International Journal of Biological Macromolecules 108 (2018) 167–176

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International Journal of Biological Macromolecules

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

Effect of duration of sonication during gelatinization on properties of

tapioca starch water hyacinth fiber biocomposite
Mochamad Asrofi a , Hairul Abral a,∗ , Yogi Kurnia Putra a , SM Sapuan b,c , Hyun-Joong Kim d
a
Department of Mechanical Engineering, Andalas University, 25163 Padang, Sumatera Barat, Indonesia
b
Department of Mechanical and Manufacturing Engineering, Faculty of Engineering, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia
c
Laboratory of Biocomposite Technology, Institute of Tropical Foresty and Forest Products (INTROP) Universiti Putra Malaysia, 43400 UPM Serdang,
Selangor, Malaysia
d
Laboratory of Adhesion & Bio-Composites, Program in Environmental Materials Science, Research Institute for Agriculture & Life Sciences, Seoul National
University, Seoul 151-921, Republic of Korea

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

Article history: This paper characterizes properties of biocomposite sonicated during gelatinization. The biocompos-
Received 8 October 2017 ite consisted of tapioca starch based plastic reinforced by 10% volume fraction of water hyacinth fiber
Received in revised form (WHF). During gelatinization, the biocomposite was poured into a rectangular glass mold then vibrated
11 November 2017
in an ultrasonic bath using 40 kHz, 250 W for varying durations (0, 15, 30, and 60 min). The resulting
Accepted 26 November 2017
biocomposite was then dried in a drying oven at 50 ◦ C for 20 h. The results of this study indicate that a
biocomposite with optimal properties can be produced using tapioca starch and WHF if the gelatinizing
Keywords:
mixture is exposed to ultrasound vibration for 30 min. After this vibration duration, tensile strength (TS)
WHF-tapioca starch biocomposite
Mechanical and thermal properties
and tensile modulus (TM) increased 83% and 108%. A further 60 min vibration only increased the TS at 13%
Moisture absorption and TM at 23%. Moisture resistance of the biocomposite after vibration increased by around 25% reaching
Vibration duration a maximal level after 30 min. Thermal resistance of the vibrated biocomposites was also increased.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction posites, as it is fast growing and abundantly available [9,10]. Some

Degradable bioplastic materials show potential as an environ-
mental pollution-reducing replacement for synthetic polymers.
Polysaccharide based bioplastics provide promise for food pro-
tection and preservation applications [1]. The use of biopolymers
based on polysaccharides substance provides promise for innova-
tive applications in food protection and preservation [2]. However,
starch based thermoplastic has low strength and thermal resis-
tance, high moisture absorption, low resistance to microbial
activity [3–5]. Many attempts to overcome these weaknesses have
been trialed. Mixing starch with ramie crystallites and cellulose
nanofibers from cassava bagasse has been found to improve the
mechanical properties and moisture resistance of biocomposites
[6,7]. When mixed with plant fibers the resulting biocomposite
could provide an attractive substitute for many synthetic polymers
[8]. The fiber of the water hyacinth plant with its high cellulose
content is one attractive reinforcement material for starch biocom-
∗ Corresponding author at: Department of Mechanical Engineering, Andalas Uni-
versity, Padang, Indonesia.
E-mail address: abral@ft.unand.ac.id (H. Abral).
previous reports have used these fibers with polyester to produce
composites with viable mechanical properties [10–13].
The introduction of air bubbles and agglomeration in the starch
matrix during pouring decreased mechanical properties of the bio-
composite [14–16]. Last works reported that applying of ultrasound
during preparing sample has created good filler dispersion and
minimized agglomeration in matrix [15,17,18]. Previous studies
have shown that applying ultrasound during sample preparation
improved performance of the biocomposite, because agglomera-
tion could be minimized and good filler dispersion created [19,20].
Ultrasound process was found superior in terms of its efficiency
of breaking the strong agglomerates of MWCNTs along with their
homogeneous distribution in the epoxy matrix [20]. Ultrasonica-
tion created good dispersion of cellulose nanofibers in polyvinyl
alcohol, yielding high mechanical properties of the composite
[17,21]. A previous study reported that SEM fractured surface was
smooth which signals good dispersion and homogeneity in the
composite [21]. Even an increase in concentration of the nanofibers
up to 10% did not lead to the emergence of signs of aggregation of
fibers in a micron-scale. In all cases, no signs of fiber pull-out could
be spotted.

