Cellulose (2021) 28:2039–2051
https://doi.org/10.1007/s10570-020-03670-0 (0123456789().,-volV)
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ORIGINAL RESEARCH
Development and characterization of biodegradable starch-
based fibre by wet extrusion
Ali Afzal . Farooq Azam . Sheraz Ahmad . Zubair Khaliq . Amir Shahzad .
Muhammad Bilal Qadir . Abdul Moqeet Hai
Received: 13 November 2019 / Accepted: 29 December 2020 / Published online: 15 January 2021
Ó The Author(s), under exclusive licence to Springer Nature B.V. part of Springer Nature 2021
Abstract The man-made fibres have the versatility
of required engineered properties. The biodegradabil-
ity is the need of the day. This study aimed at
development of biodegradable starch based fibers
using wet extrusion technique. The non-modified
natural starch is cost efficient and wet extrusion
technique will support bulk production of fibre without
any change in chemical structure of material. Multiple
additives such as plasticizers and binders were added
to the dope solution in different concentrations to
study their effect on physical properties, mechanical
performance and serviceability of the wet-spun starch
fibers. The ranges of additive concentrations in (% wt/
v) used to make the dope solutions are as follows:
starch; 38–64%, Polyvinyl Alchohol (PVA); 7–23%,
glycerol; 18–39% and styrene butadiene styrene
(SBS); 0–21%. The developed fibres had linear
density in the range of 25 tex–44 tex with fibre
diameter of about 247–301 lm. The extruded fibers
were characterized for fiber strength, surface mor-
phology, water absorption, and biodegradability. The
developed fibres have maximum tenacity of 1.56
cN/tex and water absorbency of 280 g/g. The intended
A. Afzal  F. Azam  S. Ahmad (&) 
Z. Khaliq  A. Shahzad  M. B. Qadir
Faculty of Engineering and Technology, National Textile
University, Faislabad 37610, Pakistan
e-mail: sheraz@ntu.edu.pk
A. M. Hai
University of the Punjab, Lahore 54590, Pakistan
application for these fibres is in medical textiles as
wound dressings.
Keywords Starch  Polyvinyl alcohol  Wet
extrusion  Biodegradability  Fibre
Introduction
Synthetic polymers are extensively used in various
fields of daily life from floor matt to advanced
protective clothing (Nair and Laurencin 2007). The
advantages of using synthetic polymers are the
diameter uniformity, engineered physical properties
and ease of manufacturing. However, synthetic poly-
mers are mostly petroleum based which are non-
biodegradable and can cause harmful environmental
problems. Biopolymers, owing to their biodegradabil-
ity and environmental friendly nature, have attracted a
lot of interest in recent years (Vert et al. 2002).
Starch is a biopolymer having hydrophilic semi
crystalline structure. It has granular form in its native
state which contains a mixture of two glycosidic
macromolecules (LeCorre et al. 2012) i-e amylose
(1 ? 4) a-glucopyranose and amylopectin (1 ? 4)
a-glucopyranose with (1 ? 6) branched linkages.
Starch composes of 70–80% amylopectin which
changes its structure with botanical origin (Buleon
et al. 1998). Native starch can be divided into two
categories based on crystal types of tube starches and
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cereal (Imberty and Perez 1988; Thompson 2000). A
semi crystalline structure of starch is obtained by the
presence of short chains in the amylopectin (Thomp-
son 2000).
Starch has been explored for various applications
such as filtration (Gupta et al. 2010), food products
(Han et al. 2019), food packaging (Kaewtatip and
Tanrattanakul 2012; Ren et al. 2009), drug delivery
(Fundueanu et al. 2004; Mundargi et al. 2008),
composite formation (Cheng 2019; Fitch-Vargas
et al. 2019; Owodunni et al. 2020) and textiles
(Mekala et al. 2014). Starch fibres developed with
electrospinning technique (Gordon et al. 2006) had the
disadvantage of limited production due its low
productivity. In the previous studies thermoplastic
based starch fibres were fabricated by electrospinning
and centrifugal spinning techniques as mentioned in
literature (Gordon et al. 2006; Kong and Ziegler
2014). In electrospinning technique, formic acid and
dimethyl sulfoxide has been used as solvent to
dissolve the native as well as modified starch types
(Wang et al. 2019b). A number of trials had been done
to developed starch fibres using various content of
amylose and amylopectin using electrospinning tech-
niques (Fonseca et al. 2019; Vasilyev et al. 2019). In
addition, wet electrospinning method has also been
reported where starch fibres were coagulated in
ethanol bath to develop fibre matt (Wang et al. 2019a).
In other studies, starch fibres were developed by
blending modified or native starch with crosslinkers,
plasticizers, polymers or additives (Curvelo et al.
2001; González and Alvarez Igarzabal 2015). How-
ever, larger contents of non-starch materials domi-
nated the starch properties (Curvelo et al. 2001;
Gordon et al. 2006). Pure starch fibres were developed
recently by electro wet spinning technique (Kong and
Ziegler 2012, 2014). However, this method is only
applicable to those starches which contain below 65%
amylopectin. This method has limited spinning con-
centration range and cannot be used for thicker and
shorter fibres having amylopectin content greater than
65% (Kong and Ziegler 2012).
The development of the fibres with native starch by
using wet spinning technique still needs attention. The
non-modified natural starch is cost efficient and wet
extrusion technique will support bulk production of
fibre without any change in chemical structure of
material. This study is focused on the development of
starch-based fibres by using wet spinning technique
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Cellulose (2021) 28:2039–2051
having native starch as major component with plas-
ticizer and binders at different concentrations. The
effects of multiple concentrations on different prop-
erties are investigated. These properties include sur-
face morphology using scanning electron microscope
(SEM), X-ray diffraction (XRD), swelling behaviour,
mechanical properties and biodegradability of the
fibres.
Experimental
Materials
The unmodified waxy corn starch chemical grade of
essentially pure amylopectin and polyvinyl alcohol
(PVA) (C 99.2% purity) were purchased from Dae-
jung Korea. Glycerol (purity C 99.5%), poly(styrene-
co-butadiene) (SBS) (butadiene 4 wt%) and acetone
(purity C 99.8% laboratory grade) were purchased
from Sigma Aldrich, Germany.
Experimental design was made using the Full
Factorial method for the development of biodegrad-
able fibre to investigate the effect of different levels of
input factors on output. PVA used to impart strength to
fibres, has three levels (2, 3 and 5 wt%), glycerol used
to provide the flexibility to the fibres, also have three
levels (5, 7 and 9 wt%) and Binder used to bind the
chains of PVA with starch having 2 levels (0 and
5 wt%). Table 1 shows 18 experiments with different
combinations of levels. All experiments were carried
out according to run order.
Preparation of dope solution for wet spinning
The starch solution was prepared by dissolving 10 g
pure waxy corn starch in 50 ml of water under
constant stirring at 85 °C for 10 min. PVA solution
was prepared with variable concentrations in separate
beakers by dissolving PVA in water at 60 °C with
constant stirring for 10–15 min. Then both solutions
were mixed and stirred continuously for 30 min at
80 °C. The prepared solution is shown in Fig. 1. After
30 min, binder and glycerol were added in the
prepared solution as per design of the experiment
(Table 1).
Cellulose (2021) 28:2039–2051 2041

