STUDY OF MECHANICAL PROPERTIES OF COMPOSITE

MATERIAL BASED ON POLYPROPYLENE AND

VIETNAMESE RICE HUSK FILLER
THANH DUY TRAN1 ,MAO DANG NGUYEN1 ,C.N. HA THUC1 ,H. HA THUC2 ,TAI DANG TAN3
1
FACULTY OF MATERIALS SCIENCE, UNIVERSITY OF SCIENCE, VIETNAM NATIONAL
UNIVERSITY, 227 NGUYEN VAN CU ROAD ,HO CHI MINH CITY, VIETNAM
2
FACULTY OF CHEMISTRY, UNIVERSITY OF SCIENCE, VIETNAM NATIONAL UNIVERSITY,
227 NGUYEN VAN CU ROAD HO CHI MINH CITY, VIETNAM
3
PLASTIC AND RUBBER TECHNOLOGY CENTER, 156 NAM KY KHOI NGHIA ROAD, HO CHI
MINH CITY, VIETNAM

ALYSSA SARAH E. ARENAS

LABORATORY REPORT NO. 4
Abstract
Polymer products have long caused drastic environmental impact. Because of this,
nowadays, different researches regarding the development of new materials incorporating
renewable sources to polymers were highly encouraged. Biocomposites are among these
materials. In this study, biocomposites made from polypropylene incorporated with rice husk flour
having 100-125 𝜇m size distribution would be focused. Note that the compatibilizer that was used
is maleic anhydride grafted polypropylene. The feasibility of this biocomposite as well as the effect
of the rice husk flour and the mentioned compatibilizer to this were investigated. Results then
showed that there was an improvement in the thermal stability and mechanical properties of the
composite with relatively high addition of rice husk content, as well as the maleic anhydride grafted
polypropylene.
Keywords: biocomposites, rice husk flour, compatibilizer, thermal stability, mechanical properties

Introduction
Because of its nonabrasive and biodegradable ability, low energy consumption, low
density, low cost, and high-specific mechanical properties as compared to synthetic fibers, natural
resources, rather, natural fibers have various eco-friendly applications in composite materials
nowadays (Huber et al., 2012). Rice have long been produced in several countries, especially in
Asia. Because of this, rice husk flour (RHF), which is one of the main agricultural wastes from this
production, is very abundant in this region. In fact, around 685 million tons of rice straw and around
137 milllion tons of rice husk are eliminated by many rice factories in the world per year (Lim et
al., 2012), which eventually caused some environmental problems. In response to this, many
research regarding development of applications using these agricultural wastes were made in
hope of reducing the environmental pollution caused by these. Some of these application include
using RHF as energy source (Kayal et al., 2010) and rice husk ash as filler in polymer composites
adsorbents of heavy metals, and ceramic or road-building materials(Le et al., 2013).
In this study, with narrow size of around 100-125 𝜇m narrow size distribution, RHF from
Vietnam were used in the fabrication of composites based on polypropylene (PP) matrix and a
compatibilizer which is maleic anhydride grafter polypropylene(PP-g-MA). It is expected that with
the reaction of the anhydride groups of PP-g-MA to the hydroxyl groups on the RHF surface
particles, there would be improvement in the properties of the composites. In order to verify such
claim, different characterization equipment such as thermal gravimetric analysis (TGA), scanning
electron microscope (SEM), and universal testing machine (UTM) would be performed.
Review
a. Property/Application

The property to be explored in this paper are mechanical properties specifically the
tensile modulus, flexural modulus and toughness. Tensile modulus, sometimes known as
Young’s modulus, refers to the measure of a material’s ability to refrain from having
changes in length when external forces such as tension or compression acts upon it
(Augustyn et al., 2019). On the other hand, flexural modulus pertains to the material’s
ability to bend. In a more mechanical explanation, it pertains to the “ratio of stress to strain
during a flexural deformation, or bending” (“Corrosionpedia”,2017). Lastly, toughness
could be described as the moduli of toughness and can be graphically described as the
area under the stress-strain curve up to the fracture. It pertains to the amount of energy
needed to cause a complete fracture to the material (Roylance, 2001). These properties
were then determined with the use of universal testing machine in relation to the amount
of the components incorporated on the polymer matrix.

