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Surface & Coatings Technology 202 (2008) 3427 3449

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Non-thermal plasma treatment of textiles

R. Morent a,, N. De Geyter a , J. Verschuren b , K. De Clerck b , P. Kiekens b , C. Leys a
a
Ghent University Faculty of Engineering Department of Applied Physics Research Unit Plasma Technology (RUPT)
Jozef Plateaustraat 22 9000 Ghent Belgium
b
Ghent University Faculty of Engineering Department of Textiles Technologiepark Zwijnaarde 907 9052 Ghent Belgium
Received 18 October 2007; accepted in revised form 13 December 2007
Available online 31 December 2007

Abstract

This article attempts to give an overview of the literature on the treatment of textiles with non-thermal plasmas. Because of the enormous
amount of potential uses of non-thermal plasmas for the modification of textile products, categorizing the applications is difficult, and therefore a
review is given on plasma treatment effects or results rather than on the textile applications that benefit from the treatment.
2007 Elsevier B.V. All rights reserved.

Keywords: Non-thermal plasma; Textile; Fibres; Wettability; Adhesion; Surface modification

1. Introduction aims of this are improved wettability, adhesion of coatings,

The pre-treatment and finishing of textiles by non-thermal
plasma technologies becomes more and more popular as a
surface modification technique [1]. It offers numerous advan-
tages over the conventional chemical processes. Plasma surface
modification does not require the use of water and chemicals,
resulting in a more economical and ecological process. The
enormous advantage of plasma processes concerns the drastic
reduction in pollutants and a corresponding cost reduction for
effluent treatment, so it can be considered as an environmentally
benign technology [2]. A non-thermal (or cold or low tem-
perature) plasma is a partially ionized gas with electron tem-
peratures much higher than ion temperatures. The high-energy
electrons and low-energy molecular species can initiate
reactions in the plasma volume without excessive heat causing
substrate degradation. Non-thermal plasmas are particularly
suited to apply to textile processing because most textile
materials are heat sensitive polymers. In addition, it is a versatile
technique, where a large variety of chemically active functional
groups can be incorporated into the textile surface. The possible
Corresponding author. Tel.: +32 9 2644257; fax: +32 9 2644172.
E-mail address: Rino.Morent@UGent.be (R. Morent).
0257-8972/$ - see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2007.12.027
printability, induced hydro- and/or oleophobic properties,
changing physical and/or electrical properties, cleaning or
disinfection of fibre surfaces etc. Moreover, non-thermal plasma
surface modifications can be achieved over large textile areas.
This paper on Non-Thermal Plasma Treatment of Textiles
reviews different effects than can be induced on a textile product
by a plasma treatment, and ways to obtain these effects. It spans
more than seven decades of reported treatments of textile
products in low temperature plasmas. Because of the enormous
amount of potential uses of a non-thermal plasma for the
modification of textile products, categorizing the applications is
difficult, and therefore a review is given on plasma treatment
effects or results rather than on the textile applications that
benefit from the treatment.
Due to the wide range of plasma sources used, a review of
these different plasma reactor concepts will not be given in this
paper. In literature, there is a large availability of excellent reviews
on plasma generation and plasma sources. Some of them give a
general overview of different types of plasma sources [36],
while others focus on one type of discharge [715]. It should also
be stressed that this paper tries to cover all types of non-thermal
plasma treatments of textiles. It is not the purpose to focus on only
one aspect of plasma textile processing as in [1619] or to review
plasma treatment of polymers in general [20,21].
3428 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
From the following text, it should become clear to the reader
that this subject covers a wide range of topics and that plasma
technology has seemingly limitless opportunities. Notwithstand-
ing these advantages of plasma technology, from the relevant
information gathered in literature, it is often difficult, sometimes
impossible, to do an objective scientific or industrial comparison
of different plasma processes and their effects. This can be one of
the key factors that, despite the enormous potential of plasmas
for textiles demonstrated in laboratory and industrial prototypes,
the introduction of plasma technology on an industrial scale has
not yet found its way in the textile industry. However, in order to
survive in a globalised and changing market, the textile industry
in Europe, North America and other developed countries has
more than ever need for a swing to high-functional, added value
textiles. It is in this context that plasma technology for textiles
has to take a prominent position. Moreover, the ever more
stringent national and international legislation (e.g. European
Union) will little by little lead to the substitution of traditional
wet-chemical techniques.
2. Plasma treatment effects
2.1. Increasing the hydrophilic character
The application of plasma treatments for improved wettability
has been done on all possible fibre types, with varying success.
The treatment aims at the introduction of water compatible
functional groups such as COOH, OH and NH2. Of all
plasma effects, this is without a doubt the most studied because it
influences many plasma applications. When evaluating the wet-
tability of a treated fibre surface, in most cases it is not possible to
determine the surface energy directly from contact angle mea-
surements. The irregular surface of a textile reduces the accuracy
of (large) contact angle values, while for lower contact angles
their porous structure immediately absorbs the liquid drop. That is
why wettability of textile (fibre) surfaces is usually monitored by
indirect methods such as absorption time and wicking [2225].
Apart from the demand of industry for an effective wettability
enhancement, another issue that has increased in importance and
attention over the years is the permanence of the treatment effect.
In [26], Akishev et al. showed that a remote DC glow dis-
charge stabilised by a fast airflow at atmospheric pressure is able
to modify the wettability of polyester fabrics. The treatment
effect was stable for several days. Temmerman et al. used a
similar remote reactor to treat cotton yarns [27]. The efficiency
of the air plasma treatment was tested by measuring the liquid
wicking rate based on DIN 53 923 (EDANA 10.1-72). This
wicking rate increased with treatment time and discharge power.
During the first 5 h after treatment, the plasma effect rapidly
decreased, but this decrease levelled off so that the remaining
wicking rate remained remarkably higher than the wicking rate
for an untreated yarn. Two different regimes of a remote amo-
spheric pressure air plasma DC glow discharge and surface
streamer regime were described for the treatment of different
textiles [28]. Due to the open structure of the samples, the
treatment efficiency was quantified by measuring the liquid
absorptive capacity according to DIN 53 923 (EDANA 10.1-72).
The liquid absorptive capacity is defined as the amount of water
that a fabric has absorbed after 1 min immersion in water, relative
to its own weight. This method is strongly temperature dependent,
therefore a constant water temperature is necessary. For the
treatment of polyethylene terephthalate (PET) non-wovens, the
streamer regime showed to be more efficient compared to the
glow regime. For polypropylene (PP) non-wovens, the optimal
streamer treatment time was only 0.1 s with a resulting liquid
absorptive capacity of 1170% relative to its own weight. Longer
treatment times showed no extra wettability, rather a slight
decrease in liquid absorptive capacity. PA and PET woven fabrics
in different industrial preparation stages (1) unwashed,
(2) washed and thermally stabilized, (3) finished (washed, ther-
mally stabilized and dyed) were treated in the streamer regime.
For the PA samples, the influence of the treatment is the largest on
the raw samples, while the influence on washed and thermally
stabilized fabrics is similar to the influence on the finished fabrics.
This difference was not found for PET woven samples. Akishev
et al. [29] also treated PET fabric with an atmospheric pressure air
or argon dielectric barrier corona discharge and found even after
short treatment times in argon (110 s) a substantial increase in
water uptake and water uptake rate. At identical treatment times in
air, there was a smaller effect.
Negulescu et al. treated a PET fabric in a low pressure SiCl4
plasma [30]. The SiClx groups implanted at the PET fibre
surface spontaneously hydrolyse by reaction with atmospheric
humidity, creating hydrophilic SiOH groups in addition to the
plasma created carbonyl groups. Thus, a hydrophilic fibre
surface is created. The water contact angle was reduced from an
original 86 for the untreated surface to 60 after a 30 s treat-
ment and to 46 after a 10 min plasma treatment.
PET fabric was treated by plasma initiated in various gases
(N2, O2, air, CO2 and NH3) by Wrbel et al. [31]. Evaluation of
the wettability was done by the wetting time, i.e. the time
required for a drop of distilled water, placed on the treated fabric
surface, to lose its reflective power. The wetting time of the
plasma-treated fabric considerably drops in comparison to the
untreated fabric and the best results were obtained after
treatment in oxygen, nitrogen and air plasma. Costa et al. also
studied the effects of gas composition on the wettability of PET
fabrics [32]. Molina et al. reported on an improved wettability
of keratin fibres with a water vapour plasma [284].
The one atmosphere uniform glow discharge plasma
(OAUGDP) of Tsai et al. [33] created wettability of PP melt
blown webs after a 1 to 4 min treatment in CO2 or CO2 + O2
plasmas. Addition of oxygen to CO2 improved the treatment
effectiveness, as did increasing gas temperature. They showed
that in this configuration the wettability of the webs was
determined by six critical parameters: power frequency, power
voltage, electrode gap, working gas, treatment time and tem-
perature of the working gas. More importantly, these parameters
are dependent on each other. In the same experimental system,
Dai et al. generated in air an atmospheric pressure glow dis-
charge as well as a filamentary dielectric barrier discharge [34].
They compared both configurations with a low pressure plasma
treatment and observed that the atmospheric pressure glow
discharge could compete with low pressure plasmas, while the
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
dielectric barrier discharge used was less effective. A detailed
description and evaluation of the OAUGDP for different uses in
industry was given in [35] by Roth and Bonds.
In a study on the dyeability of corona-treated cotton fabrics,
Carneiro et al. [2] evaluated the influence of the number of
passages through their reactor on the fabric hydrophilicity for raw
and desized fabrics. They showed that an increase of hydro-
philicity strongly depended on the pre-treatment state of the
fabrics: while raw fabrics require four passages before wettability
is considerable, a desized fabric has a comparable wettability after
only two passages. The effect of successive treatments was also
studied in [36] for a low pressure 8 kHz air plasma with industrial
size. A threefold 10 s treatment showed to be slightly more
efficient than a single 30 s treatment. Ryu et al. evaluated the
wettability of successive corona treatments by measuring the time
required to adsorb 0.6 l of distilled water [37]. Table 1 gives the
adsorption times for different polymer fabrics single, twofold and
threefold treated. It is clear that the effect of successive treatments
also depends on the material used.
Borcia et al. studied an 80 kHz dielectric barrier discharge
(DBD) in air for the treatment of PET and nylon fabrics [38]
and recently, a DBD in air, nitrogen or argon for the treatment
of natural, synthetic and mixed fabrics [39]. The enhanced
wettability and wickability appeared to be strongly increased
within the first 0.10.2 s of treatment. Any subsequent
surface modification following longer treatment (N 1.0 s) was
less important. The increased wettability could be attributed
to the increased level of oxidation where supplementary polar
functionalities are created on the fabric fibre surface, as
observed by X-ray photoelectron spectroscopy (XPS) also
known as electron spectroscopy for chemical analysis
(ESCA).
Recently in [40,41], Morent et al. modified PET and PP non-
wovens by a 10 kHz DBD in air, helium and argon at medium
pressure (5.0 kPa). The helium and argon discharges contained a
fraction of air smaller than 0.1%. Surface analysis and
characterisation were performed using XPS, liquid absorptive
capacity measurements and scanning electron microscopy
(SEM). The non-woven, modified in air, helium and argon,
showed a significant increase in liquid absorptive capacity due to
the incorporation of oxygen-containing groups, such as CO,
OC = O and C =O. It was shown that an air plasma was more
efficient in incorporating oxygen functionalities than an argon
plasma, which was more efficient than a helium plasma. An air
plasma treatment was the most efficient in incorporating oxygen
on the surface due to the fast reaction between the radicals on the
textile surface and the oxygen species, present in the discharge.
Table 1
Wettability of wool, polyester, and polyamide 6 fabrics treated with corona
discharge [37]
Fibre type Time of penetration (s)
Untreated Corona, Corona, Corona,
single twofold threefold
Wool N2000 1120 91 19
Polyester 877 321 134 103
Polyamide 6 332 150 47 46
3429
Fig. 1. Water contact angle of PP and PET fibres versus plasma treatment time
[285].
