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Effect of surface modication of bamboo cellulose bers on mechanical

properties of cellulose/epoxy composites


Tingju Lu
a
, Man Jiang
a
, Zhongguo Jiang
b
, David Hui
c
, Zeyong Wang
a
, Zuowan Zhou
a,
a
Key Laboratory of Advanced Technologies of Materials (Ministry of Education), School of Materials Science and Engineering, Southwest Jiaotong University,
Chengdu 610031, PR China
b
School of Light and Chemical Engineering, Xichang College, Xichang, Sichuan 610500, PR China
c
Department of Mechanical Engineering, University of New Orleans, LA 70148, USA
a r t i c l e i n f o
Article history:
Received 14 December 2012
Accepted 25 February 2013
Available online 7 March 2013
Keywords:
A. Fibers
A. Thermosetting resin
B. Mechanical properties
B. Interface
a b s t r a c t
Bamboo cellulose bers were treated with NaOH aqueous solution and silane coupling agent, respec-
tively, before they were applied into epoxy composites. The effect of surface modication on mechanical
properties was evaluated by tensile and impact tests under controlled conditions. Compared with the
untreated cellulose lled epoxy composites, the NaOH solution treatment increased the tensile strength
by 34% and elongation at break by 31%. While silane coupling agent treatment produced 71% enhance-
ment in tensile strength and 53% increase in elongation at break. The scanning electron microscopy
(SEM) was used to observe the surface feature of the cellulose bers and the tensile fractures as well
as cryo-fractures of the composites. The Fourier transform infrared (FTIR) was employed to analyze the
chemical structure of the cellulose bers before and after modications. The results indicated different
mechanisms for the two modications of cellulose. The NaOH solution partly dissolved the lignin and
amorphous cellulose, which resulting in splitting the bers into smaller size. This led to easier permeat-
ing into the gaps of the bers for epoxy resin (EP) oligmer and forming effective interfacial adhesion.
Based on the emergence of SiOC and SiOSi on the cellulose surface, it was concluded that the
enhancement of mechanical properties after coupling agent modication could be ascribed to the forma-
tion of chemical bonds between the cellulose and the epoxy coupled with the coupling agent.
2013 Elsevier Ltd. All rights reserved.
1. Introduction
The growing environmental awareness and increasing scarcity
of natural resources have provoked a growing demand for environ-
ment-friendly materials, with the desire to lower the cost of tradi-
tional synthetic ber reinforced composites [1,2]. Natural ber
reinforced green composites, virginly initiated in the automotive
industry, have regained great research interest in recent years be-
cause of its cheap price and low energy consumption [1,3]. Natural
bers exhibit many advantages over their synthetic counterparts
(e.g. carbon, glass and aramid), such as light weight, low cost, easy
processing, excellent specic strength and high specic modulus,
and especially, their renewability and recyclability [1,3]. Thus nat-
ural bers are long regarded as being promising candidates for
replacing conventional synthetic reinforcing bers in composites
for semi-structural and structural applications [4].
Cellulose, one of the most abundant natural bers on the earth,
has been studied for years in varied elds. Till now, numerous
researchers have reported advances in cellulose bers/polymer
composites. The cellulose can act as reinforcement of both thermo-
plastic and thermosetting polymers, as well as template for func-
tional composites [518]. On the basis of earlier reports, bamboo
is a very good resource of cellulose bers because of its high con-
tent of cellulose and relatively small microbrillar angle [19].
The bamboo is also very abundant and cheap in China, especially
in Sichuan province. Epoxy resin (EP), with excellent comprehen-
sive performance and a wide range of applications, has been the
most researched thermosetting matrix of cellulose reinforced com-
posites. The cellulose bers were proved to have good effect on
improving certain properties of the EP matrix. Fracture toughness
and impact behavior were reported to have signicant increase
after adding the cellulose bers, while exural strength and
Youngs Module hardly increased [2023]. The strength improve-
ment was unsatised because of the poor compatibility between
the cellulose and the matrix, which limited application of the cel-
lulose/EP composites.
Thus the poor compatibility between the cellulose ber and the
matrix is a problemwe must overcome to get composites with high
properties. The strong polarity of cellulose and high dense hydrogen
bonds between molecules and intra-molecules in its structure lead
to poor accessibility of matrix. Therefore, the interfacial tension
1359-8368/$ - see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.compositesb.2013.02.031

