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Research Journal of Textile and Apparel
Surface properties of radio frequency plasma treated wool and denim fabrics
Ahmed Hala, Gozde Yurdabak Karaca, Esin Eren, Lutfi Oksuz, Ferhat Bozduman, Melek Kiristi, Ali Ihsan Komur, Ali Gulec,
Aysegul Uygun Oksuz,
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To cite this document:
Ahmed Hala, Gozde Yurdabak Karaca, Esin Eren, Lutfi Oksuz, Ferhat Bozduman, Melek Kiristi, Ali Ihsan Komur, Ali Gulec,
Aysegul Uygun Oksuz, "Surface properties of radio frequency plasma treated wool and denim fabrics", Research Journal of
Textile and Apparel, doi: 10.1108/RJTA-02-2016-0003
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http://dx.doi.org/10.1108/RJTA-02-2016-0003
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Surface properties of radio frequency plasma treated wool and
denim fabrics
ABSTRACT
Downloaded by Cornell University Library At 07:02 16 May 2017 (PT)
The effects of hydrochloric acid (HCl), hydrazine, methyl methacrylate (MMA), styrene and
hexamethyldisiloxane (HMDSO) treatment by radio frequency (rf) plasma grafting on surface
properties of wool and denim fabrics were investigated. During plasma treatments, processing time
was varied under optimized plasma conditions (50 W, rf: 13.56 MHz). All fabrics were
comprehensively investigated by means of scanning electron microscopy-energy dispersive X-ray
spectroscopy (SEM-EDS) and contact angle measurements. Our experimental data show that the rfplasma processing has an important effect on the wettability properties of wool and denim fabrics. The
results indicated that HCl plasma treatment significantly improves the hydrophilicity of wool and
denim fabrics.
Keywords: Surface modification, wool, denim, rf plasma
1. Introduction
Plasma has diverse applications in many
branches of science and technology, including
the production of many modern household
objects [Plasma, 2001]. Plasma is a mixture of
ions, electrons, and neutral particles (atoms,
free radicals or molecules), which give it a
distinctive potential for surface modification
[Kale & Desai, 2011]. Plasma technology can
be viewed as a low-cost, rapid processing, and
eco-friendly technology [Shadi, 2014]. Thus,
plasma technology also provides several
advantages over conventional chemical
processes. Plasma technology has been used in
many areas such as electronics, manufacturing,
biomedical devices, thin film technology and
automotive
[Kale
&
Desai,
2011].
Additionally, plasma provides efficient, fast,
and low cost processing technique for coating,
painting, whitening, and other processes
particularly in the textile industry [Prysiazhny,
2013]. Non-thermal plasmas are especially
suitable for textile processing because most
textile materials are heat sensitive polymers
[Morent et al., 2008]. The textile industry is
moving toward the application of waterless or
low-water-based processing technologies for
ecological reasons [Samanta et al, 2014].
Plasma treatment has diverse effects depending
on the experimental conditions including
cleaning (removal of contaminants from the
surface), etching (changes in surface roughness
and morphology) and functionalization
(production of new functional groups at the
surface) [Peršin et al., 2012], this allows it to
provide desired properties on targeted
application areas such as less shrinkage for
wool or improved hydrophobic/hydrophilic
coatings [Canal et al., 2007]. To evaluate the
improvement in water uptake of polyester and
acrylic fabrics obtained by plasma treatment,
the capillary rise method was applied and
wettability of samples were investigated
[Ferrero, 2003]. In addition, hydrophilizations
of cotton fabrics were developed by oxygen
plasma treatment [Poll et al., 2001]. Another
study for surface modification using different
plasma gases exposed wool and cotton fabrics
to a low temperature plasma caused changes in
surface roughness [Sun & Stylios, 2006]. The
effect of plasma treatments on the surface
properties of textile fibers, air plasma and
dichlorodifluoromethane (DCFM) plasmas
were studied. Air plasma produced enhanced
water wicking, DCFM plasma resulted in
producing
a
highly
water-repellent,
hydrophobic surface [Bhat et al., 2011].
