MAY 2005 437

Influence of Fiber Surface Purity on Wicking Properties of Needle-Punched

Nonwoven after Oxygen Plasma Treatment
JO VERSCHUREN,1 PETER VAN HERZELE, KAREN DE CLERCK, AND PAUL KIEKENS
Department of Textiles, Ghent University, Belgium

ABSTRACT
Polyester and meta-aramid nonwoven samples were treated at reduced pressure in a
radiofrequency oxygen plasma for between 5 and 30 seconds. The hydrophilic effect of
the plasma treatment was assessed by three consecutive vertical wicking tests on each
sample. The influence of cleaning of the fiber surface before as well as after the plasma
treatment was determined. The presence of fiber surface additives had a positive influence
on first-time wicking. On the other hand, when the layer of surface additives is plasma
treated rather than the fiber polymer surface, the treatment effect is easily washed away.
Log(time) wicking curves and summed wicking height plots are introduced as a means to
help the interpretation of wicking data.

In the course of the last five decades numerous pub-
lications and patents have reported on the successful use
of an electrical discharge– under vacuum or at atmo-
spheric pressure–for the improvement of a wide range of
textile properties, such as hydrophilicity [1, 14], dye
exhaustion [9, 16, 18], adhesion [10, 11] and shrink-
proofing [4, 5]. Generally, the fiber surface is cleaned
from fiber surface additives (fiber processing chemicals)
prior to plasma treatment. These surface additives im-
prove frictional and electrostatic properties as required
during fiber processing, such as web formation and nee-
dle-punching. Their removal from the fiber surface oc-
curs via various methods, ranging from industrially fea-
sible processes such as gentle washing with a detergent
[21], as well as scouring and bleaching [2, 19], to exten-
sive laboratory (Soxhlet) extraction in one or more sol-
vents (acetone [15], benzene and water or methanol [8,
12], perchloroethylene, CCl4 and ethanol [6], CCl4, ac-
etone and dimethyl sulfoxide (DMSO) [13], etc.) Al-
though the latter cleaning methods are often required for
fundamental studies, they are not feasible in the textile-
industry context due to time, cost and environmental
constraints. As a consequence, when one has the ambi-
tion to introduce a plasma technology into the textile
industrial setting, the actual state of the fiber surface
should be taken into account, and pre-plasma cleaning of
1
To whom correspondence should be addressed: Jo Verschuren
(Mr.) Ghent University Department of Textiles Technologiepark
907 9052 Gent Belgium Telephone: ⫹32 9 264 57 40 (direct), ⫹32 9
264 57 35 (secretary) Fax: ⫹32 9 264 58 46 e-mail: jo.
verschuren@UGent.be
the fiber surface should be done in a feasible washing
step.
The textile structures treated in this study were made
of 15 micron thick fibers. In this case a 0.4% weight-of-
fiber (%w.o.f.) addition of surface additives covered the
fibers with a layer of average thickness 15 nm. This
thickness is comparable to the widely acclaimed instant
working depth of a plasma (5 to 20 nm). Accordingly, for
most as-received industrial fabrics it is the surface addi-
tives that are plasma treated, rather than the fiber poly-
mer surface. Only when this layer has been removed by
plasma physical and chemical etching is the full fiber
polymer surface exposed and treated. The purpose of this
study was to assess the influence of fiber surface addi-
tives on the result of a standard plasma treatment aimed
at improving the hydrophilic properties of a hydrophobic
fiber polymer surface. Both wettability and rewettability
were tested through the wicking properties of the (un)-
treated samples. Wicking properties were shown to be of
use in the assessment of plasma-induced changes in fiber
surface hydrophilic properties [3, 7, 20].
Experimental
SAMPLING AND PLASMA TREATMENT
The samples were 490 g/m2 poly(metaphenylene
isophthalamide), (meta-aramid/MA) or 550 g/m2 poly-
(ethylene terephthalate), (polyester/PET) nonwoven fab-
rics. Both needle- punched nonwovens were reinforced
by a wide maze fabric of the same fiber type, ensuring
dimensional stability. Surface additives were present at a
concentration of 0.40 ⫾ 0.05 %w.o.f., as determined

