3. lucrare_fibra de cocos
TRANSCRIPT
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Surface treatment of coir (Cocos nucifera) fibers
and its influence on the fibers physico-mechanical properties
M. Mizanur Rahmanaa, Mubarak A. Khanb
b
aDepartment of Applied Chemistry and Chemical Technology, University of Dhaka, Dhaka
1000, Bangladeshb
Nuclear Radiation and Polymer Chemistry Laboratory, Institute of Nuclear Science and
Technology, Bangladesh Atomic Energy Commission, P.O. Box 3787, Dhaka 1000, Bangladesh
Received 29 May 2006. Revised 21 December 2006. Accepted 19 January 2007. Available
online 31 January 2007.
Abstract
Coir, an important lignocellulosic fiber, can be incorporated in polymers like polyacrylate in
different ways for achieving desired properties and texture. But its high level of moisture
absorption, poor wettability and insufficient adhesion between untreated fiber and the polymer
matrix lead to debonding with age. In order to improve the above qualities, adequate surface
modification is required. In our present work, fiber surface modification by ethylene
dimethylacrylate (EMA) and cured under UV radiation. Pretreatment with UV radiation and
mercerization were done before grafting with a view to improve the physico-mechanical
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performance of coir fibers. The effects of mercerization on shrinkage and fiber weight losses
were monitored at different temperature and alkali concentration. We observed that, fiber
shrinkage is higher at low temperature and 20% alkali treated coir fibers yielded maximum
shrinkage and weight losses. It was found that higher shrinkage of the polymer grafted fiber
showed enhanced physico-mechanical properties. The grafting of alkali treated fiber shows an
increase of polymer loading (about 56% higher) and tensile strength (about 27%) than 50% EMA
grafted fiber. The fiber surface topology and the tensile fracture surfaces were characterized by
scanning electron microscopy and were found improved interfacial bonding to the modified
fibermatrix interface.
Keywords
Coir fiber; Mercerization; Photocuring; Surface pretreatment; UV radiation; Physico-mechanical
properties .
1. Introduction
Coir fibers can be incorporated in polymers to form a biodegradable matrix. But a high level of
moisture absorption and insufficient adhesion between untreated fibers and the polymer matrix
may lead to bio-composites having high water absorption characteristics that reduce their utility
in many applications since major restriction in the successful use of natural fibers in durable
composite applications is their high moisture absorption and poor dimensional stability
(swelling) [1]. Coir is a versatile lignocellulosic fiber obtained from coconut trees (Cocos
nucifera), which grow extensively in tropical countries. The chemical constituents and the
mechanical properties of coir fibers are included in Table 1. Because of its hardwearing quality,
durability and other advantages, it is used for making a wide variety of floor-furnishingmaterials, yarn, rope, etc. [5] and [6]. However, these traditional coir products consume only a
small percentage of the total world production of coconut husk. Coir is a cheap fiber, even
cheaper than sisal and jute [7]. Coir fibers are not as brittle as glass fibers, are amenable to
chemical modification, are non-toxic and possess no waste disposal problems, but unfortunately
the performance of coir as a reinforcement in polymer composites is unsatisfactory and not
comparable even with other natural fibers. This inferior performance of coir is due to various
factors such as its low cellulose content, high lignin content, high microfibrillar angle, and large
as well as variable diameter.
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2. Experimental
2.1. Materials
Coir fibers were collected from the local market of Bangladesh. The fiber was subjected to
various surface modifications like UV ageing, alkali treatment and grafting with acrylate
monomer (EMA) using UV radiation. The monomer ethylene dimethacrylate (EMA) having
molecular weight 198 was procured from Fluka Chemica (Switzerland). Photoinitiator, Irgacure-
500 was procured from Ciba-Geigy, Switzerland.
2.2. Experimental procedure and data analysis
Coir fibers were cut into small pieces (1015 cm in length). The coir fibers were washed in 2%(commercially available washing powder, Surf, Unilever, UK) detergent solution at 70 C for 1
h, then washed overnight with rinsing tap-water and finally thoroughly washed with distilled
water followed by a drying process in a vacuum oven at 70 C. The detergent washed fibers were
aged with UV radiation to measure the effect of radiation on coir properties. The fibers were then
grafted with different concentration monomer + MeOH solution at different grafting conditions
and cured under same UV light (model IST Technik, Germany) at 254313 nm wavelengths of
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radiation and 2 kW power at 50 A current. The UV radiation source contains a conveyor belt
which moves around the mercury lamp and after moving once to the lamp it was considered one
pass. The optimum grafting condition with respect to different physical properties was measured
in this method.