Plasma treatment affects/modifies only the
material surface without any molecular
fragmentation at the inner layers [Poll et al.,
2001]. Wettability is one of the important
features for many applications such as dyeing,
finishing and detergency [Gotoh & Yasukawa,
2010]. As a result of the plasma modifications,
wettability of the textiles can be firmly boosted
because of the increased amount of functional
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groups on the surface such as –COOH, -OH
and -NH2 [Morent et al., 2008]. Plasma
treatment influenced the surface topography,
which further increases the impact of the
surface chemistry on the contact angle.
Hydrophilization is typically temporary, and
either a partial or whole hydrophobic recovery
is generally observed [Jokine et al., 2012]. A
variety of configurations of plasma processing
such as atmospheric-pressure plasma and lowpressure (vacuum) plasma have been used to
modify textile surfaces by generating active
species of plasma on the surface. Non-thermal
radio-frequency (rf:13.56 MHz) powered
plasma sources provide advanced control for
surface properties and good stability of fabrics
at low cost [Radetic et al., 2009].
Among these techniques, atmospheric pressure
rf plasma systems are widely used for textile
surface modifications because of their rapid
and efficient processing. Additionally, it is
environmentally friendly since it saves water
and energy [Park & Koo, 2014]. On the other
hand, vacuum plasma provides easier control
of the parameters such as air permeability,
moisture and the elimination of the volatile
toxic chemicals for the treatments [Samanta et
al., 2012].
2. Materials and methods
2.1 Materials
Denim and Wool fabrics were obtained from
Middle Anatolia T.A.S. Kayseri / Turkey and
YUNSA T.A.S. Tekirdag / Turkey.
Hexamethyldisiloxane (HMDSO, 98.5%),
Styrene (99%), and Hydrazine (% 98) were
purchased from Sigma-Aldrich Chemistry.
Methlymethacrylate (MMA, 99%) and
Hydrochloric acid (HCl, 37%) were received
from Merck-Schuchardt and Riedel-deHaen,
respectively.
2.2 Low Pressure RF Plasma Treatment
In-situ plasma treatments of denim and wool
using different chemicals were carried out by
the homemade Plus plasma capacitively
coupled plasma (RF-CCP) reactor (Fig. 1). The
upper electrode was powered with 13.56 MHz
rf voltage while the bottom electrode was
grounded.
The aim of this study is to investigate the
surface properties of rf plasma modified denim
and wool fabrics, comparatively. The
hydrophobic and hydrophilic properties of
denim and wool fabrics were improved using
different chemicals such as hydrazine, methyl
methacrylate (MMA), styrene, hydrochloric
acid
(HCl),
and
hexamethyldisiloxane
(HMDSO) depending on their potential
applications. Wettability properties of denim
and wool fabrics were studied with different
chemicals by time intervals then surface
properties were investigated by contact angle
measurements, scanning electron microscopyenergy dispersive spectroscopy (SEM-EDS).
The results showed that rf plasma processing
has significant effect on the targeted fabrics.
Fig. 1. Rf plasma setup.
Denim and Wool substrates were prepared in
4x2 cm2 dimensions and placed in the quartz
glass plasma vacuum reactor. Denim and wool
fabrics were treated with HCl, hydrazine,
styrene, MMA and HMDSO vapors in the
vacuum plasma reactor in Fig. 1. Plasma
treatment time was 15, 30 and 45 minutes in
optimized plasma conditions (50 W and
rf:13.56 MHz). The abbreviations of all fabrics
are given in Table 1.
2
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Table 1. The abbreviations of all wool
(WF) and Denim (DN) fabrics
2.3 Instrumental studies
Surface morphology and elemental analysis of
the samples were examined using SEM-EDS
system, Tescan Vega II L Su and Oxford
Swift. Contact angle measurements were
examined by Sessile drop method (Clear View
Instruments). A light source was kept behind
droplet to enhance the boundary of the droplet
for the precise measurement of the contact
angle.
