Composites: Part A 39 (2008) 1632–1637

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Composites: Part A
journal homepage: www.elsevier.com/locate/compositesa

Characterization of natural fiber surfaces and natural fiber composites

N. Sgriccia a,*, M.C. Hawley a, M. Misra b
a
Department of Chemical Engineering and Materials Science, Michigan State University, 2527 Engineering Building, East Lansing, MI 48824, USA
b
Composite Materials and Structures Center, Michigan State University, 2100 Engineering Building, East Lansing, MI 48824, USA

a r t i c l e i n f o a b s t r a c t

Article history: Experiments have been performed to further the development of natural fiber reinforced composites as a
Received 8 January 2007 replacement for glass fiber composites. Untreated and treated surfaces of natural fibers were character-
Received in revised form 30 June 2008 ized using FTIR, XPS, and ESEM. Changes in the peaks in the FTIR spectrum at 1730, 1625 and 1239 cm 1
Accepted 14 July 2008
indicated that the alkali treatment removes hemicellulose and lignin from natural fiber surfaces. ESEM
indicated the presence of silane on treated hemp and kenaf. XPS shows that hemp has a lower O/C ratio
than kenaf. Water absorption experiments were also conducted to determine saturation mass gain. Alkali
Keywords:
treated fiber composites absorbed more water than silane treated or untreated composites. The natural
A. Fibers
A. Polymer-matrix composites
fiber composites absorbed more water than the glass fiber composites. Hemp composites, in general, per-
D. Electron microscopy formed worse in flexural testing than kenaf composites.
E. Surface treatments Ó 2008 Elsevier Ltd. All rights reserved.

1. Introduction
Lignocellulosic natural fibers such as sisal, coir, jute, ramie,
pineapple leaf (PALF), and kenaf have the potential to be used
as a replacement for glass or other traditional reinforcement
materials in composites. These fibers have many properties
which make them an attractive alternative to traditional materi-
als. They have high specific properties such as stiffness [1], im-
pact resistance [2], flexibility [3], and modulus [4]. In addition,
they are available in large amounts [5], and are renewable and
biodegradable. Other desirable properties include low cost, low
density, less equipment abrasion [3,6], less skin and respiratory
irritation [7], vibration damping[1,2], and enhanced energy
recovery[7,8]. The hydrophilicity of natural fibers results in high
moisture absorption and weak adhesion to hydrophobic matrices.
The natural fibers can be treated to improve the adhesion to ma-
trix materials. Additionally, most natural fibers have low degra-
dation temperatures (200 °C), which make them incompatible
with thermosets that have high curing temperatures. This also re-
stricts natural fiber composites to relatively low temperature
applications. There are several other challenges presented by nat-
ural fibers such as large variability of mechanical properties [2,4],
lower ultimate strength [6], lower elongation [6], problems with
nozzle flow in injection molding machines [6], bubbles in the
product [6], and poor resistance to weathering [9]. Natural fibers
can be grouped into three categories; bast, seed and leaf. In this
study, three types of bast fibers (kenaf, flax and industrial hemp)
* Corresponding author. Tel.: +1 517 432 5488; fax: +1 517 432 1105.
E-mail address: sgricci1@msu.edu (N. Sgriccia).
and one kind of leaf fiber (henequen) were used. These fibers
were chosen because they are all grown in the United States.
US auto makers are interested in these fibers because they can
avoid the cost of transporting them from overseas. Fiber treat-
ments such as silane and alkali are required to increase the adhe-
sion between the hydrophilic natural fibers and the hydrophobic
epoxy matrix.
X-ray photoelectron spectroscopy (XPS) and Fourier transform
infrared spectroscopy (FTIR) has been used to study the surface
composition of treated and untreated natural fibers and their com-
posites. George at al. used XPS to examine bleached Kraft pulp and
thermomechanical pulp fibers [10]. They found that the bleached
fibers were more hydrophilic because they have a higher O/C ratio.
Zafeiropoulos et al. studied flax fibers treated with acetic anhy-
dride and steric acid and found that treating the fibers resulted
in an increase of carbon on the fiber surfaces [11]. Khan and Drzal
looked at modified and unmodified jute fiber with XPS [12]. XPS
showed that the 2-hydroxyethylmethacrylate bonded with the jute
fibers. The effect of the alkali treatment on hemp fibers was stud-
ied by Ouajai and Shanks [13]. It was found that pectin and hemi-
celluloses were removed by the treatment. Mwaikambo et al. used
FTIR to confirm that hemicellulose was removed by the alkali treat-
ment [14]. FTIR was used to confirm fiber/matrix bonding by Moh-
anty et al. [15]. Water absorption experiments are important for
natural fiber composites studies. Caulfield et al. found that maleic
anhydride decreased the amount of water absorbed in hemp and
sisal polypropylene composites [16]. Dash et al. studied jute/poly-
ester composites in outdoor weathering conditions and found that
bleached fiber composites absorbed less water than the untreated
fiber composites [17].

