International Journal of Biological Macromolecules 101 (2017) 75–83

Contents lists available at ScienceDirect

International Journal of Biological Macromolecules

journal homepage: www.elsevier.com/locate/ijbiomac

Cassava/sugar palm fiber reinforced cassava starch hybrid

composites: Physical, thermal and structural properties
Ahmed Edhirej a,b , S.M. Sapuan a,c,∗ , Mohammad Jawaid c,d , Nur Ismarrubie Zahari a
a
Department of Mechanical and Manufacturing Engineering, University Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia
b
Department of Chemical and Material Engineering, Sabha University, Libya
c
Laboratory of Biocomposites Technology, Institute of Tropical Forestry and Forest Products, University Putra Malaysia, 43400 UPM Serdang, Selangor,
Malaysia
d
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: A hybrid composite was prepared from cassava bagasse (CB) and sugar palm fiber (SPF) using casting
Received 22 September 2016 technique with cassava starch (CS) as matrix and fructose as a plasticizer. Different loadings of SPF (2,
Received in revised form 24 February 2017 4, 6 and 8% w/w of dry starch) were added to the CS/CB composite film containing 6% CB. The addition
Accepted 8 March 2017
of SPF significantly influenced the physical properties. It increased the thickness while decreasing the
Available online 10 March 2017
density, water content, water solubility and water absorption. However, no significant effect was noticed
on the thermal properties of the hybrid composite film. The incorporation of SPF increased the relative
Keywords:
crystallinity up to 47%, compared to 32% of the CS film. SEM micrographs indicated that the filler was
Cassava film
Hybrid composite
incorporated in the matrix. The film with a higher concentration of SPF (CS-CB/SPF8) showed a more
Cassava bagasse heterogeneous surface. It could be concluded that the incorporation of SPF led to changes in cassava
Sugar palm fiber starch film properties, potentially affecting the film performances.
Physical properties © 2017 Elsevier B.V. All rights reserved.
Thermal properties

1. Introduction
In recent years, the use of natural fibers as reinforcing mate-
rials in polymers and composites has attracted much attention.
The depletion of petroleum resources and the awareness of global
environmental problems triggered the search for new green and
environment-friendly alternatives [1]. New bio-products derived
from renewable plants and agricultural residues, have various
advantages, such as low cost, low density, less tool wear, availabil-
ity, biodegradability and eco-efficiency. Bio-based products enjoys
wide applicability in construction, automotive, furniture and pack-
aging industries, which are currently dominated by products based
on petroleum feedstock. Therefore, natural fiber is now becom-
ing a new alternative material that can replace petroleum-based
products either alone or combined with other materials to pro-
duce green composites. The advantages of natural fibers, such as
low cost, low density, availability, sustainability, recyclability and
biodegradability, make them an interesting research area and con-
siderable efforts are being made to tap their full potential [2,3].
∗ Corresponding author at: Department of Mechanical and Manufacturing Engi-
neering, University Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia.
E-mail address: sapuan@upm.edu.my (S.M. Sapuan).
Cassava is ranked the fifth most widely produced starch crop
in the world, and the third among the food sources consumed in
tropical regions. The value of harvested cassava can be enhanced
by processing cassava to produce cassava starch (CS), thus con-
tributing to the development of rural economies. Among natural
polymers, starch has been considered as one of the most promis-
ing environmentally friendly materials due to its low cost, easy
availability and biodegradability. One of the major by-products
of cassava starch is pulp or bagasse. Cassava bagasse (CB) con-
tains 50–60% residual starch (dry weight basis) [4,5]. Biodegradable
composite films have been developed from cassava starch/bagasse
by casting and dehydration method, using 30% w/w fructose as
plasticizer. The results indicated that the addition of 6% bagasse
constituted the most efficient reinforcing agent, leading to remark-
able physical and mechanical properties of the final product.
Although this bio-composite exhibit acceptable properties but still
has poor water resistance. In order to overcome this problem,
hybridization the CB with lower hydrophilic natural fiber, the natu-
ral fiber that known for their high durability and resistance to water
is sugar palm fiber.
Sugar palm fibers (SPF) are known for their high durability and
resistance to sea water, which are their major advantages. Tra-
ditionally, sugar palm fibers were used to make ropes for ship
cordages, which were proven to have good properties in sea water.

