Progress in Natural Science: Materials International 32 (2022) 314–327

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Progress in Natural Science: Materials International

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Surface characterization of polyimide and polyethylene terephthalate

membranes toward plasma and UV treatments
Thi Sinh Vo a, *, Tran Thi Bich Chau Vo b
a
School of Mechanical Engineering, Sungkyunkwan University, Suwon, 16419, South Korea
b
Department of Industrial Management, Can Tho University, Can Tho, Viet Nam

A R T I C L E I N F O A B S T R A C T

Keywords: This study is to bring an overview on various methods regarding the surface treatment performed on different
Plasma treatment polymeric membranes in relation to a deference between the treatment mechanism and their chemical structure.
UV treatment Herein, plasma and UV surface treatments (PST and UST) were utilized to treat the surfaces of two commercial
Polymeric membrane
membranes, i.e., aromatic polyimide and polyethylene terephthalate for various durations using a discharge
Aromatic polyimide
Polyethylene terephthalate
electrode and an UV LED curing system, respectively. Based on the effects of PST and UST processes on the surface
of these membranes, their surface properties have been characterized to surface morphology and hydrophilicity
(or wettability), at same time the changes have probably occurred on their surface during the PST and UST
processes. As a result, their hydrophilic behavior was significantly enhanced after conducting these treatment
processes based on the investigation of water contact angle. Moreover, Fourier-transform infrared and Raman
spectroscopy manifested the changes in the chemical bonds, interactions and orientations of molecules, which
confirmed the apparition and insertion of polar functional groups after the surface treatments, and accordingly,
their wettability was enhanced significantly. Also, optical microscopy images showed direct impactions on their
surface and the evidence of slight surface aging/damage during the treatment processes based on the presentation
of the strange streaks on the treated surfaces. In particular, the peel forces exhibited an increase comparing to the
initial membranes, which is characteristically for enhancing their adhesion behavior. Hence, these results are
needful for improving the surface properties of a material, and obtaining better adhesion behavior on the
membrane-like materials and recycling polymer materials.

1. Introduction disordering the bulk properties of materials [9,10]. Specifically, plasma

As known, polymeric material system has been widely utilized in
various practical applications and research fields [1–8]. Usually, an
important factor is required to possible interactions of these polymeric
materials generated at the interface surface, at same time these polymeric
materials often contain low surface energies that can be inert with
chemical activities on the surface of materials corresponding to invalid of
polar and actively functional groups. Thus, they are truly needful to
undergo the corresponding surface treatments to improve the adhesive
properties for interacting with other materials [9–11]. Among various
surface treatment methods, plasma and ultraviolet (UV) treatments are
commonly used to improve the surface properties of polymeric materials,
i.e., physical and chemical surface changes in polymers. Actually, the
polymeric materials exposed to plasma or UV technologies is considered
to be the approaches of reaching relative surface treatments without
surface treatment (PST) is considered as a complex method for control-
ling and modifying the surface properties of materials, which exhibits
also a chemically active media to induce chemical reactions on interface
surfaces of various materials, i.e., ionized molecular and atomic, photons,
radicals, etc., meaning a formation of oxygenated chemical groups on the
surface to probably allow higher surface chemical reactivity [12–14].
Besides, an atmospheric pressure plasma treatment is concerned signif-
icantly, owing to the lower cost and simplified operation [15]. Behaviors
of hydrophilicity (or wettability), adhesion, and surface morphology are
able to improve and enhance effectively through the use of PST method
on the material surface [16,17]. Specially, its outstanding advantage
regards to a chemical effect, an example for nylon 6,6 membrane with the
use of PST method, their adhesion and surface properties markedly
improved through a conversion of carbonyl and hydrocarbon groups into
carboxylic groups [18], at same time that this surface treatment does not

* Corresponding author.
E-mail addresses: vtsinh92@skku.edu (T.S. Vo), vttbchau@ctu.edu.vn (T.T.B.C. Vo).

