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Superhydrophobic EVA copolymer fibers: the impact of chemical composition

on wettability and photophysical properties

Article in Colloid and Polymer Science · November 2018

DOI: 10.1007/s00396-018-4395-7

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Colloid and Polymer Science (2018) 296:1759–1766
https://doi.org/10.1007/s00396-018-4395-7

ORIGINAL CONTRIBUTION

Superhydrophobic EVA copolymer fibers: the impact of chemical

composition on wettability and photophysical properties
Gokhan Acik 1 & Musa Kamaci 1 & C. Elif Cansoy 1

Received: 25 July 2018 / Revised: 14 August 2018 / Accepted: 19 August 2018 / Published online: 28 August 2018
# Springer-Verlag GmbH Germany, part of Springer Nature 2018

Abstract
Fibers of poly(vinyl acetate) (PVAc) homopolymer and ethylene vinyl acetate (EVA) copolymers with varying vinyl acetate
(VAc) contents between 25 and 40 wt.% have been prepared to investigate wettability and photophysical properties. At lower
VAc contents, it was difficult to prepare fibers without any beads due to the presence of crystalline ethylene groups at higher
concentrations. EVA copolymer composition strongly affected the wettability of fibers; all EVA copolymer fibers exhibited
superhydrophobic behavior and CA values varied between 150° and 160° depending on copolymer composition while hydro-
philic PVAc homopolymer fibers exhibited hydrophobic behavior with a CA of 134°. Photophysical properties of PVAc homo-
polymer and EVA copolymers were evaluated in terms of transmittance and emission intensity. Emission intensity and transpar-
ency of EVA copolymers were decreased with the increase of VAc contents due to its amorphous behavior.

Keywords VAc fibers . EVA fibers . Wettability . Contact angle . Photophysical properties

Introduction
In recent years, a wide range of interest has been generated in
the development and application of block copolymers due to
their both special structure and availability of synthesis
methods related to material science [1–7], nanotechnology
[8, 9], medicine [10–12], etc. Ethylene vinyl acetate copoly-
mers (EVA), known as poly(ethylene vinyl acetate), having
wide range physical properties are obtained via copolymeri-
zation of ethylene and vinyl acetate by high pressure process.
After the incorporation of the more polar vinyl acetate seg-
ments to the polyethylene backbone, solubility and glass-
transition temperature of obtained polymer shift to higher
values. There are three types EVA according to percentage
of vinyl acetate known as up to 4% vinyl acetate modified
poly ethylene, between 4 and 30% thermoplastic ethylene
vinyl acetate copolymer and greater than 40% ethylene vinyl
acetate rubber. EVA, being non-biodegradable but biocompat-
ible and highly elastomeric, used wide range industrial appli-
cation including road construction, hoses, coatings, adhesives,
* C. Elif Cansoy
ecansoy@pirireis.edu.tr
1
Piri Reis University, Tuzla, 34940 Istanbul, Turkey
scratch films, and especially electric cables due to the flame
reterdancy characteristic [13–18].
There are a number of processing technique to obtain poly-
meric fiber such as template synthesis [19, 20], drawing [21,
22], self-assembly [23, 24], phase separation [25, 26], and
electrospinning [27, 28]. Electrospinning has been recognized
as a very simple and easily controlled technique to process
continuous fibers with diameters ranging from micrometer to
nanometer or from single to ordered arrangements which have
complex structure such as shell and hollow. This process not
only can be applied to synthetic or natural polymer but also
can be applied to metals, ceramics, and glasses in academic
investigations and broad range of industrial fields including
sensor technology [29, 30], filtration [31, 32], optoelectronics
[33, 34], textiles [35, 36], and medicine [37–40]. In principal,
typical electrospinning instrument composes of nozzle, pump,
voltage supply, and collector. In the electrospinning process,
applied voltage which generates electrostatic force has to
overcome the surface tension of spinning solution in order to
form fiber. By defeating the surface tension, a droplet forms at
the needle tip and transforms to conical shape knowns as
Taylor cone [41]. The polymeric jet reaches the collector sub-
sequent to the formation of conical shape at the end of the
electrospinning process by means of potential differences.
Provided that process parameters such as feed rate, surface
tension, concentration, humidity, temperature, and
1760 Colloid Polym Sci (2018) 296:1759–1766