Corresponding author.
E-mail address: zwzhou@at-c.net (Z. Zhou).
Composites: Part B 51 (2013) 2834
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between the cellulose ber and the matrix is quite high, which leads
to the peeling off the bers, and increasing of the porosity in the
composites [24,25]. To improve the compatibility, physical, chemi-
cal or other modications of the cellulose are very necessary
[26,27]. In the blending systemof natural ber and polymer matrix,
alkali treatment, acetylation, cyanoethylation and coupling agent
treatment have been included in the modication methods. Bledzki
et al. reported that alkali and coupling agent treatments of cellulose
ber had relatively better effects on the mechanical properties of
cellulose/PP composites [28], but no mechanisms or explanations
were mentioned. Based on the earlier reports, the APS and GPS (also
named KH560 in China) could be the silanes used for the natural -
ber/polymer composites [29]. We chose KH560 to modify the bam-
boo cellulose because the glycidoxy organofunctionalities in KH560
make the reactionbetweenthe ber andthe silane milder and lower
energy consumption.
In this work, the bamboo cellulose bers were pretreated with
silane coupling agent and NaOH aqueous solution respectively.
The effects of the modication of cellulose bers on mechanical
properties of cellulose/epoxy composites were comparatively stud-
ied, and the distinct mechanisms of the two modications were
put forward. The materials were very cheap and the experiments
were simple and low energy consumption, but the results were
positive.
2. Experimental part
2.1. Materials
The bamboo cellulose bers (BCFs) used in the experiments
were smashed bamboo bers pulp procured from Sichuan Anxian
Paper Co., Ltd. The bamboo ber pulp was dried for 4 h at 105 C
in the electric blast oven (Model 101-1A) after cut into small
blocks, then crushed the cellulose blocks for 3 min with a high-
speed universal grinder (FW-400A, 26,000 r/min), kept the cellu-
lose powder under sealing after drying again.
The epoxy-E44, acetone, and the curing agent-T31 were com-
mercial products that were procured from Chengdu Shunmei
Composite Materials Co., Ltd. The silane coupling agent (commercial
code: KH560), NaOHand ethanol were of chemically purity and pro-
vided by Chengdu Kelong Chemical Reagent Factory. Deionized
water was laboratory-made.
2.2. The treatment of the bamboo cellulose
The alkali treatment of BCF was carried out in a conical ask
with 2 wt% NaOH aqueous solution and 10 g of cellulose powder.
The container was placed in a magnetic stirrer for 4 h at 60 C until
the reaction was completed. The NaOH treated BCFs were ltrated
and washed several times to neutral before dried at 80 C.
The silane coupling agent treatment of cellulose was treating
BCF for 3 h at room temperature with 3% of KH560 solution. The
KH560 solution was mixed by 2.5 ml KH560, 77.5 ml deionized
water and 120 ml anhydrous ethanol, stirred continuously for 1 h
to fully hydrolyze. Next, the BCFs were soaked in the solution for
3 h, and then washed and dried at 100 C in an electric oven.
2.3. Preparation of test samples of epoxy and composites
The EP was prepared by casting method at room temperature.
The initial EP was heated at 60 C for 5 min to a better uidity, fol-
lowed by adding the curing agent, then stirred and poured into the
mold and cured for 24 h at room temperature. The BCF/EP compos-
ites were prepared by adding BCFs to the diluted EP oligmer, and
cured after adding curing agent and stirring. Composites with
different modications and gradient loadings of BCFs were accord-
ingly prepared. The details for the composites preparation in the
experiments are shown in Table 1.
2.4. Mechanical properties
In order to evaluate the mechanical properties of composites, a
tensile testing machine (AGS-J, Suzhou, China) was employed to
study the tensile strength and elongation-at-break of the compos-
ites; a pendulumimpact tester (XC, Chengdu, China) was employed
to test the impact strength of composites. The samples for tensile
testing were standard dumbbell-shaped with a 112 mm gauge
length, the tensile speed was 10 mm/min. The size of the samples
for impact test was 65 10 4 mm, the maximum impact energy
was set to be 1 J. All the tests were carried out at 25 C. Values of
the mechanical properties of each sample were decided by the
means of ve tests. The percentage of error as determined by per-
centage error (Standard Deviation/Mean)