In an argon and helium plasma containing oxygen traces, plasma
treatment led to an oxidized cross-linked structure on the textile
surfaces. Since the cross-linking reaction inhibits the incorpora-
tion of oxygen and since only traces of oxygen were present, a
helium and argon plasma were less efficient in oxidation of the
textile surfaces. The argon plasma used contained more ions than
the helium plasma resulting in a higher degree of cross-linking
and a faster incorporation of oxygen-containing groups. SEM
pictures of the plasma-treated non-wovens showed that the
hydrophilicity of the non-wovens could be increased to a
saturation value without causing physical degradation of the
surface. The ageing behaviour of the plasma-treated textiles after
storage in air was also studied in detail. The ageing effect was the
smallest for the argon plasma-treated fabrics, followed by the
helium plasma-treated fabrics, while the air plasma-treated
fabrics showed the largest ageing effect. During the ageing
process, the induced oxygen-containing groups re-orientated
from the surface into the bulk of the material. A restriction of the
polar group motion and therefore of the ageing process can be
obtained by cross-linking of the polymer chains during plasma
treatment. An air-plasma treated non-woven was not cross-
linked and therefore showed a large ageing effect. A helium
plasma treatment of the non-wovens led to cross-linked textile
surfaces resulting in a less pronounced ageing effect. Argon
plasma-treated non-wovens had a higher degree of cross-linking
resulting in an even smaller ageing effect.
The after plasma treatment observed faster uptake of water
and oil of cotton cellulose fibres, inspired Benerito et al. to
study the surface with XPS [42,43] and for all the plasmas used
they saw an increased O/C ratio. Electron spin resonance
revealed the presence of free radicals at the surface [43]. Cheng
et al. developed a new plasma jet system and obtained similar
results of increased wettability and O/C ratio for PP and PET
fibres [44]. Fig. 1 shows the change in contact angle for PP and
PET as a function of plasma treatment time, while Fig. 2 shows
the ageing behaviour of PP and PET samples treated for dif-
ferent times.
It is well known that plasma treatment changes the outermost
layer of a material without interfering with the bulk properties.
However, textiles are several millimetres thick and need to be
3430 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
Fig. 2. Water contact angle of different time plasma-treated PP (left) and PET (right) fibres versus storage time at ambient temperature [285].
treated homogeneously throughout the entire thickness. To
control the penetration depth of the plasma effect, it is necessary
to study the influence of operating parameters. Therefore, De
Geyter et al. [41,45] published a study about three layers of a
100% PET non-woven treated in the medium pressure range
(0.37 kPa) with a 50 kHz dielectric barrier discharge in air to
study the influence of pressure and treatment time on the
penetration depth. Current and voltage waveforms and Lichten-
berg figures were used to characterize the discharge. Process
pressure showed to be a crucial parameter to obtain the optimal
plasma penetration. In the pressure range 0.31 kPa, increasing
pressure resulted in a better treatment of all three layers. In the
pressure range 17 kPa, higher pressure demanded longer
treatment time to reach half of the saturated wetted area for layer
1 and 2, in contrast with layer 3, which reached this wetted area
faster with increasing pressure. This was due to two facts. The
first one was the diffusive transport of active species through the
layers. If the mean free path of a textile modifying particle is
close to or larger than the mean pore size of the textile, the loss of
active species is low, resulting in a high diffusive transport. In
contrast, smaller mean free paths cause substantial losses, which
limit diffusive transport. The second one was a different
behaviour of the DBD. In the pressure range 0.31 kPa, plasma
was burning above the textile layers using the upper textile layer
as the dielectric surface. No microdischarges typical for DBD
discharges were seen on a photographic film, placed under the
textile layers. Therefore the change in hydrophilicity of layer 2
and 3 was solely a result of diffusive transport of the active
species generated in the plasma above layer 1. In the pressure
range 17 kPa the barrier discharge went through the textile
layers using the glass plate as dielectric surface, and individual
microdischarges were seen on the Lichtenberg figures. There-
fore, in this pressure range the generation of active species also
occurred between the fibres and, together with the diffusive
transport, this was responsible for the hydrophilicity. With
increasing pressure, the number of microdischarges increased,
while the diameter and the distance between them decreased.
Poll et al. also showed that pressure is a critical parameter in
penetration of plasmas into textile structures and they were not able
to detect any penetration of the plasma effects at atmospheric
pressure [46]. Opwis et al. also published a short study on pene-
tration of plasma into textile structures in terms of increased wet-
tability of the treated layers [47]. Verschuren et al. reported on an
experimental plasma reactor that enabled the study of the effect of
gas flow around and through textile structures during plasma
treatment [48]. Only few other authors reported on the penetration
of plasma in textiles [4953]. In the latter cases, the purpose of their
work was always hydrophobicity enhancement (see Section 2.4).
Different other papers were published about the enhance-
ment of hydrophilicity of a wide range of textile fibres or
fabrics: PET [5459], PP [6068], silk [69], nylon [19,7072],
linen [73], meta-aramid [74], carbon fibres [75], wool [7679],
cellulose [80], etc. Also mixed fabrics containing eg. cotton and
polyester were treated [81].
Closely related to direct wettability, moisture regain is a
parameter that is clearly affected by plasma treatment. Hwang et
al. found that plasma-treated PP fabrics gained weight during
storage and then lose it after drying [82]. This implies that
surface oxidation plays an important role in moisture adsorption
from air and it corresponds to surface wettability enhancement
with plasma.
2.2. Enhancing adhesion
Adhesion enhancement aims at the introduction at the fibre
surface of functional groups that show affinity for, or form
chemical bonds with a product, such as a coating or a composite
matrix.
2.2.1. Composite materials
The interface between fibre and matrix plays an important role
in transferring the forces towards the fibres and determines the
composite's mechanical and chemical properties to a large extent.
Plasma treatments are known from a large amount of
publications to improve interlaminar shear strength (ILSS) of
composite materials as well as their resistance to fatigue, de-
lamination and corrosion. Such improvements are due to
enhanced interactions in the interphase, by a combination of a
plasma induced increase in bonding surface (micropitting, me-
chanical interlocking) and change in surface chemistry. When
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
treatment conditions are well chosen, the loss in fibre strength is
minimal (12%); while in some cases the fibre strength even
increases. Each combination of fibre and matrix requires a
specific set of fibre surface properties. In many publications, the
matrix is an epoxy resin; the functions introduced at the rein-
forcing fibre's surface (NH2, OH, COOH) are to react with
the epoxy function. The fact that high performance composite
structures are often used in high-end aerospace applications, and
that the starting materials are often very expensive, makes the
extra batch vacuum plasma processing step economically
feasible. Because a plasma treatment itself produces non or a
negligible amount of waste, the environmental impact and the
ever increasing costs related to it are very small.
2.2.1.1. Carbon fibres. The surface treatment of carbon fibres
[83] is required because of their low reactivity. The surface
structure and reactivity depends on which precursor has been
used and to what temperature and oxidative atmosphere the
fibres have been exposed. Jang and Kim [84] treated materials
made from co-woven carbon and polyetheretherketone (PEEK)
fibres in a 13.56 MHz oxygen plasma at low pressure for 1, 3, 5
and 7 min. They saw an increase of carbon fibre surface rough-
ness up to 3 min of treatment time; longer treatments resulted in
overall smoothing. The treatment did not increase the function-
ality of the carbon fibre surface; possibly the initial fibre surface
was already oxidized. After molding of the fabrics the composite
structure showed a considerable increase in both the flexural
strength (up to 52%) and the ILSS (up to about 17%), with a clear
maximum after a 3 min plasma treatment. This indicates that in
this system the adhesion strength was mainly determined by
mechanical interlocking.
Oxygen and ammonia plasmas were applied to improve the
interfacial adhesion between carbon fibres and bismaleimide
(BMI) resin [85]. Ammonia plasma showed to be better in
enhancing the interfacial adhesion without producing an
undesirable reduction in fibre strength. Oxygen plasma resulted
in a greater etching of the carbon fibre surface. For oxygen
plasma, the improved carbon fibre-BMI adhesion was attributed
to the improved level of mechanical keying, the increased
surface wettability and chemical bonding. For ammonia plasma,
chemical bonding between amine groups and bismaleimide, and
enhanced surface energy are the two important factors in
controlling interfacial adhesion. A similar study on the
interfacial bond formation in carbon fibre/epoxy composites
was done by Kettle et al. [86].
Yuan et al. studied the treatment of carbon fibres to improve
the interfacial adhesion with polyphenylene sulphide [87,88].
The carbon fibres were plasma etched by an oxygen or an argon
plasma resulting in an increased interfacial shear strength
(IFSS) up to 2.5 times compared to non-treated fibres.
A uniform treatment of carbon fibre surfaces by an oxygen
plasma was described by Huang et al. [89] and they reported on
the improvement of the mechanical properties of their phenolic
composites. The IFSS of the composites was strongly increased
and the treated fibres exhibited a very significant increase in
wettability. XPS results revealed a much higher oxygen
percentage on the surface of the treated fibres. Sun et al. [90]
3431
showed an enhancement of ILSS of carbon fibre reinforced
epoxy composites due to a similar oxygen plasma treatment.
Radio-frequency (RF) plasma copolymerisation of acrylic-
acid/hexane, allyl-alcohol/hexane and allylamine/octadiene gas
mixtures showed the ability to deposit thin coatings on carbon
fibres to improve the adhesion. This enhanced adhesion was
attributed to the introduction of oxygen- and nitrogen-contain-
ing functionalities which have known reactivity to epoxy
groups. Regarding the generally recognised reactivity of
carboxylic acid and amine groups to epoxides, these groups
were more effective than hydroxyl groups.
Nay et al. coated a polyimide film with a thin, visco-elastic
and reactive interlayer to improve the adhesion between the
coated film and carbon fibres [91]. Zhang et al. [92,93] treated
with success carbon fibres to enhance the interfacial properties
between carbon fibres and the polyarylacetylene resin.
Dagli and Sung [94] treated carbon fibres in a 13.56 MHz
acrylonitrile and styrene plasma at low pressure, depositing a
transparent polymer layer at 1.4 to 3.7 nm/min. The residence
time of the monomer in the reactor can be estimated at 12 s. The
determined increase in fibre tensile strength of up to 12% cannot
be due to the coating itself as it is too thin to add such strength.
Possibly, the deposited plasma polymer healed some of the
randomly distributed surface flaws that control the fibre strength.
The abundant surface polar groups combined with the improved
tensile properties of the plasma treated fibres made them attractive
reinforcements for advanced composite materials.
2.2.1.2. Polyolefinic fibres. Another application of plasma is
the surface chemical modification of high modulus polyethy-
lene (HMPE) fibres, from very low initial surface energies to the
higher surface energies required for optimum interaction with
the matrix resin (epoxy in most cases). Tissington et al. [95]
suggested that there are three contributions that lead to an
improved adhesion after an oxygen plasma treatment. First, at
short treatment times a surface oxidation occurs, while secondly
after intermediate treatment durations also cross-linking takes
place, which increases the cohesive strength of the surface.
Finally, after long plasma exposure pitting of the surface occurs,
which causes a mechanical keying effect. This mechanical
keying (interlocking) between the resin and the micropitted
fibre surface is considered as an influential factor in the
improved bond strength, though usually improving adhesion of
polyolefinic fibres is clearly linked to the introduction at the
fibre surface of polar functional groups (carboxylic, amine, ).
Gao and Zeng studied the fibre/epoxy adhesion after plasma
treatment of ultrahigh molecular weight polyethylene
(UHMWPE) [96,97]. They concluded that apart from increase
in surface energy and mechanical keying, also the non-polar
dispersion force plays a role in the adhesion of modified fibres
to epoxies; optimum results are obtained when their respective
contributions are about 60%, 30% and 10% respectively [96].
Holmes and Schwartz treated fabrics made of ultrahigh strength
polyethylene (UHSPE) fibres in an ammonia plasma and
showed that the adhesion to epoxy resin was improved [98].
