Air-Plasma treatment of bamboo fiber for polypropylene composite application
Air plasma treatment has increased remarkably the tensile properties of bamboo
fiber. Both mean stress and Young’s modulus in suitable condition increased more than 101.15
and 101.5%.
Plasma treatment also has changed the surface of fibers for a better adhesion.
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196
Journal of Chemistry, Vol. 45 (5A), P. 196 - 200, 2007
Air-plasma treatment of bamboo fiber
for polypropylene composite application
Received 16 August 2007
Ta thi Phuong Hoa, Do Thi Cuc, Nguyen Hoang An
Polymer Centre, Hanoi University of Technology
summary
In this study, the air-plasma generated by radio-frequency was used to treat bamboo fiber.
The treatment parameters were studied to find the suitable condition. The testing on tensile
strength, tensile modulus, module Weibull and elongation to break of the fiber, the measurement
of contact angles and the SEM analysis showed that at the high frequency of 12 kHz, power 50 W
and treatment time of 5 minutes, after air- plasma treatment the tensile strength and tensile
modulus of bamboo fiber increased more than double (101.1% and 101.5%), the contact angles
increased remarkably and treated fibers have cleaner surface. The adhesion between bamboo
fiber and polypropylene (PP) as well as PP containing maleic anhydride grafted PP evaluated by
droplet method showed that the interfacial shear strength (IFSS) of the treated fiber increased
18.2% at PP and 39.4% at PP-MA-PP compared with untreated fiber; SEM image showed a
better adhesion between fiber and polymer. Compared to treatment by silane coupling agent, air-
plasma treatment can improve both the mechanical properties of fiber and adhesion while silane
coupling agent only the adhesion.
I - Introduction
In recent years there has been renewed the
interest in using the natural fiber to replace glass
fiber to get polymer composite which is eco-
friendly. Vietnam is the country where bamboo
is abundantly available and of diversified
species, polypropylene (PP) has a wide range of
application and a high value of property/price
therefore there is a good potential to use
bamboo fiber for polypropylene composite
application to get a motivated combination of
environmental friendliness and economical
feasibility. However, due to very different
natures of natural fiber and polymer there is a
poor wet ability and weak interfacial adhesion
between fiber and polymer which leads to poor
mechanical properties of composite. Surface
treatment of reinforcement fiber is one of the
effective solutions. Recently cold plasma
treatment, which is environmental friendly, is
considered as a promising physical treatment
method to modify the fiber surface for a better
adhesion. In this paper air-plasma has been used
to treat bamboo fiber surface for PP-composite
application. The mechanical properties,
morphology of fiber and adhesion between fiber
and PP have been investigated and compared
with that of silane treatment [1, 2, 4].
II - Experimental
1. Material
- Bamboo fiber was separated from bamboo
using mechanical method.
- Polypropylene.
- Yeniosil Silane GF31.
2. Plasma treatment
197
Usually surface treatment is under low-
pressure. However this study is carried out at
atmosphere pressure and room temperature in
order to simplify as much as possible the
technology for application.
Plasma is generally created by supplying a
sufficient amount of energy to a volume
containing a neutral gas. The energy may be
supplied in the form of electrical energy, heat,
ultra violet radiation or particle beams. In
technical plasma device, the input energy is
generally supplied as electrical energy [1, 2].
The major structural components of self-
made plasma device for this study are a bell
(chamber) and an excitation source (Fig. 1)
connecting with gas line, vacuum pump and
pressure controller.
Fig. 1: Plasma treatment device
Bamboo fibers reside directly in the
chamber housing the plasma. The chamber was
filled by air. Plasma excitation sources in this
test having high frequency of 12 KHz with the
plasma power of 50 W. The investigation was
carried out at room temperature, atmospheric
pressure.
3. Silane treatment
The bamboo fibers were treated with a
silane solution (the ratio 10 water to 90
methanol, 0.5% dicumine peroxide, 3% silane
by weight). CH3COOH solution was used for
adjusting the pH of around 3.5 to 4. After 1 hour
treatment fibers were dried at room temperature
and then heated for 1 hour at 120 degree
Celsius.
