Processing and characterization of rotomolded high-

density polyethylene with rice husk particles as

reinforcement
Abhilash S S1,2, Prabha Sankar A1, D Lenin Singaravelu1*
1
Department of Production Engineering, National Institute of Technology Tiruchirapally, India
2
Department of Mechanical Engineering, SCT College of Engineering Trivandrum, India
*Correspondence to be addressed to dlenin@nitt.edu

Abstract. Rotational moulding is a plastic processing technology used to

manufacture large hollow products economically with short production runs.
High-density polyethylene or HDPE is widely used for rotational moulding
because of its excellent chemical resistance, high stiffness, good processability,
and low cost. However, its application is limited due to its modest mechanical
properties. This limitation can be overcome by the incorporation of fibers or
fillers as reinforcement. In the present study, Rice Husk (RH) is used as the
reinforcement filler. The different weight percentage of rice husk is added to
HDPE and is roto moulded to get polymer composites. The physical,
mechanical, morphological, and vibration damping characteristics are then
studied to determine the effect of rice husk in the HDPE matrix. Mechanical
properties were investigated as per ASTM standards, and the best values of
tensile and flexural properties were obtained for the composite with 10% rice
husk powder. The impact strength and hardness values were found to be less
significant for reinforced composites. The Thermo Gravimetric Analysis (TGA)
reported that the degradation of RH particles happens at 263 oC and hence the
processing temperature of the composites is kept below this degradation
temperature to get defect-free composites. The experimental modal analysis
results proved that the incorporation of Rice husk particles improves the natural
frequency of the composites from 24.8 Hz to 55.7 Hz.

Keywords: Rotational moulding, HDPE, Rice husk, Modal Analysis.

1 Introduction
Rotational moulding of HDPE is done to produce products like pontoons, sea toppers,
water tanks, etc. which are large, hollow, and seamless. Rotational moulding results in
parts that are stress-free and uniform wall thickness. It is a high-temperature low-
pressure process that involves biaxial rotation of mould containing plastic powder in
an oven. As a result, the plastic powder melts on the inner surface of the mould and
fuses in layers until the entire powder is used up, to form the desired product1.The
quality of a rotationally moulded part depends on different process parameters like
mould material, the rotational speed of mould, oven temperature, cycle time, cooling
medium, powder size, pigments, etc.It is observed that warpage of rotationally
moulded part increases with increase in oven temperature, part cooling rate, thermal
diffusivity of mould material and use of mould release agent whereas the warpage
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decreases with the thickness of the part, the diameter of venting pipe, and mould
pressurization 2. Many research publications recommend the use of natural fibers since
they are biodegradable, eco-friendly, and low cost34.

The modest physical and mechanical properties of HDPE pose a hindrance to the
application of rotational moulding. The initial solution of increasing the wall thickness
of the product affects the economic feasibility for short production runs. An increase
in mechanical properties of HDPE is observed when the processing temperature is
increased 5. However, the use of reinforcement fillers is a more adequate solution.
Jayaraman et al.6 added sisal and wood fibres into LMDPE and the rotationally
moulded product showed significant mechanical properties. Ortega et al. 7 studied the
effect of banana and abaca fibre in the rotational moulding process and found an
increase in tensile and flexural modulus. Similar results were also obtained by
Oliveira et al.8 when hemp fibres were added to polyethylene in rotational moulding.
Mechanical properties were reported to be improved up to 10% fiber addition with the
use of bamboo, coir, and Tampico fibers in Linear Low-Density Polyethylene
(LLDPE) matrix9,10. The natural fibers, if undergoes a fiber treatment before
composite preparation can have enhanced mechanical properties especially tensile and
flexural strength[11-12].

In this study, rice husk powder is used as the reinforcing filler with HDPE during
rotational moulding. Initially, a lab model rotational moulding machine is designed
and fabricated for carrying out the experiments. Then products with 5%, 10%, and
15% of rice husk in HDPEmatrixare developed with the help of the lab model
rotomoulding machine. The physical, mechanical, and morphological characteristics
are then investigated. Density is measured as per ASTM D 792 standards. Tensile test
is carried out following the ASTM standard of D 638 and Flexural strength as per
ASTM D 790. Impact properties were investigated following the ASTM standard of
D256. The vibration damping properties of all the composites were estimated
following ASTM standards to determine the effect of fiber content in altering the
natural frequency of the composite prepared. Therefore the objective of this study is to
develop and characterize HDPE polymer composite with rice husk powder as
reinforcement.