conductivity and molecular parameters such as melting point, 26 mm dimensions) were used to accumulate fibers in
glass-transition temperature, solubility, molecular weight, electrospinning process.
chain entanglement density, and pH value are correctly used,
almost all fusible or soluble polymers can be processed by Preparation of electrospinning solutions
electrospinning. Each of those parameters either directly or
indirectly affects the various properties of final product [35]. The parameters used for the preparation of the copolymer
In this work, we have prepared fibers of PVAc homopoly- solutions are summarized in Table 1.
mer and EVA copolymers with varying vinyl acetate (VAc)
contents. VAc contents of EVA copolymers varied from 25 to Electrospinning procedure
40% and PVAc homopolymer has also been used as 100% VA
content. After 25% VA content, electrospinning of the copol- Laboratory scale NE-100 model equipment (Inovenso,
ymer solutions was not possible due to the increase in ethylene Turkey) was used in the electrospinning process. This equip-
percentage. Ethylene homopolymer and also EVA copolymers ment consists of a syringe pump (New Era Pump Systems
with higher ethylene contents are not soluble in their solvents Inc., USA), high DC voltage power supply which can gener-
at room temperature. Because our electrospinning equipment ate current from 0 to 40 kV (Elektrosis, PW1010, Turkey), and
does not contain temperature apparatus, it was not possible to mobile aluminum ground collector. The distance between alu-
use the electrospinning solutions rather than room tempera- minum plate collector and needle tip was immobilized at
ture. Therefore, EVA copolymers with higher ethylene content 20 cm during the electrospinning process, and the potential
were not used within this study. Wettability of the fibers has difference voltage value was fixed at 21 kV by using an ad-
been changed depending on copolymer composition. At lower justable voltage supply while mass flow rate was 2 ml/h for all
VA contents, fibers exhibited superhydrophobic behavior. polymer solutions at room temperature. Electrospun fibers
Even PVAc is a hydrophilic polymer, the fibers of PVAc have were accumulated on glass slides which were stuck on the
shown hydrophobic behavior with a water contact angle of collector. All glass slides were cleaned in chromic acid solu-
134°. This was due to the incorporated roughness and thus tion before use. Electrospun fibers were stored in a desiccator
air pockets within the surface topography of the fibers. at room temperature for 1 day in order to remove the residual
Photophysical properties of homopolymer and copolymers solvents before characterization.
fibers were evaluated by using transmittance and fluorescence
spectroscopies. EVA copolymers have become more opaque Characterization
with the increase of VAc content in copolymer matrix due to
the amorphous properties of VAc. Fourier transform infrared (FT-IR) analysis was performed to
verify specific groups of PVAc and EVA copolymers by using
the Perkin-Elmer (Lambda 25, Waltham, USA) FT-IR
Spectrum Two Spectrometer equipped with a diamond ATR
Materials and methods device at room temperature, scanning range covered 4000 to
400 cm−1. Photophysical properties of electrospun fibers were
Materials measured by using Ultraviolet-visible (UV-Vis) and fluores-
cence spectrophotometers. Transmittance spectra were record-
Poly (vinyl acetate) (PVAc, Mw = 100.000 g/mol) was pur- ed using a Perkin-Elmer Lambda 25 UV-Vis spectrophotom-
chased from Sigma Aldrich (Steinheim, Germany). Ethylene eter in the range from 300 to 800 nm. Fluorescence measure-
vinyl acetate copolymer (EVA-40, Mw = 42.000 g/mol) was ments were carried out using a Perkin-Elmer LS-55 fluores-
purchased from Sigma Aldrich (Steinheim, Germany). All cence spectrometer in the range from 300 to 800 nm. The
the other copolymers, EVA-33, EVA-28, and EVA-25 were
supplied from Arkema (Colombes, France). According to Table 1 Solution preparation parameters
the ASTM D1238 (2.16 kg, 190 °C) guideline, melt flow
index values of copolymers (from EVA-40 to EVA-25), quot- Entry Polymer Concentration Solvent Temperature Time
(mg/ml) (°C) (hour)
ed from suppliers’ catalogs, were 57 g/10 min, 350–400 g/
10 min, 5–8 g/10 min, and 1.8 g/10 min respectively, and all 1 PVAc 380 Chloroform r.t. 2.5
polymers were used as received. Numbers of abbreviations 2 EVA-40 240 Chloroform r.t. 2.5
express the percentage of VAc in the copolymer. For example, 3 EVA-33 240 Chloroform r.t. 3
EVA-40 contains 60% ethylene and 40% vinyl acetate. 4 EVA-28 200 Chloroform 60 1.5
Chloroform (≥ 99.5%, Sigma Aldrich, Germany) was used 5 EVA-25 120 Chloroform 60 2
