Cellulose (2010) 17:417426

DOI 10.1007/s10570-009-9369-y

Chemical and physical analysis of cotton fabrics

plasma-treated with a low pressure DC glow discharge
S. Inbakumar R. Morent N. De Geyter
T. Desmet A. Anukaliani P. Dubruel C. Leys

Received: 26 May 2009 / Accepted: 4 October 2009 / Published online: 22 November 2009

Springer Science+Business Media B.V. 2009

Abstract This paper focuses on the modification of
cotton fabrics using a low pressure DC glow
discharge obtained in air. The influence of different
operating parameters such as treatment time, dis-
charge power and operating pressure on the chemical
and physical properties of the cotton fabrics is studied
in detail. Surface analysis and characterization of the
plasma-treated cotton fabrics is performed using
vertical wicking experiments, X-ray photoelectron
spectroscopy (XPS), scanning electron microscopy
(SEM) and weight loss measurements. The cotton
fabrics show a significant increase in wicking
behaviour; an effect which increases with increasing
treatment time, increasing discharge power and
increasing pressure. Results also show that low
pressure DC glow treatment leads to surface erosion
of the cellulose fibres, accompanied by an incorpo-
ration of oxygen-containing groups (CO, C=O,
S. Inbakumar
A. Anukaliani
Department of Physics, Kongunadu Arts and Science
College, Coimbatore 641029, Tamilnadu, India
R. Morent (&)
N. De Geyter
C. Leys
Research Unit Plasma Technology (RUPT), Department
of Applied Physics, Faculty of Engineering, Ghent
University, Jozef Plateaustraat 22, 9000 Ghent, Belgium
e-mail: Rino.Morent@Ugent.be
T. Desmet
P. Dubruel
Polymer Chemistry and Biomaterials Research Group,
Department of Organic Chemistry, Faculty of Sciences,
Ghent University, Krijgslaan 281, 9000 Ghent, Belgium
OCO and OC=O) on the cotton fibres. The DC
glow treatment has thus the potential to influence not
only the chemical but also the physical properties of
cotton fabrics and this without the use of water or
chemicals.
Keywords Glow discharge
Cotton
Wicking

X-ray photoelectron spectroscopy
Process
parameters
Introduction
Cotton is the most important textile fibre in the world
despite the inroads made into its market by synthetic
fibres (Johansson 2007). Cotton is mainly composed
of cellulose with some non-cellulosic components
including proteins, waxes, pectic substances, organic
acids, sugars, (Karahan and Ozdogan 2008). Cellu-
lose has traditionally been modified through reactions
of the various hydroxyl groups, leading to esterifica-
tion and etherification. In the last decades, non-thermal
(or cold) plasmas are gaining popularity as a cellulose
modification technique since this technique varies
significantly from the traditional esterification and
etherification routes (Johansson 2007). A non-thermal
plasma contains activated species, such as electrons,
ions, radicals, photons, which are able to abstract
hydrogen from either carbon or oxygen atoms present
on the cotton surface. In this way, cellulose can be