1359-835X/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesa.2008.07.007
 N. Sgriccia et al. / Composites: Part A 39 (2008) 1632–1637
Experiments were conducted to characterize the surfaces of
treated and untreated fibers and to investigate the absorption of
water in natural fiber composites. XPS and FTIR were used to deter-
mine the chemical composition of the fiber surfaces. ESEM images
were taken to show the effect of the silane. Water absorption tests
were used to determine the saturation point of natural fiber
composites.
2. Experimental
The natural fibers (kenaf, flax, industrial hemp supplied by Flax
Craft Inc. and henequen supplied by Dr. Pedro Herrera Franco from
Mexico) were soaked in hot distilled water for 1 h, dried for 48 h in
air at room temperature, and dried in the oven at 373.15 K for 3 h.
The 1/4 in. epoxy compatible chopped glass fibers were supplied
by Johns Manville (JM) Company and were used as such.
Diglycidyl ether of bisphenol-A (DGEBA), supplied by Adtech
Corp., cured with diaminodiphenyl sulfone (DDS), supplied by
TCI, was used to produce the epoxy. The DGEBA was mixed with
the DDS in the ratio of 2.79:1. Next 15% wt of fibers were mixed
into the epoxy. The mixture was degassed in a 373.15 K vacuum
oven for 20 min. The composites were cured in a convection oven.
The composites in these experiments had 15 wt% fiber loading.
Several grams of composite were placed in a silicone rubber mold.
The composites were cured in a 418.15 K oven for 2 h.
Fibers were treated using 5% solution of sodium hydroxide. The
fibers were submerged in the sodium hydroxide solution for 1 h at
room temperature, rinsed with tap water, and then neutralized in a
2% glacial acetic acid and tap water solution. The fibers were then
rinsed with deionized water and dried at room temperature for
24 h.
Fibers were treated using a 1% solution of 3-glycidoxypropyltri-
methoxysilane (Z-6040 from DOW Corning) in deionized water
and ethanol in a 1:1 ratio. The pH of this solution was adjusted
to 4 using 2% glacial acetic acid. The solution was stirred for 2 h be-
fore the fibers were added. The fibers were washed with deionized
water after the silane treatment. The fibers were then dried for
12 h in air and then cured in a convection oven for 5 h.
The samples were observed in Philips ElectroScan 2020 ESEM.
The sample chamber pressure was reduced to approximately
586.6 Pa. The working distance ranged from 6–9 mm. ESEM is used
to examine the morphology of the fibers and the composites.
The fibers were tested with FTIR using a Perkin Elmer Instru-
ments Spectrum One with the Attenuated Total Reflectance (ATR)
technique.
XPS was performed with Physical Electronics PHI 5400 ESCA
system, with a non-monochromatic Mg source operating at
Fig. 1. Spectrum of treated and untreated hemp fibers.
1633
300 W. The spot size of the analyzer was 250 lm2 and the operat-
ing pressure was approximately 3.386  10 4 Pa. The samples
were mounted onto a stainless steel stub using a Mo mask. The
take off angle was 45 deg.
Composites with dimensions 25.4 mm  38.1 mm  3 mm
were immersed in distilled water. Before taking weight measure-
ments, the composite surfaces were blotted with paper towels to
remove surface water. Measurements were taken at 6, 24, 48, 72,
and 144 h for untreated samples. The weight was then measured
weekly until the composites were saturated. The treated samples
were weighed at 5, 24, 48, 120, and 168 h and thereafter weighed
weekly until saturated.
Kenaf and hemp fibers were prepared with three different fiber
treatments; alkali, silane, and alkali and silane. The untreated and
treated fibers were analyzed using ESEM, FTIR, and XPS. Water
absorption experiments were also performed on untreated and
treated fiber composites. Only hemp and kenaf were selected to
be treated with alkali and silane based on previous experiments
on natural fiber composites [18]. Hemp and kenaf showed im-
proved curing times with microwaves. Also hemp reached a great-
er extent of cure with microwave curing than with convection
oven curing and had a relatively high degradation temperature
compared to the other natural fibers. Kenaf was more compatible
with the epoxy matrix materials.
For flexural testing, a support span to depth ratio of 16:1 was
used in accordance with the ASTM D 790-03 standard. The com-
posite is bent until it breaks or 5% strain is reached. The crosshead
speed used was 0.5 in/min, the span was 2.1 in and the loadcell
used was 1000 lb.
3. Results and discussion
The FTIR peaks are baseline corrected to 3323 cm 1 (see Figs. 1
and 2). The CH stretch at 2900 cm 1 is present in all fibers. The car-
bonyl peak at 1730 cm 1 can be seen in all the fibers not treated
with alkali. The lignin peak (1500 cm 1) is present in kenaf fibers
but not present in any hemp fibers. COOH bending peaks
(664 cm 1) are present in all fibers. CH2 symmetric bending peaks
at 1432 cm 1 are also present. The peak at 1625 cm 1 in hemp is
present in the non-alkalized fibers only. In the kenaf, and silane
treated kenaf fibers the peak at 1239 cm 1 is much larger than
the peak in the alkali treated samples.
The effects of fiber treatment on the natural fiber surfaces were
also studied using FTIR. The peak 1730 cm 1 is attributed to the
C@O stretching of the acetyl groups of hemicellulose [19,20]. This
peak is not present in the alkali treated samples. The removal of
hemicellulose from the fiber surfaces causes this peak to disappear
1634 N. Sgriccia et al. / Composites: Part A 39 (2008) 1632–1637