Textile Res. J. 75(5), 437– 441 (2005) DOI: 10.1177/0040517505054170 © 2005 Sage Publications www.sagepublications.com
438
from a 1 hour Soxhlet extraction with acetone
(DIN54278-1-1995).
A 20 cm ⫻ 20 cm sample area was plasma treated
centro-symmetrically between two perforated aluminum
plate electrodes that were 4 cm apart [17]. Pumpdown to
13 Pa (100 mTorr) took 3 minutes, after which a flow of
oxygen increased the pressure to 53 Pa (400 mTorr). The
estimated gas flow velocity at 53 Pa was 18 to 20
cm/second perpendicular to the nonwoven surface. Two
minutes after pressure equilibrium a 13.56 MHz, 71
mW/cm3 (375 mW/cm2 nonwoven) plasma was ignited
for 5, 10, 15 or 30 seconds. The short treatment durations
reflect industrial productivity. For a treatment length of
10 or 15 m in commercial vacuum plasma reactors a 5 to
30 second treatment corresponds to a fabric speed be-
tween 120 to 20 m/minute and 180 to 30 m/minute,
respectively. After the plasma treatment the oxygen gas
flow was maintained for another 2 minutes before vac-
uum break.
WICKING TESTS
The treated samples were left in a controlled climate
(20 ⫾ 2°C, 65 ⫾ 2% R.H.) for 24 ⫾ 2 hours before
proceeding with DIN 53924 vertical wicking tests. The
result of the test is a wicking curve, expressing the
wicking height (a.k.a. capillary rise, in mm) in a verti-
cally positioned sample as function of wicking time (up
to 600 seconds). In this study the abscissa is expressed as
log (time), by which the wicking curves are more or less
linearized. The use of a logarithmic time scale has the
advantage of (a) stressing the industrially important early
moments of wicking, and (b) avoiding the pile-up of data
points at short wicking times. From the plasma-treated
sample, four 3 cm ⫻ 20 cm repeat subsamples were cut.
The influence of the plasma treatment duration on wick-
ing can further be presented by integration of the wicking
height over the full wicking time, resulting in “summed
wicking height” (SWH) plots.
An overview of the experimental setup for wicking is
given in Table I. Wicking tests were done for both the
MA and PET nonwovens on as-received samples and on
samples of which the fiber surface was cleaned prior to
the plasma treatment. Pre-cleaning of samples was done
in a 1% solution of isopropanol in water at 40°C to
remove all water-soluble matter. After rinsing, and gen-
tle centrifuging to remove capillary water, the samples
were oven dried for 2 hours at 105 ⫾ 2°C. The influence
of plasma treatment duration was assessed by compari-
son with a non-plasma-treated sample with similar sam-
ples plasma treated for 5, 10, 15 or 30 seconds. All of the
samples were subjected to three consecutive wicking
tests (runs). First-time wicking of as-received and
TEXTILE RESEARCH JOURNAL
TABLE I. Overview of wicking test procedure.
as-received pre-cleaned
first run first run
3 drying 4
second run second run
3 washing 4
third run third run
plasma-treated samples produced a brown-yellowish
band moving with the rising water front. This band was
presumed to consist of water-soluble products created or
modified during the plasma treatment. The possible in-
homogeneities in hydrophilicity thus created were fixed
on the fiber surface by overnight drying of the wetted
samples, and assessed during a second wicking run. The
same samples were then gently hand-washed in a 1%
isopropanol solution as described before. Then a third
wicking run was done on these washed samples. The use
of isopropanol was required to prevent traditional surface
active agents from interfering with the spectroscopic
analysis performed on the samples in parallel with the
wicking tests (results to be published later). Special care
was taken not to change the nonwoven structure during
the different sample handling steps. Whereas the consec-
utive wicking runs for as-received samples reflect the
stability of the plasma-treated layer of surface additives
towards water, the runs for pre-cleaned samples reflect
the stability of the plasma-modified fiber polymer sur-
face.
From the four repeat determinations, the following
ranges of 95% confidence limit were determined for the
wicking height in as-received MA samples: 0.5–1.3 mm
(first run), 0.5–2.9 mm (second run) and 0.5–1.7 mm
(third run). For the pre-cleaned samples the confidence
limits are: 0.5–1.5 mm (first and second runs), 0.5–1.9
mm (third run). For each of the wicking times separately
the corresponding wicking heights are significantly in-
fluenced by the treatment duration, as determined from a
one-way ANOVA. Results for the PET samples are very
similar.
Results and Discussion
WICKING OF AS-RECEIVED SAMPLES
The averaged wicking curves for as-received MA
samples are presented in Figure 1. Fiber surface additives
create an environment for considerable first-time wick-
ing, even without plasma treatment. The influence of
treatment duration is modest. The wicking height in-
creases in a reasonably linear manner with log (time) up
to 3 to 5 minutes of wicking, after which it becomes
constant. In the second run the influence of plasma
MAY 2005 439