123
418
oxidized, reduced and/or substituted in new, unique
ways (Johansson 2007).
In the last decades, the application of cold plasmas
to modify the surface properties of textile materials is
experiencing rapid growth (Chen et al. 2008; De
Geyter et al. 2006; Morent et al. 2008; Samanta et al.
2009). Non-thermal plasmas are able to alter the
physico-chemical properties of a polymer surface: the
main effects of interaction between active plasma
species and polymeric surfaces is breaking polymer
molecular chains, inducing new functional groups
and altering morphological properties (Caiazzo et al.
1996; Keil et al. 1998; Toufik et al. 2002). Some of
the possible effects include improved hydrophilic
properties (De Geyter et al. 2006; Pandiyaraj and
Selvarajan 2008; Vesel et al. 2008), an improved
adhesion to coatings and to polymer matrices (Liston
1989; Liston et al. 1993; Dumitrascu and Borcia
2006; Zhang et al. 2009), an improved dye ability
(Jocic et al. 2005; Ren et al. 2008), induced
hydrophobic properties (Hodak et al. 2008; Leroux
et al. 2008), . Apart from creating interesting
textile properties, plasma processing is a rapid and
environmentally friendly technique producing virtu-
ally no waste (Verschuren et al. 2007; Yip et al.
2002). Moreover, plasma treatment only changes the
uppermost layers of a material surface without
interfering with the bulk properties (Poll et al. 2001).
Plasma modification of cotton fibres and textiles
has been extensively studied in numerous scientific
papers (Karahan and Ozdogan 2008; Pandiyaraj and
Selvarajan 2008; Samanta et al. 2009; Sun and Stylios
2004; Ward and Benerito 1982), however, there is a
lack of literature describing the effects of different
process parameters such as discharge power, operat-
ing pressure, exposure time, on the chemical and
physical properties of cotton textiles. Therefore, in the
present work, the effect of different operating param-
eters on cotton plasma modification will be studied in
detail. Plasma treatment will be performed on cotton
woven fabrics using a low pressure glow discharge
operated in air in order to improve their hydrophilic-
ity. This improved water wetting is essential for
effective processing (dyeing and finishing) and main-
tenance (cleaning) of cotton assemblies involving
aqueous media, because it facilitates the transport
of active reagents between and into the fibres (Topal-
ovic et al. 2007). An evaluation of the hydrophilic
behaviour will be performed using wicking rate
123
Cellulose (2010) 17:417426
experiments. The untreated and plasma-treated cotton
fabrics will also be characterized using X-ray photo-
electron spectroscopy (XPS) in order to correlate the
hydrophilic properties with the chemical composition
of the cotton surfaces. To gather information on the
plasma-induced physical changes, weight loss mea-
surements and scanning electron microscopy (SEM)
experiments will be carried out. The above-mentioned
experiments will be performed for selected plasma
exposure times, operating pressures and discharge
powers in order to study the influence of these plasma
parameters on the hydrophilic behaviour of cotton
fabrics.
Materials and methods
Materials
Commercially available woven grey cotton (warp
count = 29, weft count = 23), supplied by the South
Indian Textile Research Association (Coimbatore
India) is used in this study. Before plasma treatment,
the grey cotton samples were scoured by treating
them in a 2% aqueous NaOH (Nice Chemicals
India) solution for 2 h at 95 C followed by washing
in distilled water and drying in air. This pre-treatment
is used to remove waxes, pectins and other impurities
from the fabric surface (Chung et al. 2004).
Non-thermal plasma treatment
The plasma system used in this paper is schematically
shown in Fig. 1 and consists of a cylindrical plasma
chamber (length 0.5 m, diameter 0.25 m), a vacuum
pumping system (VS-114D, Hindhivac India) and a
DC power supply (Devi Electric Corporation
India). Inside the vacuum chamber, plasma is gener-
ated between two copper electrodes with a diameter
of 8 cm and a thickness of 1 mm. One electrode is
permanently fixed, the other one is variable in height
and the distance between both electrodes is set at
3 cm. Before putting the fabric sample into the
system, the chamber is first cleaned with distilled
water and afterwards with acetone. After this clean-
ing step, a cotton fabric sample is fixed in a sample
holder and inserted into the plasma chamber by using
an adjustable rod. For all experiments performed in
this paper, the cotton fabric is placed parallel with the
Cellulose (2010) 17:417426
Fig. 1 Schematic diagram of plasma system (1anode; 2
cathode; 3cotton sample; 4sample holder; 5plasma
chamber; 6pumping equipment; 7needle valve; A
ammeter; PPirani gauge)
electrodes at 1 cm from the cathode. This distance
was found to be adequate to avoid thermal alteration
of the fabric during plasma processing. The plasma
chamber is firmly closed after introduction of the
cotton fabric and the vacuum pumping system
consisting of a rotary vacuum pump and a diffusion
pump is switched on. The pressure inside the plasma