Sample
Chemical
Treatment
Plasma
treatment
time (min)
WF, DN
untreated
-
WF,DNHCl-15
HCl
15
WF,DNHCl-30
HCl
30
3. Results and Discussion
WF,DNHCl-45
HCl
45
3.1 SEM Results
WF,DNHDMSO-15
HMDSO
15
WF,DNHDMSO-30
HMDSO
30
WF,DNHDMSO-45
HMDSO
45
WF,DNHYD-15
Hydrazine
15
WF,DNHYD-30
Hydrazine
30
WF,DNHYD-45
Hydrazine
45
WF,DNMMA-15
MMA
15
WF,DNMMA-30
MMA
30
WF,DNMMA-45
MMA
45
WF,DNSTY-15
Styrene
15
WF,DNSTY-30
Styrene
30
WF,DNSTY-45
Styrene
45
Plasma is a partially ionized gas that contains
ions, electrons, and other neutral species at
many different energy levels. When energized
by an electrical field, free radicals, ions, and
atoms are formed that can interact with solid
surfaces that have been placed in the plasma
(Ramos, Runyan, and Christensen, 1996).
SEM images of plasma treated and untreated
wool fabrics are shown in Fig. 2. Longitudinal
striation reveals the fibril structure of the
fibers. The interstitial space of textile fiber
increased on WF-HDMSO-45 fabric (Fig. 2c).
Therefore, it can provide an easy pathway for
the liquid to enter the fibers resulting in
enhanced
hydrophilicity
[Navaneetha
Pandiyaraj & Selvarajan, 2008]. Fig. 2e show
the surface morphology of the MMA plasma
treated wool fabric by different time. After
plasma treatment pore size and roughness of
the wool fibers increased significantly (Fig. 2e)
and resulted in increments of hydrophilic
surface property. The surface of styrene
modified wool (Fig. 2f) showed smoother
morphology by increasing treatment time.
Wool fibers possess a scale-like cuticle on the
cortex along the fiber length [Zimmerman et
al., 2011]. The external surface of wool fiber
contains some boundaries such as escarpments
[Kan, 2007]. After plasma treatment, the
escarpments were slightly lifted in fiber
surface. But, there was no severe damage, i.e
complete scale removal on all plasma treated
wool fiber surface.
3
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Fig. 2. SEM images of WF (a), WF-HCl-15
(b), WF-HDMSO-45 (c), WF-HYD-45 (d),
WF-MMA-45 (e), WF-STY-30 (f).
Fig. 3. SEM images of DN (a), DN-HCl-15
(b), DN-HDMSO-15 (c), DN-HYD-15 (d),
DN-MMA-45 (e), DN-STY-30 (f).
Fig. 3 shows the variation in the surface
morphology of plasma-treated and untreated
denim fabrics. As seen in Fig. 3b, HCl-treated
denim fabrics displayed rougher surface
compared to the untreated one (Fig. 3a). As
shown the porous areas of plasma treated
denim fabrics especially DN-HCl-15 have
been partially removed. Fig. 3b shows that the
size coverings were broken severely after
plasma treatment. Presumably, the size film or
particles among fibers and/or coated on the
denim fabric fibers were physically bombarded
and chemically modified via the active and
high energetic plasma species, and then
removed partially via a direct gas vaporization,
or even took away via plasma gas after an
ablation, which resulting in the broken of the
size covering (Wang et al., 2013). The surface
roughness of DN-HMDSO do not change
effectively by plasma treatment time (Fig. 3c).
Hydrazine modification improved roughness of
the fiber surface, facilitating hydrophilicity
(Fig. 3d). MMA treatment at 45 minute, it was
observed that spaces between denim fibers do
not change. SEM images of styrene treated
denim (Fig. 3f) show a smooth fiber surface.
After plasma treatment, each fabric showed
different smooth and rough surface because of
different surface modification on plasma
treated fabric (Nithya et al., 2011, Pandiyaraj
and Selvarajan, 2008). Plasma treatment etches
the surface of fabric and induces both physical
changes due to the etching effect of plasma
species on the fabrics and chemical changes
due to the formation of polar groups and free
radicals on the fabric surface (Nithya et al.,
2011). The formation of polar groups such as
C=O group on fabric surface and physical
etching of the fabric surface are two important
factors
affecting
hydrophobicity
and
hydrophilicity of the fabric (Nithya et al.,
2011).
