Accepted Manuscript
Influence of Depositing Nano-SiO2 Particles on the Surface Microstructure and
Properties of Jute Fibers via In Situ Synthesis
Xuan Liu, Yihua Cui, Senjie Hao, Haiyan Chen
PII: S1359-835X(18)30128-3
DOI: [Link]
Reference: JCOMA 4983
To appear in: Composites: Part A
Received Date: 25 December 2017
Revised Date: 17 March 2018
Accepted Date: 17 March 2018
Please cite this article as: Liu, X., Cui, Y., Hao, S., Chen, H., Influence of Depositing Nano-SiO2 Particles on the
Surface Microstructure and Properties of Jute Fibers via In Situ Synthesis, Composites: Part A (2018), doi: https://
[Link]/10.1016/[Link].2018.03.026
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Influence of Depositing Nano-SiO2 Particles on the Surface Microstructure and
Properties of Jute Fibers via In Situ Synthesis
Xuan Liu, Yihua Cui*, Senjie Hao, Haiyan Chen
(Institute of Materials Science and Technology, Nanjing University of Aeronautics and Astronautics,
Nanjing 210000, China)
Abstract: Jute fibers are finding much interest as the reinforcement of polymer composites. However,
surface flaws not only affect the properties of jute fibers, but also lead to the interfacial defects of jute
fiber reinforced composites. This study aims to improve the properties of jute fibers, the surface flaws of
which were filled up by nano-SiO2 particles via in situ synthesis. The waxy substance covering on jute
fibers was removed by alkali pre-treatment, ethanediamine/alkali pre-treatment and acid/alkali
pre-treatment, respectively. The acid/alkali pre-treatment was the most effective method among three
pre-treatments. The nano-SiO2 particles deposition was prepared by the sol-gel technique. The results
showed that the surface flaws of jute fibers could be filled up by nano-SiO2 particles with the
tetraethylorthosilicate (TEOS) concentration of 0.015 mol/L. Compared with acid/alkali pre-treated fibers,
the surface free energy and tensile strength of nano-SiO2 deposited fibers were increased by 11.7% and
17.9%, respectively. Moreover, the presence of nano-SiO2 particles contributed to the significant
enhancement on the thermal stability of jute fibers.
Keywords: Fibers; Surface properties; Surface analysis; Surface treatments
1. Introduction
In recent years, the development and applications of natural fibers have been paid extensive attention
with growing concern about the environmental issues [1,2]. Natural fibers are renewable materials with
low cost, wealth of sources and degradation, which are regarded as the preferred reinforcements of
composite materials due to their excellent specific strength and specific modulus. In some fields, there
will be a real tendency to substitute natural fiber reinforced composites for synthetic fiber reinforced
composites [3,4]. However, massive hydroxyl groups on the surface of natural fibers not only increased
the hydrophilicity of natural fibers, but also impacted on the compatibility with polymer matrices [5-7]. In
addition, the surface flaws of natural fibers were not easily filled up by polymer matrices, which resulted
in the formation of voids at the interface of composites [8,9]. The voids of interface as stress
concentration location caused the initiation of the cracks on the composite. Based on previous research
works [10,11], a great many approaches including physical and chemical treatments have been applied to
improve the surface properties of natural fibers, while the surface flaws of natural fibers have not been
healed yet, so that the reinforcing effect of natural fibers was limited.
Some studies [12-14] showed that nano-particles deposition could be a novel method to heal the
surface flaws of natural fibers. The surface of natural fibers could be treated as the substrate, which
promoted the nucleation and growth of nano-particles [15]. On the other hand, nano-particles with large
specific surface area and high surface energy could transform the surrounding water molecules to the
dissociative state (-OH groups) on the surface of nano-particles, and formed the physical or chemical
bonds with the hydroxyl groups on the surface of natural fibers [16,17]. The natural fibers with the
nano-particles deposition not only improved the mechanical properties of natural fibers, but also healed
the interfacial voids between fibers and matrices [8,18]. Rabbe et al. [12] deposited nano-SiO2 particles on
the surface of cellulose fibers by the sol-gel technique, the thermal stability of cellulose fibers possessed a
noticeable improvement. Compared with the control fiber, the moisture adsorption capacity of cellulose
fibers with deposition was decreased by 50%. Ye et al. [13] found that the wood fibers were coated with
nano-ZnO particles, the tensile strength of wood fiber reinforced composites were enhanced from 20.42
MPa to 38.73 MPa, and water absorption was reduced by 3.37%. Wang et al. [14] grafted nano-TiO2
particles on the surface of flax fiber, the tensile strength of flax fiber and the interfacial shear strength of
composite were improved by 23.1% and 40.5%, respectively.