chamber is measured using a pirani gauge P
(A6STM-D Hindhivac India) and during plasma
processing, the desired pressure (0.030.07 kPa) is
maintained by using a needle valve. After reaching
the preset pressure in the plasma chamber, the DC
power supply is switched on applying the desired
voltage (250400 V) between both electrodes. In
order to calculate the discharge power, the discharge
current is measured using an ammeter A (OSAW
India) connected between the lower electrode and the
DC power supply. The typical operating parameters
for the cotton plasma treatments performed in this
work are shown in Table 1.
Table 1 Typical plasma operating parameters
Discharge potential (V) 250400 V
Discharge current (I) 719 mA
Pressure (P) 0.030.07 kPa
Exposure time (t) 110 min
Electrode separation (d) 3 cm
Gas Atmospheric air
419
Wicking rate experiments
For surfaces with a closed structure, for example
polymer foils, the surface energy can be derived from
the measurement of the static contact angle of small
droplets of distilled water or other liquids (like pure
glycerin) on the treated surface (Temmerman et al.
2005). However, for surfaces with a more open
structure, like non-woven and woven fabrics, contact
angle measurements are difficult due to the roughness
and porous structure of the fabrics. Therefore, in this
work, the hydrophilic behaviour of the untreated and
plasma-treated cotton samples will be determined by
performing wicking rate measurements based on the
standard DIN 53 923 (EDANA 10.1-72). A cotton
fabric strip (2 cm 9 7 cm) is suspended vertically
with the lower end dipped in a water-dye liquor (1 ml
Royal Blue (Industrial Research Corporation India)
dissolved in 100 ml distilled water) and as a result, a
spontaneous wicking occurs due to capillary forces
(Harnett and Mehta 1984; Wong et al. 2001; Ferrero
2003). The blue coloration of the dye solution on the
cotton fabric clearly indicated the capillary rise
height and a ruler (in millimetres) assembled along
the cotton strip enables the height measurements.
Height readings were made at time intervals of 30 s
in the first 3 min and at time intervals of 60 s for
longer wicking times. Since natural materials are very
variable by nature, the capillary rise results shown in
this work are the average of 10 independent mea-
surements performed on cotton samples treated under
the same conditions. Moreover, also the standard
deviation on these average values will be reported in
the following sections.
XPS measurements
XPS analysis is used to determine the chemical
composition of the untreated and plasma-modified
cotton samples in order to correlate the hydrophilic
behaviour of the samples with the chemical compo-
sition of their surfaces. XPS measurements are carried
out on a S-Probe monochromatized XPS spectrometer
of Surface Science Instruments (VG), using mono-
chromatic Al Ka-radiation (hm = 1486.6 eV). The
angle between the photoelectron emission direction
and the plane of the sample is kept constant at 45.
The pressure in the analyzing chamber is maintained
at 1 9 10-9 Pa or lower during analysis and the size
123
420
of the analyzed area is 250 lm 9 1,000 lm. The
high-resolution spectra are collected in the constant
analyzer energy mode and the value of 285.0 eV of
the C1s core level is used for calibration of the energy
scale. Curve fitting of the C1s peak is performed using
CasaXPS software.
Weight loss experiments and SEM measurements
Upon exposure to plasma, some degradation reactions
could potentially be initiated on the cotton surfaces
due to ion and electron bombardment (Inagaki et al.
2004). As a result, weight loss of the cotton fabrics
and morphological changes of the fibre surfaces can
occur. In order to examine the etching effect of the
low pressure glow discharge on the cotton fabrics,
weight loss experiments and SEM measurements are
performed. To obtain the weight loss percentage of the
plasma-treated cotton fabrics, the weight of the
samples is measured before and immediately after
plasma exposure using a Shimadzu AUY220 analytic
balance. The weight loss percentage is then calculated
according to the following equation:
Wut  Wpt
Wloss % 100
Wut
where Wut and Wpt are the weight of the untreated and
plasma-treated samples respectively. The weight
measurements are repeated 10 times for each
plasma-treated sample in order to obtain an average
weight loss percentage.
In order to visualize the plasma-induced morpho-
logical changes on the fibre surfaces, SEM measure-
ments are performed using a Quanta 200F scanning
electron microscope (FEI Japan). Prior to SEM
investigation, the cotton samples were coated with a
thin layer of gold since non-conducting specimens
(such as polymers) will charge under electron
bombardment.
Results and discussion
Wicking rate results
Effect of exposure time
In a first series of experiments, the operating param-
eters pressure and discharge power are kept constant
123
Cellulose (2010) 17:417426
at 0.03 kPa and 4.2 W respectively, while the expo-
sure time is varied between 1 and 10 min. Figure 2
shows the evolution of the average wicking height as
