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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- the fiber surface should be done in a feasible washing
lications and patents have reported on the successful use step.
of an electrical discharge– under vacuum or at atmo- The textile structures treated in this study were made
spheric pressure–for the improvement of a wide range of of 15 micron thick fibers. In this case a 0.4% weight-of-
textile properties, such as hydrophilicity [1, 14], dye fiber (%w.o.f.) addition of surface additives covered the
exhaustion [9, 16, 18], adhesion [10, 11] and shrink- fibers with a layer of average thickness 15 nm. This
proofing [4, 5]. Generally, the fiber surface is cleaned thickness is comparable to the widely acclaimed instant
from fiber surface additives (fiber processing chemicals) working depth of a plasma (5 to 20 nm). Accordingly, for
prior to plasma treatment. These surface additives im- most as-received industrial fabrics it is the surface addi-
prove frictional and electrostatic properties as required tives that are plasma treated, rather than the fiber poly-
mer surface. Only when this layer has been removed by
during fiber processing, such as web formation and nee-
plasma physical and chemical etching is the full fiber
dle-punching. Their removal from the fiber surface oc-
polymer surface exposed and treated. The purpose of this
curs via various methods, ranging from industrially fea-
study was to assess the influence of fiber surface addi-
sible processes such as gentle washing with a detergent
tives on the result of a standard plasma treatment aimed
[21], as well as scouring and bleaching [2, 19], to exten- at improving the hydrophilic properties of a hydrophobic
sive laboratory (Soxhlet) extraction in one or more sol- fiber polymer surface. Both wettability and rewettability
vents (acetone [15], benzene and water or methanol [8, were tested through the wicking properties of the (un)-
12], perchloroethylene, CCl4 and ethanol [6], CCl4, ac- treated samples. Wicking properties were shown to be of
etone and dimethyl sulfoxide (DMSO) [13], etc.) Al- use in the assessment of plasma-induced changes in fiber
though the latter cleaning methods are often required for surface hydrophilic properties [3, 7, 20].
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- Experimental
tion to introduce a plasma technology into the textile
SAMPLING AND PLASMA TREATMENT
industrial setting, the actual state of the fiber surface
should be taken into account, and pre-plasma cleaning of The samples were 490 g/m2 poly(metaphenylene
isophthalamide), (meta-aramid/MA) or 550 g/m2 poly-
(ethylene terephthalate), (polyester/PET) nonwoven fab-
1
To whom correspondence should be addressed: Jo Verschuren rics. Both needle- punched nonwovens were reinforced
(Mr.) Ghent University Department of Textiles Technologiepark by a wide maze fabric of the same fiber type, ensuring
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. dimensional stability. Surface additives were present at a
verschuren@UGent.be 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 TEXTILE RESEARCH JOURNAL

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

FIGURE 3. Averaged wicking curves for pre-cleaned MA samples as
function of plasma treatment duration. The top and bottom graphs are FIGURE 4. Summed wicking height (SWH) plots for pre-cleaned MA
for the first and third wicking runs, respectively. Legend: plasma (white) and PET (black) samples, as function of treatment duration.
treatment of 0 seconds (X), 5 seconds (E), 10 seconds ({), 15 seconds Legend: first (E,F), second (‚,Œ) and third (䊐,■) wicking runs.
(‚), 30 seconds (䊐).

hydrophilic layer of surface additives was removed dur- partial aliphatic and complete aromatic structures of PET
ing the washing treatment, exposing a more hydrophobic and MA, respectively the difference in wicking behavior
fiber polymer surface. After the plasma treatments of of pre-cleaned samples is possibly the consequence of
varying duration the separation of the first-time wicking the formation during the plasma treatment of low molec-
curves is clear for both fiber types and from the shortest ular weight products with a different solubility in water.
wicking times onwards. The curves are linear with log- Note that using SWH values for summarizing wicking
(time), indicating a homogeneous fiber surface. Results data has the advantage over the maximum wicking
for the second run of the MA samples were nearly height (MWH, for example, after 10 minutes wicking) of
identical to those for the first run, which is due to a better better representing the behavior of the total wetted textile
stability of the plasma treatment effect to water in com- fiber surface. As an example, samples showing or not
parison with an as-received surface (Figure 4). Such showing an inhibition period could have the same MWH,
surface stability was not found in the pre-cleaned PET although the SWH value will be lower for the sample
samples, for which second run wicking results were showing inhibition.
reduced considerably. The behavior of pre-cleaned PET
samples was similar to results for first and second wick- Conclusions
ing runs for as-received samples; namely, reduced max-
imum wicking heights, an inhibition of about 30 seconds The purpose of this study was to assess–with the use
and a loss of curve parallelism (not shown). It is sug- of consecutive wicking tests–the influence of fiber sur-
gested that the plasma treatment causes the PET polymer face additives on the effect of an oxygen plasma treat-
surface to become partly water soluble, resulting in elu- ment, and on the stability of the effect towards a treat-
tion-induced inhomogeneities and loss of hydrophilic ment in water. The presence of a layer of surface
properties. The SWH plots show that for pre-cleaned additives was shown to have a profound influence on the
samples even the shortest plasma treatment is effective in efficiency of the plasma treatment. This observation is
giving the hydrophobic fiber surface a considerable hy- expected to be as significant for atmospheric plasma
drophilic property. They also clearly indicate how the processing as it is for plasma processing in vacuo, and
successive wicking and washing procedures have a lim- valid for all textile fiber surfaces covered with water-
ited influence on MA sample properties and a larger soluble additives. However, it is obvious that not all
influence on PET sample properties. In view of the plasma applications “suffer” from the presence of sur-
MAY 2005 441

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