The coir fibers treated with EMA was immersed in acetone for 5 min t o remove unreacted
monomer. After drying in an oven the fiber samples were weighed and wrapped with stainless
steel net and finally put in a soxhlet. Homopolymers are removed through extraction in hot
acetone for 72 h in the soxhlet. In this process the homopolymer will remove from the surface of
the fiber and only the grafted molecules will remain. The amount of grafting was determined by
the following equation:
2.3. Fiber surface treatment
Coir fibers were soaked in 550% NaOH (before treatment with EMA) for about 0.5 h at
temperature ranges from 0 to 100 C in order to activate the OH groups of the cellulose and
lignin in the fiber. The appropriate concentration of NaOH solution used in mercerization before
each type of chemical treatment was completed in the initial work [14] indicated that a 1030%sodium hydroxide solution produced the best effects on natural fiber properties. The fibers were
then washed many times in distilled water and finally dried.
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Water absorption properties of treated and untreated fibers were determined by placing the
sample in a static water bath at room temperature, and water uptake for different swelling time
were measured by the formula:
2.4. Fiber surface morphology
In order to evaluate changes in the surface morphology, all investigated natural fibers were
analyzed by scanning electron microscopy (SEM) using a Hitachi S-2700 scanning electron
microscope (Nissei Sangyo GmbH, Rathingen, Germany). The excitation energy was 10 keV
with a beam current of 0.5 nA.
3. Results and discussion
Lignocellulosic fillers offer attractive properties, but are used only to a limited extent in
industrial practice [15]. Natural fibers are strongly hydrophilic materials and moisture absorption
leads to a significant deterioration of their mechanical properties. Furthermore, most polymers
are hydrophobic and due to this divergent behavior, the interface in natural fiber composites is
rather poor. Any alteration of the characteristics of the cell wall, either chemical or
morphological, has an effect on the mechanical properties of the fibers. By limiting the
substitution reaction to the fiber surface, the good mechanical properties are preserved and a
degree of biodegradability is maintained.
The tensile properties (tensile strength, elongation at break and Youngs modulus were
measured) of the untreated virgin raw fiber was measured and the average values for twenty
samples were; TS 117.5 MPa, Eb 14.8% and Youngs modulus (M) 628 MPa. Tensile strength
and elongation factors are the enhancement of these properties after polymer treatment with
EMA compared with the virgin raw fibers. Each of the data presented in this report were the
average value of at least five samples and the results obtained were with in the accuracy of 2%.
4. Effect of UV radiation on tensile properties of virgin coir fiber
Detergent washed virgin coir fibers were irradiated under UV radiation of different intensities
(represented by number of passes) to investigates its effect on the mechanical properties. The
values of tensile strength; TS (MPa), elongation at break; Eb (%) and modulus; M (MPa) were
graphically represented in Fig. 1 against the doses of UV radiation by which the raw coir fiber
was aged. These factors are the ratio between UV pretreated and untreated fibers. We observed
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significant change of mechanically properties after coir fibers were pretreated by UV radiation.
Increasing UV doses to the fiber also increases tensile strength, elongation at break and Youngs
modulus. Highest tensile strength (156.3 MPa) was achieved after the fiber was aged by 125
passes of UV radiation, which is 33% higher than the tensile strength of virgin fiber. This also
gives highest elongation (20.5%) which is about 39% higher than virgin coir fiber. Increase of
tensile properties with increasing radiation doses could be due to the inter-crosslinking between
the neighboring cellulose molecules occur under UV radiation and the decrease at higher
radiation doses could case due to the photo-degradation of cellulose backbone at higher UV
doses. During photo-degradation there will be loss in strength due to primary bond breakage in
the cellulose constituent.
Fig. 1. Tensile properties of UV pretreated coir fiber at various radiation intensities (tensile
properties) are represented as the ratio of the tensile properties of the UV pretreated coir fiber to
that of untreated one. Tensile strength of virgin raw coir fiber is 117.5 MPa. The elongation at
break and Youngs modulus are 14.8% and 628 MPa.
