Applied Surface Science 356 (2015) 408415

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Applied Surface Science

journal homepage: www.elsevier.com/locate/apsusc

Reactive-ion etching of nylon fabric meshes using oxygen plasma for

creating surface nanostructures
Hernando S. Salapare III, Thierry Darmanin, Frdric Guittard
Universit Nice Sophia Antipolis, CNRS, LPMC, UMR 7336, Parc Valrose, 06100 Nice, France

a r t i c l e i n f o a b s t r a c t

Article history: A facile one-step oxygen plasma irradiation in reactive ion etching (RIE) conguration is employed to
Received 6 May 2015 nylon 6,6 fabrics with different mesh sizes to achieve surface nanostructures and improved wettability
Received in revised form 25 June 2015 for textile and ltration applications. To observe the effects of power and irradiation time on the samples,
Accepted 28 June 2015
the experiments were performed using constant irradiation time in varying power and using constant
Available online 10 August 2015
power in varying irradiation times. Results showed improved wettability after the plasma treatment. The
FTIR spectra of all the treated samples exhibited decreased transmittance of the amide and carboxylic
Keywords:
acid groups due to surface etching. The changes in the surface chemistry are supported by the SEM data
Nylon fabric
Reactive-ion etching
wherein etching and surface nanostructures were observed for the plasma-treated samples. The etching
Oxygen plasma of the surfaces is enhanced for higher power plasma treatments. The thermal analysis showed that the
Surface modication plasma treatment resulted in decreased crystallinity. Surface chemistry showed that the effects of the
Texturing plasma treatment on the samples have no signicant difference for all the mesh sizes. However, surface
DC self-bias voltage morphology showed that the sizes of the surface cracks are the same for all the mesh sizes but samples
with larger mesh sizes exhibited enhanced etching as compared to the samples with smaller mesh sizes.
Higher power induced higher negative DC self-bias voltage on the samples that favored anisotropic and
aggressive etching.
2015 Elsevier B.V. All rights reserved.

1. Introduction susceptibility of poly(ethylene terephthalate) (PET) and nylon

Nylon 6,6 (polyhexamethylene adiamide) fabrics are semi-
crystalline polyamides that possess outstanding versatile proper-
ties that are used in textile, automobile, military, electronics, and
medical industries. Although the bers possess excellent mechan-
ical, chemical, and thermal properties, there are still some limita-
tions on its uses and applications [110]. In general, to extend the
use and applications of polymers, several treatments are employed
and some of them uses atmospheric pressure plasma to improve the
dye uptake of nylon 6 bers with different absorbed moisture [1]
and to enhance the antibacterial activity and natural dyeing proper-
ties of nylon 6 fabrics [6]; direct low-pressure and low-temperature
plasma to enhance the adhesion of carbon nanotubes on nylon
6,6 fabrics [3], to improve the mechanical properties of nylon 6
plain woven fabrics [5], to correlate the crystallinity and plasma
Corresponding author. Tel.: +334 92 07 61 59; fax: +334 92 07 61 56.
E-mail addresses: salapare@unice.fr (H.S. Salapare III), darmanin@unice.fr
(T. Darmanin), Frederic.GUITTARD@unice.fr (F. Guittard).
6,6 bers [10], and to achieve superhydrophilic or super-
hydrophobic properties for lignocellulosic seagrass, PET, and
poly(tetrauoroethylene) (PTFE) materials [1114]; gas discharges
in improving the wettability, superhydrophobicity and antibacte-
rial properties of PTFE [1518]; laser to improve the dyeability of
poly(amide) 6,6 knitted fabrics [19]; and microwave jet plasma for
the functionalization of electrospun poly(amide) 6 nanobers to
improve the adhesion properties during the production of com-
posites in tissue engineering [7].
In this study, RF oxygen plasma in reactive-ion etching (RIE) con-
guration was used to modify the chemistry and morphology of the
nylon 6,6 samples. This technique has some advantages over the
other techniques since it is an extreme form of direct plasma treat-
ment and it has an increased DC bias level that favors anisotropic
and aggressive etching on the samples [20,21]. The plasma cong-
uration under vacuum is favorable in the processing of materials
since the integrity of the plasma and the materials are maintained
throughout the irradiation process [1113,1518]. Plasma treat-
ments were found to be favorable over non-plasma techniques
since the plasma may contain different species such as electrons,