4. Tensile test of fiber
Bamboo fibers were separated from bamboo
and cut approximately 40 mm in length. Both
fiber ends were glued on the pieces of paper
(paper tabs of size 40x40 mm) for handing
purposes. During pulling, the specimens were
handled only by paper tabs and the working
zone of the fiber was not touched. Before
experimenting, fiber diameter was measured on
optical microscope with an optical objective of
4-40 times magnification. The test was carried
out on a computer connected LLOYD LRX Plus
machine. Measurements of load and
displacement were used to compute stress strain
curves for the fibers. All tests were
displacement controlled with the loading rate of
2 mm/min.
5. Determination of Fiber to Resin Interfacial
Shear Strength
The mechanical adhesion between
reinforcing fibers is usually characterized by the
interfacial shear strength (IFSS) determined by
such test methods as fiber pull-out,
microdebond test, fiber fragmentation test etc.
In this study droplet pull-out test was conducted
to evaluate the interfacial shear strength (IFSS)
between the fiber surface and resin.
Fibers were dried to allowable moisture
content and mounted on the cardboard. Drops of
PP resin was heated to melting point and then
dripped directly on the fiber. It would solidify in
several seconds. The maximal dimension of the
drops and embedded length of the fiber were
measured using an optical microscope with a
gratitude.
The separation of the droplet from the fiber
surface was made possible by use of two blades
adjusted laterally using vernier gauges.
Resistance of the droplet against the blades
provided the necessary force for generating the
shear stress between the resin droplet and the
fiber surface.
The IFSS,, is estimated as :
Cl
d
2
. =
198
where: d is the fiber diameter, m; is the
average fiber strength at critical, MPa; lC is the
critical length related to the average fiber length
at saturation fragmentation process, l as:
ll C 3
4
=
with lC is the average embedded length [3].
Fig. 2: Pull-out test
III - Results and discussion
1. Effect of plasma treatment on the
mechanical properties of fiber
Table 1 presents some mechanical properties of
bamboo fibers after plasma treatment with
various times.
Tab.1: Effect of plasma treatment on the
mechanical properties of bamboo fiber
Plasma treatment time, min
0 1 5 7
Mean stress
(), MPa 181.8 357.8 365.7 235.9
Young’s
modulus, GPa 19.72 27.79 39.73 26.32
, %
2.00 1.84 1.48 1.55
Weibull
modulus (m) 1.54 1.52 1.44 1.38
Normalizing
stress (0), kPa
15.57 16.81 25.38 98.15
The results show a significantly increase of
tensile property of fibers after air-plasma
treatment. Namely, mean tensile stress of
untreated fiber was 181.84 MPa and of treated
were 357.87 MPa (after 1 minute) and 365.77
MPa (after 5 minutes), respectively. Thus, stress
increased more than double after treated 5
minutes (up to 101.1%)
In the same conditions, Young’s modulus
increased 101.5% and elongation decreased
25.6%.
The tensile fracture surface of bamboo fiber
was observed in the scanning electronic
micoroscope and shown on the figure 2. We can
see that each bamboo fiber was even if small
(the average diameter was about 0.1 to 0.4 mm)
also set from many single fibers. The fiber
bundles arranged quite tightly and isotropic so
that sensating as a single fiber. However, the
orientation and bond on the whole fiber wasn’t
the same and fiber would be demolished at the
point that the bond was weakest.
Fig. 3: SEM image of the tensile fracture
surface of bamboo fiber
When producing plasma, there are not only
charged and neutral particles bombarding
samples, but it also produced light, such as UV
and others which may cause the polymerization
of lignin, making a significant increase in
mechanical properties of fiber due to
polymerized lignin- cellulose composite fiber
structure.
2. Contact angle
It can be seen that plasma treatment can
improve the contact angle of fiber with ethylene
glycol at nearly the same level as silane
treatment, however less in the case of water.