5. Treatment of coir fiber with EMA
5.1. Polymer loading and grafting
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The PL values of the coir fibers were calculated as the weight gain (%) after they were cured
under UV radiation. The PL values of EMA treated fibers at different radiation intensities are
given in Fig. 2a as a function of monomer concentration. The values are relatively low at low
monomer concentration and it increases with increasing monomer concentration up to 50% inmethanol. But at 70% EMA it showed reduction of PL values. PL increases with increasing UV
intensities up to a certain value and after attainment of maximum values it again decreases with
increasing radiation doses. The highest PL (19.12%) is observed for the coir sample treated with
50% EMA in methanol and at 125 passes of UV radiation.
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Fig. 2. Polymer loading (a) and grafting (b) of EMA treated coir fibers at different UV radiation
doses as a function of monomer concentration.
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The amount of grafted polymer was determined after the extraction of homopolymer through the
extraction of the EMA treated fibers in hot acetone for 72 h. This will gives exact percentages of
grafted polymer on coir fiber surface. The results of grafting efficiencies are graphically
represented against UV radiation doses as a function of monomer concentration and are plotted
in Fig. 2b. We have observed that grafting efficiencies are also increases with UV doses and the
highest efficiency (76.5%) was obtained for the coir sample grafted with 50% monomer and
cured at 125 passes of UV radiation. We have also found that at low monomer concentration and
at low UV doses the grafting efficiencies are low because at lower monomer concentration the
vinyl monomer promotes rapid propagation reaction with the help of photoinitiator leading to
network polymer structure through graft copolymerization reaction via their double bond [16].
As EMA concentration is increases the amount of residual unsaturation is also increased with the
consequence of faster rate of formation of three dimensional network structures causing
restricted mobility. After maximum value of PL the reduction of values at higher monomer
concentration may be caused by two factors. At higher EMA concentration radicalradical
recombination processes may be dominating creating more homopolymers rather than monomer-cellulose backbone reaction. Another reason could be the swelling of cellulose backbone with
MeOH is insufficient due to lower amount solvent; methanol. As a result monomer molecules
are incapable of penetrating the cellulose molecules in presence of low solvent which may cause
a smaller number of reacting sites at the cellulose backbone and thus continue to reduce the
active sites as MeOH amount reduces at higher EMA concentration.
5.2. Tensile properties
The chemical processing directly influences the cellulosic fine structure of plant fiber.
Consequently, the chemical treatments (grafting with monomers) and have a lasting effect on the
mechanical behavior of coir fibers, especially on fiber strength and stiffness. Mohanty et al. [17]
showed that the higher strength treated fibers compared to untreated fibers may be a result of the
removal of surface imperfections after the treatment. The increased uniformity of the fibers
would give an increase to strength, as points of nonconformity are removed during the treatment
and this changes the deformation. The tensile strength of coir fiber-reinforced composites is
determined both by the tensile strength of the fiber and by the presence of weak lateral fiber
bonds. The variations in the tensile strength at yield of the composites on different modification
were attributed to the changes in the chemical structure and bondability of the fiber. Many of the
modifications decrease the strength due to the breakage of the bond structure, and also because
of the disintegration of the non-cellulosic materials [14]. The reinforcing ability of the fibers didnot just depend upon the mechanical strength of the fibers but on many other features, such as
polarity of the fiber, surface characteristics and presence of reactive centers. These factors
control interfacial interaction. The improved stiffness of the fibers was attributed to the
crystalline region (cellulosic) of the fiber. The fiber also showed very good elongation
properties, with values increasing upon modifications. Lower elongation of the untreated fiber
may be due to the three dimensionally cross-linked networks of cellulose and lignin. Treatment
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broke this network structure giving the fiber higher elongation and lower strength properties.
Misra et al. [18] investigated the tensile properties of untreated, chemically modified and AN-
grafted sisal fibers. Chemically modified fibers showed an appreciable decrease in the tensile
properties. This decrease was attributed to the substantial delignification and degradation of
cellulosic chains during chemical treatment.