http://dx.doi.org/10.1016/j.apsusc.2015.06.185
0169-4332/ 2015 Elsevier B.V. All rights reserved.
 H.S. Salapare III et al. / Applied Surface Science 356 (2015) 408415
neutral species, charged species, and excited species that can inter-
act with the materials surface [22].
2. Experimental procedures
2.1. Materials and plasma treatment
Sefar Nitex nylon 6,6 fabrics (Sefar AG, Switzerland) of differ-
ent mesh sizes ranging from 25 m to 1550 m were used in the
experiments. Different mesh sizes were used because the pressure
that a fabric can support is highly dependent on the mesh size.
Before plasma treatment, the nylon 6,6 fabrics were soaked in ace-
tone for 10 min followed by air-drying for 2 h at room temperature
in order to remove any impurities on the surface. The cleaned and
dried samples were then irradiated using oxygen plasma produced
in reactive ion etching conguration of a BSET EQ NT-1 plasma
device (Digit Concept Microelectronics and High Tech Equipment,
France) operating at an excitation frequency of 13.56 MHz. The
plasma device operates on the principle of a capacitive coupled
plasma (CCP) reactor where the RF current through the oxygen
gas maintains a steady state discharge by heating the electrons.
The samples were placed on the power electrode, which is paral-
lel to the ground electrode at 50 mm distance from each other. A
20 m3 /h rotary pump evacuated the system, and the base pressure
was kept at 100 mTorr. Oxygen gas was fed into the chamber at
a ow rate of 20 sccm. The plasma sheath produced between the
power and ground electrodes induced negative DC self-bias volt-
age on the samples that was measured using a voltmeter with a
low-pass lter.
In order to determine the effects of power and irradiation time
on the treatment of the fabrics, two sets of plasma parameters were
used. The rst experiment was done with constant irradiation time
of 600 s but with varying powers of 100 W, 200 W, and 300 W, and
the second experiment was done with constant power of 600 W but
with varying irradiation times of 100 s, 200 s, and 300 s. The exper-
imental parameters used in the rst set have the same incident
energy as the second set ranging from 60 kJ to 180 kJ.
2.2. Characterizations
2.2.1. Contact angle measurements
A DSA-30 goniometer (Krss GmbH) equipped with a drop shape
analysis (DSA4) software was used to study the changes in the
wettability of the samples. Sessile drop method was used to deter-
mine the apparent contact angles. 2 L of Milli-Q deionized water
was dropped vertically onto the samples using a motorized syringe
mechanism. For each samples, contact angle measurements were
performed at three different sites.
2.2.2. Fourier transform infrared spectroscopy
The changes in the samples chemical functionalities were
obtained using a Spectrum 100 FT-IR spectrometer (Perkin Elmer,
USA) with a diamond attenuated total reectance (ATR) top plate
accessory. The samples were scanned 5 times at 4 cm1 spectral
resolutions over the range of 450 cm1 to 4000 cm1 . The spectra
reported in this paper were obtained by subtracting the background
spectra from the measured spectra.
2.2.3. Differential scanning calorimetry
Melting and crystallization proles were determined for each
sample using a Jade Differential Scanning Calorimeter (DSC) (Perkin
Elmer, USA). Samples were lled in a measurement cell of the DSC
and the temperature was rst heated from 25 C to 300 C at the rate
of 20 C/min and held for 3 min. The samples were then quenched to
25 C from 300 C at the rate 100 C/min. The glass transition tem-
perature (Tg ), melting temperature (Tm ), and enthalpy of melting
409
(Hm ) were extracted from the melting prole and the crystalliza-