In this paper, nano-SiO2 particles were deposited on the surface of jute fibers by the sol-gel technique to
heal the surface flaws of jute fibers, based on scanning electron microscopy (SEM), transmission electron
microscopy (TEM), X-ray diffraction (XRD), wettability measurement, tensile strength test and thermal
stability analysis, the effects of depositing nano-SiO2 particles on properties of jute fibers were evaluated.
2. Experimental
2.1 Materials and reagents
Jute fibers with the average diameter of 15 μm and the length of 15~25 cm were purchased from Hunan
Shangke Co. Ltd., China. Tetraethylorthosilicate (TEOS) and ethanol were obtained from Chemical
Reagent Co. Ltd., China. Ammonia, sulfuric acid (98%) and sodium hydroxide were provided by Nanjing
Share Ltd., China.
2.2 Jute fiber pre-treatment
The pre-treatment was an important factor, which affected depositing nano-SiO2 particles on the
surface of jute fibers. Three pre-treatments including alkali pre-treatment, ethanediamine/alkali
pre-treatment and acid/alkali pre-treatment were selected in this study.
2.2.1 Alkali pre-treatment
The jute fibers (2 g) were soaked in 8 wt.% sodium hydroxide solution for 1 h at 98 °C. Then they were
washed for three times by distilled water, and dried at 70 °C for 2 h.
2.2.2 Ethanediamine/alkali pre-treatment
Ethanediamine (57.5 ml) and Urea (5 g) were mixed with distilled water (57.5 ml). Then the jute fibers
(2 g) were immersed in the mixture for 1 h at room temperature. After rinsing with distilled water for
three times, the jute fibers were soaked in 8 wt.% sodium hydroxide solution for 1 h at 98 °C. Finally, the
jute fibers were washed by distilled water for three times, and dried at 70 °C for 2 h.
2.2.3 Acid/alkali pre-treatment
The jute fibers (2 g) were treated with 4 g/L sulfuric acid solution for 30 min at room temperature.
After rinsing with distilled water, the fibers were soaked in 8 wt.% sodium hydroxide solution for 1 h at
98 °C. The fibers were then washed for three times by distilled water, and dried at 70 °C for 2 h.
2.3 Deposition of Nano-SiO2 particles on the jute fibers
TEOS was mixed with ethanol (30 ml) in the presence of 0.1 g acid/alkali pre-treated fibers (the TEOS
concentration of 0.005 mol/L, 0.015 mol/L, 0.025 mol/L, 0.035 mol/L and 0.065 mol/L, respectively).
Ethanol (10 ml) /distilled water solution and ethanol (5 ml) /ammonia solution (0.6 mol/L) were slowly
dropped into the mixture, respectively. The volume ratio of TEOS and distilled water was 1: 2. Then the
solution was kept for 1 h under sonification with frequency of 40 kHz. Afterward, the mixture was under
constant and moderate mechanical stirring for 5 h at 40 °C. Finally, the fibers were washed 3 times by
distilled water, and dried at 70 °C for 2 h.
2.4 Characterization
2.4.1 Morphology analysis
To observe the difference between the qualities of deposition on the jute fiber surface with different
pre-treatments, the nano-SiO2 deposited fibers with different pre-treatments were observed by scanning
electron microscope (SEM, Quanta 200 FEG, FEI Co., United States). All the samples were gold coated
prior to the observation.