https://doi.org/10.1016/j.pnsc.2022.03.010
Received 29 September 2021; Received in revised form 19 March 2022; Accepted 29 March 2022
Available online 12 April 2022
1002-0071/© 2022 Chinese Materials Research Society. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
T.S. Vo, T.T.B.C. Vo
Fig. 1. Chemical structures and images of PI and PET.
almost impact to the mechanical properties during the surface treatment
for a material [19,20]. For UV surface treatment (UST), it is considered
that the treatment probably breaks up molecular bonds and interactions
on the surface of materials through high-energy UV photons; concomi-
tantly, an UV oxidation process can form several possible functional
groups in relation to hydroxyl, carboxyl, or carbonyl groups that en-
hances hydrophilicity and adhesion behaviors presented on the treated
surface of materials [21,22]. A general aim in the use of both PST and
UST are able to induce physical and chemical surface changes in poly-
mers through several concurrent processes, i.e., etching, grafting, poly-
merization, cross-linking, usually without modifying their original bulk
qualities [23]. In these approaches, low-pressure plasma and UV treat-
ments are able to be proposed to modify many surface properties of
polymers, including adhesion, friction, penetrability, wettability,
dye-ability, or biocompatibility, which adapt to specific applications
[23]. Thereby, these approaches are favorable for opening up of a wide
spectrum of surface polymers with desired compositions.
Nowadays, polymeric materials were applied widely in multiple
modern industries; however, almost all polymeric materials show the
surfaces with low hydrophilicity that can significantly impact the
wettability, biocompatibility, printability, and adhesion of the materials.
Hence, polymer materials, especially for polymeric membranes, are truly
necessary to undergo surface treatments to reach better hydrophilicity,
adhesion, and surface activities [24–26]. In particular, aromatic poly-
imide (PI) and polyethylene terephthalate (PET) are polymeric mem-
branes utilized widely in several different applications [27]. PI
membrane contains imide monomers pertaining to a high performance
plastic membrane, which is frequency applied to other rugged organic
materials, i.e., displays, fuel cells, etc., owing to its availably high
heat-resistance [28]. Whereas, PET, a polyester, which is a linear ther-
moplastic polymer, has a vast applicability based on numerous of
modification processes [27]. Overall, these polymeric membranes were
different in the chemical structure and the surface characterization, i.e.,
amine, hydroxyl, carboxyl, and aldehyde groups, which enable the polar
surface behaviors happening on the surface of both polymeric mem-
branes after the PST and UST processes [16,17]. Plasma and UV treat-
ments are powerful techniques to modify only the polymer surface.
Simultaneously, the main aim of this work is to probably give an over-
view of PST and UST approaches, which all were performed on the sur-
face of PI and PET membranes to grant a relation of the treatment
mechanism and the corresponding changes in the chemical structure of
treated membranes. In another hand, these polymeric membranes will be
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exposed directly under the discharge electrode and UV LED curing sys-
tem to be treated their surfaces becoming better hydrophilicity (or
wettability), adhesion, and surface behaviors, owing to physical and
chemical surface changes in polymers. Different treating and recovering
durations are also investigated on the analysis based on the water contact
angle (WCA) measurement, Fourier-transform infrared (FTIR) and
Raman spectroscopy, and optical microscopy (OM) images, which are
probably the support to confirm the hydrophilicity and surface properties
of the polymeric membranes after the surface treatments, and a 90
peel
test is applied to examine their adhesion behaviors.
2. Materials and methods
2.1. Materials
The commercially available polyimide (PI) (0.075 mm  750  750
mm2) and polyethylene terephthalate (PET) (0.125 mm  600  600
mm2) membranes (see Fig. 1) were purchased from Good-fellow Com-
pany. A 3M scotch brand tape (5413K) was offered by a Korean company.
2.2. Plasma and UV surface treatments
Both PI (0.075 mm  150  150 mm2) and PET membranes (0.125
mm  150  150 mm2) were treated by an atmospheric plasma generator
(FEMTO SCIENCE, plasma power ¼ 150 W, gas pressure ¼ 1.5 torr) and
an oven UV instrument (MS TECH, UV power ¼ 5000 mW/cm2, λ ¼ 365
nm). The distance between the membrane surface and the electrode, and
UV LED curing system was 100 mm and 30 mm, respectively. All mem-
branes were surveyed with different tested times (t ¼ 0; 2; 5; 10 min) by
plasma and UV instruments. Then, the surfaces of treated polymeric
membranes were recovered corresponding to the above treated times (t
¼ 2; 5; 10 min). The experimental systems of PST and UST utilized in this
study are shown in Fig. 2.
2.3. Water contract angle measurement
In order to determine the hydrophobic–hydrophilic behavior of the
polymeric membranes after PST and UST, a drop technique was applied
to investigate the water contact angle (WCA) [SEO Phoenix MT(M)] by
using a distilled water drop (volume ¼ ~5 μL; average values, n ¼ 3). The
WCA values were calculated by analyzing the captured drop images
basing on the ImageJ® program.
T.S. Vo, T.T.B.C. Vo