Rostami et al. [99] treated UHMWPE with an inductively
coupled plasma and found a fivefold enhancement in interfacial
3432 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
strength between the fibres and the epoxy matrix. Optimum
conditions were reached with a 15 s etch in argon plasma,
followed by a 3 min allylamine plasma polymerization. Martin
et al. studied the mechanical behaviour of high-density poly-
ethylene composites [100]. Moon and Jang reported in different
papers [101103] on the influence of oxygen plasma treatment
on the interfacial adhesion of ultrahigh modulus polyethylene
(UHMPE) fibre and vinylester composites. Masse et al. treated
HMPE fibres in an oxygen RF plasma at low pressure for
improved adhesion to a polyester resin matrix [104]. The results
demonstrated that adhesion was enhanced for plasma treatment
times as short as 2 s, mostly because of chemical bonding.
Interfacial shear resistance gradually increased for the longer
times considered, up to 10 min. In the latter case, the better
results were attributed to fibre surface etching and roughening,
rather than chemical bonding. Also corona treatments have been
done for improved fibre-matrix interaction [105]. Ma and Qi
treated PP fibres for fibre reinforced cement composites [106].
Rahel et al. used an atmospheric pressure plasma for the
treatment of ultrahigh molecular weight polypropylene
(UHMWPP) and tested the adhesion to rubber [107].
A particular problem with olefinic surfaces is that they are
easily overtreated in a direct plasma, which leads to an unuseful
modification. The use of remote (or afterglow) plasmas offers a
solution in this respect [108]. In an attempt to introduce primary
amines on a polyethylene surface only a remote plasma of
nitrogen/hydrogen leads to positive results. A direct nitrogen/
hydrogen plasma would also graft nitrogen-containing groups,
but no primary amines.
2.2.1.3. Aramid fibres. The surface of aramid (Kevlar 69)
fibres was modified by NH3, O2 or H2O plasmas in order to
improve the adhesion to epoxy resin [109]. After plasma
treatments, the IFSS of aramid/epoxy composites, as measured
with the microbond pull-out technique, was substantially
improved (4383%) depending on treatment time and gas.
The fibre strength was only little affected (less than 10% loss).
This significant improvement in IFSS principally resulted from
the formation of covalent bonds between the newly reactive
functionalities at the modified fibre surfaces and the epoxides of
the resin. Improvements in ILSS and flexural properties were
also found after treatment of aramid fibres in an ammonia or
oxygen treatment [110].
Liu et al. studied the influence of moisture regain of aramid
fibres on the adhesion between the fibres and epoxy [111]. With
a treatment in atmosphere, the substrate could contain a sub-
stantial amount of moisture and therefore the authors treated
aramid fibres with different moisture regains with plasma. They
concluded that moisture regain promoted the plasma treatment
effect on the improvement of adhesion between aramid fibres
and epoxy.
Shaker et al. [112] optimized low pressure RF plasma
polymerization of allylamine onto sized para-aramid fibres. The
processing is done in two steps: a 5 min treatment with argon
plasma followed by a 15 to 45 min allylamine plasma poly-
merization. The fibre-matrix interfacial adhesion was enhanced
when allylamine was coated on the fibre surface. The IFSS
between allylamine plasma coated Kevlar showed fivefold in-
crease over untreated fibres.
2.2.1.4. Glass fibres. Glass fibres are being replaced in many
composite applications by fibre materials with a lower density,
such as carbon fibre. Some applications, however, require the
composite structure to have ultra low conductivity and high
resistance to electrical breakdown. Therefore, glass fibres are
for example still used in electronic circuit boards.
In some cases, a plasma treatment can reduce interfacial
strength, such as has been noted when extracted borosilicate
glass fibres were treated in ammonia plasma at low pressure for
improved adhesion to epoxy resins [113]. The high level of UV-
radiation as well as the bombardment with highly energetic
plasma species were considered to lever the equilibrium
between formation and destruction of functional groups towards
their destruction. Other reasons for a decrease in adhesion were
the reduced surface roughness (removal of non-fibrous
material) and the formation of paramagnetic defect centres
both at the fibre surface and in the fibre bulk [114]. The latter
effect also leads to an increase in fibre surface conductance,
which lowers the glass fibre's performance for application in
electronic circuit boards.
2.2.1.5. Miscellaneous. Cernak et al. [115] continuously
treated a polyester monofilament in a pulsed surface discharge
in nitrogen or dry air at atmospheric pressure for 0.2 s. Within
60 s, they inserted the filament in an epoxy resin matrix. The
pull-out strength was improved by up to 800%. Simor et al.
[283] treated polyester cord threads used as reinforcing
materials of rubber blend with an atmospheric pressure water
plasma in order to enhance their adhesion to rubber. The
adhesive strength of the treated PET cord/rubber interface
doubled due to the introduction of surface polar groups and due
to the increased surface area of the fibres.
Morales et al. treated cellulose fibres for the use in com-
bination with a polystyrene matrix [116]. The results showed
that the adhesion in the fibre-matrix interface increases with
time in the first 4 min of treatment. However, at longer plasma
exposures, the fibre was sometimes degraded reducing the
adhesion with the matrix.
2.2.1.6. Combination with coupling agents. During the
production of composite materials, it often happens that the
fibre surface is not directly put in contact with the matrix. First,
the yarns are coated with an adhesive resin (a coupling agent),
whose surface forms the interface that interacts with the matrix
resin. Plasma treatments can be performed to optimize fibre-to-
coupling agent interaction. This is typically done for textile
reinforced rubber materials [16]. Pitt et al. combined a plasma
treatment with the use of a coupling agent to improve adhesion
between aramid fibres and a silicone rubber matrix [117]. The
role of the plasma treatment was both the purification of the
fibre surface and its oxidation. Bartos and Rakowski [118]
described the improvement of the adhesion of methanol
extracted PET fibres and fabric to different rubber types by
plasma treatment in different non-polymerising gases. After the
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
plasma treatment the textile structures are impregnated in a bath
containing a resorcin-formaldehyde-vinylpyridin latex. A 60 s
nitrogen plasma treatment increased the adhesive forces of fabrics
to an apolar rubber by a factor of 2.75 (8 N/cm to 22 N/cm),
which is still not enough for most intended applications. The
adhesive force to high polarity rubber however increased from
15 N/cm to 7090 N/cm (a factor of 4.76). From an adhesive
force of 7090 N/cm onwards the adhesive failure is not situated
at the fibre-rubber interface but in the rubber bulk itself.
Treatments in argon, carbon dioxide or hydrogen plasmas were
far less efficient than treatments in air or nitrogen. Krump et al. did
similar experiments in air and nitrogen on adhesion enhancement
between atmospheric pressure corona plasma-treated PET fibres
and a rubber matrix [119].
Janca et al. reported on a plasma surface treatment of PET
fabrics for the reinforcement of car tires [120]. Oiling of the
original synthetic cord fibres is the main technological problem.
The fibres were treated to increase the adhesion of the PET
fibres with the rubber matrix and the best results were obtained
with a nitrogen plasma at atmospheric pressure. The authors
suggest that a small addition of ammonia enhanced the adhesion
even more. Addition of other gases containing fluorine and
chlorine were labelled as unuseful due to their toxicity and
ecological unacceptability in industry.
2.2.2. Coated and laminated textiles, application of glues
The definition of coating in the following paragraphs is a
polymeric layer usually more than 100 m thick deposited
on top of a textile structure, penetrating only the outer few fibre
layers. This stands in contrast to fibre coating with a thickness
of several nanometres to a few micrometers (see Section 2.5). A
textile laminate is a structure that usually consists of two (non-)
woven or knitted fabrics with a polymer layer in between. Many
laminate applications aim at combined protective and comfort
properties. As is the case with fibre-matrix interaction in com-
posite materials, a plasma treatment of a textile structure aims at
improving adhesion between the structure and the deposited
coating. Plasma accomplishes this via an improved wetting of
the textile surface by the coating, and by an increase in attractive
surface-coating interactions. For applications in which a poly-
mer is deposited on a textile structure for fixation purposes, a
surface treatment can increase the penetration depth, thus
enlarging the contact surface between the textile parts that are to
be fixed to each other. Shishoo states that an improvement in
adhesive properties results from an overlap of the following
effects [121]: (1) the removal of organic contamination and of a
weak boundary layers by (reactive) cleaning and (physical)
ablation; (2) cohesive strengthening of the polymeric surfaces;
and (3) creation of chemical groups on the surface that result in
acid-base interactions and in covalent bonds; the latter are
believed to yield the strongest bond.
Recently, the adhesion of conductive polypyrrole coating on
wool and polyester fabrics was improved by an atmospheric
plasma glow discharge in [122].
Currently, most coatings are deposited via an aqueous
dispersion of a polymer and evaporation of water, as is the case
for most polyurethane coatings or polyethylene-co-vinyl acetate
3433
copolymers. Other coatings are transferred from a coated paper
onto the textile structure through hot pressing (transfer coating).
Finally, a decreasing but still considerable amount of (mainly)
polyvinyl chloride (PVC) are deposited from solvent disper-
sions of the polymer, followed by the evaporation of the solvent.
The latter method is said not to require a fabric surface treatment
if the solvent assures a good wetting of the fibre surface and a
sufficient interlock between fabric and coating material.
An atmospheric pressure nitrogen plasma was used to render
a 0.1 mm thick PET non-woven hydrophilic and facilitate
absorption of a palladium catalyst in order to provide a catalytic
surface for the deposition of electroless nickel plating [123].
While PET-nickel adhesion was inexistent for untreated
samples, an optimal adhesion was obtained after 1 s of plasma
treatment. The standard industrial peel test (ASTM D 3359-78
Method B) removed fibres from the (loosely structured) non-
woven before removing nickel from the fibre surface. A similar
study on electroless nickel plating of a polyester fabric was
recently done by Yuen et al. [124].
In [125], Dumitrascu and Borcia developed a method for
contact angle measurement between a liquid and a fibre to
compare and analyse the adhesion properties of PA-6 fibres,
before and after DBD treatment. The contact angle was found
by numerically solving a scalar equation of the drop profile
which included the experimentally measured drop dimensions.
2.3. Improving dyeing and printing properties
Plasma treatment modifies or removes the fibre's hydro-
phobic outer layer, improving dye-fibre interaction and increas-
ing the flux of dye molecules through the fibre surface into the
fibre bulk. An improvement of the dyeing properties of textiles
has many aspects: (a) increase in dyeing rate, (b) increased
dye bath exhaustion, and (c) improved dyeing homogeneity.
Improvements in dyeing properties have been reported on all
fibre types. Two types of plasma processing can be distinguished
for this purpose: depositing plasmas or non-depositing plasmas.
In the former, the required functional groups are part of a coating
that is plasma polymerised in situ at the fibre surface. Non-
depositing plasmas (e.g. O2 plasma) introduce functional groups
that interact with an (ionic) dye molecule directly at the fibre
polymer surface by chemical reaction, or alter the hydrophobic
character of the fibre surface to improve diffusion of (ionic) dye
molecules.
ktem et al. [126] introduced carboxylic acid groups at a
PET fibre surface with a 13.56 MHz low pressure plasma
treatment in two ways. In the first case, fabrics were directly
treated in an acrylic acid plasma, while in the other case they
were first treated in an argon plasma and then immersed in an
aqueous acrylic acid bath. The argon plasma creates a large
amount of surface radicals that initiate the polymerisation
reaction. Dyeing with a basic dye caused the dyeability to
increase from 0.34 K/S for the untreated fabric to 0.82 K/S for a
5 min in situ plasma polymerization. A value of 1.48 K/S was
obtained for a 15 min plasma treatment in argon followed by a
5 min incubation time in an acrylic acid solution. ktem et al.
[127] also reported on the treatment of PET/cotton fabrics with
3434 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
acrylic and water plasma and the treated fabrics showed a much
higher dyeability than the untreated PET/cotton fabrics.
In a similar study on an identical reactor, zdogan et al.
[128] treated scoured and bleached cotton jersey knit in a
13.56 MHz ethylene diamine (EDA) or triethylene tetramine
(TETA) plasma. Another treatment was done in argon, after
which the fabric was immersed in a solution of EDA or TETA.
The purpose of these treatments was the introduction and
protonation of amine functional groups at the fibre surface
resulting in an increasing affinity of anionically charged
reactive dye molecules for the cotton fibres. An increase of
colour strength K/S between 6.6% and 29.0% for EDA and
between 0.3% and 33.9% for TETA was observed, with best
results obtained after a 15 min treatment in a TETA plasma.