Table 1 Design of experiment which acetone was used as coagulant in spin bath at
Sample code PVA (wt%) Glycerol (wt%) Binder (wt%)
room temperature. After extrusion, fibres were col-
lected and dried at room temperature.
1 2 5 0
2 5 Physical characterization
3 7 0
4 5 Surface morphology
5 9 0
6 5 The morphology of the fibres was investigated using
7 3 5 0 Quanta 250 FEI scanning electron microscope (SEM).
8 5 The samples are non-conductive in nature. Therefore
9 7 0 gold coating was done on the surface using sputter
10 5 coater. The SEM images were taken mainly at two
11 9 0 magnification levels (100 9 and 400 9) at 10 kV
12 5 applied voltage.
13 5 5 0
14 5 X-ray diffraction analysis
15 7 0
16 5 The crystallographic information of starch fibre was
17 9 0 investigated using X-Ray diffractometer (XPert Pro
18 5 manufactured by PANalytical). The copper anode was
used as X-Ray source supplied with current of 30 mA
at 40 kV voltage supply to generate 0.1540 nm
characteristic wavelength. The data were collected at
5–55°2h, 0.01°2h and 1 s/step of scan range, scan
depth and time per step respectively. The developed
filament sample was tightened into an entangled small
ball and placed in cavity of zero diffraction plate
sample holder to analyse the crystallographic peaks.