in a linear fashion, indicating a regained homogeneity of

the fiber surface throughout the sample. The separation
of the curves with regard to treatment duration was good,
indicating how longer treatment durations were required
before the actual fiber polymer surface can be modified
by the reactive plasma species. It can be expected that
optimized plasma treatments of possibly several minutes
will result in good wicking properties of the as-received
samples, even after washing.
The SWH plots for as-received samples (Figure 2)
show a systematically lower wicking performance for
PET samples in comparison with MA samples, in the
first as well as the second wicking run. This could be due
to a difference in porous structure and the use of surface
additives with a lower hydrophilicity. In the second run
the influence of plasma treatment duration has increased,
but more so for the MA samples. The wicking properties
of washed samples were far inferior even to the wicking
properties of as-received samples that were not plasma
treated, and this was true for both fiber types. The third
wicking run SWH plots show that for the combination of
textile structures and plasma treatment conditions ap-
plied in this study it required a plasma treatment of
longer than 30 seconds before the fiber polymer surface
began to be modified through the layer of surface addi-
tives.

FIGURE 1. Averaged wicking curves for as-received MA samples, as

function of plasma treatment duration. The top and center graphs are
for the first and second wicking runs, respectively. The bottom graph
presents the four repeat wicking curves for the third run (washed
samples). Legend: plasma treatment of 0 seconds (X), 5 seconds (E),
10 seconds ({), 15 seconds (‚), 30 seconds (䊐). The arrows indicate
increasing plasma treatment duration. Note the difference in ordinate
scale.

