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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 OCO and OC=O) on the cotton fibres. The DC
cotton fabrics using a low pressure DC glow glow treatment has thus the potential to influence not
discharge obtained in air. The influence of different only the chemical but also the physical properties of
operating parameters such as treatment time, dis- cotton fabrics and this without the use of water or
charge power and operating pressure on the chemical chemicals.
and physical properties of the cotton fabrics is studied
in detail. Surface analysis and characterization of the Keywords Glow discharge  Cotton  Wicking 
plasma-treated cotton fabrics is performed using X-ray photoelectron spectroscopy  Process
vertical wicking experiments, X-ray photoelectron parameters
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 Introduction
treatment time, increasing discharge power and
increasing pressure. Results also show that low Cotton is the most important textile fibre in the world
pressure DC glow treatment leads to surface erosion despite the inroads made into its market by synthetic
of the cellulose fibres, accompanied by an incorpo- fibres (Johansson 2007). Cotton is mainly composed
ration of oxygen-containing groups (CO, C=O, of cellulose with some non-cellulosic components
including proteins, waxes, pectic substances, organic
acids, sugars, (Karahan and Ozdogan 2008). Cellu-
S. Inbakumar  A. Anukaliani
lose has traditionally been modified through reactions
Department of Physics, Kongunadu Arts and Science
College, Coimbatore 641029, Tamilnadu, India of the various hydroxyl groups, leading to esterifica-
tion and etherification. In the last decades, non-thermal
R. Morent (&)  N. De Geyter  C. Leys (or cold) plasmas are gaining popularity as a cellulose
Research Unit Plasma Technology (RUPT), Department
modification technique since this technique varies
of Applied Physics, Faculty of Engineering, Ghent
University, Jozef Plateaustraat 22, 9000 Ghent, Belgium significantly from the traditional esterification and
e-mail: Rino.Morent@Ugent.be etherification routes (Johansson 2007). A non-thermal
plasma contains activated species, such as electrons,
T. Desmet  P. Dubruel
ions, radicals, photons, which are able to abstract
Polymer Chemistry and Biomaterials Research Group,
Department of Organic Chemistry, Faculty of Sciences, hydrogen from either carbon or oxygen atoms present
Ghent University, Krijgslaan 281, 9000 Ghent, Belgium on the cotton surface. In this way, cellulose can be

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418 Cellulose (2010) 17:417426

oxidized, reduced and/or substituted in new, unique experiments. The untreated and plasma-treated cotton
ways (Johansson 2007). fabrics will also be characterized using X-ray photo-
In the last decades, the application of cold plasmas electron spectroscopy (XPS) in order to correlate the
to modify the surface properties of textile materials is hydrophilic properties with the chemical composition
experiencing rapid growth (Chen et al. 2008; De of the cotton surfaces. To gather information on the
Geyter et al. 2006; Morent et al. 2008; Samanta et al. plasma-induced physical changes, weight loss mea-
2009). Non-thermal plasmas are able to alter the surements and scanning electron microscopy (SEM)
physico-chemical properties of a polymer surface: the experiments will be carried out. The above-mentioned
main effects of interaction between active plasma experiments will be performed for selected plasma
species and polymeric surfaces is breaking polymer exposure times, operating pressures and discharge
molecular chains, inducing new functional groups powers in order to study the influence of these plasma
and altering morphological properties (Caiazzo et al. parameters on the hydrophilic behaviour of cotton
1996; Keil et al. 1998; Toufik et al. 2002). Some of fabrics.
the possible effects include improved hydrophilic
properties (De Geyter et al. 2006; Pandiyaraj and
Selvarajan 2008; Vesel et al. 2008), an improved Materials and methods
adhesion to coatings and to polymer matrices (Liston
1989; Liston et al. 1993; Dumitrascu and Borcia Materials
2006; Zhang et al. 2009), an improved dye ability
(Jocic et al. 2005; Ren et al. 2008), induced Commercially available woven grey cotton (warp
hydrophobic properties (Hodak et al. 2008; Leroux count = 29, weft count = 23), supplied by the South
et al. 2008), . Apart from creating interesting Indian Textile Research Association (Coimbatore
textile properties, plasma processing is a rapid and India) is used in this study. Before plasma treatment,
environmentally friendly technique producing virtu- the grey cotton samples were scoured by treating
ally no waste (Verschuren et al. 2007; Yip et al. them in a 2% aqueous NaOH (Nice Chemicals
2002). Moreover, plasma treatment only changes the India) solution for 2 h at 95 C followed by washing
uppermost layers of a material surface without in distilled water and drying in air. This pre-treatment
interfering with the bulk properties (Poll et al. 2001). is used to remove waxes, pectins and other impurities
Plasma modification of cotton fibres and textiles from the fabric surface (Chung et al. 2004).
has been extensively studied in numerous scientific
papers (Karahan and Ozdogan 2008; Pandiyaraj and Non-thermal plasma treatment
Selvarajan 2008; Samanta et al. 2009; Sun and Stylios
2004; Ward and Benerito 1982), however, there is a The plasma system used in this paper is schematically
lack of literature describing the effects of different shown in Fig. 1 and consists of a cylindrical plasma
process parameters such as discharge power, operat- chamber (length 0.5 m, diameter 0.25 m), a vacuum
ing pressure, exposure time, on the chemical and pumping system (VS-114D, Hindhivac India) and a
physical properties of cotton textiles. Therefore, in the DC power supply (Devi Electric Corporation
present work, the effect of different operating param- India). Inside the vacuum chamber, plasma is gener-
eters on cotton plasma modification will be studied in ated between two copper electrodes with a diameter
detail. Plasma treatment will be performed on cotton of 8 cm and a thickness of 1 mm. One electrode is
woven fabrics using a low pressure glow discharge permanently fixed, the other one is variable in height
operated in air in order to improve their hydrophilic- and the distance between both electrodes is set at
ity. This improved water wetting is essential for 3 cm. Before putting the fabric sample into the
effective processing (dyeing and finishing) and main- system, the chamber is first cleaned with distilled
tenance (cleaning) of cotton assemblies involving water and afterwards with acetone. After this clean-
aqueous media, because it facilitates the transport ing step, a cotton fabric sample is fixed in a sample
of active reagents between and into the fibres (Topal- holder and inserted into the plasma chamber by using
ovic et al. 2007). An evaluation of the hydrophilic an adjustable rod. For all experiments performed in
behaviour will be performed using wicking rate this paper, the cotton fabric is placed parallel with the