Mechanical characterization

Tensile strength and fibre elongation properties

The samples were conditioned in the standard atmo-

Fig. 1 Prepared solution for wet spinning
Wet extrusion of starch fibres
The dope solution was stirred for 10 min at 85 °C
followed by transfer in dope tank of wet extrusion
machine which was thermally regulated at 90 °C. The
fibres were extruded using wet spinning technique in
sphere according to ASTM D 1776. The tenacity of the
fibres was measured by using the tensile strength tester
according to ASTM D3822 method. Single fibre
strength tester (Testometric M250-2.5CT, Rochdale,
England) was used for tensile strength testing. The test
was conducted at a gauge length of 25 mm using load
cell of 50 N and speed of 10 mm/min at the temper-
ature of 21 ± 1 °C and 65 ± 2% relative humidity.
Five measurements of each sample were conducted,
and average value was recorded.

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Serviceability/comfort characterization
Water absorption
Water absorption of prepared fibers was measured
according to the ASTM D570 standard with inclusion
of different salt solutions. The specimens were oven
dried for 24 h at 50 ± 3 °C and then placed into the
desiccator to cool and weighed (Wd) on an analytical
balance capable of reading up to 0.1 mg. The condi-
tioned samples were immersed in three different liquid
mediums i.e., de-ionized water, solution A (0.9298%
NaCl ? 0.0368% CaCl2), and saline solution (0.9%
NaCl) for 24 h at 23 ± 1 °C. Specimens were
removed after 24 h, patted dry with the lint-free dry
cloth and finally weighed (Ww). The water absorption
was calculated by using the Eq. 1 (Peng et al. 2016).
 
g Ww  Wd
Water absorption ¼  100 ð1Þ
g Wd
Swelling test
Swelling test was performed using high definition
optical microscope (MICROS MC-50) at 40 9 mag-
nification installed with a digital camera. A minimum
of 10 fibres of more than 1 cm in length were placed on
glass slide. The swelling was tested for three different
swelling solutions i.e., de-ionized water, solution A
(0.9298% NaCl ? 0.0368% CaCl2), and saline solu-
tion (0.9% NaCl). The selected swelling solution drops
(1 * 2) were poured near the fibres on the glass plate
and let it to absorb for 2 min. The fiber diameter was
measured before (Dd) and after (Dw) swelling. The
swelling percent was measured by using the Eq. 2
(Hussain et al. 2016; Miraftab et al. 2011).
Dw  Dd
Swelling% ¼  100 ð2Þ
Dd
Degradation test
Degradation of fibres was evaluated using amylase
solution in water. For this purpose, specimens having
minimum lengths of 25 mm were dried in oven at
50 ± 3 °C for 24 h and weighed (W1). Then speci-
mens were immersed in enzymatic solution in a
shaking incubator having 120 rpm at 30 °C for 60 h.
The fibres were removed and gently rinsed with
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Cellulose (2021) 28:2039–2051
distilled water to remove enzymatic mixture and again
dried in desiccator for 24 h and weighed (W2).
Percentage degradation was measured using the Eq. 3:
W1  W2
Degradation% ¼  100 ð3Þ
W1
Results and discussion
Physical characterization
Surface morphology
Figures 2 and 3 shows the SEM images of the fibres at
100 9 and 400 9 magnification respectively for dif-
ferent samples. Figure 2 and 3a, e indicates that the
surface roughness of fiber decreases with increasing
PVA content with an increase in polymer grain size.
These results indicate that starch, the main constituent
has been coated with PVA which increases the grain
size and ultimately the roughness decreases. The
influence of glycerol on fibre surface can be visualized
by comparing (c & d) of Figs. 2 and 3. The results
concluded that porosity and rough appearance of fibre
surface had been reduced with an increase in glycerol
content. The increase in binder concentration also
influences the surface morphology of starch fiber as
depicted in Fig. 3a, b and e, f. It was observed that a
smooth surface was achieved by the incorporation of
binder content in the starch fibres.
Fibre diameter
The fibre diameter was measured using the Image J
version 1.51n software. The software was used for
image analysis of the SEM images to measure fibre
diameter. The fibre diameter measured for developed
fibres lies in the range of 247–301 lm.
Linear density
The linear density of the fiber was calculated using the
standard test method ASTM D 1059 for short test
specimens (ASTM 2001). Ten specimens were taken
to determine the mean linear density of fibres. The
graphical representation of obtained linear densities
against sample codes is shown in Fig. 4. The
Cellulose (2021) 28:2039–2051 2043