http://dx.doi.org/10.1016/j.ijbiomac.2017.03.045
0141-8130/© 2017 Elsevier B.V. All rights reserved.
76 A. Edhirej et al. / International Journal of Biological Macromolecules 101 (2017) 75–83
The preparation of such fibers is effortless as it does not require any
secondary processes, such as water retting or mechanical decorti-
cating to yield the fiber [3,6–8]. In the field of material engineering,
SPF has been used as reinforcement in polymer matrix composites.
Several studies have shown that sugar palm fibers have great poten-
tial to be used in many composite applications like other natural
fibers such as kenaf, jute, oil palm, sugarcane bagasse, pineapple
leaf and banana pseudo-stem fibers [9–11]. SPF is known to possess
water resistance; therefore, the hybridization of SPF with cassava
bagasse (CB) seems to be a good combination to improve the prop-
erties of the material. The incorporation of two or more different
types of fibers into a single matrix is referred to as hybrid com-
posites. The behavior of hybrid composites is a weighed sum of
the individual components, in which there is a more favorable bal-
ance between the inherent advantages and disadvantages. Also, in
a hybrid composite that contains two or more types of fiber, the
advantages of one type of fiber could complement what is lacking
in the other. Consequently, a balance in cost and performance could
be achieved through proper material design [12]. The properties of
a hybrid composite mainly depend upon the fiber content of indi-
vidual fibers, their orientation, extent of fiber intermingling, fiber
to matrix bonding and arrangement of both types of fibers. The
strength of the hybrid composite is also dependent on the failure
strain of individual fibers. Maximum hybrid results are obtained
when the fibers are highly strain compatible [13]. Recently, the
study of hybrid composites has become an active area in composite
material research, the hybrid effect being considered a critical issue
in dealing with hybrid composites. The hybrid effect can be positive
or negative depending on whether the property in the hybrid com-
posite is greater or smaller than in the non-hybrid composite [14].
However, to the best of our knowledge, there is no information on
the preparation and characterization of cassava bagasse/sugar palm
fiber reinforced cassava starch hybrid composite films using fruc-
tose as plasticizer. The main objective of this work is to investigate
the influence of different sugar palm fiber loadings on the physi-
cal, thermal and structural properties of the hybrid composite. It
should be noted that the fibers used in this study were not chemi-
cally treated or modified, which would lead to the development of
a more environmentally friendly and cheaper production process
and materials. The use of CB and SPF as reinforcement agents for
CS thermoplastic film added value to these waste by-products and
increase the suitability of CS composite films as environmentally
friendly food packaging material.
2. Materials and method
Starch was extracted from native cassava tubers, as described in
a previous work [15]. Cassava bagasse was obtained from the same
extraction process and was used as filler. Sugar palm fiber was col-
lected at Jempol, Negeri Sembilan, Malaysia. Fructose was supplied
by LGC Scientific Sdn. Bhd, Malaysia, and was used as plasticizer.
2.1. Characterization of fibers
2.1.1. Chemical composition
The methods described by (Versino and García, 2014), was used
to investigate Acid Detergent Fiber (ADF), Neutral Detergent Fiber
(NDF) of cassava bagasse and sugar palm fiber. NDF and ADF were
used to determine the Cellulose and Hemicellulose of the fibers.
[16]. The proportions of cellulose and hemicelluloses were calcu-
lated by using Eqs. (1) and (2), respectively.
Cellulose = ADF − lignin
Hemicelluloses = NDF − ADF
2.1.2. Water content (WC)
The weight loss was determined to calculate the Moisture con-
tent of CB and SPF. Powder samples were weighed (W1 ), dried at
105 ◦ C for 24 h, and weighted again (W2 ), WC was calculated as the
percentage of initial powder weight lost during drying and that on
a wet basis as shown in Eq. (3).
W1 − W2
WC (%) = × 100 (3)
W1
2.1.3. Water absorption (WA)
The water absorption of CB and SPF were determined as per the
method explained by Yaich et al. [17]. The samples (3.0 g) were
dissolved in 25 ml of distilled water and placed in pre-weighed
centrifuge tubes. After being kept in the centrifuge for 25 min at
3000 rpm, the dispersions were mixed and were left at room tem-
perature for 1 h. The supernatants were removed and the residue
was dehydrated in an oven for 25 min at 50 ◦ C, to determine the
moisture content of the samples. The water absorption capacity
was denoted as grams of water bound per gram of the sample on a
dry basis using Eq. (4), [17].
Mfinal − Mintial
WA (%) = × 100 (4)
Mintial
2.1.4. Thickness swelling (TS)
To determine the percentage of thickness swelling, the samples
diameter were measured using a digital micrometer (having 0.01
accuracy) before (di ) and after (df ) immersed the fibers in water for
24 h, following the method explined by María et al. (2011) [18]. The
thickness swelling ratio was calculated using the following Eq. (5):
di − df
TS (%) = × 100 (5)
df
2.1.5. X-ray diffraction (XRD)
Rigaku D/max 2500 X-ray powder diffractometer (Rigaku,
Tokyo, Japan) was used to study X-ray diffraction patterns of the
cassava bagasse and sugar palm fiber. The relative crystallinity
index (RC) was calculated according to Eq. (6) proposed in a previ-
ous work Frost et al. [19], based on the amorphous area (Aa) and
crystalline areas (Ac ).
Ac
Rc = (6)
Ac + Aa
2.2. Film preparation and characterization
Starch films were prepared by casting technique, using a film-
forming solution containing 5 g of cassava starch/100 ml distilled
water. Fructose was used as plasticizer, in concentrations of 0.30 g/g
dry starch. Bagasse was used as filler at 6% w/w of dry starch,
the dried fibers were cut and crushed by a Lab grinder and the
particle size of cassava bagasse and sugar palm fibers were deter-
mined using a 50/100 mesh sieve to obtain powder with particle
sizes of 150–300 ␮m. Sugar palm fiber was added in different con-
centrations: 2, 4, 6 and 8% w/w of dry starch and were termed
CS-CB/SPF2, CS-CB/SPF4, CS-CB/SPF6 and CS-CB/SPF8, respectively.
The composition of the films is shown in Table 1. The mixture was
heated to 80 ◦ C in a thermal bath and kept at this temperature for
20 min under constant stirring. The air bubbles that formed during
heating were removed by placing the film-forming solution into a
desiccator under vacuum until there were no more bubbles; then,
the solution was poured homogenously onto 10 cm diameter circle
plates. The plates with the film-forming solution were then dried in
an oven with air circulation, at 45 ◦ C. The dry films were removed
(1) from the plates and stored at ambient conditions (around 25 ◦ C
and 60% relative humidity) in a plastic bag for two weeks before
(2) characterization.
 A. Edhirej et al. / International Journal of Biological Macromolecules 101 (2017) 75–83 77

Table 1
Compositions of TPS matrix based on cassava starch (CS film), its composites with cassava bagasse (CS/CB) and cassava bagasse/sugar palm fiber reinforced cassava starch
hybrid composite (CS-CB/SPF).

Film Fructose g/g dry Starch g/100 ml CB g/100 g of dry SPF g/100 g of dry
starch distilled water starch starch