The tensile properties represented by tensile strength factor (Tf) and elongation factor (Ef) at
different UV intensities are graphically presented in Fig. 3a and b as a function of EMA
concentration. Tf and Ef are ratio of tensile strength and elongation at breaking point of grafted
and ungrafted virgin fibers. We observed that both Tf and Ef increases with UV radiation doses
and after attainment of maximum values the tensile properties decreases with increasing UV
intensities. This decrease of Tf and Ef at higher radiation dose could be caused due to the
degradation of polymer at higher UV doses [19]. The tensile property increases with monomer
concentration and after the maximum values Tf and Ef decreases with increasing EMA
concentration. This phenomenon can be explained by the same reason as described in polymer
loading section. The highest tensile strength (Tf = 1.5) is given by the sample treated with 50%
EMA and at 125th pass of UV followed by the sample grafted with 30% monomer and after 50
passes of UV radiation only. The lowest tensile strength (Tf = 1.06) which is almost similar to
that of virgin fiber is given by the coir fiber treated with 5% monomer and at 125 passes of
radiation.
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Fig. 3. Tensile properties of EMA treated coir fibers at different UV radiation doses as a function
of monomer concentration; (a) shows tensile strength factor and (b) shows elongation factor.
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The enhancement of elongation up to breaking point of coir fiber samples were expressed as
elongation factor (Ef) and is depicted in Fig. 3b against the doses of UV radiation with respect to
different EMA concentration. As usually the highest elongation (Ef = 1.39) is observed for the
sample treated with 50% monomer and after 125 passes of UV radiation and the lowest by the
sample treated with 5% monomeric solution. This case highest value after 125 passes is almost
similar to the virgin fiber (Ef = 1.02)
6. Effect of mercerization (alkali treatment) on coir fiber
Alkali treatment of cellulosic fibers, also called mercerization, is the usual method to produce
high quality fibers. Alkali treatment improves the fibermatrix adhesion due to the removal of
natural and artificial impurities from the fiber surface as well as it change the crystal structure of
the cellulose [18]. Moreover, alkali treatment reduces fiber diameter and thereby increases the
aspect ratio. Therefore, the development of a rough surface topography and enhancement in
aspect ratio offer better fibermatrix interface adhesion and an increase in mechanical properties
[17]. Alkali treatment increases surface roughness resulting in better mechanical interlocking andthe amount of cellulose exposed on the fiber surface. This increases the number of possible
reaction sites and allows better fiber wetting. The following reaction takes place as a result of
alkali treatment:
Fiber-OH+NaOHFiber-O-Na++H2O
Consequently, mercerization or more general alkali treatment had a lasting effect on the
mechanical behavior of coir fibers, especially on fiber strength and stiffness [4]. Several other
studies were conducted on alkali treatment [14], [18] and [20]. They reported that mercerization
led to the increase in the amount of amorphous cellulose at the expense of crystalline celluloseand the removal of hydrogen bonding in the network structure.
The coir fiber was mercerized by different alkali concentration (550%) and at different
temperatures ranges from 0 to 100 C. The weight loss and shrinkage was measured before it
was treated with EMA solution and was graphically presented in Fig. 4a and b. We observed that
at low temperature shrinkage is higher. But as the temperature is increased shrinkage become
insignificant. The highest shrinkage (5.88%) is observed for the sample treated with 20% alkali
and at 0 C. When the fiber is soaked in strong caustic solution (NaOH), different Na-cellulose
complexes are formed. These transformations do not change the cellulose chain length but takes
a large amount of NaOH and water in the crystal structure and is there by swollen. Thus, the
fiber becomes shorter. So, shrinkage is proportional to swelling. But swelling is the result of ion-
exchange process where cellulose acts as a weak acid. The overall process of ion-exchange-
complex formation-phase transformation involves heat of hydration and neutralization so the
process is exothermic. By basic thermodynamics, lowering the temperature should favor the
equilibrium in the positive direction. So, lowering the temperature should produce increased
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swelling and therefore increased shrinkage. The weight loss due to alkali treatment is increased
with increasing temperature up to a certain value and then decrease after attainment of maximum
value. The highest weight loss (12.65%) is obtained at temperature 25 C and for 20% alkali
solution. The coir fibers treated with 20% alkali solution at 25 C were thoroughly washed and
dried. After drying the fiber was grafted with 50% EMA solution and cured under UV radiation
of different intensities. The results of PL and tensile properties at this condition was compared
with out alkali treated grafted coir fiber. The results clearly showed that alkali treated fiber
showed increased PL and tensile strength and alkali treatment increases about 56%PL to the fiber
and 27% of tensile strength. The elongation at break is slightly lower than untreated fiber and the
reduction amount is negligible.