tion temperature (Tc ), and enthalpy of crystallization (Hc ) were
extracted from the crystallization prole. The crystallinity of the
fabric samples were then calculated using the following equation:
Hm Hc
% Crystallinity = o 100%
Hm
where Hm o is a reference value and represents the heat of melting
if nylon 6,6 were 100% crystalline [23].
2.2.4. Scanning electron microscopy
A JSM 6700F NT (JEOL Ltd., Japan) scanning electron microscope
was used to determine the morphology of the surface of the mate-
rial. The samples were scanned at 250, 10,000, and 25,000
magnications.
3. Results and discussion
Control nylon 6,6 fabrics of mesh sizes 25 m, 100 m, 200 m,
and 400 m exhibited high wettability since the water contact
angles are less than 10 and the water droplet spread on the surface
within 1 s of contact. This was expected since the nylon 6,6 fabrics
used in this study are usually used for ltration applications. For
the control nylon 6,6 fabrics of 700 m and 1550 m mesh sizes,
the contact angle is 84 and 43 , respectively, since the volume of
the water droplet used in the measurement is 2 L. This means
that the ber spacing is an important factor when studying wett-
ability, for example, when the material is used for ltration, the
selection of an appropriate lter is necessary for different types of
ltrates. After the plasma treatment, all the nylon 6,6 fabric sam-
ples exhibited improved wettability, especially for samples of mesh
sizes 700 m and 1550 m. This improvement in the wettability
is favorable when dealing with ltration using different types of
ltrates.
For the FTIR, DSC, and SEM data, only the nylon 6,6 fabric with
mesh size of 100 m will be shown, since it was found in the study
that the effects of the plasma treatment on the samples have no
signicant difference for all the mesh sizes (i.e., the same trend and
behavior on the surface chemistry, surface morphologies, thermal
properties, and crystallinity were observed for samples of mesh
sizes 25 m, 100 m, 200 m, 400 m, 700 m and 1550 m).
Fig. 1 shows the superimposed view of FTIR spectra of the con-
trol and plasma-treated nylon 6,6 fabric samples with 100 m mesh
size. For spectra b, c, and d, the plasma treatment was performed
with constant irradiation time (600 s) of varying power (100 W,
200 W, and 300 W). The spectrum of the control sample veries
that the material is nylon 6,6 since it contains the following chem-
ical functionalities: N H stretching (3264 cm1 ), C H asymmetric
stretching (3085 cm1 ), asymmetric and symmetric stretching
(2962 cm1 and 2851 cm1 , respectively), C O stretching from car-
boxylic acid groups (1734 cm1 ), amide I band and amide II and
CH2 asymmetric deformation groups (1650 cm1 and 1539 cm1 ,
respectively), N H deformation and CH2 scissoring (1452 cm1 ),
amide III band and CH2 wagging (1347 cm1 ), CCH symmet-
ric bending and CH2 twisting (1145 cm1 and 1130 cm1 ), C C
stretching (962 cm1 ), N H wagging and CH2 rocking (742 cm1 ),
C C bending (600 cm1 ), and O C N bending (548 cm1 ).
For all the peaks except the C C stretching, it was found that the
transmittance intensities decreased which are proportional to the
values of the incident energy. The existence of the amide I, amide
II, and carboxylic acid groups which are polar and hydrophilic sup-
ports the over-all hydrophilic properties of the nylon 6,6 fabrics.
The decrease in the transmittance peaks can be associated with the
breakage of some amide linkage in the nylon 6,6 fabrics which cre-
ates free amino groups, this change in the chemistry of the material
410 H.S. Salapare III et al. / Applied Surface Science 356 (2015) 408415

