Materials Today: Proceedings 38 (2021) 682–687

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Materials Today: Proceedings

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Mechanical properties of high density polyethylene matrix composites

reinforced with chitosan particles
O.O. Daramola a,c,⇑, A.S. Taiwo a, I.O. Oladele a, J.L. Olajide b, S.A. Adeleke a, B.O. Adewuyi a, E.R. Sadiku c
a
Department of Metallurgical and Materials Engineering, Federal University of Technology, Akure 340001, Nigeria
b
Department of Mechanical Engineering, Mechatronics and Industrial Design, Tshwane University of Technology, Pretoria, South Africa
c
Institute of Nano Engineering Research (INER), Department of Chemical, Metallurgical and Materials Engineering (Polymer Technology Division),
Tshwane University of Technology, Pretoria, South Africa and the Tooling Centre Soshanguve Campus, Tshwane University of Technology, Pretoria 117, South Africa

a r t i c l e i n f o a b s t r a c t

Article history: High Density Polyethylene (HDPE) matrix composites reinforced with chitosan particles were developed
Received 7 October 2019 by compression moulding technique. Chitosan particles extracted from deep sea squid with 90% deacety-
Received in revised form 21 March 2020 lation, bulk density of 0.3 g/cm3 and particle size of 90 lm were used as reinforcement. HDPE and various
Accepted 27 March 2020
weight fractions (2, 4, 6, 8 and 10 wt%) of chitosan particles were melt-compounded in a single screw lab-
Available online 17 April 2020
oratory extruder with rotational speed of 50 rpm and temperatures of 190–220 °C. The blends were then
moulded into different test specimens using carver laboratory press at a temperature of 230 °C for 12 min
Keywords:
under applied pressure of 0.2 kPa. The mechanical properties (flexural, tensile and impact) of the devel-
Mechanical properties
High Density Polyethylene
oped composites were studied. The results showed that there were improvements in the mechanical
Compression mouding technique properties of the composites. The optimal values for the tensile strength and tensile modulus of the com-
Chitosan particles posites were observed at 2 wt% chitosan particles reinforcement with values of 23.14 MPa and
Composites 828.38 MPa respectively while that of flexural strength and flexural modulus were noticed at 4 wt% with
values of 83.90 MPa and 1690 MPa respectively. The impact strength of the composites increased linearly
from 2 to 10 wt% Chitosan particles reinforcement with an optimum value of 229.20 KJ/m2. The scanning
electron microscope (SEM) examination of the composites revealed that there were homogeneous parti-
cles dispersion at lower weight fractions (2–6 wt%) while particles agglomerations were noticed on the
SEM images at higher weight fractions (8–10 wt%).
Ó 2019 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Sympo-
sium on Nanostructured, Nanoengineered and Advanced Materials.

1. Introduction understand some mechanisms, specific behaviour and influence

Through the span of years, there has been an extensive interest
in polymers and polymer-based composites because of some
unique and desirable features such as biocompatibility, less diffi-
culty in processing, light weight, low cost and sometimes
biodegradability which has caused them to replace many of the
conventional metals and materials for a wide range of applications
in medicine, aerospace, appliances, food processing and preserva-
tion and many more. Several researches have been conducted on
polymer composites by incorporating some natural or synthetic
materials in the form of fillers and fibers to modify their properties,
⇑ Corresponding author at: Department of Metallurgical and Materials Engineer-
ing, Federal University of Technology, Akure 340001, Nigeria.
their performances consequently, helping us to determine the
most suitable areas of application for such composites [1–3].
Also, there has been a keen scientific and technological interest
in the use of natural reinforcements. Examples of such is the use of
animal fiber, rice husk, bamboo stem, banana fiber, cow bone, cow
hair and chitosan to reinforce polymers [4–7].
Chitosan is a product from chitin by deacetylation process
which is a naturally occurring polysaccharide that is available in
enormous amounts from the epidermis of crustaceans such as
crabs, shrimps, lobsters, corals, jellyfish and insects such as butter-
flies, ladybugs, mushrooms and fungi [8]. Their shells are widely
used as primary sources for the production of chitosan [9].
Chitin and chitosan polymers are natural amino-
polysaccharides [10] and virtually non-toxic polymer with a wide
safety margin having unique structures, multidimensional

