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Original Article
03-Mar-2016
ameer, muhammad; national textile university, Textile Composite Materials
Research Group
Shaker, Khubab; National Textile University, Weaving department
Nawab, Yasir; National Textile University Pakistan, Textile Engineering
Ahmad, Sheraz; National Textile University, Textile Composite Materials
Research Group
Ashraf, Munir; National Textile University, Textile Processing department
Nasir, Muhammad; University of Engineering & Technology, Taxila,
Mechanical Engineering Department
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JRP-16-0171
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Abstract:
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Keyword:
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Page 1 of 22
Reduction in the moisture regain of jute composites and studying their ageing
properties
Muhammad Haris Ameer1, Khubab Shaker1, Yasir Nawab1*, Sheraz Ahmed1, Munir Ashraf1,
Muhammad Ali Nasir2
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Textile Composite Materials Research Group, Faculty of Engineering and Technology, National
Textile University, Faisalabad-Pakistan
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The natural fibers reinforced composite materials tend to absorb the moisture when they are
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exposed to humid environment. The aim of this study was to lower the moisture regain of natural
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fiber (jute) and the subsequent composite samples by using the fluorocarbon, hydrocarbon and
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hybrid fluorocarbon treatments. A significant reduction in the moisture regain was observed for
the treated reinforcements and their respective composites. The treated fabric reinforced
composites also showed good mechanical (tensile and flexural) properties as compared to
untreated fabric composite. The ageing of jute composites was conducted by water immersion
tests and its effect on the mechanical properties was studied. It was concluded that treated fabric
composites especially hybrid fluorocarbon and fluorocarbon retain their mechanical properties
even after moisture ageing, and their diffusion coefficients are also lower than the untreated
fabric composites.
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Introduction
A composite can be defined as a combination of two or more chemically distinct materials
which when combined, have improved properties over the individual materials
1, 2
. Bio-
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composites are the materials in which plant based natural fibers such as jute, hemp flax kenaf
and/or sisal are reinforced with either biodegradable or non-biodegradable matrices. In polymer
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matrix composites, the use of natural fibers as reinforcement, to produce the low cost materials,
has generated much interest recently 3, 4. The environmental concerns and the consumer demand
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compelled the material manufacturers to think about the environmental friendly materials. These
materials are also a better choice as replacement of nonrenewable materials such as glass fiber.
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The advantages of natural fibers over traditional glass fibers are: environmental friendly, low
density, biodegradability, ease of availability, annually renewable, less respiratory irritation, and
durability without using toxic chemicals and low cost 5, 6.
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A number of researchers developed their studies in the field of natural fiber reinforced plastics.
Some studies are focused on the mechanical properties of short fiber reinforced plastic, mostly
used as structural composites in automotive industry such as panels, doors, roofs and covers 7.
There are also some demerits of using natural fibers which are non-uniform quality, swelling due
to moisture regain, incompatibility with resin, dimensional instability 8. Among the different
treatment procedures, acetylation, mercerization, Sodium chlorite treatment, enzymatic,
Benzoylation, per oxide, graft copolymerization, and plasma treatments etc. are a few systems
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for surface treatments of natural fibers that have been used. Acetylation of natural fibres
introduces plasticization to natural cellulosic fibres, mostly applied to stabilize the cell wall of
wood cellulous against the moisture, environmental degradation and for improving the
dimensional stability. When apply the acetic anhydride on ligno cellulosic material it reacts with
hydroxyl groups of cellulose and also prevent the diffusion of the reagents. A flax/PP composite
made after treating the flax fibre showed 18% increase degree of acetylation and also increase in
tensile and flexural strengths 9.
