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DOI 10.

1515/secm-2013-0318Sci Eng Compos Mater 2014; aop

Vinay K. Singh*

Mechanical behavior of walnut (Juglans L.) shell


particles reinforced bio-composite
Abstract: In the present work walnut particle reinforced
composite material was developed. Ten wt%, 15 wt%,
20wt% and 25 wt% (weight percentage) of walnut particles were mixed with epoxy resin (CY-230). Scanning electron microscopy (SEM) shows that the walnut particles
were well dispersed in the epoxy resin matrix. Addition
of walnut particles increased the modulus of elasticity
of the bio composite. Addition of walnut particles in bio
composite decreased the ultimate strength both in compression and tension. However, addition of walnut particles in bio composite increased the hardness. Flexural
modulus of elasticity also increased with increasing walnut particles weight percentage, whereas flexural strength
and strain decreased with increased weight percentage of
walnut particles.
Keywords: composite material; environment; polymer;
walnut particles.

*Corresponding author: Vinay K. Singh, College of Technology,


G. B. Pant University of Agriculture and Technology, Pantnagar,
Uttarakhand-263145, India, e-mail: vks2319@yahoo.co.in

1 Introduction
Composite is a material formed with two or more components, combined as a macroscopic structural unit with
one component as a continuous matrix, and other as reinforcements with significantly different physical or chemical properties, which remain separate and distinct on a
macroscopic level within the finished structure. Normally,
the matrix is the material that holds the reinforcements
together and has lower strength than the reinforcements.
Most commercially produced composites use a polymer
matrix material called as resin solution [1].
Composite resin technology has continuously evolved
since its introduction by Bowen [2] as a reinforced Bis-GMA
system. A major breakthrough in composite technology
was the development of photo-curable resins [3]. Continued development resulted in materials with reduced
particle size and increased filler loading that significantly
improved the universal applicability of light-cured composite resins [4].

As epoxy resins are a good solvent they are widely used


in industrial applications because of their high mechanical and adhesion characteristics and chemical resistance
together with their curability in a wide range of temperatures without the emission of any volatile byproducts.
The properties of epoxy-based organic/inorganic filled
composites can be finely tuned by an appropriate choice
of the structures of epoxy pre-polymer and hardener, type
and amount of inorganic filler. The composites have many
advantages over traditional silica powder or inorganic
mineral filled materials, including lower cost, lighter
weight, environmental friendliness and recyclability.
With growing environmental awareness, ecological concerns and new legislation, bio particle reinforced
plastic composites have received increasing attention
during recent decades. Particleboards are of very recent
origin. The important aspect that has impacted favorably
on the development of these composite materials is the
possibility of incorporating waste agro-waste (agricultural residues including stalks of most cereal crops, rice
husks, coconut fibers, bagasse, maize cobs, peanut shells,
and other wastes) product and recycled plastics with the
advantage of a positive eco-environmental impact. Due to
a worldwide shortage of trees and environmental awareness, research on the development of composite preparations using various waste materials is being actively
pursued [57]. Based on a literature search [6, 810],
among the possible alternatives, the development of composites using agricultural byproducts or agro-waste materials are currently the center of attention.
Particleboards are among the most popular materials
used in interior and exterior applications such as floor,
wall and ceiling panels, office dividers, bulletin boards,
cabinets, furniture, counter tops and desk tops [11]. The
production of particleboard can be related to the decided
economic advantage of low cost raw wood material,
inexpensive agents and simple processing. Therefore,
agro-waste instead of wood is widely used in the manufacturing of particleboard. Among the raw materials are
almond shell [12], wheat straw [13], bamboo [14], cotton
seed hulls [15], flax shiv [16], rice straw-wood [17], vine
prunings [18], coir pith [19] and wood flour [20]. Polymers
such as urea-formaldehyde, phenol-formaldehyde, melamine formaldehyde, polyethylene and polyvinylidene are

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2V.K. Singh: Mechanical behavior of walnut shell particles reinforced bio-composite

commonly used as binders. Urea formaldehyde is the most


economic and useful adhesive among these binders.
The aim in the preset investigation with the objectives
was to develop a composite material containing different
percentages of walnut particle as the filler material and
investigate the mechanical behavior of different composites.

at 8 wt% of hardener (HY-951) when mixed with resin (CY230). Therefore in the present study 8 wt% of HY-951 has
been used.