Morphology changes can cause wettability
changes, but the wettability changes produced
by this modification are small. Plasma
oxidation reactions produce oxygen-containing
functional groups (OOH, OH, CO), which are
attached to the surface. These functional
groups form and play an important role in
increasing the hydrophilic properties of the
fabrics (Sun and Stylios, 2006).
4
wool fabrics due to the abrupt absorption of the
water drops. Plasma etching has an important
effect on roughening of fiber surfaces and
increasing the surface hydrophilicity [Ma &
Hill, 2006]. The decrease of the MMA
modified contact angles with increasing
plasma time lead to an associated variation of
the surface tension of wool fabric that allow it
to have a penetration of the water drop in the
wool fabric and the consequent hydrophilic
behavior [Correia et al., 2015].
The above result is consistent with hydrazine
plasma modification. However, there is an
increase in contact angle for WF-STY fabrics
due to the other modificated wool fabrics with
increasing plasma treatment time. STY plasma
etching did not induce the hydrophilicity of
wool fabric.
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3.2 EDS and Contact angle results
EDS and contact angle measurement results of
wool fabrics are given in Table 2 and Fig. 4(af). Elemental analysis results of HDMSOtreated wool fabrics for different plasma
treatment times demonstrated the presence of
Si content on the fabric surface and also other
elements such as C, O, and S. The highest Si
element content was obtained for WFHDMSO-45 fabric. These results indicate that
increasing time of exposure in plasma there is
an increase of Si-O-Si, Si-(CH3)2 and Si-C
bonds relatively to untreated wool fiber. The
change in chemical composition for all fabric
can be attributed to plasma interaction with the
surface that leads to modification of its
chemical structure and morphology (Ji et al.,
2008). The fiber diameter of untreated WF
fabric was ~ 20µm. The fiber diameter of WFHDMSO-30 fabric decreases to ~ 19.7 µm.
The interstitial pore size of WF-HDMSO-30
was found to enhance with plasma (Nithya et
al., 2011). The fiber diameter shrinkage can be
due to elimination of the material from the
substrate surface, etching contaminant layer
via plasma application. Thus, the absence of
contaminant layer can tend to decrease the
contact angle value [Molina et al., 2015,
Pandiyaraj and Selvarajan, 2008].
Table 2. EDS and contact angle results of
untreated and treated wool fabrics
C
O
S
Si
Contact
Angle
Sample
(o)
Weight
Weight
Weight
Weight
%
%
%
%
WF
52.228
47.712
2.362
-
127
WF-HCl-15
64.776
32.022
3.202
-
0
41.413
31.545
0.998
26.044
101
WF-HYD-45
67.004
28.781
4.215
-
24
WF-MMA-45
66.758
29.747
3.494
-
77
WF-STY-15
64.809
31.312
3.880
-
62
WF-STY-30
72.135
24.470
2.996
-
98
WF-HDMSO-
Water contact angle for untreated wool is ~
127 o. This value is higher than that of treated
wool fabric due to the surface-bound fatty acid
layer and limited capacity to absorb water
[Carran et al., 2013]. Surface layer of wool,
which composes of specific exocuticle and
epicuticle features, is naturally hydrophobic.
due to the disulfide bonds in its structure
[Montazer et al., 2011].