100 was less than 10%
[30].
2.5. Fourier transform infrared (FTIR) of cellulose
The virgin bamboo cellulose ber (BCF), NaOH treated bamboo
cellulose ber (N-BCF) and KH560 treated bamboo cellulose ber
(K-BCF) were submitted to FTIR analysis to nd out the transfor-
mation in their chemical structures. The powders of the three dif-
ferent BCF were completely dried at 105 C in a drying oven before
prepared as KBr pellet and being tested by FTIR (Nicolet 5700,
America) on the sample holder. All spectra were recorded in the
wave number range of 4004000 cm
1
with resolution of 4 cm
1
.
2.6. Scanning electron microscopy (SEM)
The tensile fractures and the cryo-fracture surfaces of the com-
posites as well as the pure EP were studied by SEM (QUANPA200,
Netherlands) operating in the high vacuum mode at accelerating
voltage of 20 kV. The morphologies of those three kinds of BCFs
were also characterized by SEM observations. Prior to examination,
the samples were sputtered with gold using JEOL Fine Coater JFC-
1200 for 50 s at argon pressure of 8 Pa and current of 30 mA.
3. Results and discussion
3.1. Pretreatment of cellulose ber
Before preparation of the composites, SEM observations of BCF,
N-BCF and K-BCF were applied to learn about the size and surface
features of the cellulose bers. From Fig. 1, one could see that the
virgin cellulose displayed a bril shape, having an average diame-
ter of 8 lm, and the modications led to obvious differences in
morphology. As shown in Fig. 1a, the surface of the untreated cel-
lulose was found to be considerably covered with impurities and
amorphous cellulose [31,32]. Comparatively, the cellulosic microf-
ibers treated with NaOH displayed a neat and ordered surface
(Fig. 1b), which demonstrated dislodging of impurities and amor-
phous cellulose, agreeing to the observation of Peng et al. [33].
Table 1
Different composites in the experiments.
Cellulose content (wt%)
10% 20% 30%
Untreated BCF10/EP BCF20/EP BCF30/EP
NaOH treated N-BCF10/EP N-BCF20/EP N-BCF30/EP
KH560 treated K-BCF10/EP K-BCF20/EP K-BCF30/EP
T. Lu et al. / Composites: Part B 51 (2013) 2834 29
Particularly, the NaOHtreatment of cellulose resulted in the forma-
tion of nano-sized cellulose brillations (also indicated in Fig. 8b).
As reported, the natural cellulose bers were composited by crys-
talline cellulose in nanosize and para-crystalline, surrounded by
amorphous cellulose [34]. Gaps between the nanobers were
formed after the removal of amorphous cellulose, resulting in split-
ting the bers into smaller sizes. From Fig. 1c, one can see that a
tinny thin lm appears on the cellulose surface after KH560
modication, which was ascribed to the coupling agent.
The chemical structures of the virgin and treated cellulose were
investigated by FTIR, as shown in Fig. 2. The FTIR spectrum of the
virgin BCF (Fig. 2a) was associated with the typical spectrum of
cellulose [23]. Weak characteristic peaks of lignin were found, the
peak at 1633 cm
1
indicated an absorption peak of carbonyl group
in lignin. Comparing Fig. 2b with a, no new functional groups were
introduced to the cellulose structure by NaOH treatment, but some
absorption peaks in N-BCF shifted from the corresponding peaks in
the virgin BCF as marked in curve-b. The OH stretching vibration
absorption peak at 3407 cm
1
had a left shift by 13 cm
1
, while
the CH
2
bending vibration absorption peak shifted from
1436 cm
1
to 1422 cm
1
after the NaOH modication. Associated
with the SEM observations in Fig. 1, it can be concluded that the
structure of the BCF might have been changed because of the
remotion of amorphous cellulose and other impurities after NaOH
treatment. Two new peaks appeared in curve-c at 1103 cm
1
and
802 cm
1
after KH560 modication, wherein 1103 cm
1
corre-
sponded with the stretching vibration of SiOC, and 802 cm
1
related to SiOSi stretching vibration. These results demonstrated
that chemical bonds have been formed after the cellulose being
modied by the coupling agent of KH560, and CH
2
CH(O)CH
2-
O(CH
2
)
3
SiO group had been grafted onto the cellulose molecules.
The process can be described as follows:
3.2. Mechanical properties of the composites
The mechanical properties of the pure EP and the composites
with different loadings of cellulose bers are shown in Figs. 35.
The composites lled with unmodied BCF increased the impact
strength and elongation at break, while decreased the tensile
strength. This might be caused by the poor compatibility between
BCF and EP matrix, which could be reinforced by the SEM observa-
tions as shown in Fig. 6. From Fig. 6bd, relating to BCF10/EP,
BCF20/EP and BCF30/EP respectively, cellulose bers were found
to be dispersed in the matrix, and the surface of the BCFs were
smooth and clean, not coated by matrix EP. In general, clear pull
out, detachment or debonding of some of the BCFs could be ob-
served (as indicated with arrows), which indicated the poor inter-
facial adhesion. Failure rstly occurs at the interfaces, thus virgin
BCF produced defects in the composites rather than reinforced
the matrix, leading to reduction in the tensile strength. At the same
time, the tensile fracture of pure epoxy (Fig. 6a) was very at,
H
2
C CHCH
2
OCH
2
CH
2
Si (OCH
3
)
3
+ H
2
O
O
H
2
C CHCH
2
OCH
2
CH
2
Si(OH )
3
O
H
2
C CHCH
2
OCH
2
CH
2
Si(OH)
3
+Rcell
O
OH H
2
C CHCH
2
OCH
2
CH
2
Si
__
O
__
Rcell
O
Fig. 1. SEM micrographs of (a) virgin BCF, (b) N-BCF and (c) K-BCF.
30 T. Lu et al. / Composites: Part B 51 (2013) 2834
showing a brittle fracture. The fractures of the composites were
rougher than pure EP, indicating a higher degree of toughness that
resulted in enhancing the impact strengths of the BCF lled com-
posites. This could be ascribed to the loose structure of cellulose -
bers that can absorb more impact energy.
After NaOH solution treatment, the tensile strength and the
elongation at break increased by different degrees with varying
loadings of the bers (N-BCF). KH560 modication caused signi-
cant increases both in tensile strength and elongation at break.
Both modications decreased the impact strength slightly com-
pared with BCF/EP composites. The N-BCF or K-BCF reinforced EP
composites still had much higher impact strength than those of
pure EP. For all the three kinds of composites, increasing the
content of the ller, the magnitudes of tensile strength, impact
strength and elongation at break increased at rst. When the
contents of cellulose bers were 20 wt%, the composites had the
ultimate mechanical properties. More loading of BCFs, such as
30 wt%, resulting in the reduction of mechanical properties. We
speculated this phenomenon on the higher lling that caused poor
dispersion of the bers, leading to more and/or larger defects, as
shown in Fig. 7b and d.
The tensile strength of BCF20/EP increased by 34% and elonga-
tion at break increased by 31%, while impact strength just de-
creased by 8%, still 1.97 times higher that of the pure EP after
NaOH solution treatment. The increments of tensile strength and
elongation at break caused by KH560 treatment were 71% and
53% respectively, while decrement in the impact strength was only
3% for the composites with 20 wt% cellulose content. Lvia et al.
reported considerable decreases in interfacial adhesion between
cellulose and PP after benzylation treatment [4]. Nearly no
enhancement in mechanical properties of cellulose composites
by surface modication of cellulose bers was reported by both
Abdelmouleh et al. [35] and Lu et al. [34]. Compared with these
studies, the results in our work were quite positive.
3.3. The effect of ber modications
The fracture morphology of the composites with 20 wt% loading
of cellulose bers were observed by SEM. From Fig. 8a, related to
BCF/EP composite, small pieces of polymeric matrix was found
on the bers, which further demonstrated that there was poor
combination between the bers and the matrix. In contrast, a good
link between the lled bers and the epoxy could be seen from the
tensile fracture of the N-BCF/EP composite. From Fig. 8b, we could
see that it displayed a lot of burrs on the surfaces of the cellulose
bers. In addition, it seems that some of the bers were broken
by tensile loading (as shown by arrow in Fig. 8b). These results
0 10 20 30
3
4
5
6
E
l
o
n
g
a
t
i
o
n

