Available online at ScienceDirect

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J. Mater. Sci. Technol., 2014, -(-), 1e7

Properties of Xanthoceras sorbifolia Husk Fibers With Chemical

Treatment for Applications in Polymer Composites
Hongyu Wang1), Xudan Yao1), Guoxin Sui1)*, Liming Yin2), Lihua Wang2)
1) Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
2) Shenyang Institute of Applied Ecology, Chinese Academy of Sciences, Shenyang 110016, China
[Manuscript received October 29, 2013, in revised form March 6, 2014, Available online xxx]

Surface science of natural fibers plays an important role in polymer/natural fiber composites. The Xanthoceras
sorbifolia husk fibers were selected and chemically treated by sodium hydroxide (NaOH) solution, coupling
agents, their combination, and the mixtures of acetic acid with hydrogen peroxide, respectively. 3-
aminopropyltriethoxysilane (KH550), g-methacryloxypropyltrimethoxylsilane (KH570) and organic titanate
(JN-9A) were used as coupling agents in this work. Cellulose content was found to be increased after
alkalization due to the removal of the non-cellulose substances, which was evidenced by attenuated total
reflectanceeFourier transform infrared (ATReFTIR) spectroscopy spectrum analysis and thermogravimetric
analysis (TGA) measurements. The highest cellulose content was obtained in the bleached fibers. TGA
analysis revealed an improvement in thermal stability of the treated fibers, especially for alkali-KH570 treated
fibers. The tensile strength of the alkali-KH570 treated fiber and the alkali-bleached fiber were higher than
that of other fibers due to high cellulose content and high crystallinity.

KEY WORDS: Xanthoceras sorbifolia husk fibers; Chemical treatment; Thermal property; Tensile strength

1. Introduction Xanthoceras sorbifolia (Fig. 1) belongs to the Sapindaceae

In the past decade, a number of researchers have focused on
exploring natural fibers as reinforcements in polymer composite
materials. The natural fiber is regarded as an alternative of the
synthetic fiber in reinforced plastics. It could ease the shortage of
non-renewable resources, reduce the usage of plastic, improve its
recycling levels, expand the application of the natural fibers, and
increase the added value of agricultural products. Natural fibers
are currently considered as an alternative to synthetic fibers due
to their good thermal stability, non-corrosive nature, low density,
low cost, less abrasion to processing equipment, renewability
and biodegradability[1,2]. Some of the efforts have been made on
the use of new waste sources such as corn straw, soy stalk and
wheat straw[3], aiming at obtaining biologically active com-
pounds which can be applied in different fields and applica-
tions[4]. A number of manufacturing industries such as
automotive, packaging or construction have shown great in-
terests in developing new bio-composite materials[5e7].
*
Corresponding author. Prof., Ph.D.; Tel./Fax: þ86 24 83978040; E-
mail address: gxsui@imr.ac.cn (G. Sui).
1005-0302/$ e see front matter Copyright Ó 2014, The editorial office of
Journal of Materials Science & Technology. Published by Elsevier
Limited. All rights reserved.
http://dx.doi.org/10.1016/j.jmst.2014.07.004
family, and is an important oil plant in China because of the
abundant oil content (55%e65%) in the seed kernels[8,9] and
oil’s richness (85%e93%) in unsaturated fatty acids[9]. Recently,
biodiesel made from X. sorbifolia are getting more and more
attentions. However, abundant residues of the fruit husk have not
been used yet. The exploitation of the husks for industrial ap-
plications will no doubt widen the full use of the natural waste
resources to increase added values, and therefore to reduce the
cost of biological diesel oil, and finally to promote the sustain-
able development of the biological energy industry.
The main components of the X. sorbifolia husk are cellulose,
lignin, hemicellulose and so on. It is meaningful to adopt the X.
sorbifolia husk fibers as fillers in the plastics. On the one hand,
the cost of the biological diesel oil made from the X. sorbifolia
could be reduced because the residues were exploited; on the
other hand, filling the X. sorbifolia husk fibers into plastics
contributes saving of the plastics. The new composite are more
environmental friendly and have the immense potential appli-
cation prospect. Due to the low processing temperature of the
natural fibers, the most commonly used thermoplastic matrices
are polypropylene, polyethylene and poly vinyl chloride[2].
The inherent polar and hydrophilic nature of natural fibers and
the non-polar character of most thermoplastics result in com-
pounding difficulties, and cause non-uniform dispersion of fibers
within the matrix[6]. Fiber-matrix interfacial adhesion could be