Other than the mechanical properties, the morphology and the thermal stability of the
material were also observed. Morphology is study of the structure, shape and size of an
organism or material as well as the relationship among its parts(Villee,2018). This was
described through the use of a scanning electron microscope (SEM) in relation again to
the amount of components used. Thermal stability, on the other hand, was shown in the
study in terms of the loss mass rate of the materials in relation to temperature and the
amount of components as well.

b. Experimental Design

In order to remove some rocks, dust, and soil, RHF was first washed, then treated
for a duration of 72 hours, by 1% NaOH solution. Neutralization of the solution by 0.1 M
hydrogen chloride solution comes next. After this, the RHF was again washed but this
time, 3 times with water. For 24 hours, the RHF was then dried in a vacuum oven at 80 °C
in order to remove moisture. Afterwards, in order to attain size distribution ranging from
100-125 𝜇m, RHF was grinded and screened in two types of sieves with meshes of 100
and 125 𝜇m. The remaining components namely maleic anhydride grafter polypropylene
(PP-g-MA) and polypropylene (PP) matrix, together with the acquired RHF were then
blended using a Haake PolyLab mixer for a duration of 6 minutes at a temperature of 170
°C and stir rate of 60 rpm. The resulting melted compound is then inserted to a hot press
for about 5 minutes at 3kPa and 180 °C. These were then cooled down to room
temperature and cut into 17 cm x 17 cm x 2 mm dimensions for mechanical testing.

To investigate the tensile and flexural modulus of the composites, QC-505A1

(Comtech, Taiwan) universal testing machine (UTM) with 5 mm/min crosshead speed was
used. Note for accuracy and precision, at least 5 pieces for each composition were used.
For observation of the composite’s morphology, a JSM 6600 (JEOL co., Japan) scanning
electron microscope was used. Lastly, a thermogravimetric analyzer TGA Q500 (TA
Instruments co., USA) was used to characterize the thermal stability of the materials. Note
 that the samples were exposed to nitrogen atmosphere and the parameters used were 10
°C /min heating rate and 35-800°C temperature range.

c. Results

In Figures 4 and 5, the effect of the PP-g-MA content or compatibilizer on the

mechanical properties of the composites was determined. As seen here, generally, the
improvements of these properties were improved with the addition of such content similar
to the study of Xiuju, et al. (2013). From 0 to 4% wt of PP-g-MA content, there was increase
in the mechanical properties but at 6 and 8% wt there was a sudden decrease. However,
note that this is still higher than composites without the compatibilizer. At lower
concentration, the anhydride groups of PP-g-MA interacts with the hydrophilic hydroxyl
groups of the RHF through esterification reaction. This then helps improve the interfacial
adhesion between the matrix and the filler, and thus strengthens the bond and provides
higher mechanical properties (Zabihzadeh, 2011). On the other hand, in higher
concentration of PP-g-MA, a new PP-g-MA phase may have been formed from the
agglomeration of the excess amount of compatibilizer and may have caused inhibition on
the desired interfacial adhesion between the filler and the matrix(Kim,2007).
 Similar to figures 4 and 5, the above figures also showed the mechanical properties
of the composites but this time, in reference to the incorporation of the RHF content. Here
the compatibilizer was kept constant at 4 wt%. As the figures suggest, improved stiffness
of the composite was achieved with the addition of the RHF filler as compared to the pure
PP matrix. Such is a normal behavior when polymer matrices are incorporated with rigid
fillers (Thanh et al., 2012). However, a sudden decrease in the stress was observed upon
the addition of fillers higher than 100 phr. This could be explained by the fact that from 40
to 100 phr, under the chemical linking effect of the compatibilizer, RHF disperses well into
the polymer matrix and act as the nucleus to absorb the external load’s energy. However,
once the concentration of the filler increases too much, there might be agglomerations of
it which may appear on the matrix and cause hindrance to the interfacial adhesion
between the filler and the matrix. Since the compatibilizer was only at 4wt% this were not
able to fully disperse the filler into the matrix thus, the sudden decrease in the materials’
stress.