2.3.2 Walnut particles


It was mixed with the resin up to the limits and the flowability of the mixture was maintained for the purpose of
pouring the mixture into the vertical mould. No compression load was applied in this arrangement. The size of the
walnut particles was controlled by sieving with ASTM 40
and ASTM 80.

2 Materials and methods


2.1 Matrix material
2.1.1 Epoxy resin CY-230
Epoxy resin is widely used in industrial applications
because of its high strength and mechanical adhesiveness
characteristic. It is also a good solvent and has good chemical resistance over a wide temperature range. Araldite
CY-230 purchased from M/s Petro Araldite Pvt. Limited
(Chennai, India) was used in the present investigation.
2.1.2 Hardener HY951
Hardener HY-951 purchased from M/s Petro Araldite Pvt.
Limited (Chennai, India) was used as the curing agent. In
the present investigation 8 wt% hardener HY-951 with epoxy
resin (CY-230) was used in all the material developed. The
weight percentage of hardener used in the present investigation was as per recommendation of Singh and Gope [21].

2.2 Reinforcing element


2.2.1 Walnut particles
The walnut particles are residues widely generated in
high proportions in the agro-industry by the grinding of
walnut shell. It is generally light to dark brown in color.
The walnut shells are underutilized, renewable agricultural material. In the present study weight fraction (Vf ) of
walnut particles varied from 1025. Walnut particle purchased from Allied Buss., Haldwani, India.

2.4 Method
Epoxy resin (CY-230), hardener (HY-951), and walnut particles with different weight percentages were used. Different weight percentage (wt%) of walnut particles (15, 20,
25, 30 wt%) and epoxy resin were mixed by mechanical
stirring at 3000 rpm. Based on the curing curve [23], the
solution obtained by mixing of walnut particles with resin
was kept in the furnace at a temperature of 90 10C for
2h [21]. At intervals of 30min the solution was taken out
of the electric furnace and remixed by a mechanical stirrer
at the same speed. After 2h the whole solution was taken
out and allowed to cool to 45C. When a temperature of
45C was attained the hardener HY-951 (8 wt%) was mixed
immediately [21]. Due to the addition of hardener a highly
viscous solution was obtained which was remixed at high
speed by the mechanical stirrer. The viscous solution so
obtained was poured into different moulds for sample
preparation. Tensile, compression and bending tests were
conducted on a 100 kN servo hydraulic universal testing
machine (ADMET, USA) under displacement mode of
control of 1 mm/min. The results are presented and discussed in subsequent sections.

3 Results
3.1 Density

2.3 Optimization of weight percentage


2.3.1 Hardener (HY-951)
According to Misra and Singh [22] the per cent elongation,
yield strength and Young modulus reached the maximum

Density is one of the most important properties of the particle board material. The density of walnut particles reinforced composite for various weight percentages along
with density of epoxy resin are presented in Table 1.
Table 1 reveals that increase in weight percentage of
reinforced particles, i.e., the walnut particles in the resin

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V.K. Singh: Mechanical behavior of walnut shell particles reinforced bio-composite3

Table 1Density of walnut particle reinforced composite.


S. no.

Walnut particle
(10 wt%)
(g/cm3)

Walnut particle
(15 wt%)
(g/cm3)

Walnut particle
(20 wt%)
(g/cm3)

Walnut particle
(25 wt%)
(g/cm3)

Epoxy
(g/cm3)

1
2

Mean
SD

1.169
1.172
1.168
1.168
0.0020

1.161
1.167
1.163
1.161
0.0031

1.159
1.164
1.159
1.159
0.0029

1.157
1.156
1.157
1.156
0.0006

1.179
1.184
1.186
1.179
0.0036

solution decreases the density. This decrease in density of


25 wt% is about 1% of 10 wt%. The decrease in density can
be related to the fact that the walnut particles are light but
occupy a substantial amount of space. Hence there is a
general decrease in the density of all the composite materials with regard to the epoxy resin.