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2 H. Wang et al.: J. Mater. Sci. Technol., 2014, -(-), 1e7

improved with several chemical modifications such as alkaliza-

tion, acetylation, adding compatibilizer or coupling agent. The
researchers have done lots of work to improve the properties of
the natural fiber reinforced polymer composites. In the research
of Sawpan et al.[10], different modifications containing alkali-
zation, silane treatment, maleic anhydride treatment and acety-
lation have been compared with the raw material to investigate
the difference in mechanical properties of the composites. The
alkali treated agro-residue reinforced polymer composites proved
an enhancement in the properties of the composites[3]. The most
common alkalization was still processed in the research of Aziz
and Ansell[11]. The effects of acetylation on the surface of flax
fiber[12], coconut fiber[13] have also been reported in recent years.
Besides that, the effects of maleic anhydride grafted poly-
Fig. 1 Tree of Xanthoceras sorbifolia.
propylene[14], lignin[15], and different coupling agents[16] were
also studied by many researchers. mixtures of deionized water and ethanol at the ratio of 1:1, 1:1
In this work, several surface modifications such as alkaliza- and 0:1, respectively, as the JN-9A is insoluble in water. The
tion, coupling agents and their combination were carried out on concentration of the coupling agent was 3% of the fiber weight.
the X. sorbifolia husk fibers. Bleaching process was also applied The weight of the solution was 20 times as that of the fibers. The
on the fibers after alkalization treatment. The influences of pH value of the solution was adjusted to 3.5e4.5 with acetic
modifications on the properties of the fiber were investigated. acid. After static laying for about 5e10 min, the fibers were
The fiber without any treatments was prepared for comparison. soaked in the solution for about 30 min. The soaked fibers were
The variation of components in the alkali and alkali-bleached put in the oven at 65  C for 12 h, then washed with water until
fibers were tested in this study. The attenuated total reflec- pH ¼ 7, finally dried at 80  C for 48 h. A combination of
tanceeFourier transform infrared (ATReFTIR) spectroscopy alkalization followed by coupling agent treatment was also
was aimed at testing the changes of the functional groups on the applied to the fibers. In addition, a bleaching treatment was also
surfaces of the modified fibers. Thermal property and decom- done. The hydrogen peroxide (30%) and acetic acid (pure) were
position temperature of the components of the fibers were mixed together with the volume ratio 1:1. The alkali treated fi-
analyzed by thermogravimetric analysis/derivative thermal bers were then soaked in the solution at 60  C until the solution
gravimetry (TGA/DTG) measurement. The morphologies of the became transparent. The bleached fibers were washed with water
fiber surfaces were analyzed by scanning electron microscopy several times until the pH ¼ 7.
(SEM). The tensile strength of the fibers was tested at last.
2.3. Characterization
2. Experimental
The components of the untreated, alkalized, and alkali-
2.1. Materials bleached X. sorbifolia husk fiber were tested according to the
GB/T-5889-1986.
The fibers were obtained by smashing the X. sorbifolia husks. TGA were conducted with an SETSYS evolution18 integra-
The smashed fibers were sieved to the size of 16e32 meshes tive analyzer under nitrogen atmosphere. The mass of each
(about 0.6e1.18 mm), then the raw fibers were obtained. Sodium sample was around 10e16 mg. The curves were recorded in the
hydroxide, the 3-aminopropyltriethoxysilane, g-methacrylox- course of heating from ambient temperature up to 500  C at a
ypropyltrimethoxylsilane (KH570), organic titanate (JN-9A), rate of 5  C/min.
acetic acid and hydrogen peroxide were all purchased from The spectra of ATReFTIR (NEGOLET560) were recorded in
Sinopharm Chemical Reagent Co., Ltd. a range of 4000e600 cme1 at a resolution of 4 cme1 with 100
scans.
The different treated surfaces of X. sorbifolia husk fibers were
2.2. Chemical surface treatment
coated with a thin layer of gold and then examined by using a
JSM-6301F scanning electron microscope.
Before the chemical surface treatment, the untreated fibers
were rinsed with water at the room temperature to remove the
dirt and impurity on the surface. Then the fibers were dried in the
oven at 80  C for 48 h.
Alkalization was considered as the pretreatment. The fibers
were immersed in 5 wt% sodium hydroxide solution at ambient
temperature according to a solution/fiber ratio of 20:1 (by
weight). A continuously stirring for 60 min was carried on in
order to make sure the adequate treatment of the soaked fibers.
After treatment, the fibers were rinsed with water for several
times to remove the traces of alkali on the fiber surface and
subsequently neutralized with 1 wt% acetic acid solution. The
treated fibers were then dried in the oven at 80  C for 48 h.
KH550, KH570 and JN-9A titanate were chosen as the
coupling agent. The coupling agent solution was dissolved in the
Fig. 2 Seed and husk of Xanthoceras sorbifolia.