https://doi.org/10.1016/j.ijbiomac.2017.11.165
0141-8130/© 2017 Elsevier B.V. All rights reserved.
168 M. Asrofi et al. / International Journal of Biological Macromolecules 108 (2018) 167–176
Gelatinization during the manufacture of starch based plastic
is achieved by heating and gently stirring the starch dispersion
in excess water, and is characterized by hydration, swelling, and
loss of birefringence and crystallinity of the starch chains [22,23].
However, undamaged amylopectin-rich fractions often remain
resulting in incomplete starch solubility. These insoluble fractions,
known as ghosts, are dispersed throughout the film’s microstruc-
ture in a similar way to micro-filler. Cheng et al. [24] studied
the impact of ultrasonic treatment on properties of starch film-
forming dispersion and the resulting film. Ultrasound treatment
ruptured the swelling starch granules disintegrated all the ghosts
in gelatinized maize starch dispersions increased the amount of
solubilized amylose and enhanced free mobility of polymers in the
starch dispersions, resulting in a drastic decrease in apparent vis-
cosity and increase in solubility even for a 10% starch dispersion.
This process yielded films with good transparency, improved ten-
sile strength and moisture resistance, and stronger structure [24].
An ultrasonic bath generates mechanical forces as a result of
cavitation. The collapse of the microbubbles created by cavita-
tion produces sound waves which propagate through the solution
resulting in strong shear forces [5,18,25,26]. Several works have
reported the effect of intensity and time of ultrasound dur-
ing formation on the performance of a range of composites
[5,21,23,27–32]. However, no investigations of the impact of ultra-
sound duration in a starch based biocomposite sonicated during
gelatinization exist. There is insufficient information on the effect
of vibration of gelatinized biocomposites. Therefore, in this present
research, the effect of various vibration durations during gela-
tinized on the properties of a 10% WHF pulp and tapioca starch
biocomposite was studied. The benefit of this study is to discover
the duration of 40 kHz, 250-W ultrasonic bath radiation necessary
to optimize both the mechanical properties of gelatinized 10% WHF
pulp and tapioca starch, and energy consumption. The properties
of the biocomposite measured were tensile testing, thermal stabil-
ity, and moisture absorption. Meanwhile, X-ray diffraction (XRD),
Fourier transform infrared spectroscopy (FTIR), SEM photograph of
the surface was used to identify chemical features, interactions of
all functional groups, and defects in the biocomposite.
2. Materials and methods
2.1. Extraction of WHF
WHF obtained from a swamp in 50 Kota district, Indonesia was
cut into 1 cm lengths and cleaned in fresh water. These were then
placed in a ventilated drying space with plastic roof and walls
exposed to sunlight for 5 days until dry. The dried WHF samples
were treated with 25% NaOH solution in a digester for 6 h at about
130 ◦ C, and 2 bar. Finally, the pulp was washed until the pH was
neutral, and blended for 10 min using an electric mixer. The pulp
was screened by using a printing screen with T61 mesh, then dried
using sunlight.
2.2. Preparation of biocomposite
Local commercially produced Cap Pak Tani brand tapioca pow-