P
e
r
c
e
n
t
a
g
e

(
%
)
Cellulose Content (wt%)
KH560 treated
NaOH treated
Unmodified
Fig. 4. Elongation at break of BCF/EP composites with different loadings of
cellulosic bers.
0 10 20 30
2
4
6
I
m
p
a
c
t

S
t
r
e
n
g
t
h

(
k
J
/
m
2
)
Cellulose Content (wt%)
Unmodified
KH560 treated
NaOH treated
Fig. 5. Impact strength of BCF/EP composites with different loadings of cellulosic
bers.
0 10 20 30
12
18
24
T
e
n
s
i
l
e

S
t
r
e
n
g
t
h

(
M
P
a
)
Cellulose Content (wt%)
KH560 Treated
NaOH Treated
Unmodified
Fig. 3. Tensile strength of BCF/EP composites with different loadings of cellulosic
bers.
4000 3500 3000 2500 2000 1500 1000 500 0
1
6
3
3
1
2
6
8
1
1
0
3
1
4
2
2
1
4
3
6
1
2
5
3
8
0
2
3
4
2
0
3
4
0
7
I
n
t
e
n
s
i
t
y
Wave number (cm
-1
)
(a)
(b)
(c)
Fig. 2. FTIR spectra of the celluloses: (a) virgin BCF, (b) N-BCF and (c) K-BCF.
T. Lu et al. / Composites: Part B 51 (2013) 2834 31
(a)
Pulled out Fiber
(b)
(c) (d)
Fig. 6. Tensile fractures of (a) Pure EP, (b) BCF10/EP, (c) BCF20/EP and (d) BCF30/EP.
Cellulose Reunion
Separated with matrix
(a) (b)
(c) (d)
Fig. 7. Cryo-fracture of (a) K-BCF20/EP, (b) K-BCF30/EP, (c) N-BCF20/EP and (d) N-BCF30/EP.
32 T. Lu et al. / Composites: Part B 51 (2013) 2834
suggest that the interfacial adhesion between BCF and EP matrix
become much more favorable and stronger upon the treatment
of the cellulose with NaOH solution. The removal of impurities
and amorphous cellulose in BCF by alkaline treatment has led to
smaller sized bers and increasing the surface area available for
contact with the matrix. Whats more important, after the cellulose
ber being treated by NaOH solution, the epoxy resin will perme-
ate into the gaps of cellulose brillation and then strongly joint the
bers together. As after the removal of the cementing materials,
originally a whole ber become cellulose brillation, partly with
nanometer sizes (as shown by arrow in Fig. 8b). The NaOH solution
modication broke the loose structure of cellulose bers and the
epoxy lled the gaps between the brillations, so the impact en-
ergy absorbed by them was lower.
Fig. 8c showed that the K-BCF well trapped by the EP matrix
after KH560 treatment. The bers were covered with a layer of ma-
trix, demonstrating a ne linking between the ber and EP. Com-
pared with the BCF/EP (Fig. 8a), the coupling agent caused a
signicantly wetting of the BCF through the matrix (Fig. 8c). This
was because of the chemically interaction between BCF and matrix
coupled by KH560. The action mechanisms for KH560 modication
can be suggested as: the epoxy groups in KH560 that have grafted
onto the cellulose can react with the matrix molecules and form
chemical bonds, as it has been illustrated in FTIR spectra (Fig. 2),
which will signicantly improve the adhesive force between the
interfaces of the components. Secondly, the reaction between the
OH group in cellulose molecules and the SiOH in KH560 will
weaken the hydrogen bonds in celluloses, resulting in improving
the compatibility between the cellulose and EP. While the chemical
bonds would generate more crosslinking points in the composites
and embrittle the material, the impact strength has slightly de-
creased after KH560 modication.
4. Conclusions
The epoxy composites reinforced by unmodied bamboo cellu-
lose bers, NaOH treated and KH560 treated cellulose ber were
respectively prepared. Both coupling agent modication and alkali
treatment apparently improved the tensile strength and the values
of elongation at break. The K-BCF/EP composites exhibited better
mechanical properties than those of N-BCF/EP composites having
the same cellulose content. For all these three kinds of composites,
the ultimate mechanical properties were obtained with 20 wt%
loading of cellulose bers. The result indicated optimum cellulose
content and selected modications were positive to the mechani-
cal properties of the cellulose composites.
Two different modifying mechanisms were suggested in this
study. After beingtreatedwithNaOHaqueous solution, celluloseber
became cellulose brillation with much smaller diameters, thus eas-
ier permeating for EPas well as increasing effective surface area avail-
able for contact with the matrix. After the reaction of KH560 with
both the cellulose and EP happened during KH560 modication, the
silane molecules linked the EP and the cellulose together by chemical
bonds, and signicantly improved the interfacial interactions.
Acknowledgements
This work was nancially supported by the National Natural
Science Foundation of China (Nos. 51173148, 90305003), the
National Key Technology R&D Program of China (No.
2011BAE11B01), the Fundamental Research Funds for the Central
Universities in China (Nos. SWJTU11ZT10, SWJTU11CX052), the
Science and Technology Planning Project of Sichuan Province
Broken
Fibers
Cellulose
Fibrillation
(a)
(b)
(c)
Fig. 8. Tensile fractures of (a) BCF20/EP, (b) N-BCF20/EP, and (c) K-BCF20/EP.
T. Lu et al. / Composites: Part B 51 (2013) 2834 33
(Nos. 2010GZ0251, 2011GZX0052) and the Applied Basic Research
Programs of Sichuan Province (No. 20095Y0064).
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