2 Experimental
2.1 Experimental setup

The basic requirements of a rotational moulding machine are, the mould and its
contents are heated, rotated, and cooled. The rotation of the mould should be biaxial
with a definite speed ratio between the two axes. Also, the rotation should be uniform
throughout the moulding process. Fig. 1 shows the 3-D model of the rotational
moulding machine.
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Fig. 1. (a) 3-D model of the rotational moulding machine (b) The lab model rotational
moulding machine fabricated.

The simulation and compatibility of the machine are done and are followed by
fabrication. The machine was made using 20mm × 10mm mild steel rods. The primary
frame is of dimensions 280mm × 280mm and the secondary frame is of dimensions
230mm × 230mm. The primary frame is driven by a 12V DC motor at a speed of 40
rpm. The chain drive with sprockets provides the necessary rotational motion to the
bevel gear pair that drives the secondary frame. The bevel gear pair is having a gear
ratio of 4 : 1. During the rotational moulding process, the entire setup is transferred
inside the hot air oven after mounting the mould. The oven provides the required heat
input to the mould as the machine rotates bi-axially. This heat is transferred to the
mould, then to the charge particles, and finally to the air inside the mould. The peak
internal air temperature is measured at a regular interval to monitor the processing
conditions.

2.2 Materials

Rice husk powder is used as the reinforcing filler. Rice husk is organic waste and is
the by-product of rice milling. It is a cellulose-based fibre. Rice husk powder is
collected from the rice milling industry in Kerala, a state in India. It is then sieved to
obtain fine powder from the mix. The rice husk contains 75-90% organic waste such
as lignin and cellulose. The matrix material used is High-Density Polyethylene
(HDPE). The mould required for the present study is made from a stainless steel sheet.
The speed ratio for the machine was fixed based on the shape of the mould. During
the rotational moulding process, the plastic melts and adheres to the mould surface.
Hence the de-charging of mould might be a problem. This is overcome using a mould
release agent. The mould release agent used in this study is silicone spray
manufactured by Stella. One spray over the mould surface produces a barrier of few
microns thick between the molten plastic and mould surface. The oven used for
heating the mould is a hot air oven made by LabTech. The oven has a hot air
circulating fan which ensures hot air accessibility in every part of the oven. The
temperature inside the oven is controlled by a thermostat coupled with a digital panel
to set the temperature. The maximum temperature obtained from the oven is 250̊ C.
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2.3 Experimentation

Rotational moulding of rice husk as reinforcement with HDPE matrix is done to

develop samples. Each sample had a heating cycle time of 35 minutes and a cooling
cycle time of 30 minutes. The composite designation is shown in table 1.

Table 1. Composite Designation

Weight of rice Weight of Oven

Sample Composition
husk (g) HDPE (g) temperature (̊ C)

HDPE 100% HDPE 0 120 230

5% rice husk + 95%

RH1 6 114 230
HDPE

10% rice husk + 90%

RH2 12 108 230
HDPE

15% rice husk + 85%

RH3 18 102 230
HDPE

TGA of rice husk. TGA is conducted using Perkin Elmer STA 6000 Thermo -
Gravimetric Analyzer with a resolution of 0.1μg. The heating rate is selected as 10-
degree Celsius per minute starting at room temperature to 650 oC. The nitrogen gas is
supplied at the rate of 20ml/minute. TGA is done to characterize the materials by
measuring the change in mass as a function of temperature. 15g of rice husk is heated
at a rate of 10oC per minute for analysis.

Mechanical characterization. Tensile and flexural strength is determined as per

ASTM D638 and ASTM D790 standards, respectively. Tests are conducted for five
samples each for different compositions of rice husk and HDPE and the mean value is
considered. Both tests are conducted in Tinius Olsen H50KL tensometer fitted with a
10kN load cell. The impact test is carried as per ASTM D256 standard in an impact
test machine with a head weight of 1 kg. A Yuzuki Shore D Durometer is used to
measure the hardness of the developed product at five different locations and the
average value is considered.

Physical characterization. Density is measured as per ASTM D 792 standard.