as solvent during the preparation of electrospinning solutions
and used without distillation. Standard glass slides (76 × All solutions were prepared under continuous and vigorous stirring
Colloid Polym Sci (2018) 296:1759–1766
excitation wavelength and slit width were adjusted as 330 and
2.5 nm, respectively during the measurements. Merck grade
water was used for equilibrium, advancing, and receding con-
tact angle (CA) measurements on PVAc homopolymer and
EVA copolymer surfaces, and CA measurements were done
by using a KSV Attension Theta Optical Tensiometer at room
temperature under air. CA measurements have been done on
three different regions on each fiber surface, and average CA
values were reported with standard deviations of ± 2°. Five-
microliter droplet volumes were used for equilibrium CA (θe)
measurements, and the needle was removed from the droplet
during the measurements. However, the needle was kept with-
in the droplet during advancing (θa) and receding CA (θr)
measurements; the volume of the droplet was increased from
3 to 8 μl during θa measurements and then decreased down to
3 μl while measuring θr values. FE-SEM (Leo Supra 35 VP),
field emission scanning electron microscope, was used for
investigation of the surface topographies of the PVAc and
EVA copolymer fibers.
Results and discussion
Characterization
FT-IR spectroscopy was used to indicate the chemical struc-
ture of PVAc and EVA fibers obtained by electrospinning
process. A representative FT-IR spectrum of PVAc and
EVA-40 is given in Fig. 1, and it clearly showed us that the
presence of characteristic bands located at around 2925 cm−1
(–CH symmetric stretch), 1740 cm −1 (–C=O stretch),
1470 cm−1(–CH bending), 1228 cm−1, and 1010 cm−1 (C–
O–C stretch) corresponds to the functional groups of PVAc
fibers [42–44]. All these peaks are observed also in the
Fig. 1 FT-IR spectra of PVAc and EVA-40 electrospun fibers
1761
spectrum of EVA-40, but additionally sharp peaks at around
both 2925 cm−1 and 2850 cm−1 attributed to aliphatic –CH
bending coming from ethylene segments verify the structure
of EVA [45, 46].
Surface characterization of fibers
Surface characterization of PVAc homopolymer and EVA co-
polymer fibers was done by SEM analysis. SEM images of
PVAc and EVA copolymer fibers, at 1.00 kX magnification,
are given in Fig. 2. The morphology of the electrospun fibers
is strongly affected from the applied voltage, tip-collector dis-
tance, and also the flow rate [47–50]. At higher flow rates,
bead fibers with thicker diameters will be formed instead of
smoother fibers with thinner diameters due to the short drying
time prior to reaching the collector. The large amount of solu-
tion is withdrawn from needle tip and residual solvent which
needs time to dry, lead to occur larger average bead size and
fiber diameter. Also, the residual solvent cause to form beads
instead of fibers due to the merge together of obtained fiber
structures.
At higher VAc contents, fibers were synthesized without
any beads; however, with the increase of ethylene content in
the copolymer structure, it was difficult to obtain fibers with-
out beads.
Polyethylene homopolymer has poor solubility in conven-
tional solvent systems at room temperature. Because our
electrospinning setup does not contain any heating system, it
was not possible to prepare solutions of copolymers with
higher ethylene contents, at room temperature. The increase
in ethylene content of the copolymers caused to form beads
instead of fibers at room temperature. This was due to the
crystalline behavior of ethylene polymer. After 28% content
of VAc, bead formation has started within the fiber structures
and due to the increase of ethylene content in EVA-25 copol-
ymer, electrospinning of the copolymer solution and thus the
formation of fibers were not possible at room temperature.
Wettability measurements
Surface roughness and chemical heterogeneity are the main
parameters that affect the wettability of the surfaces. EVA
copolymers with varying VAc contents and PVAc homopoly-
mer were used to prepare fibers to investigate the effect of
both roughness and chemical heterogeneity on the wettability
properties of surfaces. As a result of surface chemical hetero-
geneity, θe, θa, and θr, values are measured differently on the
fiber surfaces, and the results are reported in Table 2. Contact
angle hysteresis, CAH, is defined as the difference between
advancing and receding contact angles on a surface, and one
of the main reasons of CAH is the chemical heterogeneity of
the surface. CAH can also be calculated in terms of cosine of
contact angles; Δcosθ = cosθr − cosθa.
1762 Colloid Polym Sci (2018) 296:1759–1766