Fig. 2 Longitudinal SEM images of starch fibers at 100 9 magnification with 400 lm scale, [a sample 1, b sample 6, c sample 9,
d sample 11, e sample 13, f sample 16]

developed fibres had linear densities in the range of 25 wi

W%i ¼ Pn  100 ð6Þ
to 44 tex. 1 wi
The linear density was also calculated by measuring
where Wi is the weight (g) of an individual component
the diameter of the fibre using the following Eq. 4:
and W%i is the weight percent of individual compo-
M nent (g/g %). The individual volume percentage was
T t ¼ 1000 ð4Þ
L calculated using Eq. 7.
The Eq. 4 can also be written as: W%i
Vi ¼ ð7Þ
T t ¼ 1000  q  S ¼ 100000  q  p  r 2
ð5Þ qi

where, Tt is the calculated linear density (tex), M is
mass (g), L is length (m), q is the material density (g/
cm3), S is the yarn cross-sectional area (cm2), and r is
the yarn radius (cm). The material used in this study
was multi-components. Therefore composite material
density was calculated by considering the mass and
volume for each material component. The weight
percentage of individual component (W%i) was
calculated by percentage ratio of weight of individual
component (Wi) to total weight of the fibre as given in
Eq. 6.
where Vi is the volume of a component (cm3), and qi is
the density of that component (g/cm3). The density of
composite material was calculated using Eq. 8.
wc
qc ¼ Pn ð8Þ
1V i
where wc is the initially taken weight (g) of composite
and qc is the composite density (g/cm3). The fiber
surface area was calculated using the mean fibre
diameter for each sample obtained from SEM image
analysis. The random samples from experimental runs
were taken for comparison between actual and calcu-
lated linear density of fibre as shown in Fig. 5. The

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2044 Cellulose (2021) 28:2039–2051

Fig. 3 SEM images of the fiber at 400 9 magnification with 100 lm scale, [a sample 1, b sample 6, c sample 9, d sample 11, e sample
13, f sample 16]

Fig. 4 Experimental linear

density of different samples

error percentage between actual and calculated linear
density was also measured and shown in Fig. 5. It was
observed that the calculated linear density was close to
actual linear density of the composite developed fibre.
The average error percentage was less than 15% which
affirms that composite linear density can be calculated
theoretically with sufficient accuracy percentage.
X-ray diffraction analysis
Figure 6 shows the X-Ray Diffraction (XRD) analysis
of starch-based fibre containing PVA and starch as the
prime constituents. The peaks obtained in XRD
spectra are prominent at around 15°, 16.9°, 17.8°,
20.5°, and 23.2° which appear due to the crystallinity