As can be seen in Table 2, the contact angle
decreased after all plasma treatments compared
with the untreated wool fabric. Among all
wool fabrics, HCl treatment has the best
influence on the contact angle. The water
contact angle on HCl-treated wool fabric was
0o showing the superhydrophilicity function of
treated fabrics. HCl-treated wool fabric
absorbed the water drops very quickly,
indicating a superhydrophilic feature after
plasma treatment. Untreated wool does not
absorb the water drops when the contact angle
is about 127o. There is no observation for
contact angle measurements of HCl treated
45
5
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Fig. 4. Contact angle measurements of a) WF
b) WF-HDMSO-45 c) WF-HYD-45 d) WFMMA-45 e) WF-STY-15 f) WF-STY-30.
hydrazine, the presence of additional
hydrophilic functional groups (-NH2) also
induce
increased
moisture
absorption
(Zeronian and Collins, 1989). Si-C and C-H
bonds of the HMDSO monomers were caused
by plasma polymerization and it causes from
hydrophobic surface changes [Yoshinari et al.,
2009]. For MMA, it was chosen for
hydrophilic chemical for wool surface
modification [Lai, Shih, and Tsai, 1991].
EDS results of untreated denim fabrics reveal
that it consists mostly of C and O elemental
contents. For DN-HDMSO fabrics, Si content
increased with plasma exposure time (Table 3).
As seen from Table 3 and Fig. 5a, contact
angle for untreated denim fabric was 89o
(Table 3, Fig. 5a). Contact angle results of
HCl-treated denim fabrics were the same as
those of HCl-treated wool fabrics. When
plasma treatment time for DN-HDMSO fabrics
was increased from 15 to 45 min, contact angle
was increased to 122o (Fig. 5b, Table 3).
However, this value is higher than that of
untreated denim fabric. The water droplet
spread as soon as it fell, indicating hydrophilic
behavior caused by hydrazine plasma
treatment for 15 min (Fig.5c).
Plasma
treatments have an important effect on surface
tension contributing to the fabric wettability
and lead to dramatic changes of textile
properties [Hossain et al., 2006].
Table 3. EDS and contact angle results of
untreated and treated denim fabrics
Si
C
O
Weight %
Weight %
Sample
Weight
%
Contact
Angle
(o)
52.288
47.712
-
89
52.149
47.851
-
0
DNHDMSO-15
48.488
45.296
6.216
122
DN-HYD15
56.092
43.908
-
29
DN-MMA45
61.838
38.162
-
89
67.778
32.222
-
112
78.407
20.983
-
105
DN
DN-HCl-15
o
Contact angle value (89 C) of DN-MMA-45
does not indicate the wettability behavior of
the fabric after plasma treatment. As a result of
all plasma treatment on wool and denim fabric,
wetting properties of a solid surface are
alterable related to surface molecular structure
and the surface macroscopic properties
[Molina et al., 2001]. When fabrics exposed to
DN-STY-15
DN-STY-30
Fig. 5. Contact angle measurements of a) DN
b) DN-HDMSO-15 c) DN-HYD-15 d) DNMMA-45 e) DN-STY-15 f) DN-STY-30
6
Acknowledgement
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Conclusions
Authors gratefully acknowledge the 1509TUBITAK International Industrial R&D
Projects Grant Programme (Project No:
9110021) for financial support to this study
Plasma treatment is a useful method to
improve the surface properties of textiles, such
as enhancing surface roughness, formation of
power functional groups, as well as increasing
wettability, dyeing, printing and finishing
properties. Contact angle measurements show
that all chemicals except styrene have
increment hydrophilicity effect on wool fabric
surfaces. This behavior of styrene can be
attributed to polymerization of styrene on the
fibers. DN-STY fabrics indicate hydrophobic
behavior, unlike WF-STY fabric. HCl plasma
treatments were found to be most effective in
improving the hydrophilicity of denim and
wool fabrics. Therefore, we definitely believe
that the HCl plasma treatments on both wool
and denim fabric surface are promising
processes for textile finishing and dyeing
areas.
The contact angle for water on the wool and
denim surface decrease after the fabrics were
treated with HCl plasma, fabrics surface was
exposed to plasma with HCl as monomer,
which is probably attributed to the increase in
the amount of hydroxyl of fabrics surface.
Also, contact angle was found to decrease by
soaking in HCl by plasma modification.
7
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2012, ‘Oxygen and nitrogen plasma
hydrophilization
and
hydrophobic
recovery of polymers’, Biomicrofluidics,
vol. 6, 016501.
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