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Cellulose (2010) 17:417426 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
Fig. 1 Schematic diagram of plasma system (1anode; 2 performing wicking rate measurements based on the
cathode; 3cotton sample; 4sample holder; 5plasma standard DIN 53 923 (EDANA 10.1-72). A cotton
chamber; 6pumping equipment; 7needle valve; A fabric strip (2 cm 9 7 cm) is suspended vertically
ammeter; PPirani gauge) with the lower end dipped in a water-dye liquor (1 ml
Royal Blue (Industrial Research Corporation India)
electrodes at 1 cm from the cathode. This distance dissolved in 100 ml distilled water) and as a result, a
was found to be adequate to avoid thermal alteration spontaneous wicking occurs due to capillary forces
of the fabric during plasma processing. The plasma (Harnett and Mehta 1984; Wong et al. 2001; Ferrero
chamber is firmly closed after introduction of the 2003). The blue coloration of the dye solution on the
cotton fabric and the vacuum pumping system cotton fabric clearly indicated the capillary rise
consisting of a rotary vacuum pump and a diffusion height and a ruler (in millimetres) assembled along
pump is switched on. The pressure inside the plasma the cotton strip enables the height measurements.
chamber is measured using a pirani gauge P Height readings were made at time intervals of 30 s
(A6STM-D Hindhivac India) and during plasma in the first 3 min and at time intervals of 60 s for
processing, the desired pressure (0.030.07 kPa) is longer wicking times. Since natural materials are very
maintained by using a needle valve. After reaching variable by nature, the capillary rise results shown in
the preset pressure in the plasma chamber, the DC this work are the average of 10 independent mea-
power supply is switched on applying the desired surements performed on cotton samples treated under
voltage (250400 V) between both electrodes. In the same conditions. Moreover, also the standard
order to calculate the discharge power, the discharge deviation on these average values will be reported in
current is measured using an ammeter A (OSAW the following sections.
India) connected between the lower electrode and the
DC power supply. The typical operating parameters XPS measurements
for the cotton plasma treatments performed in this
work are shown in Table 1. 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-
Table 1 Typical plasma operating parameters sition of their surfaces. XPS measurements are carried
Discharge potential (V) 250400 V
out on a S-Probe monochromatized XPS spectrometer
Discharge current (I) 719 mA
of Surface Science Instruments (VG), using mono-
chromatic Al Ka-radiation (hm = 1486.6 eV). The
Pressure (P) 0.030.07 kPa
angle between the photoelectron emission direction
Exposure time (t) 110 min
and the plane of the sample is kept constant at 45.
Electrode separation (d) 3 cm
The pressure in the analyzing chamber is maintained
Gas Atmospheric air
at 1 9 10-9 Pa or lower during analysis and the size