a function of wicking time for cotton fabrics which
were plasma-treated at different exposure times. The
wicking height of the untreated cotton fabric remains
the same (i.e. zero) as a function of the wicking time
due to its poor wetting nature and is therefore not
presented in Fig. 2. This bad wicking behaviour of
the scoured untreated cotton fabrics can be explained
by the significant amount of non-cellulosic compo-
nents present on the scoured cellulose fibres, as will
be explained in detail in XPS results. Figure 2
clearly shows that initially the wicking height
increases fast with increasing wicking time for all
plasma-treated samples before levelling off at a
certain wicking time. For the upward wicking, it is
obvious that if the distance travelled by the liquid
becomes high enough, there will be a noticeable
effect of gravity on the flow rate, leading to a
reduction of wicking height increase. As seen in
Fig. 2, increasing the plasma exposure time leads to a
higher wicking rate. This observation suggests that
with increasing treatment time, the cellulose fibres
may become more hydrophilic since wettability is a
perquisite for wicking: a liquid that does not wet
fibres cannot wick into a fabric. Moreover, due to
plasma etching effects, the effective pore size present
in the plasma-treated cotton fabrics may increase and
adversely reduce the capillary pressure, thus increas-
ing the wicking ability (Sun and Stylios 2004; Wong
et al. 2001). Both of these aspects will be further
explored by performing weight loss, SEM and XPS
measurements in order to determine the chemical and
Fig. 2 Average wicking height as a function of wicking time
for cotton fabrics plasma-treated at different exposure times
(pressure = 0.03 kPa, discharge power = 4.2 W)
Cellulose (2010) 17:417426
physical properties of the plasma-treated cellulose
fibres.
Effect of discharge power
To study the influence of discharge power, a series of
experiments are performed at constant operating
pressure (0.03 kPa) and constant plasma exposure
time (6 min). To easily visualize the effect of
discharge power on cotton wettability, it is preferred
to present the average wicking height after 5 min of
wicking (H5min) as a function of discharge power
instead of presenting the wicking height as a function
of wicking time for various discharge powers.
Figure 3 shows the evolution of H5min as a function
of discharge power. Based on this figure, one can
assume that increasing the discharge power leads to
an enhanced wicking behavior of the cellulose fibres.
This can be explained by the fact that increasing the
discharge power results in an increase of the amount
of reactive plasma species. The presence of more
plasma species can lead to an increased fibre
wettability and/or an increased wicking ability due
to a more intense bombardment of active plasma
species.
Effect of operating pressure
In a final series of experiments, the influence of
pressure on the hydrophilicity of the plasma-treated
cotton fabrics is studied in detail in the pressure range
0.030.07 kPa. The pressure variation is limited to
this small range to ensure the stability of the DC glow
discharge and the discharge power and the plasma
Fig. 3 Average wicking height after 5 min of wicking (H5min)
as a function of discharge power (pressure = 0.03 kPa,
treatment time = 6 min)
421
Fig. 4 Average wicking height after 5 min of wicking (H5min)
as a function of operating pressure (discharge power = 4.2 W,
treatment time = 6 min)
exposure time are kept constant at 4.2 W and 6 min,
respectively. Figure 4 shows the evolution of the
average wicking height after 5 min of wicking (H5min)
as a function of operating pressure. As observed in
Fig. 4, increasing the plasma pressure in the range
0.030.07 kPa leads to an increase in cotton wicking
ability. It is known that while the electron energy (and
hence the average energy of the reactive plasma
particles) decreases with increasing pressure, its
density increases (Shi and Clouet 1992). The observed
wicking behavior is probably a result of these two
antagonist effects, however, since wicking proceeds
faster at higher pressures, it is likely that the density
increase dominates the energy decrease.
XPS results
XPS measurements are carried out to evaluate the
chemical composition of the untreated and plasma-
treated cotton fabrics. At first, low-resolution XPS
survey scans are performed to determine the percent-
ages of elements present at the cotton surfaces before
and after plasma treatment. As expected for cellulose
fibres, the main elements detected are carbon and
oxygen, since hydrogen cannot be detected using
XPS. Using area sensitivity factors, the oxygen-to-
carbon (O/C) atomic ratios were calculated for the
untreated fabric and fabrics plasma-treated at differ-
ent treatment times as shown in Table 2. The O/C
atomic ratio of the untreated cellulose fabric is 0.30,
while the value expected for pure cellulose is 0.83.
This observation indicates that the surface of the
untreated cotton fabric does not consist of pure
cellulose. The low O/C ratio is due to a considerable
123
422 Cellulose (2010) 17:417426