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 H. Wang et al.: J. Mater. Sci. Technol., 2014,
The X. sorbifolia husk fibers were separated from the shell
manually. The fibers were fixed onto the coordinate paper with
glue. The middle of the paper would be cut to make the fiber bear
the tensile load. Tensile testing of the fibers was carried out at a
cross-head speed of 0.5 mm/min using a 10 N load cell. The
gage length was 10 mm. The fibers were assumed to have a
cylindrical shape. Fiber diameters were measured in the gauge
range for up to 40 times for each single fiber. The final fiber
diameter was determined by particle size distribution statistics
calculation software 1.2.
3. Results and Discussion
3.1. Components
The X. sorbifolia husk is in oval shape, as seen in Fig. 2. The
structure of the cross section of the X. sorbifolia husk can be
divided into three parts. As shown in Fig. 3, the outside layer is
compact, and its color would turn from green to brown with the
time going by. The short fibers of the husk mainly distribute in
the mesosphere. The short fibers are perpendicular to the outside
surface, and many substances with loose structure distribute
among those fibers. The long fiber distribute in the internal
surface in a net form.
The appearances of the husk fibers change after the modifi-
cations, as shown in Fig. 4. It can be seen that the color of the
fibers are different. The color of the alkalized fiber is darker than
those of the others. The components of the fibers are also
changed by the modifications, by the alkalization and alkali-
bleached treatment, and the fiber properties will change
accordingly. Consequently, the alkalized and alkali-bleached X.
sorbifolia husk fibers were tested. The untreated fibers are for
comparison.
It can be seen from Table 1 that the content of cellulose in-
creases after alkalization, and high content of cellulose could be
found in the alkali-bleached husk fibers. While other components
of treated fiber such as wax, pectin, hydrotropic substances are
less than that of the untreated one. The hemicellulose decreases
after alkalization and this trend is shown obviously in the alkali-
bleached fiber. The lignin shows the similar trend to the hemi-
cellulose. The increase of the cellulose is beneficial to improving
mechanical property.
3.2. ATReFTIR spectroscopy
The ATReFTIR spectrum of the untreated fibers is shown in
Fig. 5. With reference to literature[4,10] the assignments of the
peaks in the ATReFTIR spectra is listed in Table 2. The strong
peak at 3317 cme1 is characteristic of the hydrogen bonded
hydroxyl group (eOH) stretching vibration. The peak at
2918 cme1 is considered due to CeH asymmetric and symmetric
stretching vibration in methyl and methylene group of all hy-
drocarbon constituents of the fiber. The peaks at 2385 cme1 and
2310 cme1 were observed. The appearance of these two peaks is
due to PeH stretching and PeOeH stretching. The peak at
1730 cme1 is also assigned to the C]O stretching in acetyl and
uronic ester groups or in carboxylic group of hemicellulose or to
the ester linkage of carboxylic group of the ferulic and p-cou-
maric acids of lignin[4,17]. The peak at 1600 cme1 is related to
the absorbed water. The peak appearing at 1508 cme1 is due to
CH2 stretching from cellulose. The peak at 1236 cme1 is
considered due to C]O stretching of acetyl in lignin. The peak
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-(-), 1e7 3
Fig. 3 Cross sectional view of the structure of the Xanthoceras sorbi-
folia husk.
at 1072 cme1 is assigned to CeO deformation in secondary
alcohol and aliphatic ether.
ATReFTIR spectra of alkali treated and alkali-bleached fibers
are also shown in Fig. 5. The peaks at 1515 cme1 and 1240 cme1
seen in untreated fibers disappear after alkalization. The disap-
pearance of the peak at 1515 cme1 indicates that the non-
cellulose such as pectin, and fats are removed during the alka-
lization. This conclusion was also confirmed by other re-
searchers[10,18,19]. The disappearance of the peak around
1240 cme1 after alkalization indicated that the removal of
hemicelluloses was easier than that of the lignin[17,18]. And the
peak at 1639 cme1 appears due to C]O stretching.
The spectra of KH550 treated fiber is shown in Fig. 6. The
peak at 1639 cme1 appears due to C]O stretching. The peak at
1454 cme1 is assigned to SieC6H5 stretching. According to the
characteristic infrared bands of silicon compounds[10,18], the
peaks at 821 cme1 and 765 cme1 appeared due to SieOeSi
asymmetric stretching and SieOeC stretching. Those charac-
teristic peaks confirm the reaction between 3-amino-
propyltriethoxy silane coupling agent and the natural fibers. The
spectra of KH570 treated fiber is similar to the one of untreated
fiber, except that the characteristic peaks at 821 cme1 and
765 cme1 are assigned to SieOeSi asymmetric stretching and
SieOeC stretching, while those peaks appearing in the spectra
of alkali-JN-9A treated fibers are due to CeOeH stretching.
The spectra of alkali-KH550, alkali-KH570 and alkali-JN-9A
treated fibers are shown in Fig. 7. The peaks at 1639 cme1 and
2355 cme1 appear in the spectra of alkali-KH550 treated fibers.
While the peak at 1240 cme1 disappears. The peak at 2355 cme1
appears due to SieH stretching. The peaks at 1639, 821 and
765 cme1 appear in the spectra of alkali-KH570 and alkali-JN-
9A treated fibers. The difference is that the peak at 1240 cme1
appears in the latter. ATReFTIR spectra of treated fibers illus-
trate that those chemical modifications are successfully carried
on the surface of X. sorbifolia husk fibers.
3.3. TGA/DTG
The mass change of the samples with increasing temperature
can be measured by using TGA technique[20]. Thermal degra-
dation of lignocelluloses starts by hemicellulose decomposition
between 200 and 260  C, followed by cellulose decomposition
between 240 and 350  C and lignin, from 280 to 500  C[21]. The
curves of the weight loss with increasing temperature of X.
sorbifolia husk fibers are obtained by TGA/DTG, as shown in
Fig. 8. The curve of the DTG could be divided into three stages.
4 H. Wang et al.: J. Mater. Sci. Technol., 2014, -(-), 1e7

