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Original Article

Flexural, thermal and dynamic mechanical


properties of date palm fibres reinforced epoxy
composites

Mohamed Hamdy Gheith a , Mohamed Abdel Aziz a , Waheedullah Ghori a , Naheed Saba b ,
Mohammad Asim b , Mohammad Jawaid b,c,∗ , Othman Y. Alothman c
a College of Engineering, King Khalid University, Abha, Saudi Arabia
b Laboratory of Biocomposite Technology, Institute of Tropical Forestry and Forest Products (INTROP), Universiti Putra Malaysia, 43400
Serdang, Selangor, Malaysia
c Department of Chemical Engineering, College of Engineering, King Saud University, Riyadh, Saudi Arabia

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

Article history: The aim of the present study is to improve the flexural, thermal stability and dynamic
Received 9 April 2018 mechanical properties of epoxy composites by reinforcing date palm fibres (DPF) at dif-
Accepted 1 June 2018 ferent loading (40%, 50% and 60% by wt.) and to evaluate the best loading through hand
Available online xxx lay-up technique. Three point bending dynamic properties in terms of storage modulus
(E ), loss modulus (E ) damping factor, Cole–Cole plot and thermal properties were analyzed
Keywords: by dynamic mechanical and thermogravimetric analyser, respectively. Flexural test results
Date palm fibres show that loading of 50% DPF increases both the flexural strength and modulus of pure epoxy
Epoxy composites composites from 26.15 MPa to 32.64 MPa and 2.26 GPa to 3.28 GPa, respectively. TGA results
Flexural strength revealed that reinforcement of DPF in epoxy composites also improves the thermal stability
Thermal stability and residual content. The residual content of epoxy (9.58%), 40% DPF/epoxy (12.51%), 50%
Dynamic mechanical properties DPF/epoxy (19.8%) and for 60% DPF/epoxy composites (15.2%) was noted, revealing that 50%
Damping factor DPF/epoxy composites confers the best result. Incorporation of DPF into epoxy also improves
Cole–Cole plot the E and E but 50% DPF show more remarkable improvement compared to 40% and 60%
DPF loading. Moreover, damping factor decreases considerably by the reinforcement of DPF
and are found lowest for 50% DPF/epoxy composites among all composites. Drawn Cole–Cole
plot also suggests the existence of certain heterogeneity in DPF/epoxy composites compared
to homogenous nature of epoxy composites. We concluded that 50% DPF loading is the ideal
loading to enhanced flexural, thermal stability and dynamic properties of epoxy composites.
© 2018 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier
Editora Ltda. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).


Corresponding author.
E-mail: jawaid md@yahoo.co.in (M. Jawaid).
https://doi.org/10.1016/j.jmrt.2018.06.013
2238-7854/© 2018 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier Editora Ltda. This is an open access
article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Please cite this article in press as: Gheith MH, et al. Flexural, thermal and dynamic mechanical properties of date palm fibres reinforced epoxy
composites. J Mater Res Technol. 2018. https://doi.org/10.1016/j.jmrt.2018.06.013
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DPF reinforced polypropylene (PP) composite materials are