Table 2 O/C ratio of untreated and plasma-treated cellulose
fabrics (pressure = 0.03 kPa, discharge power = 4.2 W)
Treatment time (min) O/C ratio (%)
0 0.30
2 0.38
4 0.40
6 0.42
8 0.43
10 0.46
amount of carbon atoms without oxygen neighbours,
which should not be present in pure cellulose.
However, it is well known (Topalovic et al. 2007;
Chung et al. 2004; Karahan and Ozdogan 2008) that
laminar layers of waxes, proteins and pectin cover the
natural cotton fibres and since these layers mainly
consist of unoxidized carbon atoms, one can conclude
that waxes, proteins, are still present on the
cellulose fibres, even after NaOH pre-treatment. This
result is in agreement with the results of Mitchell
et al. (2005), who also observed the presence of non-
cellulosic components on scoured cotton fibres.
Table 2 also shows that with increasing plasma
exposure time, the O/C atomic ratio gradually
increases from 0.30 for an untreated sample to 0.46
for a sample plasma-treated for 10 min. This increase
suggests that new oxygen-containing groups are
formed on the cellulose fabrics after plasma treatment
in air. Since these oxygen groups have a polar
character, one can conclude that plasma treatment
increases the hydrophilicity of the cellulose fabrics,
which can contribute to the increased wicking
behaviour observed in Effect of exposure time. It
is also important to mention that the plasma modi-
fication does not lead to a significant increase in N/C
atomic ratio. Therefore, no nitrogen-containing func-
tional groups are introduced on the cotton surfaces