CS film 0.3 5 0 0
CS/CB 0.3 5 6 0
CS-CB/SPF2 0.3 5 6 2
CS-CB/SPF4 0.3 5 6 4
CS-CB/SPF6 0.3 5 6 6
CS-CB/SPF8 0.3 5 6 8

2.3. Characterization of films Table 2

2.3.1. Physical properties
2.3.1.1. Film thickness. The film thickness was determined accord-
ing to the method of Lu et al. [20], using a digital micrometer
(Mitutoyo Co., Japan). The average of five random measurements
performed for each film was calculated [20].
2.3.1.2. Film density. Film density (␳) was determined on square
film samples (20 × 20 mm). It was calculated based on ASTM D792,
by dividing the film weight (m) by the film volume (v), using Eq.
(7), where the film volume was determined by multiplying the film
area by the thickness [21]. The values considered are the average
of ten determinations.
m
␳= = g/cm3 (7)
v 2.3.3. Structural properties
2.3.1.3. Water content (WC). Film moisture content (WC) was
determined by assessing the weight loss based on ASTM D 644-94
(1994). Film samples were weighed (w1), dried at 105 ◦ C for 24 h,
and then weighed (w2) again. The water content was determined
as a percentage of the initial film weight lost during drying and
reported on a wet basis according to Eq. (8). [22].
W1 − W2
WC (%) = × 100
W1
2.3.1.4. Film solubility in water (WS). The water solubility of the
films was determined in triplicate, following the method of Shojaee
et al. [23]. Film samples were dried at 105 ◦ C for 24 h in a laboratory
oven and then weighed to determine the initial solid content [23].
Pre-weighed film samples (1 cm × 3 cm) were immersed under
constant agitation into 50 ml of distilled water for 6 h at 25 ◦ C. After
that period, the remaining pieces of films were filtered and dried at
105 ◦ C to constant weight (final dry weight). The water solubility
(%) of the films was calculated according to Eq. (9) [24]:
Wi − Wf
WS (%) = × 100
Wi
2.3.1.5. Water absorption (WA). The water absorption test was per-
formed in accordance with ASTM D 570–98. The film samples were
first dried for 24 h at 50 ◦ C, cooled in a desiccator, immediately
weighed and then soaked in distilled water at room temperature.
After a specific immersion period, the samples were removed from
the water, all surface water was gently wiped off with a dry cloth,
and then the samples were weighed again. The differences between
the initial and final weights of the samples were calculated using
Eq. (10) [25].
Waterabsorption(%) = [(Mfinal − Minitial)/Minitial] × 100
2.3.2. Thermal gravimetric analysis (TGA)
Thermal gravimetric analysis was conducted according to the
ASTM E1131 standards, using 10 mm2 of film. The following con-
ditions were provided for the analysis: heating rate of 10 ◦ C min−1 ,
Chemical composition and physical properties of cassava bagasse and sugar palm
fiber.
Chemical Composition and physical properties of Cassava Bagasse and sugar palm fiber
No Content CB SPF
1 Cellulose (%) 10.04 43.87
2 Hemicelluloses (%) 29.26 5.57
3 Water content (%) 14.92 6.01
4 Water Absorption (%) 258.1 123.2
5 Thickness Swelling (%) 48.47 22.13
6 Relative crystallinity (%) 22.5 35.3
temperature range from room temperature to 500 ◦ C, and nitrogen
atmosphere with a flow rate of 25 ml/min [26].
2.3.3.1. Scanning electron microscopy (SEM). Scanning electron
microscopy (SEM) was carried out on a Hitachi S-3400N microscope
(Japan), operating at an acceleration voltage of 20 kV, in the high-
vacuum mode, in order to study the morphology of the fracture
surface of the samples. The surfaces fracture of the hybrid compos-
ite samples were observed using SEM and the SEM micrographs
were taken to investigate the interface adhesion between the fiber
and the matrix of the hybrid composites. For this purpose, the sam-
(8) ples were mounted on bronze stubs, using double-sided tape, and
coated with a gold layer (40–50 nm) [27].
2.3.3.2. Fourier transform infrared spectroscopy (FTIR). An IR spec-
trometer (Bruker Vector 22) was used to record the FTIR spectra, in
the frequency range of 4000–400 cm−1 . The samples were prepared
by the KBr-disk method [28].
2.3.3.3. X-ray diffraction (XRD). X-ray diffraction measurements
were performed, using reflection geometry, on a Rigaku diffrac-
tometer (Tokyo, Japan), operated at a generator voltage of 40 kV,
a current of 40 mA, and goniometer speed of 0.02 (2␪) s−1 . The
relative crystallinity index was calculated according to Eq. (11),
(9)
proposed in a previous work [19], based on the calculus of the
amorphous area (Aa) and crystalline area (Ac).
Ac
Rc = (11)
Ac + Aa
3. Results and discussion
3.1. Chemical composition of fibers
The physical, mechanical, and thermal properties of a natural
fiber are greatly affected by its chemical composition. Natural fibers
(10) mainly constitute of lignin, cellulose and hemicelluloses. Cellulose
serve as the main structural component providing strength to the
walls of the stem plant as well as to the fiber [29]. Table 2 shows
the cellulose and hemicelluloses of CB and SPF. It shows that the CB
contains low concentrations of cellulose but high concentrations of
hemicellulose content as compared to SPF.
78 A. Edhirej et al. / International Journal of Biological Macromolecules 101 (2017) 75–83
8000
7000
6000
Inensity
5000
4000 CB
3000
2000
1000
SPF
0 structural defects [16].
10 15 20 25 30 35 40 45 50 55 60
(2θ)
Fig. 1. X-ray diffractogram of cassava bagasse (CB) and sugar palm fiber (SPF).
3.1.1. Physical properties of fibers
3.1.1.1. Moisture content (MC). The MC of natural fiber is an impor-
tant criterion that needs to be considered in choosing natural
fiber as a reinforcement material. This is because moisture content
affects dimensional stability, electrical resistivity, tensile strength,
porosity, and swelling behavior of natural fiber in a composite
material [30]. The result of the moisture content of fibers indi-
cated that the MC of SPF was lower than CB with 6.01and 14.92%,
respectively.
3.1.1.2. Water absorption (WA) and thickness swelling (TS). The WA
is a critical criterion for several applications of TPS products. The