1. Introduction investigated [14]. Researchers found that the addition of DPF
in the PP composites improved the interfacial adhesion and
As far as environment is concern most of the researchers are
hence mechanical and thermal properties. Interestingly, these
focused on the biodegradable and renewable lignocellulosic
fibres are also used as effective filler in both thermosetting
or natural fibres as the most promising material for economic
and thermoplastics materials [12,15,16] and their advanced
growth [1,2]. Renewable resource utilizations provide the opti-
industrial and engineering applications, such as automotive
mistic ways for sustainability of ‘green’ environment. Natural
and airspace components were also reported in literature
fibres such as kenaf, jute, hemp, sisal, pineapple leaf, date
[12]. Some of the recently conveyed study on the date palm
palm and oil palm are considered as waste material and are
materials reinforced polymer composites are presented in
found abundantly throughout the world [3,4]. Although nat-
Table 1.
ural fibres have many advantage over synthetic fibre such as
From the literature survey, it is evident that no work has
high biodegradability, non-abrasive nature, low energy con-
been reported on the incorporation of DPF in epoxy compos-
sumption, low densities/cost and high specific mechanical
ites. The present research is aimed to explore the effect of
properties [5,6]. However, many researchers reviewed that nat-
DPF loading (40%, 50% and 60% by wt.) on flexural strength,
ural fibres can effectively be used as filler/reinforced material
flexural modulus, thermal and dynamic mechanical proper-
in varieties of thermoplastic and thermoset polymer compos-
ties of epoxy composites. Besides this, it also open a platform
ites for constructional and automotive applications [7–9].
to utilize huge deposition of DPF in the Saudi Arabian region
Concerning about the date palm, the worldwide annual
as renewable and green reinforcing filler in polymer compos-
production of date palm tree is 42% more in comparison to
ite industries like other natural fibres such as kenaf, jute or
coir and 20–10% more compared to hemp and sisal. Each stem
hemp.
of palm tree is surrounded by a mesh of single cross fibres
which appears as a natural woven mat of fibres with different
diameters. Most commonly, this mat is separated and cleaned 2. Materials and method
to make baskets and ropes. DPF is an aggregation of 2–5 ␮m
sized multicellular fibre containing a central void and its shape Epoxy resin and hardener (Jointmine 905-3S) was supplied by
and structure resembles to coir fibre [10,11]. DPF is multicellu- Tazdiq Engineering Sdn. Bhd., Malaysia. DPF were imported
lar lignocellulosic fibre containing polysaccharides cellulose from (Riyadh)-Saudi Arabia. The chemical composition of DPF
(38–40%), lignin and a few minor components of fat, wax, shown in Table 2 was made at Malaysian Agricultural Research
pectin and inorganic substance [12]. Several attempts have and Development Institute (MARDI), Selangor, Malaysia.
been made to reinforce the DPF in thermoplastics and ther-
mosets polymer to improve their physical, mechanical and 2.1. Fabrication of composites
thermal properties. But prior to reinforcement, usually sur-
face modification is necessary to purify and clean the surface In this study DPF is used as filler for the fabrication of
of the fibres from large amount of impurities and uncom- DPF/epoxy composites at different loading. Prior to this, DPF
pleted growth, as they may result in poor adhesion between is ground into 0.8–1 mm by using grinding machine having
fibre and polymer. In one study, short DPF reinforced mod- average 6–8% moisture content and DPF/epoxy composites
ified polyester and epoxy matrices has been reported with were fabricated through hand lay-up technique and are tested
better morphology and enhanced mechanical properties [13]. according to ASTM standard. The ratio of DPF and epoxy in
In other study, natural weathering and thermal stability of DPF/epoxy composites are listed in Table 3.

Table 1 – Exclusive literature reported on date palm reinforced polymer composites.


Reinforcements Polymer matrix References

Date palm fibres Polyester [17]


Date palm stem fibres Epoxy [18]
Date palm wood fronds Polyester [19]
Date palm fibres Polypropylene (PP) [20]
Date palm fibres High density polyethylene (HDPE) [21]
Short date palm fibres Poly-epoxy thermoset [22]
Date palm fibres Polyester [23]
Date palm seed particles Polyester [24]
Date seeds powder Polyester [25]
Date palm fibres PP [26]
Date palm leaflets Polystyrene [27]
Date palm fibres and graphite filler Epoxy [28]
Date palm fibres Thermoplastic starch [29]
Date palm particles Polyurethane [30]
Date palm fibres Recycled PP/low density polyethylene (LDPE)/HDPE ternary blends [31]

Please cite this article in press as: Gheith MH, et al. Flexural, thermal and dynamic mechanical properties of date palm fibres reinforced epoxy
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40 4
Table 2 – Chemical composition of DPF.
35 3.5
Constituents of DPF Value (%)

Flexural Strength (MPa)

Flexural modulus (GPa)


30 3
Cellulose 26.92
25 2.5
Hemicellulose 43.21
Lignin 27.42 20 2
Extractives 1.75 15 1.5
Others 0.70
10 1

