International Journal of Engineering Materials and Manufacture (2021) 6(4) 305-311

https://doi.org/10.26776/ijemm.06.04.2021.06

In-Situ Synthesis and Property Evaluation of High-Density Polyethylene

Reinforced Groundnut Shell Particulate Composite

Adetayo Abdulmumin Adebisi, Tajudeen Mojisola, Umar Shehu, Muhammed Sani Adam and
Yusuf Abdulaziz

Received: 09 March 2021

Accepted: 24 July 2021
Published:01 October 2021
Publisher: Deer Hill Publications
© 2021 The Author(s)
Creative Commons: CC BY 4.0

ABSTRACT
In-situ synthesis of high-density polyethylene (HDPE) reinforced groundnut shell particulate (GSP) composite with
treated GSP within the range of 10-30 wt% at 10 wt% has been achieved. The adopted technique used in the
production of the composite is melt mixing and compounding using two roll mills with a compression moulding
machine. Properties such as hardness, tensile strength, impact energy and water absorption analysis were examined.
The result revealed that addition of GSP increases the hardness value from 22.3 to 87 Hv. However, the tensile
strength progressively decreased as the GSP increases in the HDPE. This trend arises due to the interaction between
neighbouring reinforced particulate which appears to influence the matrix flow, thereby inducing embrittlement of
the polymer matrix. It was also observed that water absorption rate steadily increased with an increase in the
exposure time and the absorbed amount of water increases by increasing the wt% of the GSP. Analysing the obtained
results, it was concluded that there were improvements in the hardness, tensile strength, impact energy and water
absorption properties of the HDPE-GSP polymer composite when compared to unreinforced HDPE. On these
premises, GSP was found as a promising reinforcement which can positively influence the HDPE properties of modern
composites.
Keywords: High density polyethylene (HDPE), Groundnut shell particulate (GSP), Melt mixing, Compounding,
Compression moulding machine.

1 INTRODUCTION
In recent years, natural fibre reinforced polymers have started emerging as new eco-friendly polymeric composite
materials with superior engineering properties such as low density, acceptable specific strength and specific stiffness,
reduced tool wear and non-abrasiveness [1]. They are also commercially cost effective, environmentally friendly,
reduce dependence on non-renewable sources, reduce pollutant and greenhouse gas emissions and offer enhanced
energy recovery. The easy availability and presence of cellulose imparts good mechanical properties to natural fibres
which makes it viable for promoting natural fibre reinforced polymer composites. The presence of cellulose makes
natural fibres hydrophilic, however, the adhesion with hydrophobic polymer matrix reduces load transfer from
matrix to fibre in the composite thereby limiting the mechanical properties [2]. This limitation can be overcome by
improving the fibre-matrix interfacial adhesion through surface modification of the natural fibre through chemical or
physical treatment, use of coupling agent and chemically functionalized matrix.
These naturally occurring fibres have been extensively used as reinforcements in polymer matrices as compared
to the non-degradable synthetic fibres such as carbon, glass or aramid. They have shown to be invaluable when used
as reinforcing filler in the polymer matrix. Several natural fibres have been investigated and they include coir fibre
[3], wood fibre [4], rice straw fibre [5], sisal fibre [6], hemp fibre [7], kenaf fibre [8] and chitosan [9]. Groundnut
shell is a waste product obtained after the removal of groundnut seed from its pod, and there has not been substantial
demand for the utilization of groundnut shell for economic and commercial purpose. It is one of such natural agro
waste filler with potential to be used as reinforcement as it contains cellulose, hemicellulose and lignin. It is a valuable
product in composite production process due to its high availability in Northern Nigeria and scarce interest in other

A. A. Adebisi, A. A.1,2 , Mojisola, T.2, Shehu, U1, Adam, S. M.2 and Abdulaziz, Y1
1Department of Metallurgical and Materials Engineering, Ahmadu Bello University, Zaria, Nigeria
2Metallurgical and Materials Engineering Department, Air Force Institute of Technology, Kaduna, Nigeria

E-mail: aaadebisi@abu.edu.ng
a.adebisi@afit.edu.ng
References: Adebisi et al. (2021). In-situ Synthesis and Property Evaluation of High-Density Polyethylene Reinforced Groundnut
Shell Particulate Composite. International Journal of Engineering Materials and Manufacture, 6(4), 305-311.
In-situ Synthesis and Property Evaluation of High-Density Polyethylene Reinforced Groundnut Shell Particulate Composite