In order to distinguish the morphology and particle size of nano-SiO2 particles obtained from sol-gel
solution, 10 μL of the sol-gel solution (the TEOS concentration of 0.015 mol/L) was dipped onto the
carbon film-coated copper grips (mesh=200) and left to vaporize. Then the sample was observed by a
transmission electron microscope (TEM, Fei G2 T20, FEI Co., United States).
2.4.2 Fourier transform infrared spectroscopy (FT-IR)
The absorption spectra of control fibers, acid/alkali pre-treated fibers and nano-SiO2 deposited fibers
were recorded with a FT-IR spectrometer (Nicolet Nexus 870, Nicolet Co., United States), from wave
numbers of 4000 to 400 cm-1. The samples of FT-IR analysis were composed of the fiber powder and KBr
powder.
2.4.3 The test of deposition amount
Deposition amount was useful to characterize the quality of deposition. The nano-SiO2 deposited fibers
were pre-dried for 2 h at 70 °C, placed and weighed in an electronic balance (0.0001g precision). After
deposition, the fiber samples were dried and weighed by the same method. The deposition amount of
nano-SiO2 particles was then calculated by equation (1).
m2 m1
m(%) 100 （1）
m1
where m is the deposition amount of nano-SiO2 particles, m1 is the weight of fiber samples before the
deposition, m2 is the weight of fiber samples after the deposition.
2.4.4 X-ray powder diffraction (XRD)
The crystal phase of the control fibers, acid/alkali pre-treated fibers and nano-SiO2 deposited fibers
were shown by X-ray diffractometer (Miniflex-600, Bruker Co., Germany) with Cu Kα radiation
(λ=0.15406 Å) and the 2 range varies from 10 to 80 °.
2.4.5 Wettability test
The contact angle of the control fibers, acid/alkali pre-treated fibers and nano-SiO2 deposited fibers
were measured by a dynamic contact angle meter (JC2000D7M, Beijing Zhongyi technology Co., Ltd,
China), as Fig. 1 showed. Distilled water and ethylene glycol were selected as the test liquids. The
average values of contact angle were calculated by 5 samples.
Suggested position for Fig.1
According to Young’s equation (2-4), the surface energy of fiber samples with different treatments
could be calculated directly by contact angles [19-21].
l1 1 cos 2 sp lp1 2 sd ld1 (2)
l 2 1 cos 2 sp lp2 2 sd ld2 (3)
T sp sd (4)
Where T is the surface free energy of fiber sample, l1 (72.8 mN/m) is the surface free energy of
distilled water, l 2 (48.0 mN/m) is the surface free energy of ethylene glycol, ld1 (21.8 mN/m) is the
dispersion component of distilled water, ld2 (29.0 mN/m) is the dispersion component of ethylene
glycol, lp1 (51.0 mN/m) is the polar component of distilled water, lp2 (19.0 mN/m) is the polar
component of ethylene glycol.
2.4.6 Tensile test
A fiber tensile testing machine (YG001A, Hongda Co. Ltd., China) with 300 cN load cell was
employed to measure the tensile strength of a single fiber at a gauge length of 30 mm and the across-head
speed of 20 mm/min. The pre-tention of testing was 0.2 cN. Single fibers were separated from bundle
fibers. At least 40 single fibers in each kind of the sample were prepared for measurement. The fiber
diameter was measured by optical microscopy, and the diameter value measured at three different
locations along the fiber length were used to obtain the mean diameter of jute fibers. Then the cross
section area was calculated by the mean diameter.
2.4.7 Thermal analysis
Thermal stability analysis was performed by differential scanning calorimetry (DSC, 200F3, Netzsch
Co. Ltd., Germany) and thermogravimetric analysis (TGA, Pyris 1, PerKin Elmer Co. Ltd., America). The
sample weight of 5-10 g was taken for analysis in a nitrogen environment. For TG analysis, the sample
was heated up from 25-400 °C at a rate of 20 °C/min. DSC analysis was recorded from 25-200 °C at a
rate of 10 °C/min.