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Mercerization is a process in which natural fibres are treated with alkali which leads to
fibrillation and cause the breakdown of bundles of fibres into smaller fibres 10. There by leads to
develop a rough surface topography that results in better fibre matrix interface adhesion and an
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hydroxide gave the best results when they treated flax fibre into 2.5, 5, 10, 15, 18, 20, 25 and
30% NaOH
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. It was observed that 5, 18, and 10% were the best concentration for
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mercerization. The researcher also treated the jute fibres with 5% NaOH solution for 0, 2, 4, 6
and 8 hours at 300C. Then these fibers dried at room temperature for 48 hours followed by oven
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. Several researchers
reported that mercerization leads to increase in the amount of amorphous cellulose and also
decreases the hydrogen bonding
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Enzymatic treatment is very useful and interesting step when enzymes are used in combination
with chemical and mechanical methods for modification of materials. The fact is that enzymes
are efficient catalysts and are highly specific in their work under mild and energy saving
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hydroxide and benzoyl chlorite (C6H5COCl) solution could be used for treatment of surface of
sisal fibres. The fibres were alkaline pre-treated to activate the hydroxyl group of lignin and
cellulose of fibres. Then fibres were immersed in 10% NaOH and benzoyl chloride solution for
15 min. After that fibres were soaked in ethanol for 1 hour to remove benzoyl chloride and
finally were washed and dried at 80C0 for 24 hour, surface modification was observed and also
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Plasma treatment is very effective treatment method to modify the surface of natural polymers
without any change in their bulk properties. The plasma discharge can be generated by either
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cold plasma treatment or corona treatment. The type of ionized gas influenced the modification
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of the wood and synthetic polymer surfaces. Another study reported an avenue to activate a
wood surface for getting better adhesion with polyolefin by exposure to plasmas. The plasma
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. Further, the
recent study have the number of the polar component of surface energy of pine wood for plasma
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modification that include power, distance of samples to plasma source, treatment time, stability
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of plasma treatment and type of gas. Corona discharge was used to treat the pulp sheets having
moisture contents of up to 85% the process was carried out in the presence of air and nitrogen
atmospheres moreover, chemical modification of the sheets were evaluated by dye 20.
All the naturel fibres absorb water when they are exposed to moist environment. The diffusion
coefficient tells us what is rate of sorption of water in the material 21. It was reported that alkali
scouring exhibited good ability to remove non-cellulose materials from natural fibers, and the
results were further confirmed by the composition analysis 22. Changes in fineness and moisture
regain were obviously affected by the degree of non-cellulose removal.
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Jute is a biodegradable plant fiber widely used for structural application in composite materials.
The aim of this study was to lower the moisture regain of natural (jute) fibres by chemical
treatments and investigate the effect of these treatments on mechanical properties of
reinforcements and their subsequent composites. The moisture ageing properties and diffusion
coefficients of the composites were also investigated.
Experimental
Materials
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Plain woven jute fabric having areal density of 225 3 g/m2 was used as reinforcement. The
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warp and weft linear density was 200 tex and 350 tex respectively, while warp density was 4
and weft density was 3.5 threads/cm. Three types of hydrophobic chemical finishing was
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Fabric treatments
NaOH = 10 g/L
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Wetting agent = 2 g/L (to lower the surface tension and enhance the wettability)
Sequestering agent = 2 g/L (to remove minerals, heavy metal ions, etc.)
Mercerization of jute fabric was performed with sodium hydroxide (concentration 18g/l). The
temperature of solution temperature was kept 60 C while time of the treatment was 60 sec. The
reinforcement was then washed with hot water and subsequently with cold water.
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Three types of hydrophobic chemical finishing was performed using OLEOPHOBOL CPC
(hybrid-fluorocarbon), PHOBOL RSH (fluorocarbon), and PHOBOL CPC (hydrocarbon),
produced by HUNTSMAN. Solution of these chemicals were prepared in water at room
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temperature and acetic acid was added to the bath (to maintain pH of 5-7). The jute fabric was
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dipped in the solution and padded to achieve a liquor pick-up of approximately 80%. After that
fabric was dried at 110-130C in the oven.
Composite fabrication
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The composites were fabricated using four layers of the jute reinforcement, by vacuum infusion
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technique. The composites were cured at room temperature for 3 hours and post-cured at 120C
for 2 hours in heating oven. The fibre volume fraction (Vf) was maintained at 33% in all the
composite samples.
Six different composite samples were fabricated as shown in Table 1. The composite sample S1
is produced with untreated reinforcement, while S2 produced with mercerized reinforcement.
The samples S3, S4 and S5 composites were fabricated using reinforcements treated with
PHOBOL CPC, OLEOPHOBOL CPC, and PHOBOL RSH respectively. The concentration of
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difference between conditioned fabric mass and the oven-dry mass. The moisture regain was
calculated using the equation (1).