https://doi.org/10.1016/j.matpr.2020.03.695
2214-7853/Ó 2019 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Symposium on Nanostructured, Nanoengineered and Advanced Materials.
 O.O. Daramola et al. / Materials Today: Proceedings 38 (2021) 682–687
Table 1
Formulation for HDPE/Chitosan Composites Development.
Designation Composition Reinforcement (g)
A HDPE(Control sample) Nil
B 2 wt% chitosan 2.9
C 4 wt% chitosan 5.8
D 6 wt% chitosan 8.7
E 8 wt% chitosan 11.7
F 10 wt% chitosan 14.6
properties, highly sophisticated functions and wide applications in
biomedical and other industrial areas.
The use of chitosan as additives for polymer based composites is
beginning to receive quite some attention as researchers have been
conducting several studies on them. Daramola et al. [11] also stud-
ied the influence of green silica particles on the mechanical prop-
erties of Epoxy matrix composites and observed that there was
an improvement in the tensile strength and tensile modulus while
there was decrease in the percentage elongation as the weight frac-
tions of the silica particles increases.
Chitosan acts as a biodegradable additive and gives antimicro-
bial properties. Chitosan is a biocompatible, conducting polymer
[12] which shows many exciting features, such as a biodegradable
coating and film in food packaging industries [13], a dietary fiber, a
biomaterial in medicine either on its own or as a blend component
in medicine due to its rummaging ability against toxic ions [8] and
many more applications [14,15]. Apart from their relative abun-
dance, they are easily biodegradable, inexpensive, light weight
and have low abrasive nature, they are quite easy to process and
recycle, and they have moderate to excellent dimensional stability
[10]. Apart from its good film forming ability, chitosan application
has been observed to inhibit bacterial, yeast and fungi growth by
reducing the bacterial metabolic rate as chitosan sticks to the bac-
terial cell wall and the antibacterial properties are increased with
increasing amounts of chitosan [16].
There are several challenges that biomaterials for orthopedic
applications encounter which include its ability to be formed into
any specific desired shape using cost-effective methods and with-
out a negative effect on its mechanical properties. It must either be
free of lethal substances or those noxious substances must be per-
fectly sealed into the structure of the material. It should not
degrade in the presence of body fluids. A biomaterial must not lead
to poisoning of the patient. The biomaterial also must not fracture
as a result of an occasional acute overload or by fatigue from
dynamic service loads.
The mechanical properties must be in synergy with the shape of
the implant to ensure that stresses are brought to safe acceptable
level particularly where stress concentration and amplification
cannot be avoided [15,16]. HDPE has been known to possess good
low temperature toughness, reasonable tensile strength, minimal
moisture absorption, comparatively high softening temperatures
and good resistance to corrosion. The choice of HDPE as the poly-
mer matrix became incontestable because of their excellent ability
to be reinforced with either natural fibres and fillers [3].
However, the main disadvantage in (natural fibres)/plastic com-
posites is the poor compatibility between the hydrophobic poly-
meric matrix and the hydrophilic fibres [9]. This leads to the
formation of a weak interface, which results in poor mechanical
and thermal properties and this has prompted the use of chitosan
powders to reinforce HDPE [5].
The purpose of this research is to investigate the mechanical
properties of chitosan reinforced HDPE composite for biomedical
application.
683
2. Materials and methods
Matrix (g) 2.1. Materials
145.8
142.9 The high-density polyethylene was supplied by SASOL Polymers
141.7 South Africa while Silicon oil and was procured from Pascal Scien-
138.0
tific Chemical Ltd, Akure Ondo state, Nigeria. Chitosan powder with
134.1
131.2 bulk density of 0.3 g/cm3 was obtained from Eastman chemical
company, in South Africa while the Teflon sheet was obtained from
a material store in Arakale, Akure, Ondo state.
2.2. Mould preparation
Tensile mould with a dimension of 150  100  4 mm having a
dumb bell-shape, flexural mould of 150  50  5 mm and impact