industrial sectors [10]. On the other hand, high density polyethylene (HDPE) is one of the important grades of
polyethylene (PE) that exhibits excellent properties such as chemical stability barrier, good thermal resistance and
mechanical strength. These properties make HDPE a versatile material in the manufacture of many products and
packaging such as milk jugs, detergent bottles, margarine tubes, and garbage containers [11].
In their study, Jacob et al., [12] reported the dynamic mechanical characterization of groundnut shell powder
filled recycled high-density polyethylene composite. The experiments were conducted using treated and untreated
groundnut shell powder. Dynamic mechanical properties such as storage modulus, loss modulus and damping
parameter were found to improve with the incorporation of treated groundnut shell powder. The inherent properties
of the groundnut shell powder have made it a good reinforcing material in the development of composite. Similarly,
Olaitan et al., [13] investigated the comparative assessment of mechanical properties of groundnut shell and rice husk
reinforced epoxy composite. This investigation considered two different reinforcement groundnut shell and rice husk.
After comparing the mechanical properties of the two reinforcements, it was revealed that groundnut shell epoxy
composite displayed higher mechanical properties as compared to the rice husk epoxy composite. Musa et al., [14]
studied on the mechanical and morphological properties of high-density polyethylene (HDPE) leather waste
composites. The study shows that without additives, HDPE/Chrome tanned composites had higher modulus with
lower tensile strength and impact strength. Moreover, Souza et al., [15] investigated on the mechanical properties of
HDPE/textile fibres composites. The investigation result shows that the addition of modified fibres from industrial
residue to HDPE improve the tensile strength and modulus which means there is an improvement in the mechanical
property. Based on the studies highlighted, groundnut shell and HDPE have potential to be processed for use as
composite material. However, there is limited or no information available in the literatures on the study. Therefore,
this study aims to investigate the mechanical and water absorption properties of high-density polyethylene reinforced
groundnut shell particulate composite using compression moulding technique.

2 MATERIALS AND METHODS

2.1 Materials
The HDPE was obtained from the Department of Metallurgical and Materials Engineering, Ahmadu Bello University,
Zaria and the groundnut shells were locally sourced from Dawanau market in Kano state, Nigeria. The shells were
washed thoroughly to remove dirt and dried to enable easy crushing and grinding into smaller sizes using shredding
machine and a sieve of size less than <0.3mm (300 micrometres) was used. The sieved groundnut shell was then
immersed and treated in 5 % NaOH for 1, 2, 3 hours with continuous stirring after which the solution was decanted
off, washed several times with distilled water until the solution becomes neutral. The ground nut shell was then dried
in an oven at a temperature of 105 degrees for 6 hours.

2.2 Method
2.2.1 Composite Preparation
The mould used for the preparation of the composite is an iron mould with a dimension of 100 x 100 x 30 mm. An
equivalent volume of HDPE was weighed using analytical weighing balance for each sample size. The weight
percentage of 0-30 (0, 10, 20, and 30) wt % of groundnut shell were calculated from the weight of the control
sample of HDPE, weighed and tight up in different nylons for production of the composite.

2.2.2 Compounding and Mixing

To produce the composite, the ratio of the HDPE to the groundnut shell particles were measured 90/10, 80/20,
and 70/30 the measurement was carried out using an electronic digital weighing balance. The two-roll mill machine
was warmed up for about one hour (1hr) at a temperature of 150 0C. The materials were compounded via melt
mixing and compression moulding using two roll mill and a compression moulding machine at a temperature of
140 0C and a pressure of 5 psi to obtain a homogeneous mixture. The weight fraction of the reinforcement was
varied from 0-30 (0, 10, 20, and 30). The samples were cooled, after the composite was removed from the mould.
The procedure was repeated for all composition of the filler (particle). The compression mould process was carried
out at the NILEST Samara Zaria, Kaduna State, Nigeria.

2.3 Mechanical Property Test

2.3.1 Hardness Test
The micro indentation measurements were carried out at room temperature using Shimadzu HMV-1, Japan micro
hardness tester. The test measures the penetration of a specified indenter into the material with a load of 0.3kgf that
has a maximum hardness value of 100HV and a minimum hardness value of 010HV. It consists of an indenter, a
graduated circular tube and a flat surface which the sample to be tested was mounted. The sample was placed on the
flat surface and a load was applied on the surface of the specimen to obtain the hardness value. The measurements
were performed in accordance with ASTM standard E384 for micro-indentation hardness of materials [22]. The micro
hardness was computed at five different locations for each value of load for the prepared samples where the average
Vickers micro hardness number was calculated and recorded.

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2.3.2 Tensile Strength Test

The tensile testing machine used is the tensometer type W (with flexural fixture), Monsanto tensometer, UK. The
testing of the samples was conducted at the Department of Metallurgical and Materials Engineering, Ahmadu Bello
University, Zaria, Kaduna State, Nigeria in accordance with ASTM D638 standards. The samples were machined to
dumbbell shape and then placed in the universal tensile testing machine. The test was determined using tensile
machine by gripping the ends of a suitable prepared standard test sample, and then applying a continually increasing
uniaxial load until the sample fractured. The tensile loads together with the corresponding extensions were recorded
on the graph sheet for evaluation.