5 0.5
Table 3 – Formulation of DPF/epoxy composites.
0 0
Polymer composites Epoxy resin in wt.% DPF in wt.% Neat Epoxy 40%DPF 50%DPF 60%DPF

Neat epoxy resin 100 0 Fig. 1 – Effect of DPF loading on flexural strength and
40% DPF 60 40
modulus of epoxy composites.
50% DPF 50 50
60% DPF 40 60

epoxy composites get increased up to 32.64 MPa and 3.28 GPa,


respectively. The comparative increment in flexural strength
3. Characterizations
and modulus of 50% DPF/epoxy composite with pure epoxy
composites are recorded as 122.7% and 141.6%, respectively.
3.1. Flexural testing
However, at 60% DPF loading, reduction in the flexural strength
(27.83 MPa) and modulus (2.94 GPa) of epoxy composites are
Three-point bending flexural tests according to ASTM D790
noticed. Research findings reported that an increment of fibre
standard with the crosshead speed of 2.0 mm/min were
loading in composites can increases both the flexural strength
applied on upper and lower surface of each six replicate
of composites up to critical loading point [8,32,33]. Decline in
specimens of pure epoxy composites and each DPF/epoxy
the value of flexural properties beyond 50% loading can be
composites and the failure was calculated when bending of
ascribed on account of insufficient quantity of available poly-
specimen reach up to corresponding critical point.
mer matrix to wet or cover all reinforced DPF [32], resulting
poor interfacial adhesion between DPF and epoxy matrix to
3.2. Thermogravimetric analysis (TGA)
transfer the applied stress under observation. This argument
is in line with other researchers where date palm particles
Thermal stability of epoxy and DPF/epoxy composites were
get agglomerates on higher loading in polyurethane matrix,
characterized by using a thermo-gravimetric analyzer (TGA
due to poor wetting of the particles by the matrix besides
Q500, TA Instruments, USA) at 20 ◦ C/min under a room tem-
the incompatibility due to hydrophilicity of reinforcement
perature in the range of 30–700 ◦ C.
and hydrophobicity of polyurethane matrix [30]. Moreover,
observed highest flexural strength and modulus of DPF/epoxy
3.3. Dynamic mechanical analysis (DMA)
composites at 50% loading are also in line with other existing
findings showing better flexural properties at 50% fibre loading
DMA was executed according to ASTM D4065-01 to determine
[29,33,34].
the viscoelastic behaviour of DPF/epoxy and pure epoxy com-
posites as a function of temperature through TA Instruments
4.2. Thermal properties
Q800 DMA, operating at an oscillation frequency of 1 Hz and
temperature ranging from 30 ◦ C to 150 ◦ C with a heating rate
Comparative TGA analysis of DPF/epoxy composites and pure
of 5 ◦ C/min.
epoxy composites sample was carried out in a programmed
temperature range of 30–700 ◦ C are displayed in Fig. 2.
4. Results and discussion Incorporation of DPF into the epoxy matrix increased the
thermal stability, as evidenced by the TGA analysis in Fig. 2.
4.1. Flexural properties In the case of DPF/epoxy composites, the first weight loss
between 60 and 100 ◦ C corresponds to vaporization of water
Effect of loading DPF (40%, 50% and 60%) on the flexural molecules or moisture content as also observed in the case of
strength and modulus on the epoxy composites are presented natural fibre polymer composites [35,36]. Researchers revealed
in Fig. 1. that the presence of water molecule in the wall structure or
From Fig. 1, the flexural strength and modulus of pure void space and the water absorption at the interfacial bonding
epoxy composites are 26.15 MPa and 2.26 GPa, respectively. fibre–matrix [37] are ascribed for minimizing the mechanical
However, the addition of DPF increases consecutive both flex- strength of natural fibre composites [38].
ural strength and modulus of epoxy composites up to 50% From the Fig. 2 it is evident that pure epoxy composites
fibre loading, but beyond this loading a remarkable decre- shows relatively less weight loss at 100 ◦ C temperature, indi-
ment are observed. The flexural strength and modulus at cating the presence of less water molecules. Moreover, TGA
40% DPF loading are 28.6 MPa and 2.3 GPa, respectively, but results of pure epoxy composites and DPF/epoxy composites
at 50% DPF loading both flexural strength and modulus of are summarized in Table 4. It is evidently observed that there