Fig. 2 SEM and measured water

drop contact angle images of (a)
PVAc, (b) EVA-40, (c) EVA-33,
(d) EVA-28, and (e) EVA-25
electrospun fibers

PVAc is a hydrophilic polymer due to the presence of hy- content causes a decrease in water CA values, in all copolymer
drophilic vinyl acetate (VAc) groups in the structure. In case of films [51, 52]. Because surface roughness is introduced while
flat PVAc films, water θe value of approximately 60° is mea- preparing fibers, PVAc fiber surfaces have shown hydropho-
sured on the film surfaces [51, 52]. EVA copolymers contain bic behavior with a water CA of 134°, while EVA copolymer
both hydrophilic VAc and hydrophobic ethylene groups in fiber surfaces were exhibiting superhydrophobic behavior and
their structure. Depending on the composition of the copoly- water CA on all EVA copolymer fibers varied between 150°
mers, degree of hydrophilicity varies; the increase in VAc and 160°, depending on the copolymer composition.
The presence of hydrophobic ethylene groups in the copol-
Table 2 θe, θa, θr, and contact angle hysteresis (CAH) values of fiber
ymer structure causes an increase in the measured water CA
surfaces values due to weaker adhesion interactions between the hy-
drophobic ethylene groups and water molecules. The increase
(Co)Polymer θe (°) θa (°) θr (°) Δcosθ in VA% content (from 25 to 100 wt.% VA) in the composition
PVAc 134 146 114 0.422
of the copolymer fibers has caused a decrease in water CA
EVA-40 150 158 140 0.161
values of the surfaces (Fig. 3). The reason for this decrease is
EVA-33 155 161 143 0.147
due to the presence of higher amount of hydrophilic VA
groups on the fiber surfaces. When a water drop is put on
EVA-28 156 163 140 0.190
the fiber surface, restructuring of hydrophilic VA groups to-
EVA-25 160 163 152 0.090
wards the water drop occurs, and this results in a strong
Colloid Polym Sci (2018) 296:1759–1766
Fig. 3 Variation of θe values of fibers with the change of VA% contents
adhesion between water molecules and the hydrophilic
VA groups. Therefore the measured water CA values
decrease with the increase of VA% content in the copolymer
structure.
Both surface roughness and chemical heterogeneity cause
variations in θe, θa, and θr values of the same surface; there-
fore, contact angle hysteresis (Δcosθ) is calculated for all fiber
surfaces. Surface chemical heterogeneity increases with the
increase of VA contents in the copolymer composition. As
can be seen from Fig. 4, the increase in VA% content of
EVA copolymers has caused an increase in the calculated
Δcosθ values. PVAc homopolymer fibers exhibited the
highest Δcosθ, and this can be due to the higher roughness
on PVAc fibers, rather than EVA copolymers. In addition,
hydrophilic parts of both PVAc homopolymer and EVA co-
polymers may cause the water drop to be pinned on the sur-
faces; therefore, higher Δcosθ values have been calculated for
the copolymers, even in case of superhydrophobicity that
Fig. 4 Variation of contact angle hysteresis (Δcosθ) values versus VAc%
content
1763
corresponds low contact angle hysteresis [53, 54], with the
increase of VA contents.
Optical properties
Transmittance curves of PVAc homopolymer and EVA copol-
ymer fibers were measured by using UV-vis spectroscopy in
order to investigate the interaction of light with the prepared
fibers (Fig. 5a). As shown in Fig. 5a, PVAc homopolymer
fiber displayed a poor transparency around 5%.
Transmittance value of EVA-25, EVA-28, EVA-33, and
EVA-40 copolymers fibers was determined around 85%,
65%, 15%, and 10%, respectively. These results clearly indi-
cated that transparency of copolymer fibers containing 33 and
40% vinyl acetate (VAc) was decreased sharply, and they have
shown a poor transparency with the increase of VAc content in
copolymer matrix. When the transmittance properties of VAc
homopolymer and ethylene vinyl acetate (EVA) copolymers
were compared, it was found that EVA copolymers have
showed almost the same optical transmission as glass [55].
VAc content in the EVA copolymer matrix also affected its
properties, and copolymer structure was tend to be amorphous
and rubbery at high amounts of VAc [56]. As a result of these
properties, transparency of EVA copolymer was decreased
with the increase of VAc content, and this was due to the
amorphous behavior of VAc. At lower VAc contents, such as
25 wt.%, EVA copolymers had improved transmittances, and
this was due to the higher concentration of crystalline ethylene
content within the copolymer structure.
Figure 5b shows the relationship between light transmit-
tance values and VAc content at the visible region (700 nm).
At lower VAc contents (e.g., EVA-25 and EVA-28), copoly-
mer had shown a good transparency property whereas with the
increase of VAc content in copolymer (more than 28 wt.%),
transparency was decreased, and EVA copolymers have be-
come more opaque. This behavior can be explained as a result
of the amorphous properties of VAc polymer.
Fluorescence spectra of PVAc and EVA copolymer fibers
are given in Fig. 6. Emission intensity values of PVAc, EVA-
25, EVA-28, EVA-33, and EVA-40 were determined as 33, 69,
59, 53, and 47, respectively. According to these results, PVAc
has the lowest emission intensity value and emission intensity
of the copolymers decreased with the increase of vinyl acetate
(VAc) contents in copolymer matrix due to the decrease in the
crystallinity of copolymer at higher amounts of VAc.
Moreover, fluorescence property was directly proportional to
the crystallinity of the copolymer, and crystalline materials
have higher fluorescence intensities than amorphous materials
[57]. Our samples have shown compatible results with the
findings in the literature. At lower VAc contents, copolymers
have shown more crystalline behavior, and their emission in-
tensities were higher when compared to the ones with lower
VAc contents (Fig. 6).
1764 Colloid Polym Sci (2018) 296:1759–1766