Fig. 2. Spectrum of treated and untreated kenaf fibers.

[20]. The peak at 1239 cm 1 in the kenaf fibers is much smaller for
alkali treated samples. This peak is a CAO stretch of the acetyl
group of lignin and is reduced because lignin is partially removed
from the fiber surface [20]. The peak at 1625 cm 1 is reduced in
hemp alkali treated fibers and removed in kenaf alkali treated fi-
bers. This peak represents the C@O bonds on hemicellulose and
is further evidence that hemicellulose is removed from fiber sur-
faces by the alkali treatment [14]. FTIR does not show the presence
of silane on the fibers. Peaks should be present at 766 and
847 cm 1 [12]. It is possible that the concentration of silane on
the fiber surfaces is too small to detect by FTIR.
The ESEM images show that the interfibrillar material, hemicel-
lulose and lignin, is etched away by the alkali treatment (Fig. 3).
Electron microscopy also indicates the fibers are coated with silane
(Fig. 4).
Hemp is more hydrophobic than kenaf indicated by lower O/C
ratio (see Table 1) [21]. As shown in the following water absorption
data, kenaf composites absorb more water in the short run than
hemp. O/C ratios of untreated fibers are lower than the 0.83 of cel-
lulose, hemicellulose, and pectin. C1s (284 eV) and O1s (530 eV)
are present in all fibers. Ca, Si and Al are also present in small
quantities.
XPS spectra were obtained for treated and untreated natural
and glass fibers. The spectra for all fibers contained carbon and
oxygen, while nitrogen, calcium, silicon and aluminum were de-
tected in some samples. Cellulose, hemicellulose and pectin have
an O/C ratio of 0.83 while lignin has a ratio of 0.35. Since the O/C
of treated and untreated fibers is less than 0.83 the surface must
have a greater proportion of lignin and waxes [11,22].
Untreated henequen composites absorbed the most water (see
Figs. 5 and 6). There were 10 samples tested per data point and
the error bars represent the standard deviation. Glass composites
absorbed the least amount of water. Henequen composites ab-
sorbed water most quickly followed by kenaf, hemp and flax, and
glass composites in the short run. Long term, flax, kenaf and hemp
have the same absorption rate. Henequen, flax, kenaf, and hemp
composites reached saturation at 816 h while glass composites
reached saturation at 648 h (see Fig. 7).
The alkali treated kenaf and hemp composites absorb more
water than the silane only or alkali and silane treated samples.
The alkali and silane treated composites absorbed the least amount
of water. Kenaf composites absorbed less water overall than their
hemp counterparts. The silane treated, alkali and silane treated,
and untreated composites had similar water absorption profiles.
Water absorption experiments were conducted because the
absorption of water can cause changes in the shape, debonding,
or loss of strength in products regularly exposed to moisture
[22]. These experiments show that the untreated and treated nat-
ural fiber composites absorb significantly more water than the
glass fiber composites. This was expected as natural fiber compos-