Fig. 1. Superimposed view of FTIR spectra of the control and plasma-treated nylon 6,6 fabric samples with 100 m mesh size. The plasma treatment was performed with
constant irradiation time (600 s) of varying power (100 W to 300 W).

Fig. 2. Superimposed view of FTIR spectra of the control and plasma-treated nylon 6,6 fabric samples with 100 m mesh size. The plasma treatment was performed with
constant power (600 W) of varying irradiation times (100 s to 300 s).
 H.S. Salapare III et al. / Applied Surface Science 356 (2015) 408415
Fig. 3. Superimposed view of the FTIR spectra of the plasma-treated nylon 6,6 fabric samples with 100 m mesh size. The two spectra represent the same incident energy
equal to 180 kJ but of different power (300 W and 600 W) and different irradiation time (600 s and 300 s).
is favorable for textile applications since it improves its dyeability
as seen from the work of Bahtiyari [19] on polyamide fabric surface
modication using laser. Another possible effect of the decrease in
the transmittance peaks of amide I, amide II, and carboxylic acid
groups (which are sensitive to light and solvents) is the improve-
ment of the materials stability to light and solvents like alkali and
acids as shown by El-Garf et al. [24] on their work on treatment of
nylon 6 materials using dichlorobenzenesulfonyl chloride.
Fig. 2 shows the superimposed view of FTIR spectra of the control
and plasma-treated nylon 6,6 fabric samples with 100 m mesh
size. For spectra b, c, and d, the plasma treatment was performed
with constant power (600 W) of varying irradiation times (100 s,
200 s, and 300 s). The same observations as in Fig. 1 regarding the
transmittance peaks of all the chemical functionalities were seen
in the FTIR spectra in Fig. 2.
The main difference between Figs. 1 and 2 can be seen in Fig. 3
which shows the superimposed view of the FTIR spectra of the
plasma-treated nylon 6,6 fabric samples with 100 m mesh size
wherein the two spectra represent the same incident energy equal
to 180 kJ but of different power (300 W and 600 W) and different
irradiation time (600 s and 300 s). It can be seen from Fig. 3 that
the transmittance values of the 600 W, 300 s plasma-treated sam-
ples were higher than the 300 W, 600 s plasma-treated samples.
This observation is the same with the other samples of the same
incident energy but of different power and irradiation time. From
this data, it can be assumed that the power plays the main part in
the surface modication process. Higher power treatments create
more plasma particles than the lower power treatments [11,22]
and the effect of the irradiation time was found to be of lower sig-
nicance when dealing with the interaction of the plasma particles
411
with the materials surface. The higher the power also means that
the plasma temperature is high which would possibly increase the
materials dyeability as shown by Kamide et al. [25] on their study
of the structural factors governing the dyeability of poly(ethylene)
terephthalate (PET) bers.
Fig. 4 shows the dependence of the negative DC self-bias volt-
age on power. The negative DC self-bias voltage increases linearly
(R2 = 0.96553) with the square root of the power when the power
varies from 100 W to 600 W at constant pressure; this plasma
behavior is consistent with the capacitive sheath model proposed
by Catherine et al. [26]. By correlating the FTIR data with Fig. 4, we
can assume that the decreases in the spectral transmittance peaks
are proportional with the negative DC self-bias voltage induced on
the samples.
Fig. 5 shows the stacked view of the melting diagrams for the
control and plasma-treated nylon 6,6 fabric samples with 100 m
mesh size obtained in the heating measurement and Fig. 6 shows
the stacked view of the crystallization diagrams for the control and
plasma-treated nylon 6,6 fabric samples with 100 m mesh size
obtained in the cooling measurement. Based on the melting and
crystallization diagrams, the thermal properties and crystallinity
of the nylon 6,6 fabrics were extracted and summarized in Table 1.
The glass transition temperature of the plasma-treated samples
were found to be signicantly higher than the control sample, this
is an indication that the material after undergoing plasma treat-
ment has changed its molecular arrangement as also supported by
the signicant decrease in the crystallinity of the samples [2,8].
The decrease in the crystalline phase gives rise to the increase in
the amorphous phase of the material. This change in the materials
phase is favorable for textile applications as shown by Okuno et al.
412 H.S. Salapare III et al. / Applied Surface Science 356 (2015) 408415

Fig. 4. Dependence of negative DC self-bias voltage on power.

Fig. 5. Stacked view of the melting diagrams for the control and plasma-treated nylon 6,6 fabric samples with 100 m mesh size obtained in the heating measurement.