3.2 Water absorption capacity


Water absorption capacity is another crucial factor to be
taken into account when considering the effect of water
on the composite material developed. The soaking period
is 24h taken as constant for all combinations of material.
The effect is presented in Table 2.
The effect of water absorption was important in case
the material that has been developed when used for applications comes in contact of water. The water absorption
capacity was found to be higher for 25 wt% of walnut particle reinforced composite as compared with lower weight
percentage of walnut particles. This substantial increase
with regard to the epoxy resin could be because the
walnut particles here have maximum capacity for water
absorption compared to the resin particles.

3.3 Scanning electron microscope (SEM)


The state of dispersion of particles into the resin matrix
plays a significant role with regard to the mechanical

properties of the composite. In the present investigation SEM was carried out on LEO435V6 instrument and
voltage was kept 20kV for bio composite containing different weight percentage of walnut particles to evaluate
the particle size, particle matrix interface and dispersion
of walnut particles in the epoxy resin matrix.
Figure 1(A) and 1(B) show the SEM micrographs of different bio composite material investigated in the present
work. In all cases, good dispersion of walnut particles in
the resin matrix has been observed. Figure 1(A) and 1(B)
show the SEM micrograph of composite containing 10
wt% and 25 wt% of walnut particles, respectively. It is
seen in the figures that walnut particles are well dispersed
in the epoxy resin matrix in a preferred orientation.
Hence, from the above micrographs it is can be concluded that due to uniform dispersion of walnut particles
in epoxy resin, a remarkable effect on the mechanical
properties may be obtained.

3.4 Mechanical properties


3.4.1 Tensile stress-strain curve
The mechanical properties of the walnut particles filled
epoxy resin bio composite materials were determined
by a 100 kN ADMET Servo hydraulic Universal Testing
Machine at 1 mm/min strain rate under displacement
control mode. The tensile stress-strain curve for walnut
particles reinforced composite materials containing

Table 2Water absorption capacity.


S. no.

Walnut particle
(10 wt%)

Walnut particle
(15 wt%)

Walnut particle
(20 wt%)

Walnut particle
(25 wt%)

Epoxy resin

2
3

Mean
SD

0.554%
0.557%
0.548%
0.553%
0.000045

0.573%
0.579%
0.569%
0.573%
0.00005

0.581%
0.583%
0.582%
0.582%
0.00001

0.613%
0.629%
0.619%
0.620%
0.00008

0.543%
0.549%
0.546%
0.546%
0.00003

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4V.K. Singh: Mechanical behavior of walnut shell particles reinforced bio-composite

10wt%, 15 wt%, 20 wt% and 25 wt% of walnut particles


reinforced composite is shown in Figure 2. All tests were
conducted as per ISO in 100 kN Servo hydraulic Universal Testing Machine. Brittle behavior can be seen in the
stress strain diagram due to addition of walnut particles in the epoxy resin matrix for all weight percentages
of walnut particles. However, it is seen that beyond 10
wt% of walnut particle the stress strain behavior does
not increase, therefore there is no improvement in load
bearing capacity.

3.4.2 Tensile properties

Figure 1(A) 10 wt% of walnut particles. (B) 25 wt% of walnut


particles.

Tensile tests were carried out at strain rates of 1 mm/min.


The properties of the walnut particle of 10, 15, 20 and
25wt% reinforced composite are presented in Table 3.
The results of the ultimate tensile strength, percentage elongation in length and modulus of elasticity are
shown in the Table 3 for strain rate of 1 mm/min. Remarkable differences can be seen on the ultimate tensile
strength of the bio composite material between 10 wt%
and over 10 wt% of walnut particles. It can be noticed that
for all specimens the ultimate tensile strength is highest
for the 10 wt% of walnut reinforced composite and is
163 MPa. Also, 10 wt% of walnut reinforced composite is
shown as maximum percentage elongation from amongst
the composite materials. It is seen that addition of walnut
particles significantly affects the ultimate strength and

180
160
140

Stress (MPa)

120
100
80
10 wt% walnut powder

60

15 wt% walnut powder


40
20 wt% walnut powder
20
0
0.00

25 wt% walnut powder

0.01

0.02

0.03

0.04

0.05

0.06

0.07

Strain

Figure 2Stress-strain diagram under tension for different wt% of walnut particles.

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0.08

0.09

V.K. Singh: Mechanical behavior of walnut shell particles reinforced bio-composite5

Table 3Tensile properties of the composite materials.