der was used as a matrix for the biocomposite. This tapioca powder
consists of 19% water, 15% amylose, and 85% amylopectin. 1 g WHF
was mixed with 140 ml of the water. 10 g tapioca powder and
3 ml of glycerol were poured into the mixture which was then
mixed with a (Daihan HG 15D-Set A) homogenizer for 5 min at
5000 rpm. The solution was gelatinized using a magnetic stirrer at
150 ◦ C, 500 rpm for 18 min. Finally, the gelatinizing biocomposite
was poured into a rectangular glass mold and placed in the ultra-
sonic bath (model number PS-70AL, 40 kHz and 420 W). The mold
was only vibrated at 250 W, 40 kHz, and 100% amplitude with var-
ious duration for 15, 30, 60 min respectively. For duration 30 and
60 min, water in the bath was replaced every 15 min to keep the
water temperature lower than 40 ◦ C. A Universal oven (Memmert
UN-55) was used to dry the samples at 50 ◦ C for 20 h.
2.3. Moisture absorption
A piece of the biocomposite sample was dried in oven drying
until a constant weight was achieved. It was weighed using preci-
sion balance (Kenko) with 0.1 mg accuracy then stored in a closed
chamber with 99% relative humidity (RH) and 25 ◦ C for 30 min,
taken out and weighed again. Moisture absorption of the sample
was calculated by using [33]:
(wh − wo )
Moisture absorption (%) = × 100 (1)
wo
where wh is weight of moist sample and w0 initial weight of dried
sample.
2.4. Tensile testing
Tensile strength of the biocomposite was measured at room
temperature using a Com-Ten testing machine (95T Series) with
tensile speed of 3 mm/min. Five biocomposite samples from each
vibration duration were measured according to standard ASTM
D638 Type I. Thickness and width of the film were measured using a
dial micrometer to 1 ␮m accuracy. The tensile strain was measured
at the point of fracture of the sample.
2.5. Thermal gravimetric analyzing (TGA/DTG), differential
scanning calorimetry (DSC)
TGA and DTG measurement of samples were performed using
a thermal analyzer (TGA Q500 V20.6, USA). The samples were
weighed between 4 and 5 mg. The scans were run from room tem-
perature up to 600 ◦ C at a heating rate of 10 ◦ C/min under nitrogen
flow of 25 ml/min. DSC was measured using TA Instrument (Model
Q20) from room temperature up to 280 ◦ C at 10 ◦ C/min with nitro-
gen flow rate of 50 ml/min. The weight of each sample was 5–10 mg.
2.6. FTIR characterization
FTIR characterization was performed by using a Perkin Elmer
Frontier spectrometer to determine the functional groups of the
TSB and TSB/WHF composite. Samples were formed in the form of
thin sheets and scanned in the spectral range 4000–600 cm−1 .
2.7. SEM observation
SEM photography was performed using a Hitachi 3400 N series
SEM to scan the fracture surface of the tensile sample.
2.8. X-ray diffraction
X-ray diffraction (XRD– PANalytical Xpert PRO) measurement
was performed using CuK␣ radiation (␭ = 0.1542 nm) scanning
from 10 to 100◦ with a generator setting of 40 kV and 30 mA. Per-
centage of crystallinity index (CI) was measured as follows [34]:
(I200 − Iam )
CI (%) = × 100 (2)
I200
where I200 is intensity of the peak corresponding to cellulose I, and
Iam is intensity of the peak of the amorphous fraction.
 M. Asrofi et al. / International Journal of Biological Macromolecules 108 (2018) 167–176 169