mould of 80  10  2 mm were used to produce tensile, flexural
and impact samples respectively. A mould release agent (silicone
oil) was applied on the surface of the mould to aid easy removal
of the cured samples from the mould.
2.3. Compounding and production of composite samples
HDPE/Chitosan composites were developed by compression
moulding technique. Predetermined proportion of HDPE and vari-
ous weight fractions (2, 4, 6, 8 and 10 wt%) of chitosan particles
were melt-compounded in a single screw laboratory extruder with
rotational speed of 50 rpm and temperatures of 190–220 °C. The
blends were then moulded into different test specimens (tensile,
impact and flexural) using carver laboratory press at a temperature
of 230 °C for 12 min under applied pressure of 0.2 kPa. In this way,
the control HDPE matrix and HDPE/Chitosan composite samples
filled with various weight fractions of chitosan particles were pre-
pared. Teflon sheet was used to cover the top and bottom part of
the mould while siliconoil was applied at the inner edges of the
mould for easy release after moulding. All forms of weight mea-
surement were conducted using an analytical weighing balance
(LI-HPB 220)
2.4. Testing and structural characterization of samples
Composite samples were prepared for tensile, flexural, impact
toughness tests and morphological examination in order to study
the behavioral performance of the composite in service condition
(Table 1).
2.4.1. Ultimate tensile strength
In order to determine the maximum load bearing capacity of
the composite samples, tensile tests were carried out to determine
the ultimate tensile strength and elastic modulus using an Instron
5966 tester (Instron Engineering Corporation, USA) with a load cell
of 10 kN in accordance with ASTM D303-08 standard. Dumb bell-
shaped samples that were prepared by compression moulding
technique were tested in tension mode at a strain rate of 5 mm/
min at room temperature and relative humidity of 0.4. The gauge
length of the tensile samples was 14 mm and they were fastened
tightly at the edges of the upper and lower grip of the machine.
As the test piece were strained, cogent tensile test data was gener-
ated and the graphs were plotted automatically. The results pre-
sented were the average of three samples for each composition.
2.4.2. Impact test
The impact test was carried out by subjecting the HDPE matrix
and the HDPE/Chitosan composites samples to a Charpy impact
testing machine (Instron CEAST 9050), in accordance with ISO179
standard. Samples cut into dimension 80  10  2 mm were placed
684 O.O. Daramola et al. / Materials Today: Proceedings 38 (2021) 682–687
horizontally on the machine with the notched surface directly
opposite the swinging pendulum. The initial reading of the sample
gauge length and the thickness were entered into computer system
attached to the machine and the machine was switched on. The
pendulum of the machine swung freely through angle 180° and
fractured the sample. Three samples were tested from where the
mean value was evaluated and presented.
2.4.3. Flexural test
Flexural strength of the composite was evaluated by performing
flexural three-point bending test on the composite. The test was
performed at room temperature using Testometric Universal Test-
ing Machine operated at a crosshead speed of 3.0 mm/min. The
testing procedure and the flexural strength determination were
performed in accordance with ASTM D7264M-07 standard. Three
samples were tested from where the average value was deter-
mined and presented.
3. Results and discussion
3.1. Mechanical properties of the composites
3.1.1. Ultimate tensile strength (UTS)
Fig. 1 showed the variations in the ultimate tensile strength of
the control sample; HDPE and the chitosan-HDPE composites.
The optimum value of the ultimate tensile strength was
observed in sample B with 2 wt% chitosan particles reinforcement
with a value of 23.14 MPa; as the particles weight fraction
increases, there was gradual linear reduction in the UTS of the
composites, though the values from 4 8 wt% chitosan particles
reinforcement were higher than that of HDPE matrix (control sam-
ple), the least UTS value was observed at 10 wt% reinforcement
with a value of 19.01 MPa. The mechanism behind this behaviour
can be explained through a number of phenomena such as stress