Please cite this article in press as: Gheith MH, et al. Flexural, thermal and dynamic mechanical properties of date palm fibres reinforced epoxy
composites. J Mater Res Technol. 2018. https://doi.org/10.1016/j.jmrt.2018.06.013
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40% DPF/epoxy 60% DPF/epoxy


110 60% DPF/epoxy 27 40% DPF/epoxy
100 50% DPF/epoxy 24
50% DPF/epoxy
Pure epoxy Pure epoxy
90
21
80
Weight loss (%)

70 18

DTG (%/C)
60 15
50
12
40
30 9

20 6
10
3
0
0
-10
0 100 200 300 400 500 600 700
0 100 200 300 400 500 600 700
Temperature (ºC) Temperature (ºC)

Fig. 2 – TGA plot of epoxy and DPF/epoxy composites. Fig. 3 – DTG curve of epoxy and DPF/epoxy composites.

is weight loss in all types of composites, which typically occurs matrix with the maximum rate of degradation at 19%/min.
in most of the lignocellulosic fibre and its composites [39–42]. DPF/epoxy composites exhibited two peaks; the height of the
Pure epoxy composites showed 65.11% weight loss at first peak was lowest, which indicates the presence of water
305.02 ◦ C and the final remaining residue was 9.58%. The molecules in the hemicelluloses of DPF/epoxy composites or
degradation mechanism of an epoxy matrix can be explained the existence of voids that developed during the fabrication
on account of a two-step mechanism, starting with dehydra- of the composites. The heights of the second peak of the
tion followed by chain scission step [43,44]. 40% DPF loading DPF/epoxy are higher indicating that all DPF/epoxy compos-
composites showed weight loss of 70.99% at the temperature ites decomposed at a relatively higher temperature compared
of 299.72 ◦ C and final residue was 12.51%, quite more in com- to pure epoxy, however, 50% DPF/epoxy decomposed at rel-
pared to pure epoxy (9.58%), might be due to lignin content atively higher temperature among all. Moreover, Fig. 3 also
of DPF. 50% DPF/epoxy composites showed the highest ther- revealed that derivative weight loss of epoxy composites was
mal degradation temperature (316.9 ◦ C) and higher residual relatively higher with respect to all DPF/epoxy composites,
content (19.8%) or lower weight loss among all DPF loadings. while 50% DPF/epoxy displayed the minimal derivative weight
But beyond 50% loading, the 60% DPF/epoxy composites also loss. The observed result are also in agreement with other
confers higher thermal degradation temperature and resid- researches, where DPF and flax fibres are reinforced at total
ual content (15.2%), but relatively less in comparison to 50% 50% loading in biodegradable starch-based composites [45].
DPF/epoxy composites. Thus, it is evident that on exposure
to higher temperature all DPF/epoxy composites undergoes 4.3. Dynamic mechanical properties
weight loss due to the thermal decomposition of hemicel-
lulose, lignin, pectin and the glycosidic linkages of cellulose 4.3.1. Storage modulus (E )
of natural fibres [31]. However, 50% DPF/epoxy composites The E vs. temperature were plotted to extract important infor-
results better thermal stability, as the char content or the mation about stiffness, fibre/matrix interfacial bonding and
residual content at relatively higher temperature (∼700 ◦ C) is degree of cross linking of materials [46]. E contributes to elab-
more in compared to other composites, and the higher residue orate elasticity of composite components and has three region
content also improve the flame resistance behaviour under namely glassy region, transition region and rubbery region
investigation [43]. [47]. Fig. 4 display the effect of different DPF loading (40%, 50%
Derivative thermogravimetric (DTG) analysis of pure epoxy and 60% by wt.) on E of epoxy composites.
and DPF/epoxy composites were also carried out to investigate Research study declares that in the glassy region, com-
derivative mass loss are shown in Fig. 3. posite components are in highly compact and frozen stage
Fig. 3 shows the decomposition temperature of each com- resulting high E value [48]. Beyond glass transition region,
ponent of composites correlated with peak of DTG curves. E of all composites decreases considerably due to increase
There was only one peak located in the neat epoxy at 330 ◦ C in mobility of polymer chain above Tg temperature [49] and
in the DTG curve, which showed stages of degradation in the defined the rubbery region. From the Fig. 4, it is also evident