Fig. 2. Images and schematic diagrams of PST (A–C) and UST (D–F) systems.
2.4. FTIR and Raman analysis
The chemical characterization of the treated membrane surfaces was
analyzed by a Fourier-transform infrared (FTIR) spectrophotometer
(Nicolet 380, Ietled Co.) and a Raman spectrum (XperRam200) with a
laser wavelength of 532 nm. It was recorded at the wavenumber region of
4000–500 cm1 and the Raman Shift region of 3200–100 cm1 corre-
sponding to FTIR and Raman spectrums.
2.5. Peel strength and tensile analysis
A 90
peel test was carried out on a Peel Adhesion Strength Tester
instrument with a 50 N of universal load cell and 10 mm⋅min1 of pulling
speed. The membrane was tightly fixed on a platform, and the tape was
firmly attached in the upper clamp that would pull the tape up at 90
,
while the under platform moved to the right side to could be maintained
with the 90
of angle. With increasing a steady rate of the upper clamp,
the peeling force could be recorded through peeling the tape off of the
membrane (average values, n ¼ 3). Concomitantly, the stress-strain curve
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Progress in Natural Science: Materials International 32 (2022) 314–327
of tensile test (a utilized size ¼ 10  50 mm2) was performed by a uni-
versal tensile machine (UTM model 5565, UK) with 250 N of load cell
and 10 mm⋅min1 of pulling rate (average values, n ¼ 3).
2.6. SEM and OM measurements
The initial morphological structures of PI and PET membranes (i.e.,
top-surface and cross-section) were captured from scanning electron
microscopy (SEM) (FESEM JSM-7600F) at different magnifications and
positions. Besides, in order to observe the change in the surface
morphology of the treated membranes, their morphology surfaces were
investigated before and after PST and UST using an optical microscopy
(OM) (Olympus SZX12) and i-Solution™ IMTcamCCD Digital Camera.
3. Results and discussion
3.1. WCA and surface morphology of polymeric membranes
The morphological characterization of a membrane-like material is
T.S. Vo, T.T.B.C. Vo
Fig. 3. SEM images of initial PI (A–B) and PET (C–D) membranes: top-surface (A, C) and cross-section (B, D). SEM images of PI (E–F) and PET (G–H) membranes with
PST (E, G) and UST (F, H) (t ¼ 5 min).
one of important factors to acquire desired evaluations depending on
different studies' purposes. Herein, the morphological structure of
membranes has been detected by SEM images (Fig. 3), indicating that the
top-surface (Fig. 3 A, C) and cross-section (Fig. 3 B, D) morphologies of
the initial membranes (i.e., untreated membranes, t ¼ 0 min) were
relatively smooth and non-rough surfaces, and the pores did also not
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Progress in Natural Science: Materials International 32 (2022) 314–327
appear on their corresponding top-surface and cross-section regions.
Thereby, these initial membranes were the smooth and flat surfaces. The
surface treatment is considered as an expressing step so that it is able to
successfully coat the other materials on the treated substrates conducted
in various applications, owing to physical and chemical surface changes
in polymers. To better understand the changes of the PST- and UST-
T.S. Vo, T.T.B.C. Vo
Fig. 4. WCA images of PI and PET membranes after PST–Recovery (A) and UST–Recovery (B) processes with different tested times (t ¼ 0; 2; 5; 10 min).
treated membranes, their corresponding topography has been also
characterized by SEM images (Fig. 3E–H). It showed that the strange
streaks appeared on the surfaces of these treated membranes (t ¼ 5 min)
comparing to the initial membranes (yellow arrows were illustrated in
the SEM images), and their surfaces became rougher than that of un-
treated membranes. As such, these resulted in the evidence of slight
surface aging/damage during the PST and UST processes, especially for
the PST. Similarly, this phenomenon has been also clearly demonstrated
in relevantly previous researches regarding to surface modifications of
treated polymers [29–32]. As seen in Fig. 3E–H, the strange streaks on
the PST-treated membranes (Fig. 3 E, G) appeared more densely than
those of the UST-treated ones (Fig. 3 F, H), revealing that the effect of
atmospheric plasma treatment with the electric direction was more
effective comparing to the UV LED field. Besides, the PST- and
UST-treated PI membranes (Fig. 3E and F) were observed with the
rougher surfaces comparing to the treated PET ones (Fig. 3G and H),
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Progress in Natural Science: Materials International 32 (2022) 314–327
which could be favorable for significantly enhancing wettability and
adhesion behaviors of the treated PI membrane.
The surface treatment is known to successfully coat the other mate-
rials on the treated substrates conducted in various applications. For the
hydrophobic–hydrophilic behavior of the polymeric membranes after
PST and UST processes, a drop technique was applied to investigate the
WCA by using a distilled water drop. The WCA values were calculated
through analyzing the captured drop images. Herein, we will firstly
assess the different PST and UST treated durations (t ¼ 2; 5; 10 min), as
an investigation for possible changes on these polymer surfaces, and then
the surfaces of treated membranes were recovered corresponding to the
above treated durations. In theory, the WCA value (θ) is less than 90