3. Results and discussion
3.1 Homogeneous nucleation and heterogeneous nucleation of the nano-SiO2 particles
Suggested position for Fig. 2
As shown in Fig. 2 (a), the deposition of nano-SiO2 particles was prepared by the hydrolysis of TEOS
precursor and condensation of the hydroxyl groups on the jute fiber surface, which proceeded in the
solution of distilled water and ethanol with the catalyst of ammonia [12]. With the increase of the
hydrolytic degree, silica sol condensed to the various cross-linked structures [22,23]. Then the nucleation
of nano-SiO2 particles were occurred when the critical nucleus size r * obtained [24], as Fig. 2 (b)
displayed. A part of cross-linked structures formed stable nucleus in the homogeneous solution
(homogeneous nucleation), the other part combined with the hydroxyl groups on the fiber surface
(heterogeneous nucleation). The cross-linked structures deposited on the surface of jute fibers included
two forms, one reacted towards a three-dimensional network, another formed spherical nucleus and grew
to a spherical particle gradually.
Suggested position for Fig. 3
A nucleus forming on the substrate as can be seen in Fig. 3 [25], according to the equations of
homogeneous nucleation and heterogeneous nucleation [24,26], as follows:
4 3
G1 - r K BT ln( S ) 4r 2 (5)
V
2V
r*
3K BT ln(S ) (6)
1
G2 (2 3 cos cos 3 ) G1 (7)
4
1
f ( ) (2 3 cos cos 3 )
4 (8)
where G ( G1 for the homogeneous nucleation, and G 2 for the heterogeneous nucleation) is the sum
of the free energy of a new volume formation and a new surface created, V is the molecular volume of
the precipitated species, r is the radius of the nucleus, r * is the critical radius of the nucleus, K B is
the Boltzmann constant, S is the saturation ratio, is the surface free energy per unit surface area, f ( )
is the surface factor, is the contact angle between the nucleus and substrate.
Suggested position for Fig. 4
As can be seen in Fig. 4, the particle size of nano-SiO2 particles deposited on the jute fibers surface was
about 83.3 nm, while the particle size of nano-SiO2 particles in the solution was about 28.2 nm, there was
a difference between the two samples. According to equation (7) and (8), the free energy of heterogeneous
nucleation was lower than the free energy of homogeneous nucleation under the same condition.
Therefore, the surface of jute fibers was favorable for the nucleation and growth of nano-SiO2 particles.
3.2 Depositing nano-SiO2 particles on the surface of jute fibers with different pre-treatments
Suggested position for Fig. 5 and Fig. 6
The structure of jute fiber was mainly composed of cellulose, hemicellulose, and lignin. Cellulose,
which was considered as the major framework component of jute fiber structure, provided mechanical
properties and structural stability of the fiber. Hemicellulose, lignin, pectin and impurities, collectively
known as the waxy substance, consisted of the primary cell wall covering of cellulose[27,28]. The
presence of waxy substance may affect the properties of jute fibers. Therefore the pre-treatments were
needed to remove the waxy substance. The SEM images of the fiber with different pre-treatments were
exhibited in Fig. 5. From Fig. 5 (a), there was the waxy substance covering of control fibers obviously.
After alkali pre-treatment, the surface morphology was obviously changed, and fine fiber with surface
flaws was revealed. Whereas some waxy substance was left on the fiber surface, as shown in Fig. 5 (b), it
indicated that alkali pre-treatment was not strong enough to remove the waxy substance from the fiber.
In order to separate the waxy substance sufficiently, jute fibers were modified with
ethanediamine/alkali pre-treatment and acid/alkali pre-treatment, respectively. After ethanediamine
treatment, amino groups (-NH2) penetrated into the waxy substance breaking the hydrogen bonds between
the molecular chains, and paved the way for alkali solution to enter and improved the effect of alkali
treatment. Owing to the effect of acidic hydrolysis, the polymerization degree of waxy substance was
decreased, which helped the effect of alkali pre-treatment of jute fibers [29]. From Fig. 5 (d), the waxy
substance was removed thoroughly, and the surface flaws of jute fibers were visibly seen. Therefore,
acid/alkali pre-treatment possessed remarkable effect on the removal of waxy substance.