results of the water absorption test are presented in Table 2 for CB
and SPF. From the result, SPF absorbed a lower amount of water
(123.32%) as compared to the CB (258.05%) which indicates that CB
is highly hydrophilic [31]. CB exhibited higher retention capacity of
water than SPF due to the reduction of cellulose content in the CB,
this result is in agreement with the reported work by [32], these
results are in agreement with their chemical composition Table 2.
The swelling behavior of CB and SPF were investigated using
the swelling ratio. It is known that thickness swelling of mate-
rial stored in humidity chamber is accompanied by the moisture
absorption behavior of the respective material [33]. Table 2 shows
the swelling ratio of the fibers which indicated a similar trend with
the water absorption behavior. The thickness swelling can lead to
reduction in the adhesion between the fibers and matrix [33]. The
chemical composition of fibers are the most important variables
that determine the overall properties of the fibers. Generally, water
absorption and thickness swelling of fibers decreases with increas-
ing cellulose content [34]. The SPF shows highest chemical content
of cellulose (43.87%), which contribute to the higher strength and
thermal stability of the fiber. Table 2 exhibited that the WC, WA and
TS of the CB are higher than SPF, and this is due to the reduction
of cellulose content. The thickness swelling of SPF and CB is (22.13
and 48.47%), respectively. These results agree with the reported by
Sahari et al., they found that there are relationships between the
cellulose content and water absorption behavior [35].
3.1.1.3. X-ray diffraction (XRD). As observed in the X-ray diffrac-
tion patterns (Fig. 1), the cassava bagasse showed semi-crystalline
structure. Bagasse presented peaks at 2␪ = 15.4◦ , 17.5◦ , 18.4◦ and
23.2◦ , and according to Nuwamanya et al. [36], these peaks are
related to cassava starch present in the bagasse. From Fig. 1, it can
be observed that SPF had higher relative crystallinity as compared
to CB. This can be attributed to the higher cellulose content in SPF
as shown in Table 2. Furthermore, the crystallinity indexes of CB
and SPF were found 22.5% and 35.3%, respectively.
3.2. Physical properties of films
3.2.1. Thickness and density of hybrid films
The film thickness increased, while the density decreased upon
fiber addition and showed small variations, as shown in Table 3.
The higher the fiber concentrations in the cassava film, the thicker
the film. The CS film was the thinnest with 0.18 mm. However, the
film with 8% SPF (CS-CB/SPF8) was the thickest with 0.43 mm. The
incorporation of a high filler content resulted in thicker. According
to Versino et al., this could be attributed to the presence of large
filler particles within the polymer matrix, which could promote
The density of the composites decreased with increasing the
filler content; this could be due to the lighter density of the filler
material (1.26 g/cm3 for SPF) [6,9] and (1.45 g/cm3 for CB). The films
with a higher concentration of fiber showed lower densities. In
other words, the density of the hybrid composite film decreased
with increasing the fiber content, as compared to the CS film. Sim-
ilar results were reported by Shakuntala et al., for wood apple
shell reinforced epoxy composite [37], and by Salgado et al., for
foams based on cassava starch, sunflower proteins and cellulose
fibers [38]. In addition, the highest density was recorded for the
CS film with 1.73 g/cm3 and the lowest for the films with 8% SPF
(CS-CB/SPF8) with 1.18 g/cm3 , as indicated in Table 3.
3.2.2. Moisture content and solubility in water
When CB and SPF were incorporated in the CS films, the moisture
content slightly decreased, as shown in Table 3. The film contain-
ing a higher amount of SPF exhibited a lower MC, as compared to
the CS film and to the films with a lower SPF content. The matrix
effectively served as a barrier to the diffusion of water molecules
into the cell wall and cell lumen or at least it reduced the per-
meability of the fiber once the micro-pores were blocked by the
matrix. After bulking the OH groups of sugar palm fiber’s cell wall,
it was observed that the MC of the films containing sugar palm
fibers were significantly lower than those of the film with CS/CB
and of the CS film. This finding is in agreement with the results
of Soykeabkaew et al., who reported a decreasing moisture con-
tent of tapioca starch-based foam reinforced with jute and flax [39]
and of Kaisangsri et al., who investigated the moisture content of
biodegradable foam trays made from cassava starch blended with
natural fiber and chitosan [40]. Water solubility is an important
property of starch-based films. Potential applications may require
water insolubility or water resistance to improve product integrity
[41]. The addition SPF decreases the solubility of the films, and
also alters the interaction between the polymer chains, which may
decrease the dissolution of the polymer. The films were found to be
unable to maintain their integrity when immersed in water. How-
ever, this ability was dependent on the concentration of fiber. For
each film, the solubility decreased with an increase in fiber concen-
tration. The films containing a low fiber loading were more soluble
than those with a high fiber loading, despite the fact that these films
exhibited the highest equilibrium moisture content.
The films reinforced by 6% cassava bagasse (CS/CB) possessed
higher hydrophilicity [42]. The high propensity for water absorp-
tion of the films is due to the existence of hydroxyl groups in the
films. Fig. 2 shows the percentage of water uptake as a function of
time for the TPC starch film (CS film), CS/CB composite film and
CS-CB/SPF hybrid composite film with (2, 4, 6 and 8% SPF). It can be
observed from Fig. 2 that all the films absorbed a high amount of
 A. Edhirej et al. / International Journal of Biological Macromolecules 101 (2017) 75–83 79