indicating a hydrophilic surface of a material. Besides the smooth and flat
surface morphologies of the initial membranes (Fig. 3 A, C), the surfaces
presented the WCA of 56.7
 3.7
and 61.4
 4.3
corresponding to the
initial PI and PET membranes (t ¼ 0 min) (Figs. 4 and 5); therefore, the
T.S. Vo, T.T.B.C. Vo
Fig. 5. WCA values of PI and PET membranes after PST (A) – Recovery (B) and UST (C) –Recovery (D) processes with different tested times (t ¼ 0; 2; 5; 10 min). WCA
images of PI and PET membranes after PST–Recovery–PST process (E) (t ¼ 5 min). Schematic diagram of hydrophobic–hydrophilic behavior of membrane before and
after PST/UST–Recovery (F).
wettability of PI membrane was better than that of PET one, due to the
available hydrophilic nature of each membrane. After performing the
PST and UST processes, the WCA values of both the treated PI and PET
membranes exhibited a decrease corresponding to the increasing treated
durations, and which reached the lower WCA values comparing to the
initial membranes, especially in the PST process [Fig. 4 (A, B) and Fig. 5
(A, C)]. As such, the wettability improved significantly on the surface-
treated membranes (i.e., PST-treated PI membrane: 73.9%/2 min,
84.7%/5 min, 100%/10 min; and PST-treated PET membrane: 38.6%/2
min, 49.5%/5 min, 50.8%/10 min; and UST-treated PI membrane:
15.2%/2 min, 30.3%/5 min, 1.6%/10 min; and UST-treated PET mem-
brane: 6.0%/2 min, 2.4%/5 min, 0.2%/10 min). Moreover, the
wettability of PST-treated membranes was greater than that in the UST
process, maybe due to the contribution of polar functional groups rep-
resented on the surface of PST- and UST-treated membranes [33,34]
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Progress in Natural Science: Materials International 32 (2022) 314–327
(Fig. 5F). Actually, the modified surfaces by the atmospheric PST process
based on several factors, especially for the average energy occurring in
free electrons, which was in charge to make certain for changes in
chemical bonds, interactions and orientations of molecules in the mem-
branes being effective more than the UST process, by using UV LED field.
The wettability is considered as an especial trend of the adhesive
behavior of polymeric materials; concomitantly, it also relates to an
important relationship with surface energy. It means that the surface
energy is increased according to the wettability (or hydrophilicity) [29].
Additionally, Figs. 4A and 5A depicted the changes in the WCA for the
PST-treated polymeric membranes, resulting that the WCA for a polar
medium (water) reduced significantly after 5 min of PST, and the
remaining membranes unchanged much beyond 5 min (i.e., PI mem-
brane: 14.8
 3.3
/2 min, 8.7
 3.5
/5 min, 0
/10 min; and PET
membrane: 37.7
 3.9
/2 min, 31.0
 4.5
/5 min, 30.2
 3.6
/10
T.S. Vo, T.T.B.C. Vo
Fig. 6. OM images of PI (A–C) and PET (D–F) membranes before (A, D) and after PST (B, E) and UST (C, F) (t ¼ 5 min). Schematic diagram of surface morphology
behavior of membrane before and after PST/UST (G).
min). Whereas, the change in the WCA values of UST-treated membranes
was not according to the above-suggested regulations, such as an increase
in the treated PI membranes and an almost constant in the treated PET
membranes occurring between the treatment durations of 5 and 10 min;
in contrast, a decrease in the treated PI membranes and a rise in the
treated PET membranes happened between the treatment durations of 2
and 5 min (i.e., PI membrane: 48.1  3.9
/2 min, 39.5
 4.5
/5 min,
55.8
 3.6
/10 min; and PET membrane: 57.7
 3.3
/2 min, 62.9