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Fig. 4. Effect of alkali treatment on shrinkage and weight losses of coir fibers at different alkali
(NaOH) concentration as a function of solution temperature; (a) shows percent shrinkage and (b)
shows percent weight loss at different alkali concentration.
7. Water absorption property
Water uptake of treated (EMA grafted and alkali treated followed by polymer grafted) and
untreated coir samples were monitored at 25 C in a static water bath at different time interval
(30 s60 min). We have observed that all the samples attained maximum water uptake within
initial 15 min and then soaking of water stops for treated sample while the untreated sample still
continues to soak water slowly. The untreated samples showed the highest water uptake of 61%
and the grafted sample yielded a value of 31% while the alkali treated fiber showed only 26% of
water absorption. The reduced water uptake by the treated samples is due to the fact that the
monomer reacts with the OH group of cellulose through graft co-polymerization reaction and
hence reduces the hydrophilic nature of the coir fiber and also polymer fills the void space of the
treated fiber. By replacing some of the hydroxyl groups on the cell wall polymers with bondedchemical groups, the hygroscopicity of the lignocellulosic material is reduced.
8. Fiber surface morphology (scanning electron microscopy)
Scanning electron microscopic analysis examined the surface topology of untreated and treated
fibers. The removal of surface impurities on plant fibers is advantageous for fibermatrix
adhesion as it facilitates both mechanical interlocking and the bonding reaction due to the
exposure of the hydroxyl groups to the chemicals used in treatment. Fig. 5 shows the SEM
images of coir fiber surfaces before and after alkali treatment as well as alkali treated followed
by polymer grafted in (a), (b) and in (c). A porous structure is observed for untreated fibers.These images indicate that after chemical treatment, the surfaces of the fibers became rougher
enhancing the mechanical interlocking with resins. It is observed that grafting with EMA gave
surface coating to the fibers, and surface features of fibers were not clearly visible. Since coir
fibers exhibited micropores on their surface, the monomer penetrated into the pores and formed a
mechanically interlocked coating on their surface. Smooth fiber surface is observed due to the
substances deposited on the surface of the fiber. The surface topography is entirely modified
after treatment with monomer followed by UV curing. Therefore, the modification by EMA
treated coir fibers develops into changes in fiber surface (as shown in Fig. 5c). Comparison of
Fig. 5b with Fig. 5c showed that in the intercellular gaps as well as on the surface of the unit
cells, grafted EMA has been deposited. Again, the surface of EMA grafted coir seems to be
uniform and smooth in comparison with alkali treated coir fiber. These changes will effectively
result in improved surface tension, wetting ability, swelling, adhesion and compatibility with
polymeric materials [21]. EMA grafting on to coir is targeted with a view to improve surface as
well as the bulk mechanical properties for its potential use as a reinforcing fiber for polymer
composites.
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Fig. 5. SEM images of untreated and treated coir fibers; (a) virgin coir fiber, (b) coir fiber treated
with 20% alkali solution and (c) coir fiber grafted with EMA.
9. Conclusion
Renewable fibers like coir can be used as reinforcing materials for low cost composites, due tothe economic and environmental advantages of such materials. However, coir fiber is hydrophilic
due to the presence of hydroxyl groups from cellulose and lignin. The results of the present study
show that a useful composite with good strength could be successfully developed using coir
fibers as a reinforcing agent for the polymethacrylate matrix. A significant increase in the
strength of the composites was observed after treatment of the fibers. UV pretreatment of the coir
showed an increase of tensile properties and this increase of tensile properties with increasing
radiation doses could be due to the inter-crosslinking between the neighboring cellulose
molecules occur under UV radiation. The best improvement was observed for the 20% alkali
treated followed by grafting with 50% EMA. Alkali treatment of coir fiber also reduces the
hydrophilicity of the fiber and significant increase of tensile properties of the grafted fiber wasobserved.
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Compos Part A: Appl Sci Manufact, 31 (2) (2000), p. 143Article | PDF (1161 K) | View Record in Scopus | Cited By in Scopus (92)
Corresponding author. Present address: Department of Applied Chemistry and Biochemistry, Kumamoto University,
2-39-1 Kurokami, Kumamoto 860-8555, Japan. Tel.: +880 2 8126522/81 96 342 3662; fax: +81 96 342 3662.
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