Initially, the dry weight of the specimen is accurately measured. After mounting the
immersion vessel on the supporting grips, completely immerse the suspended
specimen and sinker. With the help of a wire, remove any bubbles that adhere to the
specimen surface. Determine the mass of the suspended specimen. Record the weight
of the sinker and sample holder in the same position without a specimen. This weight
is termed as ‘w’. The procedure is repeated for all the composite specimens prepared.
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Specific gravity,230oC = a/(a+w−b)

𝐷𝑒𝑛𝑠𝑖𝑡𝑦, 𝜌 23o𝐶 =𝑆𝑝𝑒𝑐𝑖𝑓𝑖𝑐𝐺𝑟𝑎𝑣𝑖𝑡𝑦∗997.5 𝐾𝑔/𝑚3

Where,

a = apparent mass of specimen in air

b = apparent mass of specimen completely immersed in the fluid

w = apparent mass of sinker immersed

Morphological characterization. The fractured surfaces of tensile specimens are

morphologically analyzed with Scanning Electron Microscopy (SEM), TESCAN
VEGA3. The electron interaction with surfaces is improved via gold sputtering.
Sputtering is done to initiate electron–workpiece interaction. SEM images are
obtained at different magnifications.

Experimental Modal Analysis (EMA). The dynamic characteristics of HDPE and

rice husk powder polymer composite are determined by vibration test as per ASTME
756-05. Impulsive forces are applied at the free end of the specimen. The specimen is
clamped in a cantilever position at one end and kept free at the other end. An
accelerometer of miniature size is attached with the specimen to acquire the
displacement signals. An impact hammer with a rubber bush attached is used for the
excitation of the cantilever beam. The force of hammering action is directly
proportional to the weight of the hammer and impact velocity. The signals from the
accelerometer are analyzed with the help of a computer to determine the natural
frequency of the samples. A miniature impact hammer is used for excitation, and the
magnitude of the impact is measured with a piezoelectric transducer. The signals from
the transducer are sent to DAQ (Data Acquisition System) for signal processing.
Figure 2 represents the schematic representation of the EMA test setup.

Fig.2. Experimental Modal Analysis test setup.

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3. Results and discussions

Rotational moulding of samples with 5% and 10% of rice husk with HDPE yielded
hollow cuboidal products. However, the sample with 15% of rice husk with HDPE
resulted in a foamed structure due to the type of interaction of rice husk with HDPE
and processing conditions. Fig. 3 shows the foamed structure obtained.

Fig. 3. The foamed structure obtained with 15% rice husk

3.1 Thermogravimetric analysis (TGA)

The Thermogram of rice husk is shown in Fig. 4. The TGA curve showed less loss of
weight until a temperature of about 100̊ C due to the elimination of absorbed water.
The weight loss was then very low till a temperature of 263̊ C. When the temperature
is increased beyond 263̊ C, there is a drastic loss of weight which is continued till a
temperature of 360̊ C. This is the region's active pyrolysis. Thereafter the weight loss
rate is again less. The residual weight obtained at 650̊ C is 3.862g.
 7

Fig. 4. Thermogram of rice husk heated at 10̊ C/min

From the TGA, it is found out that the stability of rice husk is affected at temperatures
above 263̊ C. Thus, the processing conditions for rotational moulding are to be under
this temperature to ensure the stability of rice husk for the process.

3.2 Mechanical characterization

The tensile strength of composite with different weight percentages of filler is

presented in Fig 5(a). It can be observed that the bending strength has improved with
the addition of rice husk powder to HDPE. It was because the rice husk powder was
completely wrapped by HDPE. This enabled the rice husk particles to restrain the
movement of polymer chains on the application of load. A similar trend is also seen in
the case of the flexural strength test. The results are as shown in Fig 5(d). It can be
attributed to the high modulus of elasticity of rice husk powder. The results of the
impact test and hardness test are presented in Fig 5(b) and (c) respectively. It is
observed that there is no appreciable improvement of both the properties of HDPE on
the addition of rice husk powder filler. It can be observed that the outer layer of the
samples is almost composed of HDPE alone. Thus, there is not much variation to the
hardness values of HDPE polymer composite.
8

Fig. 5. Mechanical characterisation results (a) Tensile strength, (b) Impact Strength, (c)
Hardness & (d) Flexural strength

3.3 Physical characterization

The density of the samples as per ASTM standards is shown in Fig. 10. The bulk
density of rice husk powder is less than that of HDPE. As a result, the density of
polymer composite is found to decrease with an increase in the weight percentage of
rice husk powder in the HDPE matrix. It was also noticed that the incorporation of RH
particles into the HDPE matrix leaves bubbles and voids on the matrix. When the fiber
content is maximum, the percentage of voids formed per unit area is very much
significant. The voids formation leads to a decrease in the density values of the
composites. The percentage decrease in density values of RH1 and RH2 composites
are very marginal whereas RH3 composites marked a significant decrement value
when compared with the unreinforced HDPE.
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Fig.6. Density values of RH reinforced composited compared with unreinforced one.