Fig. 3. Left: hemp. Right alkali treated hemp. Magnification 300, scale bar 150 lm.
 N. Sgriccia et al. / Composites: Part A 39 (2008) 1632–1637 1635

on silane treated glass fiber composites (25 wt%) and obtained a

Fig. 4. Alkali and silane treated hemp. Magnification 300, scale bar 150 lm.
ites absorb water in the fibers and matrix and water also exists in
the voids of the composite. While in glass fiber composites, water
is not absorbed into the fibers. Olmos et al. conducted experiments
saturation mass gain of 4.21–5.22% depending on the treatment
[23]. The untreated fibers in our experiments had 4.6% mass gain.
The rate of water absorption in our samples is consistent with
those in the treated fiber experiments. Williams and Wool tested
composites made using plant oil based resins and flax fibers
(30 wt%) [24]. The saturation weight for these composites ranged
from 10.4% to 12.4%. Tserki et al. made 30 wt% flax and polyester
composites with a saturation mass gain of approximately 6.5%
[22]. Our flax fiber and epoxy composites had a saturation mass
gain of 17.2%. Tserki et al. made 30 wt% hemp polyester composites
with a saturation mass gain of 6% [22]. The hemp epoxy samples
in our experiments reached 18.4% mass gain. Tajvidi et al. con-
ducted experiments on 25 wt% kenaf polypropylene composites
which had a saturation mass gain of around 2% [25]. The kenaf
epoxy samples in our experiments reached 17.8% mass gain at sat-
uration. Differences between our results and literature results can
be attributed to different fiber loading and matrix composition and
possibly due to voids present in our composite samples. In Figs. 5
and 6, it can be seen that the alkali treated composites absorb more
water than the untreated or silane treated composites. Fibers are
treated with NaOH to remove lignin, pectin, waxy substances,
and natural oils covering the surface of the fiber cell wall. This
makes the surface of the fiber rough by revealing the fibrils [14].
This change in fiber morphology may create more voids for water
to absorb into.
Flexural tests were performed to determine the flexural modu-
lus of the composites for comparison with glass fiber composites.
Trends in hemp fiber reinforced composite flexural modulus are

Table 1
Atomic concentration tables for treated and untreated fibers

Hemp Silane treated Alkali treated Silane/alkali Kenaf Silane treated Alkali treated Silane/alkali Flax Henequen Glass
hemp hemp treated hemp kenaf kenaf treated kenaf
C (1s) 76.79 71.75 83.13 78.49 62.34 63.67 64.83 49.89 83.88 78.27 63.84
N (1s) 2.19 3.45 1.84 2.81 2.68 3.65 2.1 2.13 1.87 3.58
O (1s) 20.48 23.03 14.44 18.15 27.96 27.68 27.9 40.38 16.12 19.55 24.28
Ca (2p) 0.53 0.61 0.26 0.18 0.51 0.31 0.75
Si (2p) 1.16 0.59 0.28 4.26 2.84 3.33 7.09 7.55
Al (2p) 2.76 2.15 1.65
O/C 0.27 0.32 0.17 0.23 0.45 0.43 0.43 0.81 0.19 0.25 0.38

Fig. 5. Water absorption of natural and glass fiber composites (untreated).