Fig. 4 Photos of the untreated (a), alkalized (b), coupling agent (KH570) treated (c), alkali-coupling agent (KH570) treated (d) and alkali-bleached (e)
fibers.

Table 1 Composition of different treated fibers

Components Cellulose Lignin Hemicellulose Wax Pectin Hydrotrope

Untreated (%) 25.7 31.2 25.2 3.4 4.8 9.7

Alkali (%) 46.8 26.8 19.0 1.4 3.8 2.2
Alkali-bleached (%) 63.8 11.0 14.6 0.1 6.4 4.1

The first is from the initial decomposition temperature to 230  C, the first region, the weight loss was caused by the decomposition
the second is from 230 to 290  C and the last is from 290 to of hemicellulose. The weight loss of treated fibers in the first
500  C. In Fig. 8(a), it can be seen that the initial decomposition region was much lower than that of the untreated fibers due to
temperature of the untreated fiber is 163  C. The weight loss is less content of hemicellulose. The weight loss in the second
about 4.5 wt% in the first region, about 15.1 wt% in the second, region and in the last region was due to the decomposition of the
and about 48.3 wt% in the last region. It is seen in Fig. 8(b) that lignin and the cellulose, respectively.
the initial decomposition temperature for the alkali treated fiber It can be found obviously that the DTG curves show a plat-
is 190  C. The weight loss is about 0.98 wt% in the first region, form around 230e260  C for untreated and coupling agent
about 13.2 wt% in the second, and about 52.9 wt% at last. treated fibers, but not for the fibers treated by alkalization. The
As seen in Fig. 8(c), the KH550 treated fiber is decomposed at main reason for this result was that most of the non-cellulose
172  C. The weight loss is about 2.4 wt% in the first region, about substances such as hemicellulose, fats, impurities and pectin
15.7 wt% in the second, and about 48.5 wt% in the last. The initial were removed during the alkali treatment. This point can be
decomposition temperature for the KH570 treated fiber (Fig. 8(d)) confirmed by the ATReFTIR spectra of chemical treated fibers
is 186  C. The weight loss is about 3.6 wt% in the first region, shown in Fig. 3.
about 18.9 wt% in the second, and about 46.3 wt% in the last. The
initial decomposition temperature of the JN-9N treated fiber
(Fig. 8(e)) is 176  C. The weight loss is about 1.4 wt% in the first
region, about 13.7 wt% in the second, and about 59.0 wt% in the
last.
As shown in Fig. 8(feh), the alkali-KH550, alkali-KH570 and
alkali-JN-9A treated fiber are decomposed at 182, 203 and 176  C,
respectively. The weight loss is about 2.3, 1.1 and 0.8 wt% from the
initial decomposition temperature to 230  C, about 10.7, 11.3 and
12.0 wt% from 230 to 290  C, and about 48.7, 55.2 and 50.3 wt%
from 290 to 500  C, respectively.
Fig. 8(i) shows the TGA/DTG curve of the alkali-bleached
fiber. And the initial decomposition temperature is 182  C.
The weight loss is about 0.8% in the first stage, about 11.7% in
the second, and about 50.3% from 290 to 500  C.
According to the above analysis, it could be concluded that
treated fiber showed higher thermal stability than untreated fiber. Fig. 5 ATReFTIR spectra of untreated, alkali treated, alkali-bleached
The similar results were also reported by other researcher[22]. In fibers.

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 H. Wang et al.: J. Mater. Sci. Technol., 2014, -(-), 1e7 5

Table 2 Assignments of selected bands for ATReFTIR spectra from the Xanthoceras sorbifolia husk fibers
1
Peak location (cm ) Assignment

3317 OeH stretching

2918 CeH asymmetric and symmetric stretching in methyl and methylene group
2385 PeH stretching and PeOeH stretching
1730 C]O stretching in acetyl and uronic ester groups or in carboxylic group of ferulic and coumaric acids
1600 NeH bending in primary amine or absorb water