123
Cellulose (2021) 28:2039–2051
Fig. 5 Error percentage comparison of calculated and actual linear density
Fig. 6 XRD pattern of composite starch fiber
of the PVA and starch polymer. Our results are in
agreement with previous studies which indicated that
peak around 20.2° is for PVA and around 15° and 23°
are for the starch fibre, whereas the doublet at about
17° and 18° indicates typical A-type pattern of starch
(Sadhu et al. 2015; Yu et al. 2006).
Mechanical characterization
Tensile strength
Effect of PVA concentration on the tensile strength of
the starch-based fibres is given in the Fig. 7. The
2045
Fig. 7 Surface plot of tensile strength verses PVA and glycerol
concentration in starch fibers
developed fibres have showed tenacity in range of 0.12
cN/tex–1.56 cN/tex (0.88–11.54 MPa). It is evident
that the strength of the fibres increases with increasing
the concentration of PVA (Tudorachi et al. 2000). This
is because of the reason that PVA has good mechanical
properties due to C–C backbone and OH groups in its
structure. Starch does not have good mechanical
properties. The inclusion of PVA in its structure helps
to improve the strength of the blended fiber. Also, both
polymers are polar substances having hydroxyl groups
which establish hydrogen bonding resulting in a better
fiber strength (Sin et al. 2010). Glycerol shows limited
effect on the strength of the fibres at low concentration
(Mao et al. 2000). However, a steep rise in strength is
observed with increasing its concentration. It might be
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2046
due to the increase in the flexibility of fibres by
increasing the glycerol concentration.
The effect of binder concentration on the tensile
strength of the fibres is given in Fig. 8. It can be
observed in Fig. 8 that the binder has no remarkable
effect on the fibre strength. However, it is interesting
to note that the tensile strength of fibers increases with
increasing both concentrations of binder and glycerol.
The combined effect of binder and glycerol is directly
proportional to the tensile strength of starch fibre. The
main purpose to use the binder is to bind the chains of
starch and PVA which helps the fibers for slow
degradation.
Tensile elongation
The force–elongation curve of the starch fiber is
shown in Fig. 9. The results depict an elastic region up
till 0.2 N (0.045 lbf) applied force followed by the
Fig. 8 Surface plot of tensile strength verses glycerol and
binder concentration of starch fibers
Fig. 9 Force elongation curve of starch fiber
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Cellulose (2021) 28:2039–2051
plastic deformation. The tensile modulus is high
indicating that material shows sufficient strength
without change in its physical properties. The plastic
deformation region shows high elongation which is
due to the inclusion of PVA in the fiber.
Serviceability/comfort characterization
Degradation test
The degradation percentage of the fibre is shown in
Fig. 10 which describes that the fiber degradation
decreases with increasing the amount of PVA
(Jayasekara et al. 2003). While a slight increase is
observed with increasing the amount of binder. This is
because of the reason that the rate of degradation of
PVA and starch is different. In starch fibre, binder is
used to bond the chains of starch with PVA. In the
degradation process, the binder degrades causing the
fibre structure to lose its structural strength and
ultimately degradation occurs. The crystallinity of
the fibres also affects the degradation. Starch has
amorphous regions in its structure therefore it has
good degradability. The degradation is also affected
by the temperature of liquid media (water), since both
PVA and starch dissolves in water at high temperature.
However, the experiment was carried out at room
temperature to determine its use for wound dressings.
Water absorbency
Water absorbency of fibre samples is determined for
different salt solutions. The results depicted that all the
samples have very good absorbency. The starch in the
fibre has excellent ability to absorb water due to the
Cellulose (2021) 28:2039–2051
Fig. 10 Effect of Binder and PVA content on the degradation
percentage of the fibers
presence of hydroxyl groups which attracts the water
molecules and hence the absorbency of the fibres
increases. The absorbency of deionized water was
highest followed by saline solution and solution A