1636 N. Sgriccia et al. / Composites: Part A 39 (2008) 1632–1637

walls. Lignin is a cementing agent that holds fiber ultimates to-

gether in bundles. The kenaf stalk also contains a greater percent-
age of bast fibers (40%) than the hemp stalk (25%) [27]. The single
fiber tensile strength of kenaf is 11.9 GPa while hemp is 9.0 [26].
Several peaks are present in kenaf that are not present in hemp.
The peak at 1590 cm 1 represents an aromatic bond present in lig-
nin [28]. The peak at 1501 cm 1 is an aromatic CAH bond also
found in lignin [22,29]. The peak present at 1450 cm 1 represents
an asymmetrical CAH deformation of cellulose and lignin rings
[28]. In addition, a peak present in hemp is not present in kenaf.
At 2849 cm 1 is a CH2 symmetric stretching bond present in waxes
[28]. The peak present at 2915 cm 1, CAH vibration in lignin and
waxes, has a greater relative intensity in hemp than kenaf. These
peaks indicate that hemp has more wax on the fiber surface than
kenaf. Also that kenaf has more surface cellulose and lignin than
hemp. The removal of wax increases adhesion between fibers
Fig. 6. Water absorption of natural and glass fiber composites (treated). and matrix materials [30,14]. Increasing lignin and cellulose on
the kenaf fiber surfaces provides more hydroxyl groups that can re-
act with the epoxide groups in the epoxy resin. This may account
not similar to the kenaf reinforced composites. Oven cured and for hemp’s poor performance in mechanical testing and kenaf’s rel-
microwave cured kenaf have similar flexural modulus, showing atively good performance.
both cure methods are equally viable curing methods. However Fiber storage is also a concern. Once the fibers were received by
microwave processing is superior due to the energy savings com- the university, the storage conditions (temperature and humidity)
pared to conventional ovens. Composites require 60–65 W to cure for the hemp and kenaf fibers were the same. However, prior to ar-
in the microwave where oven cured composites require 1600 W. rival at the university, the storage conditions were unknown. Stor-
However, up to 12 sets of samples can potentially be cured simul- age in high temperature and high humidity environments would
taneously in the oven so the more conservative estimate is be detrimental to fiber properties.
0.12 kW-h for microwave cure vs. 0.26 kW-h for oven curing (for
one sample). This is still a considerable energy savings. With
microwave processing, the composites reach the cure temperature 4. Conclusions
in approximately 20 min. Oven processing required approximately
95 min. Experiments were conducted to characterize the surfaces of
The properties of natural fibers depend on the source, nature, treated and untreated fibers and to investigate water absorption
and storage of fibers. This in turn affects the mechanical properties in natural fiber composites. Natural fiber composites absorb
of the composites. The hemp used in this study was grown in Can- more water than glass fiber composites. Alkali treatment re-
ada and the kenaf was grown in the United States. The age of the moves lignin and hemicellulose from the surface of natural fi-
plant, the fiber’s location on the plant, and the method used to ex- bers. ESEM indicated that the silane treatment coated the
tract the fiber from the plant can also affect the fiber properties fibers. Glass fiber composites had a greater flexural modulus
[26]. Kenaf and hemp have significantly different cellulose and lig- than untreated and treated most natural fiber composites with
nin content. Kenaf has 31–39% cellulose and 15–19% lignin while the exception of silane treated kenaf. Trends in hemp and kenaf
hemp has 70.2–74.4% cellulose and 3.7–5.7 % lignin [8]. Cellulose treated composites are dissimilar. Kenaf generally performed bet-
forms the main structural component of the natural fiber’s cell ter in mechanical testing than hemp.

7
Flexural Modulus(Gpa)

6
5
4

3
2
1
0
kenafoven

kenaf silane oven

kenafalkali silane oven

kenafalkali oven

kenafmw

kenaf silane mw

kenafalkali silane mw

kenafalkali mw

hemp oven

hemp silane oven

hemp alkali silane oven

hemp alkali oven

hemp mw

hemp silane mw

hemp alkali silane mw

hemp alkali mw

glass oven

glass mw

Fig. 7. Flexural modulus for treated and untreated composites.

 N. Sgriccia et al. / Composites: Part A 39 (2008) 1632–1637
Acknowledgements
This work was supported by the National Science Foundation
(DMI – 0200346). Biofibers from Flaxcraft Inc., Cresskill, NJ, Hem-
pline, Ontario, Canada and Dr. Pedro, Mexico, as well as glass fiber
samples from Johns Manville are gratefully acknowledged. The
authors would like to thank Per Askeland for running the XPS
experiments and Christopher Bunke for starting the water absorp-
tion experiments.
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