Fig. 5 C1 s peak of a
untreated cotton fabric and
b cotton fabric plasma-
treated for 10 min
(operating
pressure = 0.03 kPa,
discharge power = 4.2 W)

Table 3 Percentage of the

Treatment CC/CH (%) CO (%) C = O/OCO (%) OC=O (%)
different chemical groups
time (min)
present on the untreated and
plasma-treated cotton 0 72.8 18.3 7.3 1.6
fabrics
(pressure = 0.03 kPa, 2 65.4 21.2 10.1 3.3
discharge power = 4.2 W) 4 63.6 21.4 11.1 3.9
6 62.2 21.9 11.7 4.2
8 60.6 23.0 12.0 4.4
10 59.5 23.2 12.2 5.1

123
Cellulose (2010) 17:417426 423

during plasma treatment despite the abundance of

nitrogen present in the air plasma. These results
underlie the extreme reactivity of oxygen species
present in the air plasma compared to the nitrogen
species.
To obtain more detailed information, high-
resolution scans are performed on the C1s region for
all samples listed in Table 2 in order to determine the
types and relative amounts of the different carbon
oxygen bonds present on the surface. A detailed
analysis of the O1s peak is not performed, since it is
generally less useful. Figure 5 shows the C1s spectra
of the untreated cellulose fabric (a) and of the
cellulose fabric plasma-treated for 10 min (b). Both
C1s peaks can be decomposed into four components:
a component C1 at 285.0 eV due to CC and CH
bonds, a component C2 at 286.5 0.1 eV due to
CO bonds, a component C3 at 288.0 0.1 eV due
to C=O or OCO bonds and finally a component C4
at 289.0 0.1 eV due to OC=O bonds (Briggs
1990). Based on these high resolution C1s peaks, the
percentage of each chemical group present on the
cellulose fibres can be calculated and the obtained
results are presented in Table 3. It can be derived from
Table 3 that with increasing plasma treatment time,
the concentration of CC and CH groups decreases,
while the concentration of oxygenated carbon groups
(CO, C=O, OCO and OC=O) increases. The
higher amount of these polar oxygen-containing
groups yields a more polar and more wettable cotton
fibre surface, which in turn contributes to an increased
wicking ability, as observed in Effect of exposure
time.