In Fig. 6, nano-SiO2 particles were mainly deposited in the surface flaws of jute fibers. According to
previous researches [30,31], nucleation was formed more easily in a concave surface than on a convex
surface for the same surface curvature. As a result, the surface flaws of jute fibers provided the
superior nucleation condition which could even form nucleation without under cooling condition.
The surface flaws of jute fibers were covered due to the existence of waxy, which restricted the
nucleation and growth of nano-SiO2. The nano-SiO2 particles with smaller particle size (40-55 nm)
were deposited on the control fiber surface as Fig. 6 (a) showed. Compared with control fibers, the
particle size of nano-SiO2 particles on alkali pre-treated fibers changed remarkably, while the
agglomeration of nano-SiO2 particles occurred on the fiber surface as can be seen in Fig. 6 (b). The
nucleation sites were occupied by the left waxy substance, which led to the agglomeration of nano-SiO2
particles. From Fig. 6 (c), there were few nano-SiO2 particles depositing on the surface of
ethanediamine/alkali pre-treated fiber. Amino groups (-NH2) may form new hydrogen bonds with the
cellulose, which affected the deposition of nano-SiO2 particles. From Fig. 6 (d) displayed, the surface
flaws of acid/alkali pre-treated fibers were filled up by nano-SiO2 particles with the uniform particle size
(83.3 nm), achieving the desired result. Therefore, acid/alkali treatment was chosen as the pre-treatment
of jute fibers.
3.3 Fourier transform infrared spectroscopy (FT-IR) analysis
Suggested position for Fig. 7
The characteristic spectra of the fiber samples were displayed in Fig. 7. The peak at 1735 cm-1
related to the carbonyl groups of waxy substance was not presented with the acid/alkali pre-treatment,
this mainly contributed to the removal of waxy substance [32]. The result was consistent with the
analysis of SEM. After deposition, the peak of Si-O-Si (454 cm-1 and 804 cm-1) appeared which
suggested that TEOS was hydrolyzed and condensed as equation (9) and (10) showed [12]. The presence
of C-O-Si peak (1075 cm-1) provided a strong evidence for the immobilization of nano-SiO2 particles on
the fiber surface as equation (11) displayed. This result showed the agreement of previous reports
[17,33]. Moreover, the peak of hydroxyl groups on nano-SiO2 deposited fibers flattened owing to the
formation of C-O-Si peak.
Si(OC2 H 5 ) 4 4H 2O Si(OH ) 4 4C2 H 5OH (9)
Si(OH ) 4 SiO2 2H 2O (10)
Fiber OH SiO 2 OH Fiber O SiO 2 (11)
3.4 Evaluation of TEOS concentrations for nano-SiO2 particles depositing on the surface of jute
fibers
Suggested position for Fig. 8 and Fig. 9
As can be seen in Fig. 8 and Fig. 9, the deposition amount and particle diameter of nano-SiO2 particles
were both increased gradually as the increase of TEOS concentrations. The low concentration of TEOS
(0.005 mol/L) resulted in the large diffusion distance, which led to the restriction of the nucleation and
growth of nano-SiO2 particles. With the increase of TEOS concentrations, the surface flaws were filled up
by nano-SiO2 particles gradually. Dispersed nano-SiO2 particles with suitable particle size (83.3 nm) were
produced at 0.015 mol/L TEOS, which could be the most efficient level for healing the surface flaws.
With the TEOS concentration continued to increase, the deposition amount almost saturated, and the
particle size changed slightly. Owing to the limited nucleation sites, nano-SiO2 particles aggregated
seriously on the fiber surface, as Fig. 8 (e) displayed. In addition, it was worth noting that the oriented
attachment of nano-SiO2 particles occurred on the fiber surface, the driving force for this phenomenon
was that the elimination of the pairs of high energy surfaces led to a substantial reduction in the surface
free energy [24]. The interaction between nano-SiO2 particles was promoted with the TEOS concentration
of 0.065 mol/L, which caused the wilder particle size distribution of nano-SiO2 particles. It meant that the
excessive TEOS concentration possessed negligible effect on the particle size distribution of nano-SiO2
particles.