transfer phenomenon, interparticle space reduction, dislocation-
interface phenomenon, Orowan and Hall-petch phenomenon. The
chitosan particle addition was the least at 2 wt% causing an even
dispersion of the particles within the HDPE matrix which led to
the highest increase in strength of the composite. It is worthy to
note that there was no agglomeration, coarsening or overlapping
of the chitosan particles in composite at this weight fraction as
shown in the SEM image in Fig. 6 (b) because there was excessive
matrix area or interparticle spacing between the particles. This led
to an excellent load transfer from the matrix to the reinforcement
within the composite. 2 wt% chitosan particles- HDPE composite
had the best interparticle spacing suitable for effective stress trans-
fer from the matrix to the particles, best resistance to dislocation
motion, little or no agglomeration of particles. At 4 wt% particles
Ultimate Tensile Strength (MPa)
20
15
10
5 200
0 0
A B C D E F
Samples
Fig. 1. Variations of Ultimate Tensile Strength of HDPE Matrix and Chitosan-HDPE
Composites.
reinforcement, the chitosan particles were able to fill up the exces-
sive matrix area and further reduce the interparticle spacing but
there was the formation of particles agglomerates, coalescence or
overlapping of the chitosan particles which results to a decrease
in the ultimate tensile strength of the composite at this weight
fraction. At 8–10 wt% weight fractions, there was interfacial
debonding at the matrix-particle interface and high level of parti-
cle agglomerations were observed as can be seen in the SEM
images in Fig. 6(e-f) compared to other composites and this led
to an extrication of the composites under applied stress which con-
sequently led to a downslide in the tensile strength of these com-
posites. Also, the decreased interparticle spacing, due to the
increased volume fraction of chitosan reinforcement, creates
increased resistance to dislocation motion, which contributes to
the enhanced strength of the composites. This result was in agree-
ment with the work of Daramola et al. [3].
It is worthy to note that the enhancement of the tensile strength
can also be attributed to the presence of higher modulus chitosan
particles incorporated in the HDPE matrix, which behaved as a
resistance to plastic deformation when the composites were under
an applied stress. Orowan strengthening was also present; this is
because of the fact that the chitosan particles forced dislocations
to bow around them leading to a stunted dislocation motion. Con-
ferring from Hall-Petch relationship which summarizes that the
strength is inversely proportional to the particle size, the refine-
ment of the chitosan particles created more grain boundaries that
provided sufficient capacity to resist the applied stress. As the dis-
locations encountered a barrier, there was a change in the orienta-
tion of the dislocation leading to a stunted dislocation motion.
Moreover, at the particle–matrix interface, the bonding was strong
as observed at 2 wt% chitosan particles-HDPE composite (sample
B) which helped in increasing the resistance to applied tensile
stresses and impede extrication of the chitosan particles from the
matrix under tensile loading.
3.1.2. Modulus of elasticity
Modulus of Elasticity is a measure of the stiffness of a material
under an applied stress. It is the measure of a materials resistance
to elastic deformation. The modulus of elasticity of the chitosan
particles-HDPE composites are shown in Fig. 2.
The composite sample with 2 wt% chitosan particles reinforce-
ment showed the highest elastic modulus with a value of
828.38 MPa when compared with the HDPE matrix and other
developed composites and afterwards there seems to be a sharp
linear decrease in the modulus of elasticity as the weight fractions
of the particles increases. The result obtained is in consonance with
literature [8]. The apparent drop in the tensile modulus showed by
8–10 wt% chitosan particles reinforcement may be due to factors
such as uneven dispersion of the chitosan particles, poor
800
Modulus of Elasticity (MPa)
700
600
500
400
300
100
A B C D E F
Samples
Fig. 2. Variations of Modulus of Elasticity of HDPE Matrix and Chitosan-HDPE
Composites.
 O.O. Daramola et al. / Materials Today: Proceedings 38 (2021) 682–687 685