1508 Benzene ring, pyridine ring stretching, CH2 from cellulose
1236 SieCH2 stretching in alkane or C]C plus C]O plus CeO stretching
1033 CeO deformation in secondary alcohol and aliphatic ether or aromatic CeH in plan deformation plus CeO deformation
in primary alcohol

3.4. Morphology of the treated fibers
The SEM surface micrographs of treated and untreated X.
sorbifolia husk fibers are shown in Fig. 9. As shown in Fig. 9(a),
the surface of the untreated fiber is covered with a layer of
substances which may include pectin, wax, lignin and other
impurities. After alkali treatment, this layer of substances on the
fiber surface is removed, as seen in Fig. 9(b). This phenomenon
has also been reported by other researchers[10,18,19]. Besides that,
the fiber surface roughness increases too, which provides more
sites for the mechanical interlocking during compounding with
the plastics. The surface of KH550 treated fibers is shown in
Fig. 9(c). The shape of the cellulose is spiral vessel, and some of
them are not continuous. The surface looks rougher than the
untreated fiber. This is because the cellulose flakes away due to
lacking of the fixation from the outside layer. The wrinkle
appearing on the surface of the KH570 treated fiber is regarded
as the characteristic phenomenon of coupling agent treatment
(Fig. 9(d)). The structure of the fiber appears loose after the JN-
9A treatment, as shown in Fig. 9(e). On the micrographs of the
double-treated fibers, the surfaces were observed as rough as that
of the alkalized fiber, as shown in Fig. 9(fei). Among them, the
structure of the alkali-bleached fiber is more compact than that of
others.
3.5. Tensile properties
As shown in Table 3 and Fig. 10, compared with the untreated
fiber, the tensile strength of the alkalized, KH550 treated, and
KH570 treated fibers is increased by 24%, 17.2%, and only
about 6.4%, respectively. However, the tensile strength of the
JN-9A treated fiber is reduced by 25.6%. Considering the
double-treated fiber (Table 4), the tensile strength of the alkali-
KH550 treated, alkali-KH570 treated, alkali-JN-9A treated and
alkali-bleached fiber is increased by 19.4%, 42.4%, 14.9%, and
33.4%, respectively.
It can be seen from the fiber composition analysis that the
cellulose content of the alkalized fiber is increased. The ATRe
FTTR and TGA analysis results also show that the fiber com-
ponents, such as wax and hemicellulose, which are harmful to
the tensile properties of the fiber, are decreased after alkalization.
The relative increase of the cellulose content in the alkalized
fibers leads to an increase in tensile properties of the fibers. The
effect of the coupling agent on the tensile property is limited or
even worse. This is because the organic coupling agent has
different contributions to the crystallization of the fiber, which
has a direct impact on the level of the tensile property of the
fibers. Cellulose was covered with the substances such as wax
and hemicellulose, and then the effect of the coupling agent on
the crystallization of fiber is limited.
However, after alkalization the covered substances on the fiber
surface such as the hemicellulose and the wax were decreased or
removed, which helped the coupling agent to promote the
crystallization of the fiber. It could be seen from the data analysis
that the tensile strength of the alkali-KH570 treated and the
alkali-bleached fiber was improved obviously. The tensile
strength of alkali-KH570 treated fiber was obviously higher than
that of alkalized and KH570 treated fiber. While the tensile
property of the alkali-KH550 treated fiber was not improved as
that of the alkali-KH570 treated fiber. The tensile property of the
alkali-KH550 treated fiber was higher than that of the alkalized
fiber but less than that of the KH550 treated fiber. The tensile