199
Tab. 2: Contact angle of bamboo fiber with
water and ethylene glycol
Water Ethylene
glycol
Untreated 39.3 39.1
1 56.4 42.4
2 64.5 43.2
Silane
treatment,
%silane 3 66.9 44.5
Plasma
treatment, 1min
49.4 44.0
3. Interfacial Shear Strength (IFSS)
The results in the table 3 show the slightly
increasing of IFSS value between bamboo fibers
with resin after air plasma treatment.
Tab. 3: IFSS between bamboo fibers with PP
Plasma
treatment time, minAdhesion Un-
treated
1 5 7
Silan
treatment
(3% w)
Specific
shear
strength,
MPa
2,06 2,25 2,28 2,18 2.72
IFSS,
MPa
3,09 3,38 3,41 3,09 4.3
With un-modified PP, IFSS between fiber
and resin increased from 3.085 MPa of
untreated fiber to 3.38 MPa after 1 minute
treatment, to 3.41 MPa after 5 minutes treatment
and then decreased to 3.09 MPa (plasma treated
for 7 minutes).
With PP grafted MAPP (5% MA),
adherence increased from 3.12 MPa to 3.31
MPa of 1 minute treatment, to 3.41 MPa at 5
minutes and got the highest value of 4.35 MPa
with plasma treated for 7 minutes, higher than
that of silane treatment. It can be seen that for
PP plasma treament can increase IFSS only
9.7%, however for PP grafted MAPP 39.52%.
4. Bamboo fiber surface morphology
There was clear difference on the plasma
untreated fiber surface (a), plasma treated (b)
and silane treated (c). Plasma treatment caused a
cleaner and smoother fiber surface as showed in
Fig. 4.
Tab. 4: IFSS between bamboo fibers with PP
grafted MAPP
Plasma
treatment time,
min
Adhesion Un-
treated
1 5 7
Silan
treatment
(3%w)
Specific
shear
strength,
MPa
2,08
2,1
2,27 2,94 2.76
IFSS,
MPa
3,12 3,31 3,41 4,35 4.13
In addition, plasma treatment lost the sets of
non-orientation on the fiber’s surface.
Therefore, the single fibers in the fiber’s bundle
would be oriented more closely. That’s fit to
increase significantly strain strength of fiber
after treated. Simultaneously, the interstice
between very close two single fibers also
became wider and deeper creating conditions
adherence better with resin but unremarkably.
Silane treatment also lost the sets of non-
orientation on the surface of fiber but the effect
got lower at plasma treatment. Silane treatment
only made fiber’s surface changed but without
changing the inner fiber’s structure, therefore,
strain strength of silane treated wasn’t almost
changed.
IV - Conclusions
Air plasma treatment has increased
remarkably the tensile properties of bamboo
fiber. Both mean stress and Young’s modulus in
suitable condition increased more than 101.15
and 101.5%.
Plasma treatment also has changed the
surface of fibers for a better adhesion.
200
(a) (b)
(c)
Fig. 4: SEM showing the surface of fiber
untreated (a), plasma treatment (b) and silane
treatment (c)
The adhesion between bamboo fiber and PP
has improved. The effect of plasma treatment at
PP grafted MAPP is higher than at PP, however
less than that of silane treatment at suitable
treatment condition of 5 minutes.
References
1. Essay (2005). Low-Temperature Plasma
Processing of Materials: Past, Present and
Future. Plasma Processes and Polymers,
Vol. 2: 7 - 15 (2005).
2. D. Sun, G. K. Stylios. Textile Research
Journal. Vol. 75(9), P. 639 - 644 (2005).
3. Arnold N. Towo, Martin P. Ansell. Third
International Workshop on Green
Composites. P. 190 - 194 (2005).
4. X. J. Dai, L. Kviz. Study of Atmospheric
and Low Pressure Plasma Modification on
the Surface Properties of Synthetic and
Natural Fibres, Textile and Fibre
Technology (2001).
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