chitosan-HDPE adhesion or bonding, and particles agglomeration 60

which were observed in the SEM in images in Fig. 6 (e-f).
50

Flexural Strength (MPa)

3.1.3. Impact strength
Fig. 3 revealed the variations in the impact strength of HDPE 40
matrix and chitosan-HDPE composites.
Impact strength depends upon the reinforcement’s resistivity 30

during fracture. It is the ability of a material to absorb elastic strain

20
energy. The impact strength increases linearly from 2 wt% chitosan
particles reinforcement in sample B to 10 wt% reinforcement in
10
sample F, this is due to the multiple filler arrangement around
the matrix there by having the ability to absorb more strain energy.
0
The maximum impact strength was observed in sample F with a A B C D E F
value of 229.20 KJ/m2; this is evidence that the chitosan particulate Samples
reinforcement played a positive and active role in dissipating strain
energy throughout the composites. Fig. 4. Variations of the Flexural Strength of HDPE Matrix and Chitosan-HDPE
Composites.

3.1.4. Flexural strength

Flexural properties of the neat HDPE and composite samples 1800
were tested using a three-point bending test. The variation in the
1600
flexural strength of the composite as well as the HDPE matrix is
shown in Fig. 4. 1400

Flexural Modulus (MPa)

The highest flexural strength is 56.91 MPa which was observed 1200
in the 4 wt% chitosan/HDPE composite which increased sporadi-
1000
cally by 162.74% over the strength of 0 wt% (control sample). By
conferring from the SEM image at 4 wt% Fig. 6(c), there was an 800
increase in the volume of reinforcement but with very little coales-
600
cence of chitosan reinforcement particles, an evidence of even dis-
persion of the particles in the matrix which made it possess the 400
highest flexural strength. Increasing reinforcement content up 200
from 6 wt% and more, there was a gradual decrease in the flexural
0
strength. By referring to the SEM images, at 6 wt% to 10 wt% chi- A B C D E F
tosan, there had already began a congestion of the HDPE phase Samples
with chitosan particles which increased the viscosity of the HDPE
which in turn reduced the flexural strength [16]. As the reinforce- Fig. 5. Flexural Modulus of HDPE Matrix and the Composite Samples.

ment content increased up to 6 wt% the flexural strength improved

which was higher than that of the neat HDPE (21.66 MPa). This
load bearing capability is due to the fact that compressive stress
tends to close cracks and flaws that are perpendicular to the
applied stress [5].
3.1.5. Flexural modulus
The flexural modulus of the HDPE matrix and the Chitosan
particles-HDPE composites are shown in Fig. 5.
The flexural modulus was highest at 4 wt%. Chitosan with a
value of 1690 MPa. The flexural modulus increases linearly from
2 to 4 wt% chitosan particles reinforcement, this may be attributed
to the fact that the filler gives good reinforcement with the matrix
with well dispersed particulate. However, the flexural modulus
begins to drop gradually from 6 to 10 wt%, this may be due to poor
bonding and/or dispersion between the matrix and reinforcement
particularly at higher volume fraction of chitosan particles
addition.
Statistically, almost all the composites samples from 2 wt% Chi-
tosan/ HDPE to /8 wt% Chitosan/HDPE composites had higher flex-
ural modulus compared to the neat HDPE matrix. This showed that
the chitosan particles were good reinforcement materials under
flexural loading.
3.2. SEM images of the composite

The scanning electron microscopy is a resourceful instrument

accessible for the examination of microstructures of composites.
200 The surface of the matrix and chitosan based composites were
Impact Strength (KJ/m2)

examined in order to study the interfacial properties between

150 the chitosan reinforcement particles and the HDPE matrix.
Fig. 6 (a) shows the SEM image of the neat HDPE matrix. This is
an indication of ductile mode of fracture because of the presence of
100
hollow depressions somewhat rough fracture surfaces and this is in
consonance with results obtained from the mechanical tests car-
50 ried out on the composites.
Fig. 6 (b) shows complete filling of the ductile HDPE matrix by
0 chitosan reinforcement particles. There is no void formation,
A B C D E F agglomeration or particle coarsening of the chitosan reinforcement
Sample
because the particles were evenly dispersed into the matrix mak-
Fig. 3. Variations of the Impact Strength of HDPE Matrix and Chitosan-HDPE ing it to be able to impede dislocation motion and resist applied
Composites. stresses adequately.
686 O.O. Daramola et al. / Materials Today: Proceedings 38 (2021) 682–687

Fig. 6. (a-f) SEM Images of; [a] HDPE (control) [b] 2 wt% Chitosan-HDPE Composite [c] 4 wt%-HDPE Composite [d] 6 wt%-HDPE Composite [e] 8 wt%-HDPE Composite[f] 10 wt
%-HDPE Composite.