3.4 Morphological characterization

The fractured surface of the tensile specimen is investigated through scanning electron
microscopy. The SEM images of the fractured surface of polymer composite are
shown in Fig.7(a) and Fig. 7 (b). The addition of rice husk powder as the filler has
caused the formation of voids in the HDPE matrix. Also, it is found that the dispersion
of rice husk powder is not uniform in the HDPE matrix. There exists, even though a
small concentration gradient of rice husk powder from the outer layer to the inner
layer of HDPE matrix with the inner layer having a slightly higher concentration of
rice husk powder. When comparing the morphography of RH1 and RH 3 composites,
the RH particles are more closely packed and agglomerated in the matrix thereby
reducing the reinforcing efficiency. The fiber-matrix debonding is visible in figure
7(a). Figure 7(b) represents the SEM image of the RH1 composite where the
reinforcement fillers are found to be evenly distributed. Also, the fiber-matrix bonding
is satisfactory.

Fig.7. SEM image of (a) RH3 & (b) RH1 composites

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3.5 Experimental Modal Analysis (EMA)

The frequency at which the composite material resonates is called its natural
frequency. The aim of incorporating the fibers in the present study is to enhance the
natural frequency of the composites, thereby achieving better stiffness. The most used
experimental modal analysis technique is the hammer testing method. Here the
composite bar is excited with an impact hammer attached with a force transducer at
several points, and the response is measured at a single point. A fast Fourier transform
analyzer is used to generate a frequency response function (FRF) as output. The peak
indications in the FRF curve represent the natural frequency of the composites. The
results of the vibrational analysis are presented in Fig 8. It is observed that there is an
increase in modulus as the weight percentage of rice husk powder in HDPE increases.
This is mainly due to the inherent properties of natural fibers. The RH particles have a
significant amount of lignins and cellulose in their basic structure. This will act as a
vibration-absorbing medium. This inherent property of RH particles reflects in the
Frequency Response Curve. When the percentage of RH articles increases, the natural
frequency of the composites prepared is also found to be increased.

Fig. 8. Frequency response curve (FRC) plotted for the composites compared with unreinforced
ones.

4 Conclusions

In this work, the effect of rice husk powder filler on the characteristics of HDPE had
been investigated. HDPE polymer composites with rice husk powder are fabricated by
rotational moulding process by incorporating different weight fractions of rice husk
powder in HDPE matrix. Mechanical properties were investigated, and the best values
of tensile and flexural properties were found to be 16.4 MPa and 20.36 MPa
 11

respectively for the composite with 10% rice husk powder. The effect of the addition
of rice husk powder to HDPE is found to have a less significant effect on impact
energy and hardness. The density of the composites is found to decrease with an
increase in the weight percentage of rice husk powder in HDPE. The vibrational
analysis also showed an increase in moduli on the addition of rice husk powder. SEM
images of the broken tensile specimen were taken to study morphological
characteristics of composites. The presence of voids and a slight concentration
gradient of filler were observed. The maximum amount of rice husk that can be added
to HDPE is found to be between 10% to 15% of weight as RH3 yielded defective
products. In short, the rotomoulded composites proved better mechanical properties at
10% filler addition. Hence it can be concluded that the incorporation of RH particles
is very much effective in improving the mechanical strength. Hence the addition of
biodegradable material in a non-biodegradable polymer matrix is achieved thereby
reducing the usage of plastic to some extent. 10% natural fiber addition reduces the
overall cost of the rotomoulded product without compromising the strength of the
product. This is the social and economic relevance highlighted as the outcome of the
present work. Also, the EMA results proved that the RH particles are having better
damping characteristics thereby finding application in vibrating parts of automobiles
like fuel tanks, wheel arch, dashboards, etc.

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