Table 3
Physical properties of CS film, CS/CB composite film and CS-CB/SPF hybrid composites films.

No Film Thickness(mm) Density(g/cm3 ) Moisture content (%) Water solubility(%)

1 CS film 0.18 ± 0.07 1.73 ± 0.08 10.96 ± 0.08 33.9 ± 0.06

2 CS/CB 0.27 ± 0.05 1.28 ± 0.07 10.77 ± 0.06 24.47 ± 0.12
3 CS-CB/SPF2 0.33 ± 0.08 1.27 ± 0.03 10.71 ± 0.04 19.08 ± 0.09
4 CS-CB/SPF4 0.37 ± 0.07 1.24 ± 0.02 10.62 ± 0.07 16.76 ± 0.06
5 CS-CB/SPF6 0.40 ± 0.04 1.21 ± 0.06 10.47 ± 0.11 15.53 ± 0.08
6 CS-CB/SPF8 0.43 ± 0.03 1.18 ± 0.05 10.24 ± 0.09 14.37 ± 0.05

350

300
Water Absorption (%)

250 CS film
CS/CB
200 CS-CB/SPF2
CS-CB/SPF4
150 CS-CB/SPF6
CS-CB/SPF8
100

50

0
0 15 30 45 60 75 90 105 120 135 150 165 180 195 210 225 240
Time (min)

Fig. 2. Water absorption of CS film, CS/CB composite film and CB/SPF reinforced CS
hybrid composites films.

water after 30 min of water immersion at room temperature due

to the hydrophilic properties of starch and fiber.
It is well known that dry cassava bagasse immersed in water
is rehydrated like a sponge, more specifically, it absorbs water up
to about 160% of its weight in a short period of time [43]. How-
ever, it can be noted that the water uptake or absorption of the
hybrid composite decreases with an increasing SPF loading. Simi-
lar trends were also found for moisture content results. This could
be attributed to the lower hydrophilicity behavior of SPF, as com-
pared to CS and CB [44]. The CS film absorbed about 108.52%
in 90 min, while the CS/CB film and CS-CB/SPF2, CS-CB/SPF4, CS-
CB/SPF6 and CS-CB/SPF8 absorbed about 280.18, 161.33, 138.15,
102.71 and 92.27%, respectively. The films containing 8% SPF (CS-
CB/SPF8) absorbed a lower amount of water, as compared to the
other films, the maximum water uptake observed was 380.53%
after 240 min for the CS/CB film, and the minimum was 100.87%
for the CS-CB/SPF8 film after 240 min. These results are similar to
those reported by Sahari et al. for sugar palm fiber (SPF) reinforced
plasticized sugar palm starch (SPF/SPS) biocomposites [45].