Fig. 6. Stacked view of the crystallization diagrams for the control and plasma-treated nylon 6,6 fabric samples with 100 m mesh size obtained in the cooling measurement.
 H.S. Salapare III et al. / Applied Surface Science 356 (2015) 408415 413

Table 1
Summary of the thermal properties and the crystallinity for the control and plasma-treated nylon 6,6 fabric samples with 100 m mesh size.

Experimental parameters Tg ( C) Tm ( C) Tc ( C) Hm (J/g) Hc (J/g) Crystallinity (%)

Control 123.2 220.2 173.8 137.9 1.9 53.1

100 W, 600 s 132.7 219.5 173.7 133.2 4.1 50.4
200 W, 600 s 133.2 219.8 173.2 115.5 4.8 47.0
300 W, 600 s 135.4 219.9 175.0 119.5 5.2 44.6
600 W, 100 s 132.0 219.5 176.5 116.8 8.1 42.5
600 W, 200 s 133.7 220.7 181.2 107.5 1.3 42.5
600 W, 300 s 137.3 220.8 172.5 103.5 2.5 39.5

[10] on their work on the effect of the crystallinity of PET and nylon
6,6 bers on the plasma etching and dyeability characteristics by
low temperature plasma treatment, wherein they found out that
the increase in the materials crystallinity decreases its dyeability
since the dyeable area in a material lies on the amorphous phase.
The decrease in the crystallinity is supported by the FTIR data
where there is an increase in the transmittance peaks in the
C C stretching bands of the plasma-treated samples, which cor-
responds to the amorphous phase of the sample [19]. There is no
signicant change with the melting and crystallization tempera-
ture of the control and plasma-treated samples since based from the
FTIR data, the chemical composition did not changed due to plasma
treatment. However, there is a general decrease in the enthalpy
of melting and increase in the enthalpy of crystallization after the
plasma treatment, which also effected the decrease in the crys-
tallinity of the plasma-treated materials. This also means that the
energy per mass unit being absorbed or released by the sample
changed due to the decrease in the transmittance peaks of all the
chemical groups as seen from the FTIR data.
Fig. 7 shows the representative SEM micrographs of the (a, d, g)
control and plasma-treated nylon 6,6 fabric samples with 100 m
mesh size under (ac) 250, (df) 10,000, and (gi) 25,000
magnications. The SEM images of the treated samples represent
the same incident energy equal to 180 kJ but of different power
and different irradiation time: (b, e, h) 300 W, 600 s treated (c, f, i)
600 W, 300 s treated.
It can be observed that the plasma treatment induced etching
as seen from the ripple-like structures on the surface of nylon 6,6
fabrics. A closer look on the surfaces structures at 25,000 magni-
cations revealed that the plasma treatment, which induced etching,
created surface cracks with openings of sizes ranging from 0.50 m
to 1.00 m. By comparing the 300 W, 600 s plasma-treated and
600 W, 300 s plasma-treated samples reveals that the etching of the
samples surfaces also conrms the decrease in the transmittance
peaks of all the chemical groups in the FTIR spectra of the plasma
treated samples, this result is consistent with the BeerLamberts
law since the concentration of the functional groups decreased
because of the etching.