Figure 8 shows the morphology of both a PP/RHF composite (a) and a

PP/RHF/PP-g-MA composite in order to have a better observation of the effect of the
compatibilzer and filler to the composite. As seen in figure 8(a), a rough morphology of the
composite was displayed. This is because with the absence of the PP-g-MA which serves
as the compatibilizer, the filler and matrix phase have poor interaction. Furthermore, upon
the addition of 4 wt% PP-g-MA, there is a noticeable change in the morphology. There is
little to no free spaced between the two phases thus, the separating positions were
reduced. This just shows that as fillers are important in increasing the mechanical
properties of the composites, PP-g-MA improves the interfacial adhesion of the two
phases.
 As seen on figure 9, mass loss of the PP at point a, starts at 384 °C and reaches
maximum loss at about 454 °C. In the case of RHF at point b, mass loss starts 340 °C due
to the decomposition of lignin and cellulose/hemicellulose. Note that the mass loss
observed at around 250 °C was just a result of the evaporation of absorbed moisture in
RHF and should be considered irrelevant. On the other hand, the mass loss of the PP/RHF
composites and PP/RHF/PP-g-MA composite started at around 285 °C and 295 °C,
respectively. It can also be seen here that the PP/RHF/PP-g-MA has better thermal
stability than PP/RHF because the mass loss rate of the latter was faster. This may be
because the 4 wt% compatibilizer helps to have easier and faster dispersion of the RHF
to the polymer matrix which causes the PP molecules to surround and indulge the RHF.
Thus, it would be harder to disorient the structure of the composite with the compatibilizer
(Zabihzadeh,2011).

As I read through the article, I have learned that there are many factors which need
to be considered in the fabrication of a composite reinforced with agricultural wastes,
rather, by natural fillers. First, since characterization techniques would be used in
determining the properties of the composites, it is very much important to take note of the
specifications of the test sample as well as the parameters that are to be set on the
equipment to be used. This is because even with small variations of the parameters and
dimensions of the test samples may cause alterations on the expected results. Aside from
this is the percent by weight content of the materials to be used. Take for examples too
much compatibilizer and filler may cause unnecessary agglomeration of these which may
cause disruption to the interfacial dispersion of the matrix and the filler, thus, affect the
structure of the composite. Having excess amounts defeat the purpose of fabricating the
composite in the first place. Other than this, compatibility of the filler, matrix and
compatibilizer is also a huge factor in the fabrication of composites. No matter how
promising the properties of the filler is, if it is not fully dispersed to the matrix, instead of
improving the properties of the composite, it may cause a rough and uneven surface and
a faster mass loss rate. This fabrication, although a little bit tedious would be of great help
to the environment.
Conclusion/Recommendation
Since environmental problems caused by both plastic production and agricultural waste
are rampant nowadays. It would be of great help to think of ways on how to minimize both
hindrances. One of which is through the incorporation of agricultural wastes as fillers to a polymer
matrix. This study shows that it is feasible for such agricultural wastes, specifically, rice husk to
work as reinforcement fillers in the formation of composites. Note that these do not only improve
the toughness of the composites but also improve other mechanical properties such as tensile
and flexural strength of the composite. Furthermore, compatibilizers are important as it ensure
that there is uniform and stable interfacial dispersion between the matrix and the fillers. In
conclusion, this innovation could be a steppingstone for the start of a new era of renewable
sources that greatly helps in the preservation of the environment for future generations. Thus, I
would recommend future research regarding these topics exploring other agricultural wastes,
compatibilizers and polymer matrices.
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