3.3. Thermal properties of films
3.3.1. Thermal gravimetric analysis (TGA)
Fig. 3 shows the thermal behavior of SPF/CB reinforced CS
hybrid biocomposites. It was found that the fiber loading slightly
decreased the thermal stability of the hybrid composites. The first
mass loss, in the range of 31–100 ◦ C, was due to the evaporation
of moisture. Then, the mass loss between 150 ◦ C and 380 ◦ C for
the hybrid composite films was due to the decomposition of the
three major constituents of natural fibers: hemicelluloses, cellu-
lose and lignin [46]. In general, the thermal decomposition of these
fibers consists of four phases. The first phase is the decomposition
of hemicelluloses, followed by that of cellulose, of lignin and lastly
of their ash [6,47]. Yang et al. reported that hemicelluloses decom-
pose at 220 ◦ C and their decomposition is substantially completed
at 315 ◦ C. As soon as hemicelluloses are completely decomposed,
the decomposition of cellulose will take place as the second phase
of decomposition. Owing to the predominantly crystalline nature
of the cellulose chains, cellulose is relatively thermally stable. It
does not start to decompose until hemicelluloses are completely
decomposed, thus its decomposition normally starts at a higher
Fig. 3. Thermogram (A) TGA curves and (B) DTG curves of CS film (control), CS/CB
composite film (0%) and CB/SPF reinforced CS hybrid composites films.
temperature above 315 ◦ C [48]. This is supported by Reddy and
Yang [29], who reported that the critical decomposition temper-
ature of crystalline cellulose is 320 ◦ C. The third phase represents
the decomposition of lignin. It is the most difficult to decompose,
compared to hemicelluloses and cellulose. Although the decompo-
sition of lignin starts as early as at 160 ◦ C, it decomposes slowly and
its decomposition extends to a high temperature to complete [48].
This is explained by the fact that lignin is a very tough component,
known as giving rigidity to plant materials. Finally, when the lignin
is completely decomposed, the component that is left is inorganic
material, which can be assumed as ash. Inorganic materials, such as
silica (silicon dioxide, SiO2 ), in the fiber, can only be decomposed at
a very high temperature [30]. Fig. 3 (B) shows the maximum DTG
peaks located between 300 and 320 ◦ C. For the hybrid films, the
maximum DTG peak occurs at around 311 ◦ C, while for the CS film,
it occurs at 319.8 ◦ C. However, the DTG peaks decreased upon the
addition of fiber, showing very small variations, according to the
80 A. Edhirej et al. / International Journal of Biological Macromolecules 101 (2017) 75–83
Table 4
Thermal properties (obtained by TGA and DTG analyses) of CS film, CS/CB composite film and CS-CB/SPF hybrid composites films.
Film Degradation Temperature (◦ C)
T10% T30%
CS film 184.2 303.4
CS/CB 178.4 296.9
CS-CB/SPF2 172.8 296.1
CS-CB/SPF4 171.2 295.4
CS-CB/SPF6 171.1 294.1
CS-CB/SPF8 170.8 291.1
results listed in Table 4. These peaks are similar to those reported by
Versino et al., for biocomposites reinforced with cassava peel [28],
and by Ramírez et al., for cassava starch biocomposites reinforced
with green coconut fiber [26]. The last thermal event at 500 ◦ C indi-
cated the mass residue (%), which ranged from 25.1 for the CS film to
26.6 for the CS-CB/SPF8 film. The mass residue of the films slightly
increased with the addition of fiber, showing small variations.
3.4. Structural properties of films
3.4.1. Scanning electron microscopy (SEM)
SEM was used to examine the microstructure and the interfacial
adhesion of cassava starch and its reinforced biocomposites. Fig. 4A
shows the SEM micrographs of the plasticized cassava starch film
(CS film). The CS film showed homogeneous surfaces and a com-
pact structure. The addition of the filler led to the formation of more
heterogeneous surfaces, where particles of the reinforcing material
covered by the starch matrix can be observed (Fig. 4B–F). The fact
that the fibers were coated with the starch matrix indicated that
the residue was structurally incorporated in the network, owing
to a high compatibility between both components. Good adhe-
sion between the filler and the matrix leads to a resistant interface
[49], consequently reinforcing the matrix enhances the mechani-
cal properties of the material. When a higher amount of SPF filler
was used (CS-CB/SPF8), particle density increased, promoting the
interaction among filler particles, which could induce the forma-
tion of aggregates. The presence of these aggregates, together with
large fiber particles, induces defects in the matrix, which affect film
structure integrity (Fig. 4f), probably because of their high volume.
Ludueña et al. [50] stressed that the agglomerates do not allow cor-
rect matrix-filler interaction, and therefore they observed weaker
polymer-filler interfacial adhesion [50].
A SEM micrograph was used to qualitatively assess the inter-
facial adhesion of the fiber and matrix for the hybrid composites.
The fracture model of the hybrid composite in Fig. 4, can prove
that there was good compatibility between CS and SPF. SEM micro-
graphs of the hybrid film also reveal the presence of SPF as
reinforcement in bio-composite without any cracks. Good adhe-
sion between the matrix and the fibers without voids or pores. Fig. 4
shows a series of SEM micrographs of the fractured surface of the
hybrid composites containing different amounts of SPF. It is indica-
tive of the relatively homogeneous nature of these biocomposites
as seen in SEM. It can be observed that smooth fracture surfaces
with a homogeneous matrix as well as good adhesion of the SPF
to the TPS matrix, which play an important role in improving the
performance of the obtained material.
The fact that fibers were coated with the starch matrix indicated
that the fiber was structurally incorporated in the network (Fig. 4),
owing this to a high compatibility between both components.
Good adhesion between the filler and the matrix leads to a resis-
tant interface [49], consequently reinforcing the matrix enhancing
their properties. Similar observations have been reported by other
authors for starch based composites [10,51].
Mass Residue (%) at 500 ◦ C DTG peak (◦ C)
T50%
323.5 25.1 319.8
312.6 25.4 311.5
315.9 25.8 311.4
315.7 26.1 311.1
315.4 26.3 310.5
311.6 26.6 308.7
3.4.2. Fourier transform infrared spectroscopy (FTIR)
The functional groups present in the CB-SPF/CS hybrid com-
posites were analyzed by FT-IR (Fig. 5). Through this analysis,
it was possible to demonstrate the existence of certain chem-
ical constituents in the SPF-CB/CS hybrid composites, namely,
amylose and amylopectin for starch and cellulose, hemicellu-
lose and lignin for the fiber. It was found that the FT-IR spectra
for all the samples showed the same peaks, since our mate-
rials were derived from biological resources. For example, the
intense peaks at 3200–3500 cm−1 indicated the presence of O H
groups in starch and fiber, showing that starches are very sensi-
tive to water molecules due to the presence of hydroxyl groups.
This was also supported by other authors, [9,52], and these peak
ranges were attributed to the stretching of hydroxyl groups due to
hydrogen bonding between the molecules. Meanwhile, the strong
bands at 2900–3000 cm−1 were assigned to the C H stretching
and the peaks at 990–1000 cm−1 were found to be characteris-
tic of the anhydroglucose ring O C stretch [53]. Also, the peaks
at 1500–1600 cm−1 were attributed to the bending of water in
starch [54]. Furthermore, in the case of the CS film, this band is
broader than those of the composite samples due to the structure
of the polysaccharide and also to the possible association of water
with this poly-hydroxylated system. The effect of increasing the
fiber content in the composites is reflected inversely on the shape
of this band (a less defined band). According to Tongdeesoontorn
et al., the band located at 1658 cm−1 corresponds to the adsorbed
water in the samples [55]. As can be observed in the spectra
(Fig. 5), the CS film shows the most intense signal at this frequency,
which is reflected by the breadth and intensity of the O H band
at 3270 cm−1 . On the other hand, this band decreases in the CS/CB
composite sample, as well as in the hybrid (CS-CB/SPF). Besides, in
these CS film, the intensity of the band changes gradually (decreas-
ing) proportionally to the increase in the amount of fibers. This
result suggests that the starch is mainly responsible for this water
band and therefore, the SPFs do not have any observable contribu-
tion because of their low moisture content.
3.4.3. X-ray diffraction (XRD)
XRD measurements were performed to determine the effect of
fiber loading on the crystallinity of the films. The XRD spectra of
the CS film, CB/CS composite film and CB/SPF reinforced CS hybrid
composite films are presented in Fig. 6. XRD results indicated that
the crystalline structure of the CS film was increased by the incor-
poration of CB and SPF. The CS film had sharp diffraction peaks
at 17.3◦, which indicated a typical A-type pattern [56]. As can be
seen in Fig. 6, the films with a higher fiber content have a highly
crystalline structure. The relative crystallinity values of the cassava
films with various fiber loadings are listed in Table 5. The addition
of 6% cassava bagasse (CS/CB) did not significantly affect the crys-
tallinity of the films. However, the incorporation of SPF did, and as
a result, the crystallinity of the films increased from 0.33 to 0.47, as
a function of SPF content.
The result is influenced by cellulose content, where the higher
cellulose structure in the SPF contributed to the high crystallinity
 A. Edhirej et al. / International Journal of Biological Macromolecules 101 (2017) 75–83 81