2.3.3 Impact Energy Test

Impact strength of a material is the capacity to absorb energy under shock or impact load. The impact test was
conducted on the prepared GSP-HDPE composite on the treated samples using the charpy impact testing machine.
The composite samples for the impact test were prepared according to ASTM D-256 with the dimensions of 55 mm
(length) x 10 mm (width) x 10 mm (height) and also provided the V-notch at the middle of the samples. The pendulum
was raised to the test height and held there. The sample was mounted in the machine and the door of the machine
was closed. The pointer for reading the impact energy value on the calibrated scale was adjusted to zero before the
pendulum was released by means of a handle on the door of the machine. The pendulum falls from the height,
breaking the sample and hitting the pointer to the test energy value. This process was repeated for all the samples,
till all the impact test value for all the different composition was recorded and the average value was recorded.

2.4 Water Absorption Test

Water absorption test was used to determine the water absorption capacity of the synthesized composite under some
specified conditions. The test was carried out by immersion of the samples in water bath at room temperature for a
time duration. The samples were cut to dimensions 20 x 20 mm, the initial weight of the samples was taken with aid
of an electronic digital weighing balance with tolerance of 0.001 g. Then each of the samples were immersed in a
beaker containing water and the new weight of the samples was recorded. The samples were immersed in water for
a duration of 1 – 3 hrs, after immersion the surface of the specimen were cleaned dry and weighed immediately to
measure their weight. The initial weight of samples is taken as w1 and after the sample is removed from the water is
taken as w2. The percentage water absorption was obtained from the relationship in equation 1.

3 RESULTS AND DISCUSSIONS

3.1 Groundnut Shell and Developed HDPE-GSP Composite
Fig. 1(a-c) show the groundnut shell in the as received, untreated and treated conditions. The untreated groundnut
shell is bright compared to the treated groundnut which is dark due to the removal of some elements during the
treatment process. Fig. 1(d) shows the developed HDPE-GSP composite before conducting the various testing to
ascertain the properties analysis.
𝑊2 − 𝑊1
% 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐴𝑏𝑠𝑜𝑟𝑏𝑡𝑖𝑜𝑛 = 𝑥100 (1)
𝑊1

Figure 1: Groundnut shell (a) as received, (b) untreated, (c) treated and (d) Sectioned portion of developed HDPE-
GSP composite

3.2 Mechanical Properties Analysis

3.2.1 Hardness Test
Figure 2 explains the comparative analysis of the HDPE (control sample) and the GSP-HDPE composite subjected to
alkaline treatment at various time intervals ranging from 1 to 3 hours. The unreinforced HDPE shows the lowest
hardness value of 22.3 Hv. The GSP-HDPE reveals a progressive increase in hardness value as the wt% of GSP
increases from 10 wt% to 30 wt% for 1 hr alkaline treatment. However, the hardness value for the 2 hrs and 3 hrs
treated GSP-HDPE composite exhibited similar trend where there is a drop in hardness value from 71.73 to 54.2 Hv
and 42.87 to 34 Hv for the 20 wt% GSP-HDPE composite.

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In-situ Synthesis and Property Evaluation of High-Density Polyethylene Reinforced Groundnut Shell Particulate Composite

The 30 wt% GSP-HDPE composite exhibited a remarkable rise in the hardness value for both 2 hrs and 3 hrs
treated composite from 54.2 to 76.13 Hv and 34 to 67.9 Hv, respectively. The reason for the drop in hardness value
for the 20 wt% GSP-HDPE composite maybe ascribed to the poor interfacial bonding or poor adhesion of the
reinforced GSP and HDPE. The increase in hardness is attributed to the strengthening effect of the GSP incorporated
into the HDPE matrix.

3.2.2 Tensile Test

The tensile strength of the GSP-HDPE composite was found to decrease progressively as the percentage of GSP
increased from 10 wt% to 30 wt% as shown in figure 3. However, the 10 wt% reinforced GSP-HDPE treated for 3
hrs showed better tensile strength when compared to 20 and 30 wt% treated composites. The increase in wt% of
the GSP is expected to increase the tensile strength but this trend may have resulted due to poor wettability and
adhesion with uneven dispersion between the GSP and HDPE. Although, similar behaviour was previously reported
in the use of coir fibre as filler reinforcement [16].

3.2.3 Impact Energy Test

The impact strength of treated GSP-HDPE composite attained maximum at 20 wt% GSP treated for 1 hr as shown in
Figure 4. However, the 10 wt% and 30 wt% treated GSP-HDPE composite recorded poor impact strength for all
time conditions considered. The impact strength of the composite reduced after 20 wt% may be due to the reduction
of elasticity of the material due to GSP addition thereby reducing the deformability of the HDPE. Moreover,
considerable amount of energy absorption takes place through particle pull out process but after alkali treatment a
strong mechanical interlocking develops between the GSP and HDPE and particle pull out is reduced which in turn
decreases the impact strength.

