2. THEORETICAL FOUNDATIONS OF CHEMICAL ENGINEERING Vol. 53 No. 3 2019
INFLUENCE OF DIFFERENT SUGAR PALM FIBER CONTENT 455
modified composites have been found to be thermally
more stable than raw fiber reinforced composites [16].
The sugar palm fiber (SPF) reinforced with plasticized
sugar palm starch biocomposites was studied by Sha-
hari et al. A good adhesion was observed under scan-
ning electron microscopy due to homogeneous distri-
bution of fibers and polymer, which ultimately enhanced
the mechanical properties of biocomposites [17].
Arenga Pinnata is a local largely available natural
source of SPF in Indonesia, Philippines and Malay-
sia, which is potentially best for polymer compositions
in numerous applications [18]. SPF exhibits interest-
ing and unique characteristics, which are friendly in
processing with lightweight, high specific modulus,
and nontoxic with CO2 absorption during the develop-
ment [19]. SPF has limited applications in polymer
composites, except in some polyurethanes [20, 21],
epoxies [22] and high impact polystyrene [23] com-
posites. However, SPF reinforcement in thermoplastic
polyurethane composite with different fiber loading
has not been presented earlier.
The aim of this study is to observe the effect of
TPU/SPF (250 μm size) at different fiber contents
(90–10, 80–20, and 70–30 wt % TPU/SPF) on the
mechanical and physicochemical properties of
TPU/SPF composites. Surface characterization was
also used. The FTIR, SEM, and XRD were studied to
observe the effect of fiber content on the TPU matrix.
MATERIALS
Polyether-type thermoplastic polyurethane was
received from Bayer Co. (Malaysia) Sdn Bhd, Petaling
Jaya,Selangor,Malaysia.Sugarpalmfibers(ArengaPin-
nata) were harvested locally from Raub in Malaysia.
EXPERIMENTAL SETUP
Sugar Palm Fiber Preparation
The SPF fiber was dried for 14 days at 35°C after
washed, and cut to size between 1–2 cm manually by
special cutter, further crushed by grinder machine
(model Retsch ZM 200). Subsequently, pulverized
fiber was sieved by using an auto shaker FRITSCH
Analysts 3 to sieve into size 250 μm. The 250 μm SPF
size was selected as an optimum size from previous
work [21].
Preparation of TPU/SPF Composites
Various weight of TPU base composites and vari-
ous SPF (10, 20 and 30 wt %) were compound by using
extruded method and the compressing molding.
Thermo SCIENTIFIC EUROLAB 16 was used to
extrude all the composites with temperature and speed
set up at 190°C and 40 rpm, respectively [21]. LOTUS
SCIENTIFIC 25-ton compression molding was used
to press the composite pellets for 10 minutes at 190°C.
Before fully press, a preheating process was performed
for the specimen before reaching up to 190°C. The
final product was cooled down to 50°C.
Mechanical Properties Testing
Based on ASTM standards, various mechanical
properties were performed for the preparative compo-
sition system in tensile, three-point bending flexural,
and notched impact tests. The tensile and flexural
properties were established by using INSTRON uni-
versal testing (model 3369) machine. All the speci-
mens (tensile, flexural, and impact) were cut by using
special mechanical cutter according to ASTM D638,
D790, and D256, respectively [24–26]. A crosshead
speed for tensile test was 5 mm/min to test 5 specimens
for each type of new composites. While, the flexural
properties were tested according to ASTM D790, with
crosshead speed being set at 2 mm/min [25].
A ZWICK-Roell 5113 pendulum impact tester
machine was used to measure the notched impact
strength for 5 impact specimens based on ASTM
D256 [26]. The absorbed impact energy recorded was
divided by the cross-section area of specimens to cal-
culate the impact strength (kJ/m2
). All the mean val-
ues (μ), standard deviation (σ), and standard error for
the experimental results are presented in Table 1. The
following equation was used to calculate the standard
deviation (σ) for all the Y values:
Here, σ is the standard deviation, μ is the mean values
for every Y individually, xi are the individual values of
tensile, flexural, and impact properties, and N is the
number of experiments repeated (depended on the
ASTM), which was 5.
All the modulus details of the samples are given in
Table 2.
Morphological and Chemical Analysis
Fourier transform infrared spectroscopy (FTIR),
scanning electron microscopy (SEM), and X-ray dif-
fraction (XRD) were employed for chemical and phys-
ical examination of the prepared samples to study the
morphology of TPU/SPF composites.