3. Results and discussions
3.1. SEM photograph
Fig. 1 shows SEM photographs that display different fracture
surfaces of the tensile specimens irradiated for various vibration
durations. Fig. 1a and b are SEM images of the fracture surface
showing the different dimension of the porosities. The sample
vibrated for 30 min (Fig. 1b) show smaller defects than the sam-
ple vibrated for 15 min (Fig. 1a). The gap between the WHF and the
matrix of the non-vibrated sample was more distinct in compari-
son to that vibrated for 60 min. Better interfacial bonding between
WHF and the matrix was obtained after vibration (Fig. 1d). Agglom-
eration of the untreated sample was observed in Fig. 1e, but this
tends to be well dispersed through the matrix after irradiation
(Fig. 1f). This may be due to the ultrasound bath providing the
kinetic energy to expedite the depolymerization process of the
starch gel resulting in a decreased viscosity due to the destruction
of the polymer network [35]. Low viscosity would provide easier
diffusion of all substances to fill macro and micro porosities in

Fig. 1. Fracture surface of TSB WH: (a) structure of composites in 15 min, (b) structure of composites in 30 min, (c) interfacial adhesion matrix-fiber in 0 min, (d) interfacial
adhesion matrix-fiber in 60 min, (e) distribution fiber in 0 min, (f) distribution fiber in 60 min.
170 M. Asrofi et al. / International Journal of Biological Macromolecules 108 (2018) 167–176

Fig. 2. FTIR diffraction pattern in range of (a) 250–4000 cm-1, (b) OH stretching, (c) Absorbed water and –CH2 symmetrical bending, (d) C O stretching.
 M. Asrofi et al. / International Journal of Biological Macromolecules 108 (2018) 167–176
the biocomposite, thus making better interface bonding between
WHF and the matrix [22,36,37]. Furthermore, the kinetic energy
results in de-agglomeration of the WHF allowing it to be dispersed
well [24]. Better inter-facial bonding and WHF dispersion result
in an improvement in mechanical properties and moisture resis-
tance after ultrasound. The results of this work are consistent with
previous studies [20,38].
3.2. FTIR spectra
FTIR is used to identify chemical features and shifts due to
interactions between functional groups [39]. Fig. 2a displays the
FTIR spectra of all samples with and without vibration treat-
ment. Vibration in the ultrasonic bath did not change the overall
appearance of the FTIR spectra [40]. However, there was an obvi-
ous shift in wave number of the bands including magnification
of the region of 3280–3297 cm-1 (corresponding to OH stretch-
ing) and 2928–2932 (corresponding to CH stretching) in Fig. 3b,
1643–1645 (in relation to absorbed water) and 1352–1354 (corre-
sponding to CH2 symmetrical bending) in Fig. 2c, 1013–1016 (in
relation to C O stretching) in Fig. 2d, [41,42] The obvious decrease
in wave number from 3280 up to 3297 in the region of OH stretch-
ing may be due to the formation of hydrogen bonds between WHF
Fig. 3. XRD- diffraction patterns of the treated samples for a) 0, b) 15, c) 30, d) 60 min respectively.
171
and the matrix [22,43,44]. Kaewtatip et al. [45] also found strong
hydrogen bond formation between luffa fiber and a cassava starch
matrix evidenced by a shifting of the −OH stretching wave number
to a lower value [45]. As vibration duration increased the trough
associated with absorbed water became shallower. This is due to
an increase in compactness as evidenced by SEM photographs. This
shift is consistent with the moisture absorption data as shown in
Fig. 7s which displays lower moisture absorption of the biocom-
posite after vibration.
3.3. X-ray diffraction
X-ray diffraction patterns of the untreated and treated biocom-
posite after 0, 15, 30 and 60 min of vibration are displayed in
Fig. 3a–d, respectively. Fig. 3a shows that the diffraction pattern
for the untreated samples displays more peaks as can be seen in
more detail in Table 1. As vibration duration increases some peaks
disappear, for example, the peak with intensity 1121 at 2␪ = 24
in the untreated biocomposite (Fig. 3a) disappeared after vibra-
tion as shown in Fig. 3b–d. Disappearance of the peaks could be
due to gelatinization of ‘ghosts’, the previously insoluble starch,
thus increasing amylose content and the viscosity of the matrix
[23,24,46]. Another reason for disappearance of the pattern may be
172 M. Asrofi et al. / International Journal of Biological Macromolecules 108 (2018) 167–176

Fig. 4. Thermogravimetric analysis (TGA/DTG) curve of samples for a) 0, b) 15, c) 30, d) 60 min respectively.