% =
100
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(1)
The tensile testing was performed both for the reinforcement and composite samples. The
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tensile strength and elongation of jute reinforcements (treated and untreated) was tested
according to ISO 13934-1 test method while ASTM D3039 was followed to test the tensile
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The flexural properties were tested by three point bending test according to ASTM D7264. The
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flexural strength () and flexural modulus (Ef) of composites was calculated using the equation
(2), (3) and (4).
Flexural strength, =
Maximum strain, =
3'(
2*,
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(,
(2)
(3)
(4)
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Where, L is the support spam (mm), h is the thickness of the beam (mm), b is the width of beam
(mm), P is the maximum applied force, and is the mid-span deflection.
Sorption behaviour
There exist a number of models to express the moisture regain of composite materials. The
percentage water absorption is calculated with the mass difference dry composite samples and
samples dipped in water as given in equation (1). For one dimensional (1D) moisture absorption,
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when composite is exposed on both sides to the same environment, moisture regain G can be
calculated using the equation (5).
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2? + 1, = , D
Moisture regain, G =
= 1 ,>
AB
C
E
ms mi
=
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(5)
GHI
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Where, ms is the mass of moisture in saturated state, and mi is the initial moisture regain of the
material. D is the diffusivity of the composites, h is thickness of specimen, t is the time and j is
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the summation index. The diffusion coefficient is an important parameter in Ficks law. Solving
the diffusion equation for the weight of moisture, and rearranging in terms of the percentage
moisture content, the following relationship is obtained:
4K
L . ND
Moisture %, M =
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(6)
Where Mm is the equilibrium moisture content of the specimen. Using the weight gain data of the
material with respect to time, a graph of weight gain versus time is plotted. The coefficient of
diffusion (D) defined as the slope of the normalized mass uptake against and has the form of
equation (7).
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S ,
D = R
T
4K
(7)
Where, k is the initial slope of a plot of M (t) versus t1/2, Mm is the maximum weight gain and h
is the thickness of the composites.
Moisture ageing of composites
The moisture sorption of natural fibre reinforced composite measured when they are dipped in
the distilled water
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behaviour and the effect of this moisture sorption on the mechanical (tensile and flexural)
properties were also checked from one to four week.
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Moisture regain
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The moisture regain of untreated, mercerized, and chemical treated (PHOBOL CPC,
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OLEOPHOBOL CPC, and PHOBOL RSH) reinforcement was determined and the results are
shown in figure 1. It can be observed that the moisture regain of mercerised reinforcement has
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Mercerisation of the fabric causes changes in the molecular orientation, and fibre becomes
uniform due to formation of canals or spaces. The alkaline treatment is reported to have two
effects on the fibre25: (1) increases surface roughness resulting in better mechanical interlocking;
and (2) increases the amount of cellulose exposed on the fibre surface, thus increasing the
number of possible reaction sites. Due to this reason, the mercerized fabric has higher moisture
regain as compare to untreated reinforcement.
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The moisture regains of reinforcement treated with chemicals PHOBOL CPC, OLEOPHOBOL
CPC, and PHOBOL RSH were found 6%, 4.8%, and 5.3% respectively. The reinforcements
treated with the chemicals have lower moisture regain because the chemical surface tension lies
between 14-28 mN/m.
There is a significant difference in moisture regain of reinforcements and their corresponding
composites. It is because that the composites have 67% of resin which is hydrophobic in nature.
The moisture regain of neat resin samples is only 0.21%. The mercerized reinforcement has the
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improved wettability as compared to untreated and therefore will absorb more resin, and a good
interface is formed between resin and reinforcement. Therefore, the composite sample S2
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much difference in the moisture regain values. In treated composites, the S4 (OLEPPHOBOL
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CPC) have lesser moisture regain because the reinforcement is treated with a hybrid
fluorocarbon, which is soil release copolymer having fluorine and hydrophobic part. The
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hydrophobic part is involved in establishing a good interaction between resin and reinforcement,
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while fluorine has lower surface tension. It results in a composite material having lower
moisture regain as compared to the others. The S3 (PHOBOL CPC) and S5 (PHOBOL RSH)
composite samples do not have much difference in results, having 1.7% and 1.6% moisture
regain respectively. This minute difference may be attributed to the lower surface tension of
fluorocarbon as compared to hydrocarbons.
Moisture kinetics of the all the composite samples was studied and graph of moisture regain was
plotted against the square root of time as shown in Figure 3.