treatment duration was increased but overall wicking

performance was decreased. This can be expected be-
cause of the elution– during the first run– of hydrophilic
substances along the rising water front. This elution
results in a hydrophilic concentration gradient increasing FIGURE 2. Summed wicking height (SWH) plots for as-received MA
with sample height, as reflected in the non-linearity of (white) and PET (black) samples, as function of treatment duration.
Legend: first (E,F), second (‚,Œ) and third (䊐,■) wicking runs.
the log (time) plots. For the as-received samples that
were not plasma treated the maximum wicking height in
the second run was more than halved as compared to the
WICKING OF PRE-CLEANED SAMPLES
first run (from 82 to 38 mm). This indicates the high
water solubility of the applied fiber surface additives. The behavior towards consecutive wishing tests of
After washing of the samples the wicking was even pre-cleaned MA and PET samples was similar to that of
lower, with an inhibition period of at least 15 seconds. the as-received samples, although the wicking properties
For all samples treated for up to 10 seconds the maxi- themselves had changed considerably (Figure 3). Water
mum wicking height was close to zero. For the longer sorption of the non-plasma-treated sampleswas always
treatment durations the log (time) wicking curves behave minimal, as expected from the fact that a moderately
440
FIGURE 3. Averaged wicking curves for pre-cleaned MA samples as
function of plasma treatment duration. The top and bottom graphs are
for the first and third wicking runs, respectively. Legend: plasma
treatment of 0 seconds (X), 5 seconds (E), 10 seconds ({), 15 seconds
(‚), 30 seconds (䊐).
hydrophilic layer of surface additives was removed dur-
ing the washing treatment, exposing a more hydrophobic
fiber polymer surface. After the plasma treatments of
varying duration the separation of the first-time wicking
curves is clear for both fiber types and from the shortest
wicking times onwards. The curves are linear with log-
(time), indicating a homogeneous fiber surface. Results
for the second run of the MA samples were nearly
identical to those for the first run, which is due to a better
stability of the plasma treatment effect to water in com-
parison with an as-received surface (Figure 4). Such
surface stability was not found in the pre-cleaned PET
samples, for which second run wicking results were
reduced considerably. The behavior of pre-cleaned PET
samples was similar to results for first and second wick-
ing runs for as-received samples; namely, reduced max-
imum wicking heights, an inhibition of about 30 seconds
and a loss of curve parallelism (not shown). It is sug-
gested that the plasma treatment causes the PET polymer
surface to become partly water soluble, resulting in elu-
tion-induced inhomogeneities and loss of hydrophilic
properties. The SWH plots show that for pre-cleaned
samples even the shortest plasma treatment is effective in
giving the hydrophobic fiber surface a considerable hy-
drophilic property. They also clearly indicate how the
successive wicking and washing procedures have a lim-
ited influence on MA sample properties and a larger
influence on PET sample properties. In view of the
TEXTILE RESEARCH JOURNAL
FIGURE 4. Summed wicking height (SWH) plots for pre-cleaned MA
(white) and PET (black) samples, as function of treatment duration.
Legend: first (E,F), second (‚,Œ) and third (䊐,■) wicking runs.
partial aliphatic and complete aromatic structures of PET
and MA, respectively the difference in wicking behavior
of pre-cleaned samples is possibly the consequence of
the formation during the plasma treatment of low molec-
ular weight products with a different solubility in water.
Note that using SWH values for summarizing wicking
data has the advantage over the maximum wicking
height (MWH, for example, after 10 minutes wicking) of
better representing the behavior of the total wetted textile
fiber surface. As an example, samples showing or not
showing an inhibition period could have the same MWH,
although the SWH value will be lower for the sample
showing inhibition.
Conclusions
The purpose of this study was to assess–with the use
of consecutive wicking tests–the influence of fiber sur-
face additives on the effect of an oxygen plasma treat-
ment, and on the stability of the effect towards a treat-
ment in water. The presence of a layer of surface
additives was shown to have a profound influence on the
efficiency of the plasma treatment. This observation is
expected to be as significant for atmospheric plasma
processing as it is for plasma processing in vacuo, and
valid for all textile fiber surfaces covered with water-
soluble additives. However, it is obvious that not all
plasma applications “suffer” from the presence of sur-
MAY 2005
face additives. Many treatments aim only at the improve-
ment of the first-time wettability; in this case there is no
problem if the treated surface additives are washed away
during the first contact with water.
For the textile structures treated in this study, to obtain
a given wicking effect a clean fiber surface requires
longer treatment durations than a surface covered with
surface additives. This is a result of the difference in
resistance towards plasma oxidation between the surface
additives and the pure fiber polymer surface. The longer
treatment duration required for a pure fiber surface is
compensated by an improved resistance of the effect
towards a treatment with water.
In the SWH plots the wicking behavior of samples
treated in a range of plasma conditions and post-plasma
wet treatments can be evaluated, and this in a single
graph. Still, the individual log(time) wicking curves re-
main the basis for information on the industrially impor-
tant early wicking behavior, and on inhomogeneities at
the fiber surface.
Although wicking tests do not produce the surface
morphological and (physico)chemical information ob-
tained from Atomic Force Microscopy (AFM) and x-ray
Photoelection Spectroscopy (XPS) and contact angle
measurements, its value lies in the possibility to charac-
terize a textile structure in its entirety. As such, the
determination of wicking and related properties is a
complementary tool for the characterization of textiles
whose processing or application benefits from the fiber
surface modification by a plasma.
ACKNOWLEDGEMENTS
This study was supported by BOF project TW11V/
983473, Ghent University
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Manuscript received 2005; accepted 2005.