Ferrero et al. tested the dyeability of PET, polyamide (PA)
and PP woven fabrics after plasma polymerisation of acrylic
acid [129]. The overall colour strength was significantly in-
creased. However, while the wash fastness was acceptable on
PA, it was unsatisfactory on PET and PP fabrics, probably due to
the lack of penetration of the acrylic acid monomer in the fibre.
SEM and Fourier transform infrared spectroscopy (FTIR)
confirmed that grafting of polyacrylic acid had taken place
only on the surface of PET and PP, but in the case of PA the
interior of the fibre was also modified. Similar experiments on
nylon-6, with a plasma pre-treatment and a subsequent acrylic
acid or 2-hydroxyethyl methacrylate grafting process, were also
reported by Liao et al. [130].
The impact of a nitrogen plasma treatment on the dyeing
properties of wool fabric was studied in detail by El-Zawahry
[131]. The non-thermal plasma treatment resulted in etching of
the fibre surface, enhancing the hydrophilicity and wettability of
the treated wool along with creating and introducing new active
sites onto the wool surface. The treatment also improved the
dyeing rate and shortened the time to reach dyeing equilibrium.
The nitrogen plasma introduced new NH2 groups onto the
wool surface, thereby enhancing the extent of dye exhaustion.
Wakida et al. showed that atmospheric pressure plasma treat-
ment was effective for ameliorating the dyeing properties of
wool and nylon and that the effectiveness of the treatment
regarding dyeing rate strongly depended on the specific dye
used [132,133].
El-Nagar et al. performed a low pressure treatment of PET
resulting in significant improvements in water absorbance and
dyeability [134]. Recently, Raffaele-Addamo et al. applied a RF
plasma in air or argon to PET fibres and showed an increased
colour depth upon dyeing [135]. Fig. 3 shows the increase and
saturation of colour depth as a function of dyeing time for a PET
fabric. Iriyama et al. generated low pressure plasmas in different
gases (O2, N2 and H2) for deep dyeing of silk fabrics [136]. All
plasma-treated silk fabrics showed increased K/S values and the
best results were obtained with the O2 plasma. The plasma-
treated fabrics dyed in lower dye concentration, as low as 6%,
gained greater K/S values compared with untreated ones dyed in
a 10% dye solution, which could lead to great saving of dyes.
Radetic et al. [137] did a similar study on knitted wool fabrics
with different gases (O2, air and Ar) and also achieved the best
results with an oxygen plasma. The effect of the plasma treatment
Fig. 3. Increase of colour depth at 371 K as a function of time on an untreated
() and an air plasma-treated () PET fabric [286].
on the K/S values increased in the following order: argon plas-
ma b air plasma b oxygen plasma. The results on K/S of plasma-
treated fabrics were compared with a traditional chlorination
process and showed that even short plasma treatments yielded
considerable improvements in the printing properties of wool
fabric, making plasma technology a viable alternative for
chlorination.
Jin and Dai [138] reported on an increased dyeing uptake of
nitrogen glow discharge treated wool. In another study, Jocic et al.
compared the effect of plasma treatment and chitosan treatment
on wool dyeing with acid red 27 [139]. They observed that wool
treated with a RF air plasma had improved dyeing properties.
In another publication the grafting of SiClx+ cations from a
30 kHz low pressure SiCl4 plasma onto additive-free acetone
extracted PET fibres is described [140]. The highly reactive
SiClx species implanted on the surface are hydrolysed to Si
(OH)x in a post plasma reaction with atmospheric humidity.
Untreated samples showed a 0.4 K/S value. Optimum surface
modification was reached after a 1 min plasma treatment, after
which K/S values of up to 1.6 were noted following 30 s of
dyeing with a basic blue dye.
PP non-woven fabrics were activated by an atmospheric
pressure plasma treatment using a surface dielectric barrier
discharge in N2 and ambient air by Cernakova et al. [141].
Subsequently, the plasma activated samples were grafted using
a catalyst-free water solution of acrylic acid. The grafted non-
woven exhibited improved water transport and dyeing proper-
ties and the plasma activation in nitrogen was more efficient
than in air. A similar study of graft co-polymerization of acrylic
acid on DBD treated linen was done by Ren et al [142].
Covalently bonded coatings were deposited on CCl4 and
acetone extracted PP fabrics in an argon/acrylonitrile
13.56 MHz cold plasma by Sarmadi et al. [143]. The fabrics
showed both increased water uptake and increased uptake of
acid dye: K/S increased from 0.6 for the untreated fabric up to
4.25 for the treated fabric. Sarmadi and Kwon [144] studied the
O2 and CF4 plasma treatment of PET fabrics. The O2 plasma
improved both the water uptake and the surface dyeability,
while CF4 plasma resulted in excellent water repellency and
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
unexpected improved surface dyeability. They suggested that
this behaviour could be due to intense fluorination reactions and
simultaneous unsaturated bonds and trapped free radical
formation. Ageing analysis showed insignificant post-plasma
modifications under open laboratory conditions. However, as in
many other plasma textile applications, ageing of the plasma
effect often plays a role in dye uptake as shown by Malek et al.
for cotton fibres [145].
Another possible explanation for the positive influence of a
plasma treatment on the dyeing kinetics of PET fibres was
suggested by Urbanczyk et al. [146]. They treated a PET filament
yarn in a 6.5 MHz air plasma at low pressure and determined
several dyeing properties. The diffusion coefficient of a disperse
dye increased up to 28%. An explanation for the improved dyeing
properties was given by considering that the outer molecular
layers of PET fibres are markedly more ordered than the bulk
polymer, creating a barrier for molecules diffusing into the fibre.
A plasma treatment alters or removes these outer layers, thus
increasing diffusion rates of dye and solvent molecules.
In contrast to the previous studies, a plasma treatment can also
decrease diffusion rates as it has been shown that a plasma
selectively etches the amorphous domains of the fibre surface
polymer structure, thus increasing its crystalline fraction. Because
dye molecules progress through the fibres amorphous polymer
fraction, dye rates can be decreased, as was noted when PET and
nylon 6.6 were treated in an air or oxygen plasma [147].
The apparent contradiction i.e. plasma treatment improves
or slows down dyeing processes raised by the aforementioned
studies is solved by considering that depending on plasma
treatment conditions, which are often described in too little
detail in publications, a plasma of given gas type can lead to
different effects at the fibre surface, e.g. conditions which
favour, or not, the selective etching of the amorphous part of the
polymer at the fibre surface.
2.4. Hydrophobicity and oleophobicity
The treatment introduces certain functional groups via a
coating or a graft co-polymer, removes hydrophilic functional
groups or changes hydrophilic groups into non-hydrophilic
ones. The most straightforward way is the treatment of a fabric
in a non-depositing gas which grafts (or exchanges) single fibre
polymer atoms with hydrophobic groups such as fluorine
groups. In another method the fabric is immersed in a fluid
consisting of or containing the hydrophobic prepolymer with
added initiators, after which the textile is plasma-treated leading
to the grafting of the prepolymer on the fibre surface. The
method with the highest potential is the deposition of a polymer
structure at the fibre surface while the textile remains in the
plasma reactor. The deposition can occur (a) while the plasma is
ignited (plasma polymerization) or (b) in a two-step process:
(b1) creation of radicals at the fibre surface in an inert plasma
(e.g. argon) and (b2) reaction of these radicals with unsaturated
monomers (plasma grafting).
By using a corona discharge, hydrogen silicone fluid was
grafted on polyester fabric [148]. Contact angles varied with
initiator concentration and treatment duration. The untreated PET
3435
showed a contact angle of 71 and obtained the highest angle of
127 after a 30 s treatment. Reduction of contact angles after long
corona treatments is probably due to the oxidation of the silicone,
with the introduction of hydrophilic functional groups.
Iriyama et al. [149] treated a polyamide 6 fabric in various
vacuum plasmas containing fluorine in some form: saturated
(CnF2n + 2, n = 1 4 and 6), unsaturated (C2F4 and C3F6) and a
mixture of CF4 and H2. The treated samples were consecutively
machine washed for 30 min and dried at room temperature. For
all samples treated in the saturated fluorocarbon plasmas the
contact angle was equal (130), regardless of the molecular size
of the fluorocarbon, while it reduced equally to 125 after
washing. It was stated, however, that it was dangerous to draw
conclusions from contact angles alone. The water droplet
rolling-off angle (WDRA) proved to be more adequate in
notifying differences between the monomers used. The
hydrophobic effect seemed to have been lost for CF4 and
C2F6 plasmas, and largely retained for the C3F8, C4F10 and
C6F14 plasmas.
Recently, Shen and Dai studied the treatment of silk and
cotton fibres by a C3F6 vacuum plasma [150]. Table 2 shows the
contact angles before and after different treatment times. After
only a 1 min treatment, contact angles changed from 0 to 120.
Longer treatment times did not result in a substantial increase in
contact angle. Using XPS, the authors observed on both fibre
surfaces the incorporation of CF, CF2 and CF3 groups.
After washing with water and alcohol extraction, partial loss of
fluorine from the surface was observed, but contact angle
measurements on the fibres still showed largely improved
hydrophobic properties.
Zhang et al. deposited a nanoparticulate hydrophobic film
onto cotton fabrics [151] and reported contact angles of 164
after a treatment of only 30 s. In this paper, the fluorocarbon
used for plasma polymerisation was not specified, but the
authors referred to [152] for a description of the coating process
where they used perfluorohexane or octafluorotoluene. It was
not clear if these two monomers were also used in [151] to
produce a hydrophobic film.
Some authors reported on the penetration of hydrophobic
coatings induced by plasma in textile structures [4953]. Krentsel
et al. [4951] studied the penetration effects of CF4 and C2F4
glow discharge and low temperature cascade torch plasmas on
different sheets of PET non-wovens, while Mukhopadhyay et al.
[52,53] coated different layers of cellulose-based filter papers
Table 2
Contact angle of silk and cotton fabrics treated by C3F6 plasma for various
treatment times [150]
Exposure time Contact angle ()
(min)
Silk Cotton
0 0 0
1 119.4 2.0 124.2 0.9
3 123.9 2.6 127.2 1.6
5 122.1 2.1 127.5 1.6
10 122.0 0.8 127.9 1.7
3436 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
with different fluorine-containing monomers to enhance their
hydrophobicity.
Chaivan et al. used a low pressure SF6 plasma to improve the
hydrophobic properties of silk [153]. After a 3 min treatment the
contact angles increased from 70 for the untreated samples to
130140. Hydrophobic properties can also be introduced on
polyester fabric by a 10 min plasma grafting of methylmethacrylate
or vinyltrimethoxysilane [154]. Riccardi et al. developed together
with a variety of diagnostic tools a small reactor for industrial
applications based on a low pressure SF6 RF plasma reactor and
achieved improved hydrophobicity on textiles [155,156]. Hochart
et al. induced hydrophobicity with a low pressure microwave
plasma on polyacrylonile (PAN) fabrics by graft-polymerisation of
fluorinated methacrylate [157]. Vaswani et al. used CF3CHF2 and
C4F8 as monomers for plasma polymerisation on cellulose fibres
to enhance their hydrophobicity [158].
A side-effect of hydrophobic fibre coatings is that, though
the fabrics themselves are water repellent, the fibrous structure
allows water vapour to diffuse from one fabric side to the other.
This effect which improves garment comfort properties is
applied in sports and other protective garments, and can also be
obtained after fibre coating via classical wet processing. Both
plasma and wet processing for hydrophobic fibre coating
deposition compete with products such as Gore-Tex, which is a
relatively expensive microporous polytetrafluoroethylene
(PTFE) membrane requiring a supporting fabric and which
has a lower vapour permeation than a normal fabric. Largest
disadvantage of fibre coatings is their lack of durability because
very thin layers are deposited on soft substrates.
Hegemann reported on the plasma activation in a low
pressure RF discharge with Ar/O2 of PET fabrics followed by a
wet-chemical fluorocarbon impregnation to achieve oleophobic
fibres [159]. The plasma activation led first to a more wettable
surface. This increased wettability enabled an enhanced uptake
of conventional fluorocarbon liquids.