(NaCl ? CaCl2). The absorbency of starch fibres in
different solutions from low to high is deionized
water [ Na? [ Ca2?. The strength of salt type and
concentration can be expressed as ionic strength. The
Fig. 11 Effect of ionic strength on the water absorbency of the fibers
2047
ionic strength (mol ion/dm3) of solutions are Ca2?-
[ Na? [ deionized water. The relation of ionic
strength on water absorbency is expressed by Flory’s
equation (Bao et al. 2011).
 2
5=3 i=2V u S1=2 þ ð1=2  x1 Þ=V 1
Q  ð9Þ
V E =V 0
where Q is degree of swelling, i=V u is the charge
density of polymer, S is the ionic strength of the
solution, (1/2 - x1)/V1 is the polymer-solution affin-
ity, VE/V0 is the crosslinking density. The water
absorbency decreases by increasing the ionic strength
of saline solution as per Eq. 9. The obtained results are
in accordance with Flory’s equation.
The water absorbency decreases with an increase in
the concentration of different external saline solutions.
This may be caused by the cations in different salt
solutions. The osmotic pressure between external
saline solution and polymeric network decreases with
the increase of the concentration of the saline solution.
The decrease in water absorbency of starch fibres
might also be due to reduced penetration of counter
ions (Na? and Ca2?) into the polymeric network on
the anionic group (–CO) causing screening effect.
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Fig. 12 Swelling behavior of starch-based fiber
Swelling test
The swelling test was performed to analyse the change
in the physical dimension of fibre in different solutions
by using the optical microscope. Swelling in distilled
water has highest values for all the samples as shown
in Fig. 12. The highest value for swelling in distilled
water might be due to the different constituents present
in the fibre. The first reason can be the starch fibre
which is cellulosic in its nature having natural ability
to absorb water. Secondly, PVA and glycerol both
have hydroxyl groups which attract the water
molecules. In comparison to distilled water, the saline
solution and solution A (NaCl ? CaCl2) have lesser
swelling as demonstrated in Fig. 12. Starch, PVA, and
glycerol have organic nature and are less polar as
compared to salts which reduce the ion exchange
between the saline solution and fibres. The lesser
swelling might be due to the interaction of ions with
the hydroxyl groups leaving lesser hydroxyl groups for
water absorption that’s why it shows less swelling. As
the fibres absorb water, dimensions of the fibres
changes which swell the fibre in transverse and axial
direction. The pre-images (a, c and e) are the fibre
before absorption and post-images (b, d and f) are after
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Cellulose (2021) 28:2039–2051
absorption as shown in Fig. 13. It is clearly observed
that the diameter of the fibre increases, and fibre gets
swelled after the absorption of water.
Conclusion
The starch-based biodegradable fibres were developed
in this study using wet extrusion technique. The error
percentage between calculated linear density and
experimental linear density was less than 15% which
expresses good homogeneity among constituent mate-
rials. The effect of PVA and binder on tensile strength,
absorption, swelling and biodegradability was deter-
mined. The tensile strength of fibers was increased
with increasing PVA concentration. Also, the fibre
elongation was predominately depending on the
concentration of PVA and glycerol. The surface
morphology of fiber changed with the change in the
concentration of constituent materials. It was observed
that the PVA and binder had a direct relation with
surface smoothness and porosity of fiber. Addition of
the binder increased the biodegradability of the fibres
but reduced the roughness and water absorption
Cellulose (2021) 28:2039–2051
Fig. 13 Swelling of the fibers after absorption
because binder used to degrade the PVA at faster rate
so that starch and PVA can degrade at equal rates.
Acknowledgments The authors gratefully acknowledge the
financial support provided by Higher Education Commission,
Islamabad, Pakistan for the completion of this research having
research Grant Number 21-1850/SRGP/R&D/HEC/2018.
Compliance with ethical standards
Conflict of interest The authors declare that they have no
conflict of interest.
2049
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