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From the Figure 3, it can be observed that there is a steady increase in the moisture regain of all
the samples up to 36000 sec. It is clear from the graph, after 10800 sec the equilibrium is
established of all the composites. The untreated reinforced composite has more water absorption
than other composites because the interface developed between resin and reinforcement was not
as good as other composites. Another reason is that the untreated reinforcement can uptake a
higher amount of moisture. The composites reinforced with chemical treated jute have lesser
moisture absorption when they are exposed to water.
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Diffusion coefficient
The diffusion coefficient of resin and different composite samples are given in Table 2.
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From the Table 2, it can be observed that the diffusion coefficient of untreated composite is
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higher than the other composites. This is because the moisture regain of untreated composite is
highest among the other. The lowest diffusion coefficient is exhibited by the composite sample
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S4 (treated with PHOBOL CPC). It is due to the fact that the PHOBOL CPC contains hybrid
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fluorocarbon. Hybrid fluorocarbon is made of soil release copolymer and has fluorine and
hydrophobic part in it. Hydrophobic part is involved in making the good interaction between
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resin and reinforcement and the fluorine have lesser surface tension. Lower the surface tension
lowering the moisture regain of water. The diffusion coefficient of neat resin is lowest of all
because it is hydrophobic in nature.
Tensile testing
The tensile properties of simple reinforcement was performed on tensile testing machine, three
samples were tested for each and average values were reported in Figure 4.
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It can be clearly seen that tensile strength of chemical treated reinforcement (PHOBOL CPC,
OLEOPHOBOL CPC, and PHOBOL RSH) is higher than untreated and mercerized jute
reinforcement. This is perhaps due to the fact that the chemical treatment restricts the slippage
of individual yarns by developing cross linking in the reinforcement. The -OH groups present in
the cellulosic fibres are responsible for hydrogen bonding. The chains slide over each other
when cellulosic material is stretched and tends to recover back when external force is removed.
But when a higher concentration of fluorocarbons is applied, almost all of the -OH groups react
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with fluorocarbons and the hydrogen bonding within the cellulosic material is restricted; thus
prohibiting the chain sliding. The mercerized reinforcement has greater tensile strength than
untreated, because it swells the fibre and when they are stretched the swell fibres give the higher
tensile strength 26.
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The untreated composite has lowest tensile strength. Mercerized and treated with PHOBOL
CPC have almost same tensile strength. Composites treated with OLEOPHOBOL CPC and
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PHOBOL RSH composites have highest tensile strengths among composites samples.
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The effect of ageing on the tensile strength of composite materials is shown in Figure 5. It can
be observed that the tensile strength of composite fabricated with treated reinforcements is
higher, and is retained with moisture ageing. The initial strength of untreated reinforced jute
composite is 10.044 MPa, and a decrease is observed in the tensile strength when exposed to
water. The untreated reinforcement fabric absorbs water, which causes the fibers to swell and
damages the interface between matrix and reinforcement. Therefore, the exposure of untreated
composites to the environment or water results in loss of strength. The initial strength of
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Page 13 of 22
mercerized composite is 11.98 MPa. The mercerized reinforcement also have great tendency to
absorb the water but it has improved interface, as discussed earlier, and loss in strength is small.
The chemical treated reinforced composite (PHOBOL CPC, OLEOPHOBOL CPC, and
PHOBOL RSH) have tensile strength 12.54, 15.71 and 15.81 MPa respectively. The strength
loss in these composite is also small due to very low moisture uptake and improved interface
between resin and the reinforcement.
The cellulosic materials have -OH group, and develop hydrogen bonding which is responsible
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for the stretching and sliding of chains. When cellulosic materials are treated such materials with
the fluorocarbon replaces or reacts with the -OH groups and prohibits the sliding of the chains as
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shown in the Figure 6. It will result in good tensile strength of the material treated with such
chemicals (PHOBOL CPC, OLEOPHOBOL CPC, and PHOBOL RSH).
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The replacement of -OH group with the active fluorocarbon also lowers the moisture regain, and
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it retains a good interface. As a result it will not lose much strength when exposed to moist
environment.
Flexural properties
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The three point bending test method was used to determine the flexural strength of composite,
while test rate was 1 mm/min. The length of support spam was 96 mm, while width of
composite sample was 13 mm. The maximum applied force and deflection was obtained, and
flexural strength and modulus was calculated as discussed earlier. The flexural testing was
performed for the actual and aged samples, and the results are reported in Figure 7 and 8.