2.5. Deposition of fibre coatings
A plasma is used as a means to deposit nanometer thick layers
of (in)organic or metallic material at a fibre surface. Several
methods of plasma assisted deposition on textiles have been
proposed. A first group uses thermal evaporation, sputtering or
anodic arc evaporation at low pressure to vaporize metals and
polymers and to condense the gasified material onto a substrate
(physical vapour deposition PVD). A second group makes use
of monomers in gaseous or aerosole phase which are deposited
as a three-dimensional and cross-linked polymer network at the
substrate surface; this method is also called plasma polymerisa-
tion. Plasma deposition is different from plasma grafting; the
former is a one-step in-situ method, while the latter has separate
radical-forming and (non-plasma) graft-polymerisation steps.
Textiles used for plasma deposition can also be pretreated in a
plasma, but in this case rather to clean the fibre surface from
impurities than to create surface radicals. Plasma deposition is
limited to very thin layers (up to 200 nm) on the individual
fibres, and is therefore different from textile coating, which puts
a layer up to a few mm on top of a textile structure.
2.5.1. Metallic coatings
The oldest type of PVD is by thermally vaporising metals
with a relatively high vapour pressure, such as aluminium,
copper and silver. Another common technique is sputtering of a
metallic target. Dietzel et al. [160] applied PVD arc coating to
polyamide fabrics at low pressure. The samples were cleaned
and activated by an argon glow discharge, after which deposition
was performed between 15 and 45 min. Titanium and zirconium
cathodes were used as deposition material. Mixtures of argon
with nitrogen or acetylene were used to deposit layers of metal
nitride respectively metal carbide. Oxygen, which originates
from fibre adsorbed water or from polymer degradation was
found in the deposited material in high concentrations. The
zirconium based coatings showed better abrasion resistance.
Only high nitrogen content titanium nitride coatings resisted
washing tests. Electrical resistivity, which is above 1012 for
untreated polyamide, was reduced most (down to 105 ) for
titanium based coatings after long treatment durations.
Metal coated textiles are used in protective coatings (cold,
heat), in protection against electromagnetic radiation, and for
their antibacterial properties [161]. However, due to their low
adhesion, the deposited layers have to be protected by an
additional polymer coat.
2.5.2. Polymer coatings
Pane et al. [162] treated acrylic fabrics for outdoor use in a
plasma of a mixture of a fluorocarbon monomer with argon or
methane, for 15 min at low pressure. First, prior to polymerisa-
tion with a traditional wet chemical treatment, the fabrics were
pre-treated in an oxygen plasma at various pressures for 3 to
10 min. The plasma cleaning step did not significantly decrease
the surface extractable matter, but clearly improved both the
water contact angle and the water penetration properties of the
fabrics after a traditional wet chemical application of a
hydrophobic finish. Secondly, the traditional wet chemical
treatment was replaced by a plasma polymerisation. Plasma
cleaning and plasma polymerisation resulted in a water
column (i.e. resistance to hydrostatic water penetration) of up
to 37 cm and a contact angle of up to 140, as compared to 20 cm/
118 and 32 cm/133 for unwashed and washed untreated
fabrics, respectively. Mechanical properties were improved, as
compared to the untreated as well as traditionally treated fabrics.
Castelvetto et al. compared a two-step process with a what
they called one-step process for the polymerisation of
functional acrylic monomers onto cotton fibres [163]. In the
two-step process, a cotton fabric was RF argon plasma-treated at
low pressure (in-situ) and then placed in a monomer solution
(ex-situ). In the one-step process cotton fabrics were impreg-
nated with monomer and then treated by the RF argon glow
discharge. The efficiency of both processes strongly depended
on the monomers used. For the less volatile fluorinated
monomer 1,1,2,2-tetrahydroperfluorodecyl methacrylate, a
one-step plasma treatment on a pre-impregnated substrate was
required. On the contrary, with 2-hydroxyethyl methacrylate
better results were obtained by a two-step process.
Vander Wielen et al. reported on the grafting of acid
monomers on cellulose fibres initiated by a DBD [164,165].
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449 3437

The cellulose fabrics were first sprayed with an aqueous phosphate and phosphonates derivatives) on cotton fabrics
monomer solution and afterwards dried. Thereafter, the cellu- induced by argon plasma [172]. In order to produce multi-
lose sheets were treated by a DBD to enhance the polymerisa- functional surfaces, they studied in a subsequent paper the
tion and incorporation of the monomers. combination of a water repellent treatment (CF4 plasma) and fire
Chen et al. used plasma as a pre-treatment step before graft retardant finishes on cotton fabrics [173]. Fig. 4 clearly shows
polymerisation of acrylamide on PP fabrics [166] to enhance the water-repellent properties of cotton fabrics treated with
their long term water adsorption. Although the surface of the PP diethyl(acryloyloxyethyl)phosphoramidate (DEAEPN) before
fabric can be changed from hydrophobic to hydrophilic after and after grafting and polymerisation of AC8 (1,1,2,2,tetrahy-
plasma treatment, it would obviously age after some days. In droperfluorodecylacrylate), washing, and drying at 373 K.
contrast, with the UV-induced graft polymerisation of PP, the The use of non-thermal plasmas for biomedical applications is
fabrics were able to keep their hydrophilic properties during for the moment the booming branch of plasma technology.
7 days due to the covalently grafting with hydrophilic monomer. Therefore there is e.g. growing interest in making certain textiles
One of the latest developments in plasma finishing of textiles biocompatible. Chen and Chiang [174] used a DC pulsed
is atmospheric pressure plasma liquid deposition (APPLD), discharge to activate PET/PE non-woven fabrics (NWF) followed
developed by Plasma Ireland and the University of Durham, and by thermal-induced graft polymerisation with acrylic acid.
commercialised by Dow Corning Plasma, in which atomised Improved biocompatibility of the modified NWF was confirmed
liquid droplets are injected into the active plasma region with 3T3 fibroblast cells. More cells were found to attach to the
[167,168]. The atomised liquid is generated via an ultrasonic modified surface with higher growth rates, indicating that the
nebuliser. Contrary to most vacuum plasma polymerisations the treatment is beneficial for cell attachment and growth.
monomeric or oligomeric substances are not destroyed during
APPLD; thus, they can be deposited (polymerised) at the surface 2.6. Surface cleaning: desizing, removal of impurities
while retaining the original functionality of the monomer
(oligomer). Hydrophobic polysiloxane coatings were deposited When using a plasma treatment for surface cleaning,
on precleaned cotton fabrics in a helium discharge of selectivity of the plasma for the material to be removed from
tetramethylcyclotetrasiloxane (TMCTS) or octamethylcyclote- the fibre surface is required, since the fibre structure itself
trasiloxane (OMCTS) precursors, leading to a water contact should not be damaged. The use of plasmas for desizing of
angle of 140. Non-treated cotton wets immediately. By cotton and polyester-cotton was first described as early as 1973
changing to an oxidative helium/oxygen plasma, TMCTS and [175]. The technique was presented as a novel approach to the
OMCTS precursors result in hydrophilic SiOx coatings.
There are several textile related aspects which have to be
taken into account when considering plasma polymerisation as a
means to give special properties to a textile substrate. A
majority of applications aim at giving the textile superior
hydrophobic properties. This is usually done by polymerisation
of unsaturated fluorocarbons such as perfluoropropene. How-
ever, Vohrer et al. [169] concluded that oxygen species in the
plasma can considerably reduce the hydrophobic performance
of the deposited polymer. Recently, Shahidi et al. reported on
the same problem for cotton fibres with a metallic coating (see
previous section) [170]. The oxygen can be due to desorption of
water from the fibre, or from plasma ablation of oxygen-
containing fibre polymer or fibre lubricant. Washing and drying
of the textile prior to the plasma treatment, or a prolonged
vacuum treatment before plasma ignition are ways to reduce the
sources of contamination. Another aspect is the unidirectional
approach of plasma excited species at the moment of interaction
with the fibre surface, which results in the plasma polymerisa-
tion induced dyeability to be observed only for the fibre surface
directed towards the plasma. While this aspect is not relevant
when treating foils, it is essential for textile applications aiming
at modifying the textiles complete fibre surface, i.e. also the
surface that is not in direct contact with the plasma. A final
aspect is the large width of the substrate to be treated, which
requires an optimum distribution of monomer in the plasma
polymerisation zone [171]. Fig. 4. Water-repellent properties of cotton fabrics treated with DEAEPN (a)
Recently, Tsafack and Levalois-Grtzmacher reported on the before and (b) after grafting and polymerisation of AC8, washing, and drying at
grafting and polymerisation of fire retardant monomers (acrylate 373 K [287].
3438 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
environmental problems of desizing in the textile finishing
industry. Cotton, polyester and cotton-polyester fabrics con-
taining 8.4% weight of fibre (w.o.f.) polyvinyl alcohol (PVA)
size were treated in a RF plasma afterglow in O2, N2 and air at
low pressure, and in an atmospheric pressure corona discharge.
The oxygen plasma treatment was the most efficient one, while
the N2 plasma was not effective at all and air plasma caused
intermediate results. Corona treatments of identical fabrics
failed to show weight loss, even after long treatment times
(20 min). The developed plasma desizing process finally
consisted of two steps: an oxygen plasma treatment during
which the PVA polymer is degraded into gaseous compounds,
and a subsequent aqueous washing step which removes the size
which was not removed during the plasma treatment. After a
10 min plasma treatment almost 60% of the size was removed; a
subsequent cold rinse removes another 35%. A cold rinse
without a previous plasma treatment removed only 11% of the
size, while a conventional hydrogen peroxide desizing method
removed 82%. Loss of fibre mass, which should be minimised,
is less than 4% in plasma conditions were 60% of PVA is
removed. This is somewhat logical because the layer of PVA
must be removed from the yarn before the fibre surface can be
etched away. No significant loss in fabric strength was noted.
Cai et al. [176] applied air/He and air/O2/He atmospheric
plasma treatments to desize PVA on cotton. The air/O2/He
treatment showed to have a greater effect on PVA than the air/He
plasma. Both plasma treatments did not only serve to remove
some PVA size, but also to significantly facilitate PVA removal
by subsequent washing. The authors attributed this effect to the
enhanced swelling, dissolving and dispersing of PVA. The
tensile strengths of the fabrics and yarns were not statistically
significantly affected by the plasma treatment. The same authors
also applied both treatments for desizing PVA on rayon (viscose)
fabrics [177]. Both treatments were able to remove some of the
PVA on the rayon and increase PVA solubility in cold water,
resulting in a higher weight loss in cold washing. The effect of
the atmospheric pressure plasmas became greater as the treat-
Fig. 5. Effect of microwave plasma cleaning with different gas mixtures and varying pressure [288].
ment time increased. Plasma treatment followed by one cold and
one hot washing had the same effect as the conventional
chemical treatments followed by two cycles of cold and hot
washing. The plasma treatment did not have a negative effect on
rayon fabric tensile strength. In another paper, Cai et al. [178]
compared the effect of an air/O2/He plasma treatment on
desizing PVA on cotton fabric with the conventional H2O2
desizing. A 5 min plasma treatment followed by one cold wash
showed to be competitive with the H2O2 process (2 cycles of
cold and hot wash), and an 8 min plasma treatment followed by
one cold wash gave even better results.
Rakowski et al. [179] reported the desizing of glass fibre
fabrics containing 1.09% of paraffin size to levels of 0.3% after
a 5 min O2 plasma treatment. Common desizing procedures for
glass fibre fabrics involve the lengthy heating of fabric rolls in a
carefully controlled temperature regime and atmosphere, e.g.
4872 h at 620 K in nitrogen.
Wei et al. showed that low temperature plasmas are effective
in the removal of organic size from ceramic fibre surfaces [180].
The desizing of organic starch glass fibre was studied in a RF
plasma reactor donated by IBM [181]. Plasma etching of starch
size from the glass yarn/fibre surface is especially attractive
because (a) the plasma is selective for the organic matter, with
no weight loss for the glass fibres, and because (b) glass fibres
are less heat sensitive than most textile fibres, which allows for
high plasma power density levels. Traditional heat cleaning can
take up to four days in an oven; the low pressure plasma
desizing could be accomplished in about 30 s. An advantage of
the cold plasma removal of size on glass fabrics used in printed
circuit boards is that contrary to traditional heat cleaning no
surface migration of sodium, aluminium and calcium ions takes
place. This has a positive effect on the electrical resistivity of the
treated fabric.