Table 1 were reduced according to the duration of vibration. In the begin-

Quantitative data of XRD diffraction pattern of Fig. 3.
ning, CI was decreased significantly by about 61% after 15 min
No Sample 2 Theta (o ) Intensity (Count) Crystallinity Index (CI in%) vibration. For further vibration duration, the crystallinity index dis-
1 0 min 15 972 84 plays tendency of steady state. CI of 60 min vibrated sample was
2 17 1371 57% which could be categorized as high CI, yielding better mechan-
3 20 1385 ical properties [49].
4 22 1484
5 24 1121
6 26 920 3.4. TGA/DTG and DSC analyzing
7 34 848
8 15 min 17 1218 61 Fig. 4 displays the thermal stability of the present biocompos-
9 20 1213
ite. Graphs of weight loss (%) and derivative weight (%/min) for all
10 22 1379
11 30 835 specimens display similar appearances. The initial weight loss at
12 35 831 around 100 ◦ C indicates evaporation of water content in the sam-
13 30 min 15 937 69 ples [49]. The second major weight loss in the temperature range of
14 17 1243
240–370 ◦ C may be due to decomposition of celluloses [50]. Ther-
15 20 1212
16 22 1386
mal resistance of the vibrated sample is higher than that without
17 30 781 treatment. This is evidenced by increases in initial decomposi-
18 60 min 17 1179 57 tion temperature for further vibration duration. In this case, the
19 20 1099 initial decomposition temperature without vibration in Fig. 4a is
20 22 1357
269.76 ◦ C, then it improves to 273.67 ◦ C (Fig. 4b), 275.33 ◦ C (Fig. 4c),
and 275.69 ◦ C (Fig. 4d) for 15, 30, and 60 min respectively. Mean-
while, the maximum decomposition temperature shown in DTG
a disruption of the crystalline structure of clustered amylopectin curve shifted to a higher temperature after vibration. The enhance-
leading the diffraction peaks became broader [47]. The only change ment of the thermal resistance was also confirmed in DSC curve as
to the three main peaks at 17, 20, 22 (2␪) was a decrease in shown in Fig. 5. The melting temperature of the sample without
their intensity corresponding to a reduction crystallinity index (CI). vibration in Fig. 5a is 190.59 ◦ C that is lower than samples vibrated
These changes in CI are in good agreement with previous studies for 15 min (192.59 ◦ C) in Fig. 5b, 30 min (195.10 ◦ C) in Fig. 5c, and
[27,48]. Table 1 shows how the CI values for various treatments 60 min (193.33 ◦ C) in Fig. 5d. The improvement of the thermal sta-
 M. Asrofi et al. / International Journal of Biological Macromolecules 108 (2018) 167–176
Fig. 5. DSC curve of the samples for a) 0, b) 15, c) 30, d) 60 min respectively.
bility after ultrasonication was attributed to well WHF dispersion,
and better interfacial bonding between WHF and matrix [51]. More
compact microstructure after vibration results in improvement for
thermal resistance [23]. Furthermore, it is necessary to note that
significant increase in thermal resistance is clearly observed from
vibration of 0 min up to 30 min. However, it became lower for vibra-
tion 60 min that probably indicates a constant level of the thermal
stability achieved in 30 min duration.
3.5. Tensile strength (TM), tensile modulus (TM) and elongation
at break (EL)
Average TS, TM, and EL of the biocomposite for various vibra-
tion times are shown in Fig. 6a–c. The value of TS and TM improved
markedly, and EL decreased as the biocomposite became strong,
rigid and more brittle after ultrasound exposure. Up to 30 min the
stress strain relationship improved rapidly with vibration dura-
tion but further vibration appeared to provide no improvement to
these values. The average TS, TM, and EL in the untreated sam-
ples 3.41 MPa, 49.96 MPa and 22.20%, respectively. After 30 min
of vibration TS increased 83%. A further 60 min vibration only
increased the TS about 13.48% to an average of 7.07 MPa. TM
markedly improved up to 30 min of vibration then the rate of
increase was reduced reaching a maximum level (127.65 MPa) at
60 min; a 155.5% improvement compared to the nonvibrated sam-
ple. Fig. 6c shows EL of the biocomposite for different vibration
times. The EL decreased as duration of treatment increased from
173
22.20% with no vibration to 18.45% after 60 min. This change in
mechanical properties may be due to the ultrasonication vibrat-
ing all the substances within the biocomposite, leading the WHF to
separate and to distribute homogeneously throughout the matrix.
Furthermore, vibration also reduces the gaps between the matrix
and the fibers. The improved mechanical properties of the biocom-
posite are a result of both the homogeneously dispersed WHF in
the tapioca starch matrix and the strong hydrogen bonds between
fiber and matrix resulting from their closer proximity. This is sup-
ported by the SEM photographs of the fractured surfaces which
shows evidence of better interfacial adhesion (Fig. 1d), and uniform
fiber dispersion within the matrix (Fig. 1f). Previous studies have
also indicated that ultrasonic treatment improved the mechanical
properties of composites [22,24,52].
3.6. Moisture absorption
Generally, a starch based biocomposite has high moisture
absorption due to the hydrophilic nature of starch [24]. Therefore,
it is salient to observe the effect of vibration duration on moisture
absorption in these 10% WHF starch based biocomposites. Fig. 7
shows the moisture absorption of each sample after 6 h in a moist
chamber. All samples absorbed moisture rapidly until saturation
point. However, the nonvibrated samples display the highest rate
of absorption (%/time) and also have the highest moisture absorp-
tion capacity. The average value of moisture absorption of sample
decreased as vibration duration increased up to 30 min probably
174 M. Asrofi et al. / International Journal of Biological Macromolecules 108 (2018) 167–176