RESULTS AND DISCUSSION
Effect of Fiber Loading on Tensile Properties
of TPU/SPF Composites
The effect of the fiber content on the tensile
strength of SPF/TPU composition is illustrated in
Fig. 1. Pure TPU exhibited a tensile strength of
11 MPa. A lot of discrepancies existed ranging from
(10–30 wt %) fiber loading. It was observed that the
=
σ = − μ
2
1
1 ( ) .
N
i
i
x
N
4. THEORETICAL FOUNDATIONS OF CHEMICAL ENGINEERING Vol. 53 No. 3 2019
INFLUENCE OF DIFFERENT SUGAR PALM FIBER CONTENT 457
smaller fiber loading (10 wt %) shows the highest tensile
strength (~14 MPa). Higher tensile strength is imputed
to an enhanced SPF/TPU interfacial bonding, where
the fibers work as a carrier of load in a polymer matrix,
which is consistent with previous work [15, 27]. How-
ever, 20 and 30 wt % SPF loadings have shown low
strength of 10.21 and 9.89 MPa, respectively. The
lower tensile is a result of inadequate existence of the
TPU matrix, which resulted in a higher surface area of
fiber in the matrix; this ultimately leads to fiber
agglomeration and blocked the stress transfer, as evi-
dent by previous studies [28, 29].
Figure 2 illustrates the effect of fiber loading on the
tensile modulus of TPU/SPF composite. The modulus
of 30 wt % SPF loading was calculated ∼95.28 MPa,
which is the highest value recorded in this work. The
pure TPU, 10 and 20 wt % fiber loadings exhibited val-
ues of 10, 23.34, and 51.11 MPa, respectively. In other
words, the increase in fiber loading will mount in the
tensile modulus values [30]. The composites which
involve high stiffness fillers (such as SPF) in a lowstiff-
ness (TPU) matrix lead to a higher stiffness composites
by increasing the fibers loadings, as mentioned by many
previous studies [14, 15].
Figure 3 shows the effect of different fiber loadings
on the tensile strain values of pure TPU and
TPU/SPF composites. It was observed that the strain
value decreased with the increasing percentage of fiber
loadings. Pure TPU, 10, 20, and 30 wt % TPU/SPF
composites showed a decreasing pattern of strain val-
ues (67.27, 39.89, 23.43, and 12.9%, respectively).
These results are appropriate for a fact that sugar palm
fiber strain at failure is 19.6% [31], which eventually
lowers the strain values in the composites with
increasing fiber loadings [22, 32].
Table 2. Clarification of the kinds of definition for all the moduli
Mechanical
Properties
Specimen properties,
mm
ASTM Strength, MPa Modulus, MPa Strain, %
Tensile Length 33 D638
Maximum tensile stress
Young’s tensile stress
0.02–0.1 mm/mm
Tensile strain
(extension) at break
(standard)
Width 6
Thickness 3
Flexural Length 130
D790
Flexure stress at maxi-
mum flexure load
Modulus (automatic) –
Width 13
Thickness 3
Impact Length 65
D256
Impactstrengthcalculated
from the impact energy
– –
Width 13
Thickness 3
Fig. 1. Effect of fiber loading on tensile strength of
TPU/SPF composites.
16
14
12
2
0
30
20
10
0
Tensile
strength,
MPa
Fiber loading, %
10
8
6
4
TPU/SPF
TPU/SPF
TPU
TPU/SPF
Fig. 2. Effect of fiber loading on tensile modulus of
TPU/SPF composites.
120
100
20
0
30
20
10
0
Tensile
modulus,
MPa
Fiber loading, %
80
60
40
TPU/SPF
TPU/SPF
TPU
TPU/SPF
5. 458
THEORETICAL FOUNDATIONS OF CHEMICAL ENGINEERING Vol. 53 No. 3 2019
MOHAMMED et al.
Effect of SPF Loading on the Flexural Properties
of TPU/SPF Composites
The effect of fiber loading on the flexural strength
and flexural modulus of TPU/SPF composite is
shown in Figs. 4 and 5, respectively. The values of the
flexural strength and modulus for all the samples; pure
TPU, 10, 20, and 30 wt % were recorded as (4.31,
36.11 MPa), (1.14, 23.93 MPa), (2.5, 49.87 MPa),
(4.4, 97.6 MPa), respectively. An increasing trend of
flexural strength and modulus was observed with
increasing fiber loadings [15], the increment indicates
a goodinterfacialbondingoftheSPFinTPUcomposite.