A comparative study between plasma and wet chemical
cleaning of synthetic fibres was done by Keller et al. [182]. In
this work, different cleaning methods were compared in order to
remove sizes on PET multifilament fibres, namely chemical
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
cleaning by Soxhlet extraction and by cleaning in a lab-built
bath, as well as etching in atmospheric and low pressure micro-
wave plasma, and in a RF plasma. Fig. 5 shows the effect of a
microwave plasma cleaning process with different gas mixtures
and varying pressure. It was found that both parameters were
key factors for desizing. The best result was obtained with a 1:1
gas mixture of argon and nitrogen at a pressure of 0.53 kPa
(power = 18 W). Different criteria, such as efficiency, flexibility,
ecology and industrial applicability were evaluated. In terms of
these criteria, the authors claimed that the RF plasma showed
the best performance. The continuous fibre treatment in a low
pressure He/O2 RF discharge enabled the complete removal of
4.4 wt.% size at a velocity of 10 m/min. Although atmospheric
and low pressure microwave discharges showed higher
efficiencies, their application was limited due to the high heat
loads yielding degradation of the PET fibres before cleaning
was completed. Both evaluated chemical methods produced
large volumes of waste and a nanolayer of size remained on the
fibre surface. D&K Consulting also published a short com-
parative study between plasma techniques versus wet pre-
treatments for desizing textiles [183].
2.7. Inactivation of micro-organisms: disinfection/sterilization
A plasma can be an efficient sterilising tool via vacuum
pressure, highly energetic UV light and/or reactive plasma species.
The idea of using electrical discharges for sterilization is one of the
first reported plasma treatment effects, e.g. in a patent from 1938
[184] in which small insects are aimed at. More recently the
OAUGDP by Roth et al. is being used for the decontamination of
HVAC filters [185] and other non-wovens (e.g. PP melt blown
webs) [186]. Different reactor setups have been developed [187
189]. Fig. 6 shows the survival curve for the micro-organism E.
coli K12 on a PP sample. Short treatments of about 25 s were
sufficient to decrease the number by a factor 105106. Apart from
the plasma parameters, the efficiency of decontamination depends
on the micro-organism and the substrate on which it resides.
Fig. 6. Characteristic survival curve for micro-organisms on a PP sample containing
an initial loading of 6 106 E. coli K12 cells treated by an OAUGDP [289].
3439
Typically, 99.99% of captured micro-organisms were destroyed
within 5 s (direct parallel plate OAUGDP, E. coli) to 10 min
(afterglow OAUGDP, certain viruses).
When medical textiles having specific surface properties are
to be sterilized, a plasma treatment could alter these surface
properties and render the medical devise useless. Plasma
sterilisation of textiles (aimed at destroying residing micro-
organisms) seems therefore limited to non-medical applications,
such as the applications mentioned above. Nevertheless plasma
technology offers different biomedical applications for other
purposes like described in Section 2.5. Borcia et al. e.g. reported
on the DBD treatment of non-woven PE (Tyvek) medical
packaging material [190]. A DBD treatment offers the
possibility of improving seal quality of packaging materials.
This material sealing often is the most critical step in packaging
manufacture. Another medical application was reported by Virk
et al. [191]. The non-woven fabric Sontara, commonly used
for surgical gowns, was treated with antimicrobial finishes and a
plasma containing fluorocarbon gas. The plasma treatment did
not alter the weight, thickness, stiffness, air permeability,
breaking strength and elongation. Plasma-treated and water
repellent Sontara samples showed higher blood and water
resistance compared to other treatments. Plasma-treated sam-
ples also showed a zone of inhibition for Staphylococcus
aureus, thus providing a barrier against microbes. Yuranova et
al. studied the beneficial antibacterial activity of silver grafted
on textile fabrics by a RF plasma [192]. A minimum loading of
silver was necessary to inhibit the bacterial growth, like E. coli.
As is the case for many plasma-for-textiles applications, the
effectiveness of a sterilisation process depends on the ability of
the effect to penetrate in a textile structure.
2.8. Influencing physical properties of fibres
2.8.1. Optical properties
The treatment requires efficient physical removal of fibre
surface polymers for the creation of microscopic pits. Treat-
ments have been specifically done to decrease light reflection at
the fibre surface, so that a dyed treated textile acquires a deeper
shade; an effect especially looked after with (microfibre) fabrics
coloured in black and other deep colours. The colour depth of
black fabrics is usually expressed as lightness L, which is one
of the three coordinates in the CIE-Lab colour representa-
tion system. An L-value can range from zero for black, to 100
for white. The other coordinates are a (the greenred axis) and
b (the blueyellow axis); they determine the hue (h) and the
chroma (C) which is a measure of the saturation of a colour
of the textile. The colour difference, E, expresses the change
in colour after treatment, and is a function of L, a and
b. Spectral changes can be visually assessed from E = 0.5
or larger. It should be noted that, the use of plasma to deepen the
colour of a textile, requires the treatment to only change the
depth of the colour, so preferably without changing its chroma.
Strictly speaking, the values for a and b should not change
during the treatment; only the one for L should change in
casu decrease. However, most publications report only E, so
a full assessment of the plasma treatment cannot be made.
3440 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449

The decrease in reflection after a plasma treatment is caused Table 3

by the creation of ripples (a.k.a. sea-shore structure) and Change in whiteness of wool of different fineness treated with a gliding discharge
in different environments [199]
microcraters, a feature first described on PET fibres by Byrne
and Brown in 1972 [193] after a 3 h, low pressure argon plasma Fineness Treatment time Environment Change in whiteness
(s) (%)
at 3.14 MHz. The created surface roughness causes the incident
light to be scattered rather than specularly reflected. For 58s 10 air +32
20 air +8
optimum colour deepening the size of microcraters should be
10 air + water mist +13
between 0.1 and 1 m, i.e. around the visible wavelength range 20 air + water mist +7
(0.40.7 m). The influence of plasma current frequency on the 10 air + water steam +23
resulting fibre surface topography was shown by Wrbel et al. 20 air + water steam +13
[31]. For a 4 min low pressure treatment in a nitrogen plasma 20 O2 36
64s 10 air +4
the mean size of created pores decreased with increasing
20 air +5
frequency (50 Hz, 5 kHz or 100 kHz). 10 air + water mist +9
An argon plasma treatment at low pressure of black (acid) 20 air + water mist +5
dyed wool and silk fabrics induced E values of 0.25 10 air + water steam +16
respectively 0.77 after 300 s of treatment. Similar results are 20 air + water steam +22
70s 10 air +1
obtained for polyamide 6 and Chinon textiles [194], for which
20 air +6
non-reflective black textiles are created with an L value of 10 air + water mist +3
around 5, down from a value of 1520 for the untreated ones. 20 air + water mist +4
Sputter etching and argon plasma treatment was also 10 air + water steam +3
performed on disperse black dyed Technora, Kevlar (para- 20 air + water steam +2
20 O2 23
aramid), and Conex (meta-aramid) fabrics [195], and on yellow,
red and blue dyed Technora (p-aramid) and Conex (m-aramid)
fabrics [196]. Under identical conditions the microcraters
produced on Conex fibres were much smaller than the ones
created on Technora, which resulted in a smaller reduction in whiteness, it can be seen that the whiteness was enhanced for all
fibre reflection. Still, the initial lightness of Conex (L = 18.1) air treatments. The whiteness enhancement strongly depended
was lower than the lightness of Technora and Kevlar fibres after on the fineness, the treatment time and the air composition as
a 10 min sputter etching treatment (L = 24.7 respectively 23.0). seen in Table 3. The effect of gas composition was also shown by
It was noted that the overall change in colour (E) of yellow Mak et al. [200] who reported on a tremendous decrease in
fabrics was mainly due to a change in C, while for the blue and whiteness of Tencel after long argon or oxygen plasma
red dyeings the change in colour was caused by a change in both treatment. To enhance the whiteness of cotton fabrics,
L and C. Prabaharan and Carneiro [201] suggested a two-stage process,
Tsai et al. [33] reported a significant physical etching of PP where the plasma-treated cotton fabric was further treated with
melt blown fibres after treatment in the OAUGDP. Though hydrogen peroxide. In this way, they achieved an acceptable
detailed treatment conditions are not mentioned, the fact alone whiteness with the additional benefits of saving time, saving
that the creation of micro-etchings is possible at 1 atmosphere thermal energy and saving water and chemicals.
without visible thermal degradation of the fibres is worth To improve the deep colouring effect of PET fabrics, Lee
mentioning. Tsai et al. [197] also treated melt blown and elec- et al. deposited anti-reflective coatings on the PET surface with
trospun nylon and polyurethane (PU) with the OAUGDP and two different organo-silicon compounds (HMDS, TTMSVS)
showed that after a 10 s treatment the fabric strength and colour using an atmospheric pressure microwave plasma [202]. They
degrade to a noticeable extent for the electrospun, but not for the analysed the quality of their polymerized thin film with SEM
melt blown, fabrics. and FTIR. Spectrophotometry was used to measure the
The decolourization of denim fabrics after plasma treatment reflectance to confirm the deep colouring effect. It was observed
in oxygen or argon was studied by Ghoranneviss et al. [198]. The that the minimum reflective value was obtained at a film
results showed a better decolourized output for Ar than O2 after a thickness of 150200 nm on PET when using HMDS and
15 min treatment. However, after washing the treated denims, TTMSVS monomers. An addition of O2 promoted the
the O2 treated samples looked better than those treated by Ar. decomposition of organic monomers and contributed to the
Janca et al. reported on the treatment of wool with a gliding enhancement of the colour intensity on the PET surface.
arc discharge [199]. The plasma was generated in a small space Lehocky and Mracek treated PET fibres with a low pressure
between the electrodes and was drifted by a gas flow into a conic RF air plasma [203]. Due to the plasma treatment they were able
space, towards the base of which, the treated wool combed top to use a new dye bath composition without any use of sodium
moved. The gas flow could be loaded with water mist or water sulphate resulting in a coloured fibre with the same reflectance
steam. Table 3 shows the results on the whiteness of the wool of as obtained with traditional dyeing processes without plasma
different finenesses for different treatments. The whiteness was treatment, but with sodium sulphate. In this way, they showed
evaluated by a spectrometer. In contrast to the treatment with an the power of plasma treatment from both ecological and
oxygen plasma where they observed a substantial decrease in economical view.
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
2.8.2. Mechanical properties
The treatment requires physical and chemical etching
process conditions that change the frictional properties of
fibres. Changing the physical properties of yarns and fabrics,
and more in particular their increase in tensile strength, bursting
strength and wear resistance, were among the first positive
effects caused by a plasma treatment on a textile structure.
Already in 1961, Kassenbeck patented a glow discharge reactor
for this purpose [204]. Shrink-proofing of wool is also an
important example of influencing the mechanical properties of
fibres. This subject is not covered in this section. Because of the
large amount of data available in literature shrink-proofing of
wool is discussed in detail in Section 2.9.
Plasma treatments can improve properties such as (tear)
strength, elongation, stiffness, etc. A number of studies were
published by Thorsen from the second half of the 1960s
onwards on improved frictional properties of fibres by AC
corona treatment at atmospheric pressure [205207]. The
tensile strength of wool, mohair and cotton yarns increases
with 1226%, 31% and 28% respectively, even after treatment
as short as 1 s. This frictionising can further lead to improved
mohair carding and to an increase in wool fibre spinning rate
into yarns and improved cotton spinnability. McCord et al.
demonstrated the effect of gas composition of the plasma on
tensile strength of nylon [208]. They had a slight decrease in
nylon fabric tensile strength after treatment in He for 3 min,
while there was no significant change in tensile strength of the
nylon fabric treated with HeO2 after exposure times of up to
8 min. Belin et al. [209] showed that cotton sliver tenacity was
improved for a single corona passage and even more for three
consecutive passes. They also observed an improved wettability
and dye adsorption [210]. In the former case, increased felting
Fig. 7. 3D views of AFM images of PET textile surface. (a) Untreated surface; (b) 60 s treated surface; (c) 120 s treated surface [290].