Weight loss and SEM results

From the previous section, it can be concluded that

cellulose fibres become more hydrophilic after
plasma treatment due to the incorporation of oxygen-
containing functional groups. However, an increased
wettability is not the only effect that can be respon-
sible for the strongly increased wicking ability of the
samples after plasma treatment. As stated previously
at the end of Effect of exposure time, also physical
modifications caused by plasma etching could con-
tribute to the increased wicking ability. Therefore, in
this section, the physical modifications of the cellu-
lose fabrics are studied in detail using SEM and
weight loss measurements.
Fig. 6 SEM images of a untreated cotton fabric, b cotton
fabric plasma-treated for 4 min and c cotton fabric plasma-
treated for 10 min (discharge power = 4.2 W, operating
pressure = 0.03 kPa)
In order to visualize the plasma-induced morpho-
logical changes on the fibre surfaces, SEM mea-
surements are performed. Figure 6 shows (a) a SEM
image of the untreated cotton fibre, (b) a SEM image
of a plasma-treated cotton fibre with an exposure

123
424 Cellulose (2010) 17:417426

time equal to 4 min and (c) a SEM image of a
plasma-treated cotton fibre with an exposure time
equal to 10 min. The untreated cotton fabric consists
of cellulose fibres with a relatively smooth surface,
however, some grooves and cracks are already
present. After plasma treatment, the surface of the
cellulose fibres seems to become rougher with a
significant amount of tiny grooves and cracks, as
illustrated in Fig. 6b, c. Based on these SEM images,
one may conclude that the applied plasma treatment
etches the surface of the cotton fabrics. It should be
however highlighted that it is extremely difficult to
make a sound and justified conclusion based on
SEM images alone. The SEM images provided in
Fig. 6 show single fibres on local places of the
cotton fabric: other fibres in the untreated cotton
fabric seem to be as rough as the ones provided in
Fig. 6c, while fibres in the plasma-treated fabrics are
as smooth as the ones shown for the untreated
cellulose fabric. To confirm the etching behavior of
the discharge used in this paper, weight loss
measurements are performed. Table 4 shows the
average weight loss percentage for various plasma-
treated samples together with the calculated standard
deviations. Table 4 clearly shows that the weight
loss percentage increases with increasing treatment
time up to approximately 4.5% at a treatment time of
10 min. As a result, one can conclude with certainty
that the discharge used in this paper etches the
surface of the cotton fabrics. It is however very
difficult to know if the plasma removes the non-
cellulosic components from the cellulose fibres or if
the plasma etches the cellulose fibres themselves.
Most likely, a combination of both effects will take
place during plasma treatment.
This etching effect may be due to electron and ion
bombardment in addition to the contribution of
oxidative reactions with activated oxygen atoms to
degradation reactions (Inagaki et al. 2004). Table 4
also shows that the weight loss percentage increases
with increasing discharge power and increasing
operating pressure. This can be explained by the fact
that more plasma species can interact with the fabric
surface at higher discharge power and higher oper-
ating pressure. Taking into account the above men-
tioned results, one can conclude that the low pressure
DC glow discharge causes both chemical and phys-
ical modifications to the cellulose fibres, which both
attribute to the increased wicking behaviour after
plasma treatment.

Table 4 Average weight

Treatment Pressure (kPa) Discharge Average Standard
loss (%) of 10 cotton fabrics
time (min) power (W) weight loss (%) deviation (%)
plasma-treated with
different operating 1 0.03 4.2 1.68 0.08
parameters
2 0.03 4.2 2.11 0.05
3 0.03 4.2 2.70 0.10
4 0.03 4.2 3.00 0.07
5 0.03 4.2 3.34 0.06
6 0.03 4.2 3.64 0.11
7 0.03 4.2 4.20 0.05
8 0.03 4.2 4.39 0.03
9 0.03 4.2 4.48 0.04
10 0.03 4.2 4.56 0.03
6 0.04 4.2 4.00 0.11
6 0.05 4.2 4.35 0.03
6 0.06 4.2 4.43 0.33
6 0.07 4.2 4.64 0.34
6 0.03 2.1 2.91 0.05
6 0.03 2.6 3.43 0.05
6 0.03 5.6 4.08 0.07
6 0.03 7.6 4.35 0.06