Fig. 6 ATReFTIR spectra of untreated, KH550, KH570 and JN-9A Fig. 7 ATReFTIR spectra of alkali, alkali-KH550, alkali-KH570 and
treated fibers. alkali-JN-9A treated fibers.

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6 H. Wang et al.: J. Mater. Sci. Technol., 2014, -(-), 1e7

Fig. 8 TGA/DTG curves of untreated (a), alkali treated (b), KH550 treated (c), KH570 treated (d), JN-9A treated (e), alkali-KH550 treated (f), alkali-
KH570 treated (g), alkali-JN-9A treated (h), alkali-bleached treated (i) fibers.

Fig. 9 SEM images of untreated (a), alkali treated (b), KH550 treated (c), KH570 treated (d), JN-9A treated (e), alkali-KH550 treated (f), alkali-KH570
treated (g), alkali-JN-9A treated (h), and alkali-bleached treated (i) fibers.

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 H. Wang et al.: J. Mater. Sci. Technol., 2014, -(-), 1e7 7

Table 3 Tensile strength of the untreated and treated fiber (4) The combination of alkali treatment with coupling agent
treatment was effective for the husk fibers. Alkali-KH570
Surface treatment Untreated Alkalized KH550 KH570 JN-9A
and alkali-bleached fibers presented better tensile property
Tensile strength 108.8 135.2 127.5 115.8 81.0 than single method treated fibers, and these two
(MPa) treatments are more suitable for application in polymer
composites. The improvement of the tensile strength was
due to the increase of the cellulose content of the treated
fibers.

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experienced three regions. In the first region, from the [19] L.A. Pothan, C. Bellman, L. Kailas, S. Thomas, J. Adhes. Sci.
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hemicellulose and other low modulus sustained [20] N.M. Julkapli, H.M. Akil, Polym. Plast. Technol. Eng. 49 (2010)
decomposed. In the second region from 230 to 290  C, 147e153.
the lignin decomposed. The cellulose decomposed mainly [21] J.D.S. Macedo, M.F. Costa, M.I.B. Tavares, R.M.S.M. Thire,
in the last region from 290 to 500  C. Polym. Eng. Sci. 50 (2010) 1466e1475.
(3) The changes in chemical groups on the fiber surface proved [22] D.R. Mulinari, C.A.R.P. Baptista, J.V.C. Souza, H.J.C. Voorwald,
that all the modifications were achieved on the surface of in: 11th International Conference on the Mechanical Behavior of
Materials, Lake Como, Italy, 5e9 June, 2011.
the fiber, which affected the properties of the fibers.

Please cite this article in press as: H. Wang, et al., Journal of Materials Science & Technology (2014), http://dx.doi.org/10.1016/j.jmst.2014.07.004