Moreover, there are two types of stresses occurring at the
two sides of a flexible sample, parallel with shear stress at
the axisymmetric matrix plane [28, 33, 34].
Effect of SPF Loading on the Impact Strength
of TPU/SPF Composites
The effect of fiber loading on the impact strength of
SPF/TPU composites is presented in Fig. 6. The impact
strengthshowedanincreasingtrendfrom92.93kJ/m2
for
pure TPU matrix, 100.2 kJ/m2
at 10 wt %, and
113.55 kJ/m2
at 20 wt % fiber loading, before decreasing
to 41.73 kJ/m2
at 30 wt % fiber loading in TPU/SPF
composites [35]. This might be due to lack of energy
absorbance in the thermoplastics when combined with
short natural fibers causing a decrease in the impact
strength [36].
Fourier Transform Infrared (FTIR) Spectroscopy
Figure 7 shows the FTIR spectra of TPU and dif-
ferent SPF loading reinforced TPU system, where the
three sets of TPU/SPF (10, 20, and 30 wt %) showed
similar behavior with identical peaks of pure TPU
[37]. The 10 wt % SPF loading showed much lower
transmittance than 20 and 30 wt % samples, which
attributes to a high value of adherence on the polymer
surface. The H+
bonding between TPU and SPF in
TPU/SPF composites in different fiber loading causes
a minimal increase in the transmittance frequency of
C=O group, as tabulated in Table 3. The TPU poly-
mer without additive C=O absorbs at 1701.12 cm–1
,
while TPU/SPF of 10, 20, and 30 wt % showed
1701.43, 1701.45, and 1702.05 cm–1
, respectively.
There is a physical interaction between the SPF and
the TPU polymer by the hydrogen H+
bonding which
resulted in the low transmittance C=O peaks, as vali-
dated by a previous study [11].
Fig. 3. Effect of fiber loading on tensile strain of TPU/SPF
composites.
75
60
0
30
20
10
0
Tensile
strain,
%
Fiber loading, %
45
30
15
TPU/SPF
TPU/SPF
TPU
TPU/SPF
Fig. 4. Effect of fiber loading on flexural strength of
TPU/SPF composites.
5
4
1
0
30
20
10
0
Flexural
strength,
MPa
Fiber loading, %
3
2
TPU/SPF
TPU/SPF
TPU TPU/SPF
Fig. 5. Effect of fiber loading on flexural modulus of
TPU/SPF composites.
40
10
0
30
20
10
0
Flexural
modulus,
MPa
Fiber loading, %
30
20
TPU/SPF
TPU/SPF
TPU
TPU/SPF
100
90
80
70
60
50
110
6. THEORETICAL FOUNDATIONS OF CHEMICAL ENGINEERING Vol. 53 No. 3 2019
INFLUENCE OF DIFFERENT SUGAR PALM FIBER CONTENT 459
Scanning Electron Microscope (SEM) Study
The fracture surface detected a combination of
SPF breakage and fiber pull-out of all TPU/SPF com-
posites, respectively, except the glassy surface for pure
TPU (Fig. 8), which indicates that fiber-matrix adhe-
sion is moderately good. Figure 8a shows a smooth
glassy fractured surface in different places of the
orderly TPU matrix. Figures 8b–8d show poor fiber
matrix adhesion, as there are gaps between fibers and
matrix with fiber pull-outs and cracks in TPU matrix.
SEM morphology study demonstrates that fiber load-
ing at 80–20% TPU/SPF and 70–30% TPU/SPF
have a negative effect on the fiber-matrix adhesion,
which results in low mechanical properties. However,
the fiber loading 90–10% TPU/SPF exhibited a best
overlap and match withtheTPUmatrix. SEMfurnishes
an evidence that the fiber loading played an extensive
voids effect around the fibers in 10 wt % loading sample
with an increased interfacial adhesion, which results in
a uniform surface [11, 15].
X-Ray Diffraction (XRD) Study
XRD analysis is used to investigate the various
loadings (10, 20, 30 wt %) of short SPF (250 µm) rein-
forced TPU composites, and the diffractograms of the
samples are presented in Fig. 9.