100
Control - HDPE 87
90
1 hr Alkaline Treatment
80 76.13
2 hrs Alkaline Treatment 71.73
67.57 67.9
70 63.4
3 hrs Alkaline Treatment
HARDNESS (HV)

60 54.2
50 42.87
40 34
30 22.3
20

10

0
0 10 20 30
WT % REINFORCEMENT (GSP)

Figure 2: Effect of wt% GSP and alkaline treatment on hardness value of GSP-HDPE composites

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25
21.55 Control - HDPE

20 1 hr Alkaline Treatment
TENSILE STRENGTH (N/MM2)

2 hrs Alkaline Treatment

14.04
3 hrs Alkaline Treatment 13.45
15 12.7 11.86
13.17 12.36 11.74 11.99
11.12
10

0
0 10 20 30
WT % REINFORCEMENT (GSP)

Figure 3: Effect of wt% GSP and alkaline treatment on tensile strength of GSP-HDPE composites

1.6
1.43 1.45
1.37
1.4 Control - HDPE 1.07
IMPACT ENERGY (J)

5
1.2 1 hr Alkaline Treatment
1 2 hrs Alkaline Treatment
0.8
0.8 3 hrs Alkaline Treatment 0.63
0.57 0.6
0.6 0.5
0.4
0.4

0.2

0
0 10 20 30
WT % REINFORCEMENT (GSP)

Figure 4: Effect of wt% GSP and alkaline treatment on impact energy of GSP-HDPE composites

3.3 Water Absorption

The result obtained from water absorption test is plotted against the wt% of GSP as shown in Figure 5. The water
absorption rate attained maximum with 30 wt% GSP-HDPE treated for 2 hrs. When compared to the HDPE sample,
the absorption value increased from 0.653% to 9.579%. Similar trend of result was achieved by Munoz and Garcia
(17) in their study. The increase in water absorption upon addition of wt% GSP is as a result of the hydrophilic nature
of groundnut shell which absorbs water, thereby creating room inside the composite resulting in micro-cracks that
develop between the interface of the particle and the matrix giving rise to higher water absorption.

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In-situ Synthesis and Property Evaluation of High-Density Polyethylene Reinforced Groundnut Shell Particulate Composite

12
Control - HDPE

10 1 hr Alkaline Treatment 9.579

8.779
2 hrs Alkaline Treatment 8.834
WATER ABSORPTION (%)

8 3 hrs Alkaline Treatment

4 3.476

1.574 1.094 1.532

2
0.653 0.385 1.058

0
0 10 20 30
WT % REINFORCEMENT (GSP)

Figure 5: Effect of wt% GSP and alkaline treatment on water absorption of GSP-HDPE composites

4 CONCLUSIONS
In this study, effects of wt% GSP and alkaline treatment on the mechanical properties and water absorption behaviour
of GSP-HDPE composite were reported. It was found that both the wt% GSP and alkaline treatment influences the
properties of the composite. The following conclusion were drawn from the study;
1. The GSP-HDPE composite was successfully developed using the melt mixing and compression moulding
technique.
2. The hardness value of the GSP-HDPE composite shows a steady rise as the wt% GSP increases from 10-30
wt% for the 1 hr treated GSP. However, the 2 hrs and 3 hrs treated GSP experiences a decline for the 20
wt% GSP. The 30 wt% GSP attained the maximum for all treatment time with 87 Hv as the highest value.
3. The tensile strength of the composite decreases progressively as the wt% of the GSP increases from 10-30
wt%. Although, the 10 wt% reinforced GSP-HDPE treated for 3 hrs attained the maximum value at 14.04
N/mm2.
4. GSP-HDPE composite achieved optimum impact energy at 20 wt% GSP treated for 1 hr. However, the 10
and 30 wt% recorded poor impact strength due to the reduction in the elasticity of the HDPE as a result of
GSP addition.
5. Water absorption rate attained high value at 30 wt% GSP-HDPE composite for all treatment time.
However, the composite treated for 2 hrs achieved the maximum water absorption rate.
6. It is concluded that the wt% and alkaline treatment play a major role in the mechanical and water
absorption properties of GSP-HDPE composite. However, an optimization analysis study will be required
to fully achieve the best wt% composite of GSP and alkaline treatment time.

ACKNOWLEDGEMENT
The authors acknowledge the support received from the Department of Metallurgical and Materials Engineering,
Ahmadu Bello University, Zaria throughout the conduct of the research. Sincere appreciations are also extended to
the technical team in the Departmental workshop where the experimental studies reported here were conducted.

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