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420 Cellulose (2010) 17:417426

of the analyzed area is 250 lm 9 1,000 lm. The at 0.03 kPa and 4.2 W respectively, while the expo-
high-resolution spectra are collected in the constant sure time is varied between 1 and 10 min. Figure 2
analyzer energy mode and the value of 285.0 eV of shows the evolution of the average wicking height as
the C1s core level is used for calibration of the energy a function of wicking time for cotton fabrics which
scale. Curve fitting of the C1s peak is performed using were plasma-treated at different exposure times. The
CasaXPS software. wicking height of the untreated cotton fabric remains
the same (i.e. zero) as a function of the wicking time
Weight loss experiments and SEM measurements due to its poor wetting nature and is therefore not
presented in Fig. 2. This bad wicking behaviour of
Upon exposure to plasma, some degradation reactions the scoured untreated cotton fabrics can be explained
could potentially be initiated on the cotton surfaces by the significant amount of non-cellulosic compo-
due to ion and electron bombardment (Inagaki et al. nents present on the scoured cellulose fibres, as will
2004). As a result, weight loss of the cotton fabrics be explained in detail in XPS results. Figure 2
and morphological changes of the fibre surfaces can clearly shows that initially the wicking height
occur. In order to examine the etching effect of the increases fast with increasing wicking time for all
low pressure glow discharge on the cotton fabrics, plasma-treated samples before levelling off at a
weight loss experiments and SEM measurements are certain wicking time. For the upward wicking, it is
performed. To obtain the weight loss percentage of the obvious that if the distance travelled by the liquid
plasma-treated cotton fabrics, the weight of the becomes high enough, there will be a noticeable
samples is measured before and immediately after effect of gravity on the flow rate, leading to a
plasma exposure using a Shimadzu AUY220 analytic reduction of wicking height increase. As seen in
balance. The weight loss percentage is then calculated Fig. 2, increasing the plasma exposure time leads to a
according to the following equation: higher wicking rate. This observation suggests that
with increasing treatment time, the cellulose fibres
Wut  Wpt
Wloss % 100 may become more hydrophilic since wettability is a
Wut
perquisite for wicking: a liquid that does not wet
where Wut and Wpt are the weight of the untreated and fibres cannot wick into a fabric. Moreover, due to
plasma-treated samples respectively. The weight plasma etching effects, the effective pore size present
measurements are repeated 10 times for each in the plasma-treated cotton fabrics may increase and
plasma-treated sample in order to obtain an average adversely reduce the capillary pressure, thus increas-
weight loss percentage. ing the wicking ability (Sun and Stylios 2004; Wong
In order to visualize the plasma-induced morpho- et al. 2001). Both of these aspects will be further
logical changes on the fibre surfaces, SEM measure- explored by performing weight loss, SEM and XPS
ments are performed using a Quanta 200F scanning measurements in order to determine the chemical and
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


Fig. 2 Average wicking height as a function of wicking time
In a first series of experiments, the operating param- for cotton fabrics plasma-treated at different exposure times
eters pressure and discharge power are kept constant (pressure = 0.03 kPa, discharge power = 4.2 W)

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Cellulose (2010) 17:417426 421

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 Fig. 4 Average wicking height after 5 min of wicking (H5min)
as a function of operating pressure (discharge power = 4.2 W,
instead of presenting the wicking height as a function
treatment time = 6 min)
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 exposure time are kept constant at 4.2 W and 6 min,
assume that increasing the discharge power leads to respectively. Figure 4 shows the evolution of the
an enhanced wicking behavior of the cellulose fibres. average wicking height after 5 min of wicking (H5min)
This can be explained by the fact that increasing the as a function of operating pressure. As observed in
discharge power results in an increase of the amount Fig. 4, increasing the plasma pressure in the range
of reactive plasma species. The presence of more 0.030.07 kPa leads to an increase in cotton wicking
plasma species can lead to an increased fibre ability. It is known that while the electron energy (and
wettability and/or an increased wicking ability due hence the average energy of the reactive plasma
to a more intense bombardment of active plasma particles) decreases with increasing pressure, its
species. density increases (Shi and Clouet 1992). The observed
wicking behavior is probably a result of these two
Effect of operating pressure antagonist effects, however, since wicking proceeds
faster at higher pressures, it is likely that the density
In a final series of experiments, the influence of increase dominates the energy decrease.
pressure on the hydrophilicity of the plasma-treated
cotton fabrics is studied in detail in the pressure range XPS results
0.030.07 kPa. The pressure variation is limited to
this small range to ensure the stability of the DC glow XPS measurements are carried out to evaluate the
discharge and the discharge power and the plasma 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
Fig. 3 Average wicking height after 5 min of wicking (H5min)
as a function of discharge power (pressure = 0.03 kPa, untreated cotton fabric does not consist of pure
treatment time = 6 min) cellulose. The low O/C ratio is due to a considerable

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

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

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424 Cellulose (2010) 17:417426

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

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Cellulose (2010) 17:417426 425

Conclusion properties of atmospheric plasma-treated 3D aramid


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