Table 4 – Degradation temperature and residual content of composites obtained from TGA.
Composite samples Degradation temperature (◦ C) and weight loss (%) Final residue (%)


( C) (%)

Pure epoxy composites 305.02 65.11 9.58


40% DPF/epoxy 299.72 70.99 12.51
50% DPF/epoxy 316.9 75.54 19.8
60% DPF/epoxy 281.58 74.21 15.2

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40% DPF/epoxy 60% DPF/epoxy


60% DPF/epoxy 40% DPF/epoxy
50% DPF/epoxy 0.8
50% DPF/epoxy
2000 Pure epoxy Pure epoxy
Storage Modulus (MPa)

0.7
1600
0.6

Tan Delta
1200 0.5

0.4
800 0.3
0.2
400
0.1
0 0.0
20 40 60 80 100 120 140 160 20 40 60 80 100 120 140 160

Temperature (ºC) Temperature (ºC)

Fig. 4 – Storage modulus of epoxy and DPF/epoxy Fig. 6 – Damping factor of epoxy and DPF/epoxy
composites. composites.

that incorporation of DPF in epoxy composites improves the movement of the polymer chains. From Fig. 5, it is clearly evi-
E of pure epoxy composites, however, it marginal increment dent that the pure epoxy display narrow peak in the range
in 40% DPF loading in the glassy region indicating that fibre of temperature 70–80 ◦ C. However, the addition of DPF in the
loading did not confers much effect in the molecular mobil- epoxy matrix improved the loss modulus peak height of epoxy
ity of the polymer chains above Tg [50]. Furthermore, E of composites, since the ranges of peak express the diversity of
epoxy composites get improved after the addition of fibres chain segment of polymer three-dimensionally [53]. Broad-
up to 50% representing the higher stiffness and perfect distri- ening the curve of the polymer matrix after the addition of
bution of DPF within epoxy matrix of developed composites. DPF indicated that fibre played an important role above Tg.
But further increment of DPF content beyond 50% showed The broadening in E is due to enhancement in chain seg-
noticeable reduction in modulus chiefly ascribed due to weak ment as well as more free volume with the addition of natural
fibre/matrix adhesion, unevenly dispersion and agglomera- fibres [54]. Interestingly, the difference in E of 40% and 60%
tion of DPF within epoxy matrix which might reduce the DPF/epoxy composites are marginal, however, 50% DPF load-
reinforcing effect of fibre as filler in composites [51]. Recently ing shows improved E may be due to better adhesion of matrix
research study reported that the thermal properties of pineap- with fibres. The highest E peak height of 50% DPF/epoxy also
ple leaf fibre and kenaf fibre of total 50% fibres loading in indicates the possibilities of its higher mechanical properties
phenolic composites also exhibits highest E [52]. compared to epoxy composites and among all DPF/epoxy com-
posites. Similar arguments and observations are observed in
4.3.2. Loss modulus (E ) the case of kenaf hybrid composites [55].
The loss modulus curve is the measure of energy dissipated as
heat per cycle under deformation experienced in a viscoelastic 4.3.3. Damping factor
material [47]. Fig. 5 presents the effect of different DPF fibre Fig. 6 illustrates the damping factor of the pure epoxy and
(40%, 50% and 60% by wt.) loading on loss modulus of epoxy different loading (40%, 50% and 60% by wt.) of DPF/epoxy com-
composites. posites plotted vs. temperature. It is evidently clear that the
Fig. 5 clearly shows that E plot follows somehow the same incorporation of DPF at all loadings influenced the damping
trend as E verses temperature, showing improvements by the factor of epoxy composites.
incorporation of DPF. Furthermore, all E curves reach a max- It was also observed that, damping factor reaches maxi-
imum values for maximum dissipation of mechanical energy mum in a transition region and then reduced dramatically
and decreases for higher temperatures, as a result of the free in a rubbery region. This phenomenon represent the initial
frozen stage before Tg and then mobility of small groups of
Pure epoxy materials/or molecules within polymer structure after glass
40% DPF/epoxy
240 60% DPF/epoxy transition region [46]. Moreover, epoxy composites showed
50% DPF/epoxy
higher peak value of damping factor indicating higher degree
200
Loss Modulus (MPa)