It is clear from the Figure 7 that the composites treated with the chemicals have highest flexural
strength as compared to the mercerized and untreated reinforced composites. The reason behind
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is same as that of tensile strength, i.e. good adhesion between matrix and reinforcement. The
composites treated with the chemicals have good interface and there is a gradual decrease in the
flexural properties, when these composites are exposed to the environment. On the other hand a
significant loss is observed in the flexural strength of untreated composite materials.
The flexural modulus of samples shown in the Figure 8. It is clear from the results that there is a
decrease in the flexural modulus of the natural fibre reinforced composites with the passage of
time. The composite treated with chemical have good flexural modulus as compare to the
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mercerized and the untreated reinforced composites. The mercerized composites have good
modulus as compared with the untreated reinforced composites. These composites have the
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Conclusion
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The moisture regain was significantly reduced in chemical treated reinforcements and their
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subsequent composite. The hybrid fluorocarbon (Oleophobol CPC) treated reinforced composite
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showed lowest moisture regain and diffusion coefficient values, while untreated composites
showed highest. Their moisture sorption behaviour, when exposed to water, was almost double
than the chemical treated reinforced composites. A significant difference in the mechanical
properties of treated and untreated composites was also observed. The chemical treated
fluorocarbon (Oleophobol RSH) and hybrid fluorocarbon (Oleophobol CPC) composite showed
good tensile and flexural properties. The loss in strength of treated fabric composites was small
as compared to untreated composites due to good fibre-matrix interface.
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S. No.
Sample ID
Reinforcement
Fabric treatment
S1
Jute
Untreated
(g/l)
-
S2
Jute
Mercerized
18
S3
Jute
PHOBOL CPC
40
S4
Jute
OLEOPHOL CPC
40
S5
Jute
PHOBOL RSH
40
S6
Neat resin
r
Fo
Pe
er
Saturation moisture
Samples
Uptake, Mm (%)
K value, plotted
Re
Diffusion coefficient
Mm versus
D (10-5 m2/s)
0.068
1.3
25
Mercerized
17.6
0.045
1.15
PHOBOL CPC
16.5
0.042
1.14
OLEOPHOBOL CPC
14.9
0.024
0.45
PHOBOL RSH
15.2
0.032
0.78
Resin
0.93
0.0019
0.43
ew
Untreated
vi
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8
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Page 19 of 22
16
Moisture regain %
14
12
10
8
6
4
2
0
r
Fo
Untreated
Mercirized
Phobol cpc
Oleophobol cpc
Phobol RSH
Reinforcement
er
Pe
3.5
3
vi
2.5
2
ew
Moisture regain %
Re
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
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23
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25
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27
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30
31
32
33
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40
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42
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48
49
50
51
52
53
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60
1.5
1
0.5
0
Untreated
Mercirized
Phobol cpc
Resin
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30
25
Moisture regain %
20
15
Untreated
Mercirized
Phobol CPC
Oleophobol CPC
Phobol RSH
Resin
10
r
Fo
0
0
200
400
Pe
600
800
1000
1200
1400
1600
1800
er
Re
300
250
ew
350
vi
1
2
3
4
5
6
7
8
9
10
11
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200
150
100
50
0
Untreated
Mercerized
PHOBOL CPC
OLEOPHOBOL CPC
PHOBOL RSH
Reinforcements
Page 21 of 22
18
16
14
12
10
8
Untreated
Mercerized
PHOBOL CPC
r
Fo
OLEOPHOBOL CPC
PHOBOL RSH
2
0
Initial
1 Week
2 Week
Pe
3 Week
4 Week
Ageing time
er
ew
vi
Re
1
2
3
4
5
6
7
8
9
10
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60
40
30
Untreated
Mercerized
PHOBOL CPC
OLEOPHOBOL CPC
PHOBOL RSH
20
10
Pe
0
Initial
1 Week
2 Week
3 Week
4 Week
Ageing time
er
Re
3.5
vi
Untreated
Mercerized
PHOBOL CPC
OLEOPHOBOLCPC
PHOBOL RSH
ew
50
r
Fo
1
2
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2.5
2
1.5
1
0.5
0
Initial
1 Week
2 Week
Ageing time
3 Week
4 Week