Property

Walnut particle
(10 wt%)

Walnut particle
(15 wt%)

Walnut particle
(20 wt%)

Walnut particle
(25 wt%)

Ultimate tensile strength (MPa)


% Elongation in length

Modulus of elasticity (MPa)

163.00
8.49
2013.00

119.00
7.29
1388.00

114.00
6.93
1333.00

104.00
6.85
1328.00

percentage elongation. The ultimate tensile strength and


the modulus of elasticity of 10 wt% of walnut board are
almost 1.37 and 1.45 times higher than 15 wt% walnut
board, 1.43 and 1.51 times higher than 20 wt% walnut
board and 1.57 and 1.52 times higher than 25 wt% walnut
board. It is true for all particulate composite material;
no material can be fabricated which has more ultimate
strength from matrix material if reinforced material is
mixed at macro level. These behaviors are also shown in
Figure 3.
On the basis of results obtained the effect of weight
fraction (Vf ) on modulus of elasticity and ultimate strength
are shown in Equations 1 and 2 with a correlation coefficient greater than 0.99.
Modulus of elasticity (MPa) = -0.69Vf3 + 42.44Vf2
-858.1Vf + 7040.0

(1)

Ultimate strength (MPa) = -0.058Vf3 + 3.42Vf2


-66.43Vf + 544

3.4.3 Compressive strength


The compressive strength properties of the walnut particle
filled epoxy resin composite materials were determined
by 100 kN ADMET Servo controlled Universal Testing
machine at 1 mm/min strain rate under displacement
control mode.
The results of the compressive test are shown in
Table 4. All tests were conducted under displacement
control mode. Stress strain diagram obtained from compressive test is shown in Figure 4.
A remarkable difference can be noticed in the value of
the compressive strength with different weight percentage

205

9.0

190
8.5
175

Ultimate strength, MPa


Modulus of elasticity/10 MPa

160

8.0

% Elongation

145

7.5

Elongation (%)

Ultimate strength, Modulus of elasticity

(2)

130
7.0
115
6.5

100
10

12

14

16
18
20
Walnut particles (wt%)

22

24

Figure 3Variation of ultimate tensile strength, modulus of elasticity and elogation for different weight percentage of walnut reinforced
composite.
Table 4Compressive properties of the composite materials.
Property

Walnut particle
(10 wt%)

Walnut particle
(15 wt%)

Walnut particle
(20 wt%)

Walnut particle
(25 wt%)

UTS (MPa)

% Reduction in length

Modulus of elasticity (MPa)

261.00
49.95
1578.00

231.00
46.61
1668.00

191.00
45.69
2321.00

135.00
31.48
2391.00

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6V.K. Singh: Mechanical behavior of walnut shell particles reinforced bio-composite

300

Ultimate strength (MPa)=-8.36Vf +350.8.

(4)

Stress (MPa)

250
200

3.4.4 Hardness

150

As known, hardness implies a resistance to indentation,


permanent or plastic deformation of material. In a bio
composite material, filler weight fraction significantly
affects the hardness value of the hybrid composite material. Hardness values measured on the Rockwell M-scale
showing the effect of weight percentage of walnut particles on the hardness values of hybrid composite are
presented in Table 5. Variation of hardness with walnut
particles weight percentage is shown in Figure 6.
It is found that hardness of neat epoxy resin (CY-230
+8 wt% of HY-951) is 56.4 MRH. The hardness of the fabricated composite made of epoxy resin and 25 wt% is the
maximum and is 89.8 MRH. The hardness increases with
increase in walnut particles weight percentage. Figure 7
shows that with increasing of hardness, ultimate strength
in compression as well tension deceases and material
behaved in a brittle manner.