Fig. 4. SEM of A: CS film, B: CS/CB composite film and C–F: CS-CB/SPF hybrid composites films.

1500

1400

1300 CS-CB/SPF8
1200

1100

1000 CS-CB/SPF6
900
CS-CB/SPF4
Inensity

800

700

600

500 CS-CB/SPF2

400
CS/CB
300
Fig. 5. FTIR spectra of TPS matrix (CS film), CS/CB bio-composites and CB/SPF rein- 200
forced CS with different sugar palm fibers loading. CS film
100
Table 5 0
The relative crystallites (RC) of CS film, CS/CB composite film and CS-CB/SPF hybrid 10 15 20 25 30 35 40 45 50
composites films.
(2θ)
Film RC (%)
Fig. 6. XRD curves of CS film (control), CS/CB composite film and CB/SPF reinforced
CS FILM 32
CS hybrid composites films.
CS/CB 33
CS-CB/SPF 2 37
CS-CB/SPF 4 39 enhancement of relative crystallinity in the TPS based composites
CS-CB/SPF 6 43 is expected with increasing the amount of fibers [44].
CS-CB/SPF 8 47

of the films. This is due to the cellulose crystalline structure [29].
Table 5 presents the relative crystallinity of TPS based compos-
ites. It can be observed that the proportional increase of fibers in
the matrix caused enhancement of the relative crystallinity. Fibers,
synthetic or natural, are orientated materials and therefore, their
crystallinity is higher than the crystallinity of starch. Therefore, an
4. Conclusion
CB/SPF reinforced CS hybrid composites were developed with
the main objective of obtaining a material with improved prop-
erties and performance. The incorporation of SPF significantly
improved the physical properties. It decreased the water con-
tent, water solubility and water absorption. The addition of SPF
82 A. Edhirej et al. / International Journal of Biological Macromolecules 101 (2017) 75–83
also increased the relative crystallinity up to 47%. Comparing the
CB/SPF hybrid composite with the CS/CB composite film and the
CS film, it is clear that the same properties were improved with
the addition of SPF. The thermal properties were also studied and
the results demonstrated that the addition of fibers led to a slight
decrease in the degradation temperature of the hybrid. This is nor-
mal, considering the low degradation temperature of natural fibers.
Morphological analysis of the hybrid composite using SEM revealed
good interfacial interaction and dispersion of CB and SPF within
the matrix. Overall, hybridization of CB with SPF in TPS improves
the properties of the composites, which expanded the potential
application of this biodegradable material.
Conflict of interest
The authors declare that there is no conflict of interest regarding
the publication of this paper.
Acknowledgements
The authors are grateful for the financial support from Uni-
versity Putra Malaysia and for the funding this project received
through the Exploratory Research Grant Scheme (vote number
9389900).
References
[1] A.K. Mohanty, M. Misra, L.T. Drzal, Natural Fibers, Biopolymers, and
Biocomposites, CRC Press: Taylor & Francis Group, Boca Raton, FL, 2005.
[2] S.M. Sapuan, M. Maleque, Design and fabrication of natural woven fabric
reinforced epoxy composite for household telephone stand, Mater. Des. 26 (1)
(2005) 65–71.
[3] Z. Leman, S.M. Sapuan, A. Saifol, M.A. Maleque, M. Ahmad, Moisture
absorption behavior of sugar palm fiber reinforced epoxy composites, Mater.
Des. 29 (8) (2008) 1666–1670.
[4] P. Panichnumsin, A. Nopharatana, B. Ahring, P. Chaiprasert, Production of
methane by co-digestion of cassava pulp with various concentrations of pig
manure, Biomass Bioenergy 34 (8) (2010) 1117–1124.
[5] A. Edhirej, S.M. Sapuan, M. Jawaid, N.I. Zahari, Its polymer, fiber, composite,
and application, Polym. Compos. 38 (3) (2015) 555–570, http://dx.doi.org/10.
1002/pc.23614.
[6] M. Ishak, S.M. Sapuan, Z. Leman, M. Rahman, U. Anwar, Characterization of
sugar palm (Arenga pinnata) fibres, J. Therm. Anal. Calorim. 109 (2) (2012)
981–989.
[7] M. Ishak, Mechanical Properties of Treated and Untreated Woven Sugar Palm
Fibre-reinforced Unsaturated Polyester Composites, Master of Science Thesis,
Universiti Putra Malaysia, Serdang, Selangor Malaysia, 2009.
[8] R. Jumaidin, S.M. Sapuan, M. Jawaid, M. Ishak, J. Sahari, Characteristics of
thermoplastic sugar palm starch/agar blend: thermal, tensile, and physical
properties, Int. J. Biol. Macromol. 89 (2016) 575–581.
[9] J. Sahari, S.M. Sapuan, Z. Ismarrubie, M. Rahman, Physical and chemical
properties of different morphological parts of sugar palm fibres, Fibres Text.
East. Eur. (2012) 21–24.
[10] J. Sahari, S.M. Sapuan, E. Zainudin, M. Maleque, Thermo-mechanical behaviors
of thermoplastic starch derived from sugar palm tree (Arenga pinnata),
Carbohydr. Polym. 92 (2) (2013) 1711–1716.
[11] D. Bachtiar, S.M. Sapuan, M. Hamdan, The effect of alkaline treatment on
tensile properties of sugar palm fibre reinforced epoxy composites, Mater.
Des. 29 (7) (2008) 1285–1290.
[12] M.M. Thwe, K. Liao, Durability of bamboo-glass fiber reinforced polymer
matrix hybrid composites, Compos. Sci. Technol. 63 (3) (2003) 375–387.
[13] M. Sreekala, J. George, M. Kumaran, S. Thomas, The mechanical performance
of hybrid phenol-formaldehyde-based composites reinforced with glass and
oil palm fibres, Compos. Sci. Technol. 62 (3) (2002) 339–353.
[14] N. Pan, K. Chen, C.J. Monego, S. Backer, The hybrid effects in hybrid fibre
composites: experimental study using twisted fibrous structures, Proc. R. Soc.
Lond. A: Math. Phys. Eng. Sci. R. Soc. (1998) 1109–1127.
[15] A. Edhirej, S.M. Sapuan, M. Jawaid, N.I. Zahari, Effect of Various Plasticizers
and Concentration on the Physical, Thermal, Mechanical and Structural
Properties of Cassava Starch Based Films, Starch-Stärke, 2016.
[16] F. Versino, M.A. García, Cassava (Manihot esculenta) starch films reinforced
with natural fibrous filler, Ind. Crops Prod. 58 (2014) 305–314.
[17] H. Yaich, H. Garna, S. Besbes, M. Paquot, C. Blecker, H. Attia, Chemical
composition and functional properties of Ulva lactuca seaweed collected in
Tunisia, Food Chem. 128 (4) (2011) 895–901.
[18] M.G. Lomelí Ramírez, K.G. Satyanarayana, S. Iwakiri, G.B. de Muniz, V. Tanobe,
T.S. Flores-Sahagun, Study of the properties of biocomposites. Part I. Cassava
starch-green coir fibers from Brazil, Carbohydr. Polym. 86 (4) (2011)
1712–1722.
[19] K. Frost, D. Kaminski, G. Kirwan, E. Lascaris, R. Shanks, Crystallinity and
structure of starch using wide angle X-ray scattering, Carbohydr. Polym. 78
(3) (2009) 543–548.
[20] Y. Lu, L. Weng, X. Cao, Morphological, thermal and mechanical properties of
ramie crystallites—reinforced plasticized starch biocomposites, Carbohydr.
Polym. 63 (2) (2006) 198–204.
[21] K.N. Matsui, F. Larotonda, S. Paes, D. Luiz, A. Pires, J. Laurindo, Cassava
bagasse-Kraft paper composites: analysis of influence of impregnation with
starch acetate on tensile strength and water absorption properties,