Fig. 7. Representative SEM micrographs of the (a, d, g) control and plasma-treated nylon 6,6 fabric samples with 100 m mesh size under (ac) 250, (df) 10,000, and
(gi) 25,000 magnications. The SEM images of the treated samples represent the same incident energy equal to 180 kJ but of different power and different irradiation
time: (b, e, h) 300 W, 600 s treated (c, f, i) 600 W, 300 s treated.
414 H.S. Salapare III et al. / Applied Surface Science 356 (2015) 408415
Fig. 8. SEM micrographs of the plasma-treated nylon 6,6 fabric samples with mesh sizes of (a and g) 25 m, (b and h) 100 m, (c and i) 200 m, (d and j) 400 m, (e and k)
700 m, and (f and l) 1550 m under 25,000 magnication. The SEM images from (af) represents the same incident energy as of (gl) but of different power and different
irradiation time: (af) 300 W, 600 s treated (gl) 600 W, 300 s treated.
In order to compare the etching effects on the different mesh
sizes, Fig. 8 shows the SEM micrographs of the plasma-treated
nylon 6,6 fabric samples with mesh sizes of (a, g) 25 m, (b, h)
100 m, (c, i) 200 m, (d, j) 400 m, (e, k) 700 m, and (f, l) 1550 m
under 25,000 magnication. The SEM images from (af) repre-
sents the same incident energy as of (gl) but of different power and
different irradiation time: (af) 300 W, 600 s treated (gl) 600 W,
300 s treated. The surface crack openings for all the mesh sizes
ranges from 0.05 m to 0.25 m for 300 W, 600 s treatments and
from 0.50 m to 1.00 m for 600 W, 300 s treatments. The power
has a greater morphological effect on the surfaces as compared with
the irradiation time, which is also consistent with the observations
seen from the FTIR and DSC data. Although the increase in the sur-
face crack openings are relatively the same for all the mesh sizes, a
closer look on Fig. 8 reveals that there is a greater etching on the fab-
rics surfaces for larger mesh sizes (400 m, 700 m, and 1550 m)
as compared with the smaller mesh sizes (25 m, 100 m, 200 m)
as exhibited by the enhanced ripple-like surface structures. Fabrics
with larger mesh sizes are more susceptible to etching since larger
surface areas are exposed to the oxygen plasma.
The negative DC self-bias voltage also played a main role in
the etching process; high power induces higher negative DC self-
bias voltage that increases the electronic density in the plasma and
the number of plasma species that interacts with the surface of
the materials [27]. Samples treated at longer irradiation times also
showed more enhanced and aggressive etching because etching
rate is higher for samples exposed to high negative DC self-bias
voltage [28].
By visual inspection of Fig. 7, we can say that there are increases
in the surface roughness of the nylon 6,6 fabric surfaces after plasma
treatment. It can be assumed that the result of the plasma treatment
on the materials wettability is consistent with the Wenzel wetting
state where hydrophilic surfaces tend to be even more hydrophilic
(when the apparent water contact angle of a smooth surface,  Y is
less than 90 , the apparent contact angle of a rough surface,  W is
always less than ) when the surface roughness increases [2931].
4. Conclusions
A facile one-step oxygen plasma irradiation in reactive-ion
etching (RIE) conguration was employed to nylon 6,6 fabrics
with different mesh sizes in achieving nanostructured surface and
improved wettability for textile and ltration applications. The
effects of power and irradiation time on the samples were deter-
mined by using different parameters: (1) constant irradiation time
in varying power and (2) constant power in varying irradiation
times. In general, improved wettability was observed for all the
samples after the plasma treatment. The FTIR spectra of all the
treated samples exhibited decreased transmittance of the amide
and carboxylic acid bands due to surface etching. The changes
in the surface chemistry are supported by the SEM data wherein
etching and texturization of the surfaces were observed for the
plasma-treated samples. The etching of the surfaces is enhanced
for higher power plasma treatments. Increasing the irradiation time
also enhances the etching on the samples surfaces, however; it is
the power and the negative DC self-bias voltage that played the
major role in the etching process. The thermal analysis showed
that the plasma treatment resulted to decreased crystallinity and in
consequence increased the amorphous phase of the samples. The
data of the surface chemistry showed that the effects of the plasma
treatment on the samples have no signicant difference for all the
mesh sizes. However, surface morphology showed that the sizes of
the surface cracks are the same for all the mesh sizes but samples
with larger mesh sizes exhibited enhanced etching as compared
to the samples with smaller mesh sizes. Higher power induced
higher negative DC self-bias voltage on the samples that favored
anisotropic and aggressive etching. The results of this study are
favorable for applications that need properties such as improved
dyeability, increased stability to light, and increased resistance to
alkali and acid solvents.
Acknowledgements
We would like to thank the Erasmus Mundus Mobility with Asia
(EMMA-West)2013 (Lot 12) for the nancial grant (Grant No.
2012-2643/001-001-EMA 2) and the Centre Commun de Micro-
scopie Applique of the Universit Nice Sophia Antipolis and the
Microscopy and Imaging platform Cte dAzur (MICA) for the SEM
characterization.
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