100

10 wt% of walnut particle


15 wt% of walnut particle
20 wt% of walnut particle
25 wt% of walnut particle

50

0
0

0.1

0.2

0.3

0.4

0.5

Strain

Figure 4Stress-strain diagram under compression for different


wt% of walnut particles.

composition of walnut particle. It can be noticed that


addition of walnut particle improves the modulus of elasticity of composite materials. It is found that ultimate compressive strength of 10 wt% of walnut is about 261.0 MPa.
But increase in weight percentage of walnut particles, the
ultimate strength decreases considerably. Hence, taking
into consideration the requirement and the cost effectiveness various composition of the reinforced material can be
taken. Variation in ultimate strength, percentage reduction in length and modulus of elasticity with respect to
different weight percentage walnut reinforced composite
are shown in Figure 5.
On the basis of results obtained the effect of weight
fraction (Vf ) on modulus of elasticity and ultimate strength
are shown in Equations 3 and 4 with a correlation coefficient >0.9.
Modulus of elasticity (MPa)=61.84Vf +907.3

(3)

Table 5Rockwell hardness values on M-scale for various filled


hybrid composites.
S. no

Walnut
(10 wt%)

Walnut
(15 wt%)

Walnut
(20 wt%)

Walnut
(25 wt%)

Resin

Mean
SD

R-63
R-64
R-61
R-60
R-63
R-62.2
1.6431

R-67
R-65
R-66
R-68
R-64
R-66
1.5811

R-77
R-81
R-79
R-80
R-78
R-79
1.5811

R-90
R-87
R-89
R-91
R-92
R-89.8
1.9235

R-57
R-55
R-58
R-57
R-55
R-56.4
1.3416

85
45
250
40

220
Modulus of elasticity/10 MPa

190

Ultimate strength, MPa


% Reduction in length

35

160
130
10

80
Hardness (MRH)

280

Reduction in length (%)

Modulus of elasticity, Ultimate strength

90
50

310

75
70
65
60
55

30
15
20
Walnut particles (wt%)

25

Figure 5Ultimate strength for different weight percentage of


walnut reinforced composite.

50
0

10
15
Walnut particles (wt%)

20

25

Figure 6Hardness (MRH) for different weight percentage of walnut


reinforced composite.

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V.K. Singh: Mechanical behavior of walnut shell particles reinforced bio-composite7

280
Ultimate strength (compression)

260

Ultimate strength (MPa)

240

Ultimate strength (tension)

220
200
180
160
140
120
100
60.0

70.0

80.0

90.0

Hardness (MRH)

Figure 7Variation of ultimate strength with hardness (MRH).

Table 6Flexural strength properties for resin and composites materials.


Properties

Walnut particle
(10 wt%)

Walnut particle
(15 wt%)

Walnut particle
(20 wt%)

Walnut particle
(25 wt%)

Flexural modulus (MPa)


Flexural stress (MPa)

Flexural strain

1360.0
769.0
0.057

1450.0
614.0
0.042

1500.0
603.0
0.040

1560.0
439.0
0.028

The present result shows that a linear relation between


hardness and ultimate strength in tension and compression exists. The following correlation between hardness
and ultimate strength has been developed (Equations 5
and 6) with a correlation coefficient >0.9, where H is hardness in MRH scale.

flexural modulus of elasticity. But flexural stress and flexural strain was found to be higher for 10 wt% walnut filled
composites as compared with others investigated in this
report.

Ultimate compressive strength (MPa) = -4.280H + 522.3

(5)

4 Conclusions

Ultimate tensile strength (MPa)=-1.648H + 247.3.

(6)

Epoxy bio composites reinforced with walnut particles


were prepared. Such bio composites were experimentally
characterized by means of microscopy, tensile, compression, hardness and bending test. Remarkable changes
in the mechanical properties have been noticed due to
addition of walnut particles in bio composite. Addition
of walnut particles increased the hardness, which is very
important property for particles board with sustainable
tensile and compressive properties.

3.4.5 Flexural strength


The flexural strength of the walnut particle filled epoxy
resin composite materials were determined by 100 kN
ADMET make servo controlled universal testing machine
at 1mm/min strain rate under displacement control mode
using three point bend test. The results are presented in
Table 6.
As depicted by the test data, amongst the composite
materials developed the 25 wt%, walnut reinforced composite shows the best results with regard to the flexural
modulus of elasticity (1560 MPa) and also it is better than
10 wt% walnut reinforced composites with regard to the

Acknowledgments: The author expresses his gratitude


and sincere thanks to Department of Science and Technology, India, for providing finance to carry out this research
work smoothly.

Received December 16, 2013; accepted January 2, 2014

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8V.K. Singh: Mechanical behavior of walnut shell particles reinforced bio-composite

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