3.5 X-ray powder diffraction (XRD) analysis
Suggested position for Fig. 10
XRD patterns of different samples were summarized in Fig. 10. The major peaks at 22.5°and 34.5°
indexed to the lattice planes at 002 and 040 [34]. The major peaks of cellulose (002) were not shifted,
which indicated that the pre-treatment and deposition occurred on the surface of jute fibers, and did not
alter the fiber structure. Cellulose involving crystalline and amorphous regions were covered by the waxy
substance which was completely amorphous [27,28]. After acid/alkali pre-treatment, the crystallinity of
the fiber was increased due to the removal of waxy substance. The diffraction spectrogram did not
produce characteristic peak after nano-SiO2 particles deposition, which illustrated nano-SiO2 particles
were amorphous [35]. What is more, the decline of fiber crystallinity should be ascribed to the covering
of nano-SiO2 particles.
3.6 Wettability analysis
Suggested position for Fig. 11
Contact angle relating to the performance of surface energy was controlled by the structure of fiber
surface. Fig. 11 presented the wettability of fiber samples with different [Link] wettability of
fiber was improved with the removal of hydrophobic pectin on the fiber surface. Acid/alkali pre-treatment
not only helped the exposure of hydroxyl groups, but also increased the contact area of fiber with test
liquids, hence the surface free energy of acid/alkali pre-treated fiber was increased. Compared with the
control fiber, the surface free energy of acid/alkali pre-treated fiber was enhanced by 45.7%. After
deposition, the surface free energy of nano-SiO2 deposited fiber maintained upward trend. This was
because massive active groups on nano-SiO2 particles increased the interaction between the fibers and
tests liquids. Moreover, the specific surface area of nano-SiO2 particles also benefited the wettability of
fiber. Compared with acid/alkali pre-treated fiber, the surface free energy of nano-SiO2 deposited fiber
was improved by 11.7%.
3.7 Tensile properties analysis
Suggested position for Tab. 1
Table 1 showed the tensile strength of jute fibers with different treatments. Compared with
control fibers, the tensile strength and Young modulus values of acid/alkali pre-treated fibers were
decreased by 9.8% and 4.2%, respectively. Acid/alkali pre-treatment could remove the waxy
substance between unitary fibers, a certain degree of fibrillation on the fiber surface might be the
reason of the lower stiffness of fibers. Further more, the surface flaws of jute fibers were revealed
by acid/alkali pre-treatment resulting in the reduction of tensile strength and the premature failure
of fibers.
Compared with acid/alkali pre-treated fibers, the tensile strength and Young modulus values of
nano-SiO2 deposited fibers were improved by 17.9% and 12.1%, respectively. As shown in Fig.7,
new bonds of C-O-Si were formed between nano-SiO2 particles and jute fibers, which implied that a
strong interface combination was formed. This interface played a critical role in transferring of
external stress between the fibers and nano-SiO2 particles. The surface flaws on jute fibers as stress
concentration location caused the initiation of the cracks. Nano-SiO2 particles filling up the surface
flaws of fibers could be deemed as a protective layer to prevent the initiation and propagation of
crack. They may eliminate the stress concentration and increase the energy dissipation. Therefore,
nano-SiO2 particles deposition could enhance the tensile strength of jute fibers significantly.
3.8 Thermal stability analysis
Suggested position for Fig. 12
As Fig. 12 (a) displayed, the DSC curve of fiber samples exhibited an endothermic peak at the
temperature rang of 50-150 °C, which indicated the evaporation of water and the release of volatiles in
the intermolecular region of fibers [36]. The presence of waxy substance, which contained water and
volatiles, led to the highest endothermic peak of control fibers among three samples. Owing to the
removal of waxy substance, the endothermic peak of acid/alkali pre-treated fibers related to the
evaporation of water was shifted to a lower temperature. Compared with acid/alkali pre-treated fibers, the
endothermic peak of nano-SiO2 deposited fibers was changed to a higher temperature, and got broadened.
It meant the removal of water molecules from nano-SiO2 deposited fibers required higher temperature,
this was may be due to the higher surface energy of nano-SiO2 particles, as Fig. 11 showed.