Fig. 5 (a) Transmittance curves

of PVAc and EVA copolymers (b)
relationship between VAc
contents and the transmittance
values at 700 nm

Conclusion

PVAc homopolymer and EVA copolymer fibers with varying

Fig. 6 Fluorescence spectra of PVAc homopolymer and EVA copolymers
VAc contents were prepared by electrospinning method to
investigate the wettability and photophysical properties. At
higher VAc contents, copolymer fibers were successfully pre-
pared; however, when VAc content was decreased below
28 wt.%, it was difficult to obtain fibers without any beads.
Due to the increase in ethylene content in copolymer compo-
sition, and thus at lower VAc contents, crystalline behavior of
ethylene groups has caused to form beaded structures instead
of fibers.
When the effect of copolymer composition on the wettabil-
ity of the fibers was investigated, it was found that the increase
in VAc content has caused a decrease in water CA values due
to the reorientation of hydrophilic VAc groups towards the
Colloid Polym Sci (2018) 296:1759–1766
surface. Water CA values of EVA copolymers varied from
150° to 160° with the decrease of VAc content from 40 to
25 wt.%. While all EVA copolymer fibers were exhibiting
superhydrophobicity, PVAc homopolymer has shown hydro-
phobic behavior with water CA of 134°.
Photophysical properties of PVAc homopolymer and EVA
copolymers with varying VAc contents were also investigated
by using UV-Vis and fluorescence spectroscopies.
Transparency and emission intensities of EVA copolymers
were decreased with the increase of VAc contents in copoly-
mers matrix due to the decrease in the crystallinity of the
copolymers, and copolymer structure was tend to be amor-
phous and rubbery at high amounts of VAc.
Funding This research did not receive any specific grant from funding
agencies in the public, commercial, or not for profit sectors.
Compliance with ethical standards
Conflict of interest The authors declare that they have no conflict of
interest.
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