. The low compressive strength may be attributed to the pres-
ence of surface impurities on the untreated fibres as well as its inappropriate
surface texture in this state that result in poor adhesion between the untreated
fibres and the resin matrix. The presence of lignin may also explain this poor
performance as mentioned by Riedel [38] which leads to poor mechanical
interlocking and chemical bonding.
Fatigue test
Fatigue test specimens were subjected to skin stresses of 69, 46 and 32 MPa (constant
amplitude) at a frequency of 1,420 stress cycles per minute and results of the SN curves
are presented in Fig. 9. The properties of the fibre/matrix interface and fatigue life were
enhanced by better bonding brought about by alkali treatment. Composite reinforced
with untreated screwpine fibres experienced considerably more interfacial damage than
those with alkali treated fibres.
Fatigue failure of all specimens under investigation except from unreinforced
epoxy occurred in five major mechanisms: matrix cracking, crack propagation, de-
lamination initiation, de-lamination growth and fracture as shown in Fig. 10a,b,c.
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80
70
STRESS, MPa
60
50
40
30
20
0 50000 100000 150000 200000 250000
After the crack initiation, the crack propagated very slowly because the fibres
whether screwpine or glass still continues to hold the matrix as observed in
Fig. 10a; this is commonly known as crack bridging or fibre bridging and it
increases the fatigue performance of the composite. On the other hand, unreinforced
epoxy matrix had a different fracture mechanism. The material failed instantly when
the first crack appeared. Glass fibres composite have better fatigue life but fatigue
performance of treated screwpine composite is also good at low stress levels;
suggesting that the possibility of using them as substitute to glass-reinforced
composite for low load application is promising.
a Crack initiation
& propagation
on treated
screwpine fibre
composite
b Final fracture
and reduced
de-lamination
c Fracture of
specimen after
fatigue test
More cracks
observed
Fig 10 a,b,c: Observed fracture mechanism
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Conclusion
This investigation looked into the potential of using screwpine fibres for semi structural
composite materials such as automotive external mirror casing. The effect of alkali
treatment on improving the wetting property of the screwpine fibres to the epoxy matrix
has been investigated. Taguchi method was used and the optimum alkali treatment
conditions were found to be 5 % NaOH concentration for 45 min at 75 °C without any
fibre degradation. Hemicellulose, lignin and other impurities on the fibre surface were
also observed to decrease. Following the compression tests, it was found that at 10 %
fibre fraction, the composite with the treated fibres (at the optimum conditions) has
21.5 % higher compressive strength as compared to the untreated fibre composite.
Based on the fatigue behaviour, it was found that treated fibre composite had about 3
times the fatigue cycles to failure than an unreinforced composite. Glass fibre compos-
ite has slightly higher fatigue life than screwpine composite. However, it is believed
that further research in order to improve the wettability of the fibre to the matrix would
yield screwpine composites having comparable or even better fatigue life properties
than that its glass-fibre counterpart.
Acknowledgments The authors gratefully acknowledge the timely help rendered by the following staff of
the University of Mauritius: Mr. R Sheik Manoga, Ms. Vencatasamy, Mr. Awatar, Mrs. Seeruttun, Mrs.
Bissoundoyal, Mrs. Nathalie, Mr. Debiddin and his team.
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