123
Cellulose (2010) 17:417426
Conclusion
The primary aim of this study was to investigate the
effects of a low pressure DC glow discharge on the
chemical and physical properties of cotton fabrics.
The influence of different operating parameters, such
as treatment time, discharge power and operating
pressure on the plasma modification were studied in
detail using vertical wicking experiments. Results
have clearly shown that plasma treatment leads to a
significant increase in cotton wicking ability; an effect
which increases with increasing treatment time,
increasing discharge power and increasing operating
pressure. XPS measurements have demonstrated that
this enhanced wicking ability can be attributed to an
enhanced wettability of the cotton fibres since plasma
treatment introduces polar oxygen-containing groups
such as CO, C=O, OCO and OC=O groups on the
cotton fibres. However, in this paper, it is also shown
that not only chemical modifications but also physical
modifications contribute to the enhanced wicking
ability of plasma-treated cotton fabrics. Based on
SEM and weight loss measurements, it was shown
that the low pressure DC glow discharge etches the
surface of the cotton fabrics, an effect which also
increases with increasing treatment time, increasing
discharge power and increasing operating pressure.
As a concluding remark, one can state that plasma
treatment can be used as an effective method for
cotton pre-treatment with the advantage of low
application temperature, without the necessity of
any chemical substance, without any water consump-
tion and without imposing any alteration to the
interior part of the cellulose fibres.
Acknowledgments S. Inbakumar would like to thank the
Director of the Collegiate Education, Chennai 600 006,
Tamilnadu for providing a scholarship for a research study.
References
Briggs D (1990) Applications of XPS in polymer technology.
In: Briggs D, Seah MP (eds) Practical surface analysis,
volume 1: Auger and X-ray photoelectron spectroscopy,
2nd edn. Wiley, Chichester, pp 437484
Caiazzo F, Canonico P, Nigro R, Tagliaferri V (1996) Elec-
trode discharge for plasma surface-treatment of polymeric
materials. J Mater Process Technol 58:9699
Chen X, Yao L, Xue J, Zhao D, Lan Y, Qian X, Wang CX, Qiu
Y (2008) Plasma penetration depth and mechanical
425
properties of atmospheric plasma-treated 3D aramid
woven composites. Appl Surf Sci 255:28642868
Chung C, Lee M, Choe EK (2004) Characterization of cotton
fabric scouring by Ft-IR ATR spectroscopy. Carbohydr
Polym 58:417420
De Geyter N, Morent R, Leys C (2006) Surface modification of
a polyester non-woven with a dielectric barrier discharge
at medium pressure. Surf Coat Technol 201:24602466
Dumitrascu N, Borcia C (2006) Adhesion properties of poly-
amide-6 fibres treated by dielectric barrier discharge. Surf
Coat Technol 201:11171123
Ferrero F (2003) Wettability measurements on plasma treated
synthetic fabrics by capillary rise method. Polym Test
22:571578
Harnett PR, Mehta PN (1984) A survey and comparison of
laboratory test methods for measuring wicking. Text Res J
54:471478
Hodak SK, Supasai T, Paosawatyanyong B, Kamlangkla K,
Pavarajarn V (2008) Enhancement of the hydrophobicity of
silk fabrics by SF6 plasma. Appl Surf Sci 254:47444749
Inagaki N, Narushim K, Tuchida N, Miyazaki K (2004)
Surface characterization of plasma-modified poly(ethyl-
ene terephthalate) film surfaces. J Appl Polym Sci B 42:
37273740
Jocic D, Vilchez S, Topalovic T, Molina R, Navarro A,
Jovancic P, Julia MR, Erra P (2005) Effect of low-tem-
perature plasma and chitosan treatment on wool dyeing
with acid red 27. J Appl Polym Sci 97:22042214
Johansson K (2007) Plasma modification of natural cellulosic
fibres. In: Shishoo R (ed) Plasma technologies for tex-
tiles. Woodhead Publishing Limited, CRC Press LLC,
Cambridge, pp 247281
Karahan HA, Ozdogan E (2008) Improvements of surface
functionality of cotton fibres by atmospheric plasma
treatment. Fibres Polym 9:2126
Keil M, Rastomjee CS, Rajagopal A, Sotobayashi H, Bradshaw
AM, Lamont CLA, Gador D, Buchberger C, Fink R,
Umbach E (1998) Argon plasma-induced modifications at
the surface of polycarbonate thin films. Appl Surf Sci
125:273286
Leroux F, Campagne C, Perwuelz A, Gengembre L (2008)
Fluorocarbon nano-coating of polyester fabrics by
atmospheric air plasma with aerosol. Appl Surf Sci 254:
39023908
Liston EM (1989) Plasma treatment for improved bondinga
review. J Adh 30:199218
Liston EM, Martinu L, Wertheimer MR (1993) Plasma surface
modification of polymers for improved adhesiona crit-
ical review. J Adhes Sci Technol 7:10911127
Mitchell R, Carr CM, Parfitt M, Vickerman JC, Jones C (2005)
Surface chemical analysis of raw cotton fibres and asso-
ciated materials. Cellulose 12:629639
Morent R, De Geyter N, Verschuren J, De Clerck K, Kiekens
P, Leys C (2008) Non-thermal plasma treatment of tex-
tiles. Surf Coat Technol 202:34273449
Pandiyaraj KN, Selvarajan V (2008) Non-thermal plasma
treatment for hydrophilicity improvement of grey cotton
fabrics. J Mater Process Technol 199:130139
Poll HU, Schladitz U, Schreiter S (2001) Penetration of plasma
effects into textile structures. Surf Coat Technol 142:489
493
123
426
Ren CS, Wang DZ, Wang YN (2008) Improvement of the graft
and dyeability of linen by DBD treatment in ambient air. J
Mater Process Technol 206:216220
Samanta KK, Jassal M, Agrawal AK (2009) Improvement in
water and oil absorbency of textile substrate by atmo-
spheric pressure cold plasma treatment. Surf Coat Technol
203:13361342
Shi MK, Clouet F (1992) Study of the interactions of model
polymer surface with cold plasmas. II. degradation rate
versus pressure and gas flow rate. J Appl Polym Sci
46:20632074
Sun D, Stylios GK (2004) Effect of low temperature plasma
treatment on the scouring and dyeing of natural fabrics.
Text Res J 74:751756
Temmerman E, Akishev Y, Trushkin N, Leys C, Verschuren J
(2005) Surface modification with a remote atmospheric
pressure plasma: DC glow discharge and surface streamer
regime. J Phys D Appl Phys 38:505509
Topalovic T, Nierstrasz VA, Bautista L, Jocic D, Navarro A,
Warmoeskerken MMCG (2007) XPS and contact angle
study of cotton surface oxidation by catalytic bleaching.
Colloids Surf A 296:7685
123
Cellulose (2010) 17:417426
Toufik M, Mas A, Shkinev V, Nechaev A, Elharfi A, Schue F
(2002) Improvement of performances of PET track
membranes by plasma treatment. Eur Polym J 38:203209
Verschuren J, Kiekens P, Leys C (2007) Textile-specific
properties that influence plasma treatment, effect creation
and effect characterization. Text Res J 77:727733
Vesel A, Junkar I, Cvelbar U, Kovac J, Mozetic M (2008)
Surface modification of polyester by oxygen- and nitro-
gen-plasma treatment. Surf Interface Anal 40:14441453
Ward TL, Benerito RR (1982) Modification of cotton by
radiofrequency plasma of ammonia. Text Res J 52:256
262
Wong KK, Tao XM, Yuen WM, Yeung KW (2001) Wicking
properties of linen treated with low temperature plasma.
Textile Res J 71:4956
Yip J, Chan K, Sin KM, Lau KS (2002) Low temperature
plasma-treated nylon fabrics. J Mater Process Technol
123:512
Zhang CS, Chen P, Liu D, Wang BC, Li W, Kang XT (2009)
Aging behavior of PBO fibres and PBO-fibre-reinforced
PPESK composite after oxygen plasma treatment. Surf
Interface Anal 41:187192