3441
resistance was obtained by a plasma treatment in air at atmo-
spheric pressure. Belin et al. also reported on experiments
showing similar improvements when chloroform or carbon
tetrachloride was introduced to low pressure glow discharges in
air or acetylene [211]. Lee and Pavlath showed that wool yarn
became shrink resistant and stronger after an afterglow
treatment [212]. Kim and Kang also studied the dimensional
and surface properties of plasma and silicone treated wool
fabrics [213]. Abbott et al. studied the sliver cohesion [214] and,
the yarn and fabric properties [215] of plasma-treated cotton.
The plasma showed to have a positive effect on sliver cohesion,
yarn strength and fabric strength.
The increase in cotton fabric strength can change into a
weakening of the fabric when exposure time is too long
(typically N 10 min). The positive effect of plasma treatment
creation of surface roughness for an increased fibre friction
can be compensated by excessive weight loss and creation of a
brittle, cross-linked surface layer [73].
Blakey and Elalfy observed a deterioration in the tensile
properties due to plasma-etching and the creation of voids due
to the presence of delustrant particles in man-made fibres
[216,217]. In another study, the same authors reported on the
identification of animal fibres, like camel hair, cashmere,
merino wool, human hair and angora-rabbit hair [218]. The
plasma treatment removed the cuticle of the fibre and revealed
the cortex which was analysed with SEM. The observed
physical changes were typical for the animal fibre used.
The treatment of PET fabrics in a SiCl4 plasma has been
done to improve their comfort-related mechanical and surface
properties [30]. The primary effect of the plasma treatment was
on the surface roughness, in good accordance with atomic force
microscopy (AFM) roughness data. A similar AFM study was
3442 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
done by Poletti et al. [219] to quantify the effect of gas
composition on the surface roughness. Fig. 7 shows AFM
images of the untreated and the 1 min and 2 min air plasma
treated PET samples. The surface of the untreated PET textile
appeared to be flatter compared to the treated samples. The
treated samples showed that the air plasma treatment induced
pits and micropores whose density, depth and size increased as a
function of exposure time.
In a series of papers, Vander Wielen et al. [220,221] treated
cellulose fibres with a DBD discharge and analysed the effect of
the DBD on the physical strength and dimensional stability of
the fabrics. Wang et al. [222] studied basalt fibres treated with
an atmospheric pressure plasma in different gas atmospheres.
Their results suggested an increased roughness, while the
strength of basalt fibres was slightly reduced. Yip et al. studied
the treatment of nylon by low temperature plasmas in different
papers [223225] and observed physical changes on polyamide
fibres in the form of ripple-like structures of sub-micron size
that were induced by plasma etching [225].
Titov et al. reported in a series of papers about the
fundamental study on etching of PET fabrics in different
conditions [226232]. Among others, the effects of texture,
specific surface area, gas composition, afterglow and
temperature were investigated by rate of mass loss and
evolution of gaseous products. In different papers [233235],
Sun and Stylios studied a low temperature plasma treatment
of cotton and wool. Next to a changing wettability depending
on gas composition, they observed a slight loss in elasticity
after plasma treatment. The tensile strength increased after
plasma treatment, while the stretch of the material was
reduced.
Huang et al. [236] treated viscose-based activated carbon
fibres (ACFs) with a DBD plasma in nitrogen. ACFs have
attracted extensive interest to be used as catalyst or catalyst
support due to their unique properties. Chemical functionals
existing on the ACF surface can act as active centres or
adsorption sites and are responsible for the catalytic activity of
the fibres. The DBD nitrogen treatment was responsible for the
etching of the surface and for an increased roughness resulting
in a larger surface area favourable for catalyst activity. XPS
revealed that the treatment changed the distribution of the
oxygen functional groups. Su et al. [237] showed that after
plasma modification, the adsorption of carbon monoxide by the
carbon adsorbent was about 8 times better than for non-treated
carbon fibres. Wen et al. reported on the ammonia plasma
treatment of carbon fibres resulting in damage of the
microstructures of carbon fibres [238].
2.8.3. Electrical properties
The treatment requires the introduction of functional groups
at the fibre surface which, by hydrogen bonding with
atmospheric water, decrease the resistivity of the treated textile.
Rashidi et al. studied the effect of a low pressure air plasma on
the surface resistivity of cotton and PET fabrics and observed a
decrease in surface resistivity after plasma treatment [239]. Bhat
and Benjamin treated cotton and polyester fabrics at different
power levels in a 13.56 MHz air plasma for durations between 10
and 60 s [240]. Following this air plasma treatment the fabrics
were grafted in an acrylonitrile plasma or in an aqueous
acrylamide solution of different concentrations. The surface
resistivity at 70% RH was considerably reduced for the grafted
polyester fabrics. This reduction was linked to the increased
moisture content of the treated fabrics. On the other hand, Byrne
and Brown [193] deposited acrylic acid with a 3.14 MHz plasma
at low pressure. A treatment of 1 min, caused the resistivity of the
polyester fabric substrate to increase from 1012.6 m to more
than 1015 m, even though the deposited acrylic acid is
expected to increase the moisture content in the same way as
acrylamide does.
Oh et al. reported on the effect of plasma treatment gas on the
electrical conductivity of polyaniline-nylon-6 fabrics [241].
Plasma surface modifications with oxygen, ammonia and argon
were performed at low pressure on the nylon-6 fabrics to
improve the adhesion and the rate of polymerisation. After-
wards the plasma-treated fabrics were immersed in an aqueous
hydrochloride solution of aniline. Successive polymerisation
was initiated with a mixture of an oxidant/dopant solution
containing ammonium peroxydisulfate and HCl. The fabrics
treated with an oxygen plasma showed the highest conductivity.
The conductivity of the oxygen plasma-treated polyaniline-
nylon-6 fabric was more stable with repeated washing and
abrasion cycles than polyaniline-nylon-6 fabric without plasma
pre-treatment.
Hautojrvi and Laaksonen [242] studied on-line corona
treatment of PP fibres during melt spinning. Corona treatment
resulted in a substantial decrease in contact angles. With
amounts of added spin finish lower than 0.2% by w.o.f., treated
fibres had considerably better antistatic properties than
untreated fibres. Treated fibres had an electrical resistance an
order of magnitude lower and about 50% less static charge
builded up during carding.
Recently, Liu et al. [243] modified the morphology and
composition of acrylic fibres with a low pressure nitrogen glow
plasma. The overall surface roughness increased with increas-
ing treatment time. XPS analysis showed that hydrophilic
groups were inserted at the surface. Table 4 shows the contact
angles and the antistatic ability of the untreated and treated
samples for different treatment times. The static ability was
tested with a static tester and quantified via the state half-decay
time of the fibres. This value was half of the time needed for a
fibre to completely discharge the static charges imposed by the
test machine [243]. The shorter the half-decay time is, the better
Table 4
Wettability and antistatic ability of the untreated and plasma-treated samples
[243]
Samples Contact angle Half-decay time
() (s)
Untreated 77.80 9.57
N2 plasma treated
1 min 65.64 3.98
3 min 34.92 1.35
5 min 56.41 2.62
7 min 54.73 3.16
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
the antistatic ability of the fibres should be. Next to an increase
in hydrophylicity, a drastic increase in antistatic ability was
reported due to changes in surface morphology and due to the
introduction of polar groups at the surface.
Aubrecht et al. [244] treated PET fabric with a low pressure
O2/CF4 13.56 MHz plasma and surface resistance was
significantly reduced from 1014 to 108 . One week after
treatment the original surface resistance was reached again.
2.9. Shrink-proofing of wool
The treatment requires physical and chemical etching
process conditions that change the frictional properties of
wool fibres. The shrinking of woollen textiles (a.k.a. felting) in
the presence of water and mechanical agitation is due to the
occurrence of scales at the wool fibre surface. Both kinetic and
static effects are involved. Kinetically, the most important
physical property is the difference in frictional coefficients in
the against-scale and with-scale directions (differential friction)
[17]. Statically, the hydrophilic character of the fibre surface is
most important. Physically, shrink-proofing by plasma is caused
by an increase in fibre-to-fibre friction and a decrease in
differential friction. Chemically, it is cause by the increase in
surface charging via the incorporation of hydrophilic groups at
the fibre surface.
Carr et al. [245] investigated the effect of dry corona treatment
and aqueous treatments on the hygral expansion of wool. The
chemical changes at the fibre surface were characterized by XPS.
After an intensive corona treatment, they found that the extent of
oxidation of disulphide bonds to S(VI) in the form of sulphonic
acid groups (SO3H) was about 47%, as compared to 100% for
wet chlorination. This lower sulphonic acid content is compen-
sated by the formation of hydroxyl and carbonyl functions
attached to the carbon of the protein structure, the concentration of
which depends on plasma power.
Lee and Pavlath found that the shrinkage of wool yarn in a
vacuum discharge afterglow was almost equally effective in a
hydrogen plasma than in an oxygen plasma [212]. Possibly, for
a hydrogen plasma treatment the oxidation of the fibre surface
occurs by a post-plasma reaction of free surface radicals with
atmospheric oxygen and water. This apparent contradiction
stresses the importance of parameters such as post-plasma
ageing conditions.
One of the oldest and most investigated plasma effects to
date, shrink proofing of wool by plasma was initiated to replace
wet chemical processes that cause various degrees of environ-
mental stress. For this purpose plasma processes were
developed on pilot scale and industrial grade reactors, both at
atmospheric pressure [246], and at reduced pressure
[212,247,248]. Apart from vacuum batch processing of fabrics,
vacuum plasma reactors have been developed for the contin-
uous treatment of slivers and yarns, by treatment in a plasma
glow [248] and in a plasma afterglow [249]. Evaluation of wool
propensity to shrinking is assessed via the directional frictional
effect (DFE), fabric dimensional change (FDC), and the felting
ball test (FBT). Plasma and other anti-felting treatments aim at
reducing the DFE and FDC, and increasing FBT values.
3443
Thorsen published a series of studies on the AC corona
treatment of wool and mohair card webbing, top, yarn and
fabric [207,246,250] at temperatures between 373 K and 413 K.
Temperatures were kept high to reduce ozone formation.
Usually, one of the large plate electrodes was covered by a
dielectric material. When treating undried samples at higher
voltages, both electrodes where covered in order to prevent
small holes being burned in the samples and to reduce the
sticking of card webbing to the electrodes. Shrink proofing was
successful for treatment durations between 4 and 30 s,
depending on the form in which the fibres were treated (loose
fibres, card webbing or top). The increase in with-scale friction
decays slowly with time after treatment, against-scale friction
does not (up to at least 1000 h) [206]. Fabric samples could not
be made shrink-proof because the gaseous reactants did not
penetrate adequately, however, shrink-proof fabric could be
made of yarns spun from treated card webbing. All treatments
harshened the hand of the fibres, necessitating a subsequent
treatment with softeners. However, shrink proofing was lost
when using cationic softeners. In his publications, Thorsen
gives complete information on the cost and the productivity of
the treatment. A similar approach with the pros and cons of
plasma treatment of wool can be found in [251] by Ganssauge
and Thomas.
The usefulness of corona treatment for various effects can be
increased by multiple passing of the textile through the reactor
[37]. For a desized and scoured cotton/wool fabric a single,
double and threefold corona treatment led to a laundry
shrinkage of 27.1, 22.3 and 21.9% respectively, as compared
to 29.7% for untreated wool/cotton fabric. However, a 3 min
oxygen glow discharge treatment of the same fabric at low
pressure reduces the laundry shrinkage to only 3.9%.
Pavlath et al. produced a series of studies on continuous
plasma treatment of fine wool yarns, both in the plasma glow
and in the afterglow [212,249,252]. Initially the yarns were
extensively extracted with various solvents; later it was found
that cleaning is not necessary when the oil content is less than
1%. The tube-shaped glass reactor had an external electrode
system (treatment in the plasma glow) or an internal inductance
coil (treatment in the glow and in the afterglow), connected to a
13.56 MHz generator. The residence time of the yarn in the
plasma was between 0.5 and 1.2 s. Yarn shrink-proofing values
between 55% and 98% were obtained. For treatments longer
than about 1 s in the plasma glow singeing and yellowing
occurred at high energy densities. Treatments in the plasma
afterglow did not heat the yarn but were less successful in shrink
proofing (up to 73%).