It is seen that there is no diffraction peak observed
for TPU composites. The absence of the diffraction
peak in the case of reinforced composites is due to the
complete exfoliation of the SPF fiber into the TPU
network structure. The observance of peak at 2θ =
∼21° shows the amorphous nature, and the uniform
level dispersion of SPF simultaneously confirms the
efficient and effective compatibility between the SPF
and the TPU matrix. The 30 wt % fiber loading
showed the minimum intensity due to larger amount
of fiber loading. SPF dispersion is homogenously
observed in the form of individual layers within the
polymer matrix and leads to form exfoliated compos-
ites which attribute to the improvement of properties
of the resulting composites [21, 37].
Fig. 6. Effect of fiber loading on impact strength of
TPU/SPF composites.
40
0
30
20
10
0
Impact
strength,
kJ/m
2
Fiber loading, %
20
TPU/SPF
TPU/SPF
TPU
TPU/SPF
100
80
60
120
Fig. 7. FTIR analysis for different SPF loading in TPU/SPF composites.
30% TPU/SPF
20% TPU/SPF
10% TPU/SPF
TPU
300
150
100
50
0
500
2500
4000
Transmittance
(a.u.),
%
2, deg
250
200
2000
3500 3000 1000
1500
7. 460
THEORETICAL FOUNDATIONS OF CHEMICAL ENGINEERING Vol. 53 No. 3 2019
MOHAMMED et al.
CONCLUSIONS
In this study, the flexural, impact, tensile, and
physicochemical properties of new TPU/SPF com-
posites have been investigated. The results are as fol-
lows:
• The economical production of new TPU com-
posites with SPF, a naturally available fibre (natural
resource), has been successfully achieved (presented
in previous paper).
• The flexural properties witnessed an increasing
trend as the fiber loading was increased. However, the
flexural properties for the TPU are still the highest.
• The impact strength reaches the peak at the
medium fiber loading, and it decreased rapidly with
increase in the fiber loading to 30 wt %.
• The optimum fiber loading of SPF in TPU com-
posite to obtain the maximum tensile strength and
strain was found to be 10 wt %. However, there was no
significant effect of adding more than 10 wt % to the
Table 3. Main FTIR bands of pure TPU, 10, 20, and 30 wt % TPU/SPF composites
Peak location,
cm–1
Chemical
structure
Motion
Pure
TPU
10% TPU/SPF 20% TPU/SPF 30% TPU/SPF
3.420–3.200 N–H Stretching 3326.22 3326.07 3329.76 3328.72
1.590–1.650 N–H Bending 1596.29 1596. 31 1596.34 1596.14
3.000–2.800 CH2 and CH3 Stretching 2956.55 2956.46 2955.90 2955.99
1.740 C=O Non-bonded urethane
Stretching
1726.92 1726.65 1727.19 1726.66
1.690 C=O Associate urethane 1701.12 1701.43 1701.45 1702.05
1.550–1.510 H–N–CO Combined motion 1529.27 1529.22 1528.94 1528.53
Fig. 8. The SEM for (a) pure TPU, (b) 10, (c) 20, and (d) 30 wt % fiber reinforced TPU composites.
20 μm 20 μm
20 μm 20 μm
(a) (b)
(c) (d)
Pull out fiber
Pull out fiber Pull out fiber
SPF
SPF SPF
Void
Void
Void
8. THEORETICAL FOUNDATIONS OF CHEMICAL ENGINEERING Vol. 53 No. 3 2019
INFLUENCE OF DIFFERENT SUGAR PALM FIBER CONTENT 461
TPU matrix on the tensile strength and strain proper-
ties of new composites. Meanwhile, there was a dra-
matic rise in the modulus for all the composites, with
increasing fiber loading (maximum at 30 wt %), which
was later confirmed by physicochemical studies.
• The SEM showed the 10 wt % fiber loading with
less void and higher fiber intersection with the matrix
as compared to the other fiber loadings.
• FTIR analysis of TPU/SPF composites with dif-
ferent fiber loadings verified the presence of hydrogen
bonding combination between TPU and SPF.
• Therefore, it is concluded that SPF needs chem-
ical or physical treatment to enhance the physico-
chemical properties of TPU/SPF composites.
FUNDING
This work is supported financially by the Ministry
of Higher Education (MOHE) Malaysia and the Uni-
versity Malaysia Pahang (UMP) through the Funda-
mental Research Grant Scheme RDU-130138. More-
over, the authors are thankful to University of Tech-
nology, Baghdad, Iraq, for all supports.
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