The TGA curves of jute fibers with different treatments were presented in Fig. 12 (b). The TGA curves
exhibited three regions relating the thermal degradation of fibers. The first one region ranged the
temperature from 50 to 200 °C, the mass loss in this region was attributed to the sample dehydration and
the release of volatiles. The second region occurred the temperature between 200 and 350 °C due to the
decomposition of cellulose (250-350 °C), hemicellulose (25-290 °C) and lignin (150-420 °C) [28,37].
Compared with control fibers, the decomposition temperature of acid/alkali pre-treated fibers was higher,
due to the removal of hemicellulose and lignin. The third region ranging from 350 to 450 °C
corresponded to the temperature range of the oxidation of remaining organic material. Compared with
control fibers and acid/alkali pre-treated fibers, it could be clearly found that the thermal stability of
nano-SiO2 deposited fibers was improved significantly. Based on this results, it could be stated that the
nano-SiO2 particles deposited on the fiber surface formed an effective barrier against oxygen which
enhanced the thermal stability.
4. Conclusion
In this paper, nano-SiO2 particles were deposited on the surface of jute fiber via in situ synthesis, and
the influence on the properties of jute fibers was studied.
(1) The waxy substance, which hindered nano-SiO2 particles deposition on the fiber surface, were
removed by alkali pre-treatment, ethanediamine/alkali pre-treatment and acid/alkali pre-treatment
before the deposition. Acid/alkali pre-treatment was the most effective method among three
pre-treatments.
(2) The surface flaws of jute fibers were favorable for the nucleation and growth of nano-SiO2
particles. The surface flaws were filled up by nano-SiO2 particles with the TEOS concentration of
0.015 mol/L.
(3) The presence of nano-SiO2 particles was deemed to contribute to the enhanced surface free energy,
tensile strength and thermal stability of jute fibers. Compared with acid/alkali pre-treated fibers,
the surface free energy and tensile strength of nano-SiO2 deposited fibers were increased by 11.7%
and 17.9%, respectively.
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Table 1
Tensile properties of control fibers, acid/alkali pre-treated fibers and nano-SiO2 deposited fibers
Tensile strength Tensile modulus Elongation at break
Samples
/(MPa) /(GPa) /(%)
Control fiber 471.8±34.9 21.5±1.3 1.35±0.06
Acid/alkali pre-treated fiber 425.3±41.3 20.6±1.8 1.31±0.04
Nano-SiO2 deposited fiber 501.2±38.2 23.1±1.4 1.46±0.03
Fig. 1. Shape of the test droplet on jute fiber surface.
Fig. 2. (a) Preparation of nano-SiO2 by the sol-gel technique, (b) Illustration of the overall free
energy G as a function of the growth particle size r [24].
Fig. 3. Illustration of the heterogeneous nucleation [25].
Fig. 4. (a) SEM image of nano-SiO2 particles on the surface of jute fiber, (b) TEM image of nano-SiO2
particles in the reaction solution.
Fig. 5. SEM images of (a) control fiber, (b) alkali pre-treated fiber, (c) ethanediamine/alkali pre-treated
fiber, (d) acid/alkali pre-treated fiber.
Fig. 6. SEM images of (a) control fiber with nano-SiO2 particles deposition, (b) alkali pre-treated fiber
with nano-SiO2 particles deposition, (c) ethanediamine/alkali pre-treated fiber with nano-SiO2 particles
deposition, (d) acid/alkali pre-treated fiber with nano-SiO2 particles deposition.
Fig. 7. FT-IR spectra of control fibers, acid/alkali pre-treated fibers and nano-SiO2 deposited fibers.
Fig. [Link] of nano-SiO2 with different TEOS concentrations.
Fig. 9. The deposition amount (a) and particle size variation (b) of nano-SiO2 particles on the surface of
jute fibers with different TEOS concentrations.
Fig. 10. X-ray diffraction patterns of control fibers, acid/alkali pre-treated fibers and nano-SiO2 deposited
fibers.
Fig. 11. Wettability of control fibers, acid/alkali pre-treated fibers and nano-SiO2 deposited fibers.
Fig. 12. (a) DSC curves of jute fibers with different treatments, (b) TGA curves of jute fibers with
different treatments.