Gregorski and Pavlath [253] studied the shrinkage of a
woollen fabric treated in a 13.56 MHz nitrogen or oxygen
plasma at low pressure with XPS. Only for the oxygen plasma
the reduction in area shrinkage correlated well with both the
increase in oxygen and nitrogen containing hydrophilic groups
at the fibre surface and with the increase in water removable
sulphur-containing groups. After a single 10 min plasma
treatment the area shrinkage was reduced from 45% (non
treated) to 15%. Low angle X-ray diffraction of wool fibres
before and after a 5 min air plasma treatment at low pressure
3444 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
Table 5
Values of the DFE for (non) plasma-treated woollen fibres [248]
DFE method Mercer Lindbergh
Dry Wet Dry Wet
Untreated 0.325 0.352 2.125 2.143
5 min plasma-treated 0.205 0.252 0.931 0.828
showed only a change for the lipid ring, which lost its sharpness
[247]. Though the heat component of the plasma did not induce
structural changes, it is known that the equilibrium water
content of wool reduces with 3 to 4% w.o.f. [248] after a
vacuum plasma treatment. Long plasma exposure destroys the
X-ray diffraction pattern completely.
Rakowski et al. built a pilot scale air-to-air vacuum plasma
reactor [248]. The plasma treatment resulted in a reduction of
DFE, which is the basis for shrink resistance of woollen
structures (Table 5). The natural fat content is reduced with 25%
but the alkali solubility (via ISO 3073, ASTM D1283, ASTM
D1113 standards) which is a measure for fibre damage is
unchanged. The super wash label which allows for 5 to 10%
area shrinkage can be easily obtained by successive plasma
treatment and either a resin treatment or a treatment with a
quarternary ammonium surfactant in the presence of sodium
sulphite reducing agent [254].
In different papers, Kan et al. [255262] reported on the low
temperature plasma treatment of wool fibres. In [256], they
treated wool fibres with low temperature plasma, chlorination,
polymer deposition and their combinations. The plasma
treatment reduced the feltability by 70.3% compared with the
untreated sample, and the chlorination only resulted in a
decrease of 6.3%. The best results (76.6% reduction) were
obtained by a chlorination followed by a plasma treatment.
Plasma treatment, followed by chlorination and then polymer
deposition resulted in a reduction of the feltability of 56.3%.
Also the order of treatment played an important role. The same
3 treatments, but in a different order (chlorination, plasma,
polymer deposition) clearly affected the result: 73.4% reduction
in feltability. Bateup et al. also studied the application of shrink-
resist polymers to pre-treated wool in an atmospheric pressure
air plasma reactor [263]. The critical surface tension was
increased allowing the liquid pre-polymers based on poly
(propylene oxide) and poly(tetramethylene oxide) to spread
spontaneously on individual fibres. The effect of the nature of
the working gas on the plasma treatment was studied by using
three different non-polymerizing gases: oxygen, nitrogen and a
25:75 hydrogen/nitrogen mixture [257,259]. ATR-FTIR analy-
sis showed that the oxygen plasma was most efficient in the
creation of hydrophilic functional groups. The largest chemical
modification of the fibre surface was obtained after a 5 min
oxygen, nitrogen and hydrogen/nitrogen plasma treatment, for
which an area shrinkage of 1.46%, 2.06% and 1.86%
respectively was obtained, in comparison with 12.28% for the
untreated wool fabric. Kan et al. treated fabrics with an oxygen
plasma [258,262], tested its properties and compared the results
with the industrial requirements. According to them, the low
temperature plasma treatment achieved the industrial require-
ments and was found to increase extensibility and decrease
tearing strength and shrinkage tendency.
Shekar and Bajpai treated wool fabrics with a 13.56 MHz
oxygen plasma at low pressure and observed a significantly
reduced shrinkage [264]. A similar shrink resistance was
observed by Zuchairah et al. after an 8 MHz plasma treatment
and an aqueous polymer treatment [265]. Shrink resistance was
also obtained via a 3 kHz parallel plate glow discharge in 1:1
helium/argon and acetone/argon atmosphere at atmospheric
pressure [266]. After 20 cycles the laundering shrinkage of the
non-treated fabric was 39.4%. A 60 s treatment in He/Ar or
acetone/Ar plasma resulted in a shrinkage of 18.4%, while a
180 s treatment resulted in a shrinkage of 9.1%.
Osenberg et al. demonstrated the applicability of mass
spectrometry to monitor chemical reactions during a wool
treatment process in large-volume plasma sources [267]. They
showed that the ratio of partial pressures of O2, SO2 and CO
could be used to prevent burning of the wool and determined the
felting tendency.
Hcker [268] described a combined treatment with plasma
and with the use of an additional resin coverage of the wool
fibre surface to enhance the shrink-resistance. This led to an
area shrinkage after 50 simulated washing cycles in a do-
mestic washing machine of approximately 1%. This was
competitive with a standard shrink-resist treatment with acid
aqueous chlorine solution, reduction with sulfite, and applica-
tion of a thin resin (polyaminoamide) layer to the surface
(Chlorine/Hercosett process).
To further improve machine washability and handle, plasma
treatments have been combined with the application of chitosan
[269,270] or collagen [271,272] biopolymer. Shrink proofing of
wool via plasma treatment has become less urgent from an
environmental perspective due to a reduced wool fibre
consumption and new, competitive processes. Enzyme treat-
ment is one of these potential competitors, though considerable
disadvantages such as costs, limited shelf life and sensitivity to
denaturation still have to be solved before widespread industrial
use is conceivable. Shrink-proofing will probably remain a two-
step process in which a surface oxidation step (wet chemistry,
plasma, enzymes) is followed by a fibre coating step (synthetic
resin, bio-organic resin).
2.10. Improving the efficiency of wet finishing processes
The treatment effect has to optimise the interaction between
fibre surface and the finishing product that is added to a bath or
foam. The effect can be advantageous on two levels: (a) due to
improved wetting properties of the textile product, less or no
chemical wetting agent is needed, and (b) because of an improved
interaction between finishing product and fibre surface, less
finishing product is needed for identical properties (better bath
exhaustion). The properties of a plasma-treated and finished
textile can also be improved as compared to a merely finished
textile to which the same amount of finishing product is added.
An example is the improvement of wool felting resistance
even though less resin is applied [248]. The minimum effective
treatment level (METL) for a shrink proof resin is reduced from
 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
2.5% w.o.f. for non-plasma-treated wool to 1% w.o.f. for fabrics
made of plasma-treated wool top. Similar effects were found for
knitted goods. Another plasma treatment effect was that the
resin application process does not require the use of sodium
metabisulphite (Na2S2O5) as a reductans; this was an environ-
mental bonus.
In a comparison of four shrink resist polymers normally
applied in a chlorination pre-treatment, Zuchairian et al. [265]
treated hand washed wool fabric in a conventional 8 MHz
oxygen plasma at low pressure. After a 3 h laundry test,
untreated fabric shrunk about 32%; a 2 min plasma treatment
resulted in an area shrinkage of 15%. After the 2 min plasma
treatment, the polymers were applied to the wool fabric by
exhaustion from aqueous solution. The results for hydrophilic
polyamide and acrylic copolymer are better than those for less
hydrophilic polyether and polysiloxane, which suggests that the
increase in hydrophilic character of the fibre surface facilitates
the adhesion and spreading of relatively hydrophilic polymers.
Wong et al. used a 13.56 MHz plasma in oxygen or argon at
low pressure to treat linen fabrics prior to wet enzymatic
treatments [273]. The plasma pre-treatment resulted in changes
of fibre surface chemistry and morphology. The change in
morphology was studied in detail in [274]. By means of the
plasma pre-treatment, the effectiveness of the enzyme treatment
was enhanced and a faster reaction rate was achieved, while the
strength loss was acceptable. The fabric whiteness was reduced
after the plasma pre-treatment, but subsequently it could be
effectively recovered by the enzyme treatment. Also Yoon et al.
[275] reported on the combination of a plasma pre-treatment
and enzymes. Close to this research, the paper of Zanini et al.
about the comparison of the effectiveness of plasma treatments
versus biological enzyme treatments is worth mentioning [276].
2.11. Formation of radicals
The working gas and the treatment conditions must be
optimised towards maximum production of surface radicals.
Wakida et al. [277] and Chen [278] did a virtually identical
study on the creation and stabilisation of free radicals for a range
of fibre types treated in different plasma gases. Electron Spin
Resonance (ESR) spectra were used to assess the relative
amount of radicals remaining in the fibre polymer structure after
24 h of ageing in dessicator conditions. The ESR signal
increased with treatment duration and also depended on the
plasma treatment pressure, for which an optimum exists.
Following order was found for the fibres (relative intensity for
a 180 s treatment): cotton linen N mercerised cotton N polyno-
sic fibre N viscose N wool N silk N polyamide 6 N PET; after a CF4
plasma values range from 2.9 to 4.9 for cotton and linen, to 0.0
to 0.2 for PET, showing the large influence of fibre type on free
radical stabilisation. Within cellulosic fibres, free radicals
recombine more easily when the fibre structure is loose, such
as is the case with mercerised cotton as compared to native
cotton. The type of gas also had a profound influence on free
radical creation: CF4 N CO N H2 N Ar N CH4 N N2 O2. For cotton
fibres, values range from 2.9 to 4.9 after a CF4 plasma, to 0.3 to
0.5 after an O2 plasma.
3445
Molina et al. reported on the presence of stable free radicals
in merino wool fibres treated by low temperature plasmas in
nitrogen, air and water vapour [279]. The presence of radicals
depended on the treatment time and the kind of gas used for
plasma generation. Sadova identified with ESR cystine, peptide,
alanine and glycine radicals on wool fibres treated by a low
pressure glow discharge [280].
Ward and Benerito [281] associated the radicals produced on
cotton by RF plasma treatment in N2 and NH3 with the rupture of
glycosidic bonds, with the formation of activated carbonyls and
U U
with the creation of free radicals such as is -H2C , H2C-O and
RHC-OU in the glucopyranose ring. In their study, they found
that the ESR signal from NH3 plasma-treated cotton was lower
than the signal from N2 treated samples (after a 1 h treatment).
Radicals at the fibre surface initiate polymerisation processes
during (in situ) or after the plasma treatment (ex situ). Apart
from the plasma conditions the fibre type plays an important
role. The creation of radicals and the consecutive grafting of
acrylic acid on polyester fabrics was, in fact, one of the early
(1975) reported applications of industrial plasma technology on
textiles [282].
3. Conclusion
The main purpose of this review was to offer the reader a
chance to evaluate both the wide variety of obtainable effects
and the different paths to reach those effects. By stressing on the
treatment effects rather than on the application field of the
obtained effect the interested reader is offered a background
from which applications yet unthought-of can be developed.
The main conclusions from this review can be summarised into
the following points: (1) a large range of effects can be induced
on a textile by a cold plasma, including novel textile properties,
(2) a large variety of plasma treatment conditions can result in
the same effect, (3) cold plasmas have a large potential for
economic and ecologic savings, (4) plasma technology is able to
obtain good results (even) with industrial scale reactors, and
(5) plasma technology for textiles was developed during a long
period. It is therefore at least surprising that plasma processing
on an industrial scale has been slow to make an impact in the
textile industry. From this review direct observations can be
made providing a partial explanation on the current situation
of plasma technology in the textile industry: (1) the limited
information available in literature concerning the exact treat-
ment conditions, (2) the very different types of plasma sources
sometimes used, (3) the rarity of scientific reports resulting from
treatments in industrial reactors, and (4) the use of plasma effect
characterisation tools not adapted for textiles. Therefore, to
overcome the scepticism from industry, it is necessary that
researchers in plasma technology for textiles show an open-
minded attitude to the work of their colleagues. If the
researchers' own developed plasma source is not able to
achieve the desired demands from industry, referring the
industrial partner to another research group will not necessary
be harmful or unfavourable for that first research group. On the
contrary, when plasma technology for textiles becomes an
accepted and valid alternative for other processes in the textile
3446 R. Morent et al. / Surface & Coatings Technology 202 (2008) 34273449
industry, every researcher in plasma technology would benefit
from this achievement.
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