of molecular mobility [56] compared to the rest DPF/epoxy


160 composites. But the addition of DPF in epoxy substantially
120 decreases the viscoelastic damping factor as because epoxy
resin is known as bad thermal resistance and higher ther-
80
mal resistant polymers used to have minimum degree of
40 molecular mobility [57,58]. Remarkably 50% DPF reinforced
0 epoxy composites shows lower damping factor while 40%
20 40 60 80 100 120 140 160
DPF/epoxy composites convey highest among the rest DPF
reinforced epoxy composites. Moreover, peak of dynamic
Temperature (ºC)
damping of epoxy composites also get broader due to incorpo-
Fig. 5 – Loss modulus of epoxy and DPF/epoxy composites. ration of DPF indicating the higher crosslinking density in all

Please cite this article in press as: Gheith MH, et al. Flexural, thermal and dynamic mechanical properties of date palm fibres reinforced epoxy
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60% DPF/epoxy on the basis of better dispersion, wetting of fibres and inter-
40% DPF/epoxy
240
50% DPF/epoxy facial bonding between DPF and epoxy matrix. TGA and DTG
Pure epoxy
analysis also exposed that 50% DPF loading improved the ther-
Loss Modulus (MPa)

200
mal stability and residual content, explained on account of
160 better compatibility and adhesion in which polymer acts as
120 a barrier to prevent the degradation of fibres. Furthermore,
80
remarkable improvement in E and E for 50% DPF loading,
whereas noticeable reductions beyond 50% in these dynamic
40
properties are observed. Besides this incorporation of DPF also
0
results considerable reduction in mobility hence reduces the
0 200 400 600 800 1000 1200 1400 1600 1800
damping factor of all DPF/epoxy composites relative to pure
Storage Modulus (MPa)
epoxy composites.
Fig. 7 – Cole–Cole plot of epoxy and DPF/epoxy composites. The success of this work probably minimize huge date
palm wastes deposition and could provide an attempt to lower
the existing use of synthetic fibres in polymer composite
DPF/epoxy composites [55]. A wider peak of dynamic damp- industries for advanced engineering applications such as in
ing are observed for 50% DPF/epoxy, revealing the existence automotive, paper making and outdoor applications.
of more time for relaxation of molecules due to lower poly-
meric chains movement due to better interfacial interaction.
Conflicts of interest
Researcher reported in the literature that in case of fibres rein-
forced polymer composites, the damping peak height appear
The authors declare no conflicts of interest.
due to fibre’s internal energy dissipation between fibre/matrix
inter-phase [59].
Acknowledgments
4.4. Cole–Cole plot
This work is funded by Deanship of Scientific Research, King
Cole–Cole also referred as Wicket plot is the highly valuable Khalid University, Abha, The Kingdom of Saudi Arabia, Project
method to interpret the relationship between E and E [47]. No. (499) and the authors express their gratitude to King Khalid
Homogenous curves indicated by smooth, semicircular arc, University for supporting this research work.
while imperfect or irregular shape signifies the heterogeneity
in the polymeric system [41]. Fig. 7 displayed the Cole–Cole plot references
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Please cite this article in press as: Gheith MH, et al. Flexural, thermal and dynamic mechanical properties of date palm fibres reinforced epoxy
composites. J Mater Res Technol. 2018. https://doi.org/10.1016/j.jmrt.2018.06.013