Fig. 6. Effect vibration time in high loading WHF fraction in TSB matrix on mechanical properties of (a) tensile strength (b) tensile modulus (c) elongation at break.

indicating that the increased compactness of the vibrated biocom-

posite makes diffusion of water difficult [6,53–55]. A similar result
was also reported by W. Cheng et al. [24] who demonstrated that
ultrasound treatment produced a film with higher moisture resis-
tance and stronger structure in comparison to untreated film.

4. Conclusions

This study investigated properties of tapioca starch based bio-

composites reinforced by a 10% by volume fraction of WHF formed
with different periods of (40 kHz, 250 W) ultrasonic vibration. The
vibrated biocomposites were more compact, stronger, more rigid,
more thermal and moisture resistant, and more brittle after ultra-
sonication. SEM photographs demonstrated that vibration resulted
in better interfacial bonding between WHF and the matrix, and this
was evidenced by shifts of OH stretching in the FTIR curves. XRD
demonstrated that the crystal structure of the biocomposite was
also changed by vibration. TS and TM values of sample vibrated
for 30 min were improved by 83% and 108% and EL was decreased
by 15% compared to the non-vibrated sample. Further vibration
Fig. 7. Performance of moisture absorption for all studied samples.
after this point resulted in minimal changes to these mechanical
 M. Asrofi et al. / International Journal of Biological Macromolecules 108 (2018) 167–176
properties. Moisture resistance of the biocomposite after vibration
increased by around 25% reaching a maximal level after 30 min.
The results of this study indicate that a biocomposite with optimal
mechanical properties can be produced using tapioca starch and
WHF if the gelatinizing mixture is exposed to ultrasound vibration
for 30 min.
Acknowledgement
Acknowledgment is addressed to Andalas Univer-
sity, for supporting research funding with project name
“Skim Klaster Riset Guru Besar 2017”, contract number
69/UN.16.17/PP.HGB/LPPM/2017.
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