In Fig. 6 (c) there is the occurrence and manifestation of chi- the formation of large voids which means there are large stress
tosan agglomerates in the composites. This may be as a result of concentration sites which to a large extent amplifies the stress
increase in the volume fraction of the chitosan reinforcement par- applied on the composite leading to the fastest rate of fracture.
ticles. This stemmed a congestion of the ductile HDPE matrix with From the micrograph, there is a large pulling out or debonding of
chitosan particles leading to an agglomeration of the particles, for- the chitosan particles from the HDPE matrix. It is characterized
mation of less voids and stress concentration sites. Though the by the largest amount of void formation, largest amount of
presence of voids were observed but the overall interfacial prop- debonding of the chitosan particles, largest amount of stress con-
erty and strength was better largely because of the strong interface centration sites and a fastest form of fracture under the least
that still existed and the high reinforcement to void ratio. applied stress when compared to the other composites.
Fig. 6 (d) revealed that there is an increase in reinforcement
particles which led to an increase in the voids of the chitosan/HDPE
4. Conclusion
composite. The mode of fracture was somewhat brittle. This is
because the voids act as stress raisers making the material to fail
After a meticulous study of the mechanical properties of the
or fracture under decreased applied stress i.e. the more the voids,
Chitosan-HDPE composites, the following deductions were made;
the more the stress concentration and amplification and the faster
the rate of fracture under a lower applied stress. Also, the interface
i. The Chitosan particle performed effectively as a good rein-
between the particles and the reinforcement is weak, leading to
forcement by effectively transferring stresses from the HDPE
debonding and significant separation of the composite under a
matrix and thus increasing the mechanical properties of the
low applied stress. The fracture surface is smooth indicating a brit-
composites well above the neat HDPE polymer matrix.
tle fracture mode of failure.
ii. Examining the surface morphology of the composites, those
Fig. 6 (e) shows the fractured surface of the 8 wt% Chitosan-
above 4 wt% chitosan particle addition had substantial
HDPE Composite. There is the manifestation of significant popula-
amount of particle coarsening and agglomeration which
tion of voids in this composite compared to the other lower volume
did affect in a negative way the mechanical properties of
fraction 8 wt% Chitosan-HDPE composites. This was because of an
those composites.
increase in the volume fraction of chitosan reinforcement. There is
iii. Also, 4 wt% Chitosan-HDPE composite has proven to be the
also a substantial congestion of the ductile HDPE matrix. The voids
best Chitosan-HDPE composite developed because there
act as stress concentration sites i.e. they have the ability to raise
seems to be a balance and an optimization of the mechanical
the stress level significantly when a somewhat low stress is applied
properties such as having the highest flexural strength and
on the bulk composite. They can magnify and amplify the stresses
modulus, high impact strength, high elastic modulus and
acting on the composite leading to a fast fracture under a low
finally a very higher tensile strength.
applied stress. Also, the interface properties and bond strength
were low compared to other Chitosan-HDPE composites of lower
reinforcement because the grains of the chitosan were more CRediT authorship contribution statement
exposed from the HDPE matrix as if there is a falling out of the
grains by a phenomenon called debonding when under applied O.O. Daramola: Conceptualization, Supervision, Data curation,
stresses leading to weaker mechanical properties. Formal analysis, Writing original draft, Writing – review & editing.
Fig. 6 (f) shows numerous voids in the microstructure of com- A.S. Taiwo: Project administration, Writing original draft.
posites coupled with huge formation of agglomerates. There is I.O. Oladele: Supervision. J.L. Olajide: Software, Methodology.
 O.O. Daramola et al. / Materials Today: Proceedings 38 (2021) 682–687
S.A. Adeleke: Project administration. B.O. Adewuyi: Supervision.
E.R. Sadiku: Supervision, Resources, Writing - review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgement
Authors Acknowledged the Institute of NanoEngineering and
Research (INER), Tshwane University of Technology, Pretoria South
Africa and Materials Testing Laboratory, Department of Metallurgi-
cal and Materials Engineering, Federal University of Technology,
Akure, Nigeria for their support.
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