Carbohydr. Polym. 55 (3) (2004) 237–243.
[22] N. Cao, X. Yang, Y. Fu, Effects of various plasticizers on mechanical and water
vapor barrier properties of gelatin films, Food Hydrocoll. 23 (3) (2009)
729–735.
[23] M. Jouki, N. Khazaei, M. Ghasemlou, M. HadiNezhad, Effect of glycerol
concentration on edible film production from cress seed carbohydrate gum,
Carbohydr. Polym. 96 (1) (2013) 39–46.
[24] S. Shojaee-Aliabadi, H. Hosseini, M.A. Mohammadifar, A. Mohammadi, M.
Ghasemlou, S.M. Ojagh, S.M. Hosseini, R. Khaksar, Characterization of
antioxidant-antimicrobial ␬-Carrageenan films containing satureja hortensis
essential oil, Int. J. Biol. Macromol. 52 (2013) 116–124.
[25] Z. Ahmad, N.H.A. Razak, N.S.M. Roslan, N. Mosman, Evaluation of kenaf fibres
reinforced starch based biocomposite film through water absorption and
biodegradation properties, J. Eng. Sci. 10 (2014) 31.
[26] M.G. Lomelí-Ramírez, S.G. Kestur, R. Manríquez-González, S. Iwakiri, G.B. de
Muniz, T.S. Flores-Sahagun, Bio-composites of cassava starch-green coconut
fiber: part II—structure and properties, Carbohydr. Polym. 102 (2014)
576–583.
[27] L.R. Mello, S. Mali, Use of malt bagasse to produce biodegradable baked foams
made from cassava starch, Ind. Crops Prod. 55 (2014) 187–193.
[28] F. Versino, O.V. López, M.A. García, Sustainable use of cassava (Manihot
esculenta) roots as raw material for biocomposites development, Ind. Crops
Prod. 65 (2015) 79–89.
[29] N. Reddy, Y. Yang, Biofibers from agricultural byproducts for industrial
applications, Trends Biotechnol. 23 (1) (2005) 22–27.
[30] M. Jawaid, H.A. Khalil, Cellulosic/synthetic fibre reinforced polymer hybrid
composites: a review, Carbohydr. Polym. 86 (1) (2011) 1–18.
[31] D.I. Munthoub, W.A.W.A. Rahman, Tensile and water absorption properties of
biodegradable composites derived from cassava skin/polyvinyl alcohol with
glycerol as plasticizer, Sains Malays. 40 (7) (2011) 713–718.
[32] N. Razali, M.S. Salit, M. Jawaid, M.R. Ishak, Y. Lazim, A study on chemical
composition, physical, tensile, morphological, and thermal properties of
Roselle fibre: effect of fibre maturity, BioResources 10 (1) (2015) 1803–1824.
[33] J. Sahari, S.M. Sapuan, E. Zainudin, M. Maleque, Effect of water absorption on
mechanical properties of sugar palm fibre reinforced sugar palm starch
(SPF/SPS) biocomposites, J. Biobased Mater. Bioenergy 7 (1) (2013) 90–94.
[34] M.J. John, S. Thomas, Biofibres and biocomposites, Carbohydr. Polym. 71 (3)
(2008) 343–364.
[35] J. Sahari, S.M. Sapuan, Z. Ismarrubie, M. Rahman, Comparative study of
physical properties based on different parts of sugar palm fibre reinforced
unsaturated polyester composites, Key Eng. Mater. Trans Tech. Publ. (2011)
455–460.
[36] E. Nuwamanya, Y. Baguma, N. Emmambux, P. Rubaihayo, Crystalline and
pasting properties of cassava starch are influenced by its molecular
properties, Afr. J. Food Sci. 4 (1) (2010) 008–015.
[37] O. Shakuntala, G. Raghavendra, A. Samir Kumar, Effect of filler loading on
mechanical and tribological properties of wood apple shell reinforced epoxy
composite, Adv. Mater. Sci. Eng. 2014 (2014) 1–9.
[38] P.R. Salgado, V.C. Schmidt, S.E.M. Ortiz, A.N. Mauri, J.B. Laurindo,
Biodegradable foams based on cassava starch, sunflower proteins and
cellulose fibers obtained by a baking process, J. Food Eng. 85 (3) (2008)
435–443.
[39] N. Soykeabkaew, P. Supaphol, R. Rujiravanit, Preparation and characterization
of jute-and flax-reinforced starch-based composite foams, Carbohydr. Polym.
58 (1) (2004) 53–63.
[40] N. Kaisangsri, O. Kerdchoechuen, N. Laohakunjit, Biodegradable foam tray
from cassava starch blended with natural fiber and chitosan, Ind. Crops Prod.
37 (1) (2012) 542–546.
[41] M. Bertuzzi, M. Armada, J. Gottifredi, Physicochemical characterization of
starch based films, J. Food Eng. 82 (1) (2007) 17–25.
[42] R. Sothornvit, J. Krochta, Plasticizers in edible films and coatings, Innov. Food
Packag. (2005) 403–433.
[43] F. Debiagi, R.K. Kobayashi, G. Nakazato, L.A. Panagio, S. Mali, Biodegradable
active packaging based on cassava bagasse, polyvinyl alcohol and essential
oils, Ind. Crops Prod. 52 (2014) 664–670.
[44] X. Ma, J. Yu, J.F. Kennedy, Studies on the properties of natural fibers-reinforced
thermoplastic starch composites, Carbohydr. Polym. 62 (1) (2005) 19–24.
[45] J. Sahari, S.M. Sapuan, E. Zainudin, M.A. Maleque, Mechanical and thermal
properties of environmentally friendly composites derived from sugar palm
tree, Mater. Des. 49 (2013) 285–289.
[46] S. Mohanty, S.K. Verma, S.K. Nayak, Dynamic mechanical and thermal
properties of MAPE treated jute/HDPE composites, Compos. Sci. Technol. 66
(3) (2006) 538–547.
 A. Edhirej et al. / International Journal of Biological Macromolecules 101 (2017) 75–83
[47] Y. El-Shekeil, S.M. Sapuan, K. Abdan, E. Zainudin, Influence of fiber content on
the mechanical and thermal properties of Kenaf fiber reinforced
thermoplastic polyurethane composites, Mater. Des. 40 (2012) 299–303.
[48] H. Yang, R. Yan, H. Chen, D.H. Lee, C. Zheng, Characteristics of hemicellulose,
cellulose and lignin pyrolysis, Fuel 86 (12) (2007) 1781–1788.
[49] S. Kuciel, A. Liber-Knec, Biocomposites on the base of thermoplastic starch
filled by wood and kenaf fiber, J. Biobased Mater. Bioenergy 3 (3) (2009)
269–274.
[50] L. Ludueña, A. Vázquez, V. Alvarez, Effect of lignocellulosic filler type and
content on the behavior of polycaprolactone based eco-composites for
packaging applications, Carbohydr. Polym. 87 (1) (2012) 411–421.
[51] H. Ibrahim, M. Farag, H. Megahed, S. Mehanny, Characteristics of starch-based
biodegradable composites reinforced with date palm and flax fibers,
Carbohydr. Polym. 101 (2014) 11–19.
83
[52] H. Sakina, Z. Sarani, D. Khairul Zaman, Chemical characterization of
benzylated oil palm empty fruit bunches, Symposium on utilization of oil
palm tree. oil palm biomass: opportunities and challenges in commercial
exploitation, Kuala Lumpur, 2000.
[53] J. Fang, P. Fowler, J. Tomkinson, C. Hill, The preparation and characterisation
of a series of chemically modified potato starches, Carbohydr. Polym. 47 (3)
(2002) 245–252.
[54] J. Sahari, S.M. Sapuan, E. Zainudin, M.A. Maleque, Thermo-mechanical
behaviors of thermoplastic starch derived from sugar palm tree (Arenga
pinnata), Carbohydr. Polym. 92 (2) (2013) 1711–1716.
[55] W. Tongdeesoontorn, L.J. Mauer, S. Wongruong, P. Sriburi, P. Rachtanapun,
Effect of carboxymethyl cellulose concentration on physical properties of
biodegradable cassava starch-based films, Chem. Cent. J. 5 (1) (2011) 1–8.
[56] L. Zhang, W. Xie, X. Zhao, Y. Liu, W. Gao, Study on the morphology, crystalline
structure and thermal properties of yellow ginger starch acetates with
different degrees of substitution, Thermochim. Acta 495 (1) (2009) 57–62.