3.5
/5 min, 62.3
 3.0
/10 min) (Figs. 4B and 5C). Overall, besides 5
min of the treatments, 10 min was also able to use successful treating on
the surface of polymeric membranes. Although there were differences in
the changes of each surface treatment method, a tested time of 5 min is
able to be selected as an optimal time for examining essential modifi-
cations on the surface of polymeric membranes to reduce the process
time.
In the recovery processes [Fig. 4 (A, B) and Fig. 5 (B, D)], comparing
to the initial membranes, the WCA values still display a decrease with the
increasing recovered durations, as well as a significant improvement in
the wettability occurring on the membrane surfaces, excepting for the
recovered PET membrane after UST (i.e., recovered PI membrane after
PST: 72.8%/2 min, 55.7%/5 min, 73.5%/10 min; and recovered PET
membrane after PST: 40.7%/2 min, 48.5%/5 min, 49.2%/10 min; and
recovered PI membrane after UST: 14.8%/2 min, 22.5%/5 min, 2.5%/10
min; and recovered PET membrane after UST: 1.5%/2 min, 3.1%/5
min, 3.7%/10 min). Besides, according to a comparison of the corre-
sponding treated-recovered membranes, the WCA values showed a slight
increase, excepted for the 5 min - recovered PI membrane after PST (i.e.,
recovered PI membrane after PST: 4.1%/2 min, 65.5%/5 min; and
recovered PET membrane after PST: 3.4%/2 min, 1.9%/5 min, 3.3%/10
min; and recovered PI membrane after UST: 0.4%/2 min, 11.1%/5 min,
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Progress in Natural Science: Materials International 32 (2022) 314–327
0.9%/10 min; and recovered PET membrane after UST: 8.0%/2 min,
0.6%/5 min, 3.9%/10 min), meaning that the wettability of these
recovered membranes was less not much than this of treated membranes.
Obviously, the recovery ability of the polar component involved to the
unstable polar functional groups on the surface, which were able to be
oxidized and formed peroxides associating to the surrounding oxygen
and moisture [13], meaning that this decrease was attributed to an in-
crease in the molecular orientations leading to reducing the possibly
dispersive interactions [13], which was suitable and clearly analyzed by
Shaw et al. [13]. Overall, the wettability of these polymeric membranes
occurring in the PST and recovery processes was still greater than that in
the UST and recovery process, meaning that the effect of hydrophilic
surface was happened better during the PST process. The hydrophilic
groups were organized onto the surface of polymeric membranes after
PST and UST processes; in particular, these functional groups were able
to be oxidized or oriented after the recovered time, based on the increase
in the WCA values. Nonetheless, there were still some rational steps being
missed (i.e., uniformity, mobility, hydrophobicity, orientation, polarity
and interaction) [35,36], the recovery ability of the hydrophobicity
happening on the UST-treated surfaces was mainly attributed to the
mobility and orientation of the polar functional groups [13]. To further
understand, the recovered membranes after the PST process were utilized
for treating once more time (t ¼ 5 min) on the surface of these recovered
membranes (Fig. 5E). As a result, the WCA values of polymeric mem-
branes after the second PST process were almost equal with the ones after
the first PST process (i.e., 9.0
 3.9
/PI and 31.8
 4.3
/PET), sug-
gesting that their wettability was still well maintained, might be due to
the repeated physical (i.e., aging or damage) and chemical (i.e., chemical
bonds, interactions and orientations of molecules) surface changes of in
the membranes.
T.S. Vo, T.T.B.C. Vo
Fig. 7. FTIR (A, B) and Raman (C, D) spectrums of PI (A, C) and PET (B, D) membranes before and after PST and UST.
Moreover, Fig. 6 (A-F) showed the OM images of the membranes’
surface before and after the PST and UST processes (t ¼ 0 min and 5 min).
Resulting that the whole of corresponding views of the treated mem-
branes (t ¼ 5 min) indicated evenly strange streaks with different colors
on the surfaces comparing to the initial membranes (t ¼ 0 min), as
noticed by yellow dashed arrows on the OM images. In another word, the
characterization by OM images displayed direct impactions on the initial
surface of these membranes and the evidence of slight surface aging/
damage during the PST and UST processes [37], i.e., physical and
chemical surface changes in polymers, which was also appropriate with
the abovementioned SEM results. Indeed, Novak et al. [38] investigated
that the crystallinity degree of isotactic polypropylene had an influence
on the aging of PST-treated polymeric materials, indicating that
restricted mobility (crystalline polymer) decreased the aging rate effect
by reducing the surface polymer chains rearrangement. Herein, the
number of these streaks were appeared greater on the PST-treated
membrane surfaces comparing to the UST-treated one, meaning that
the effect of modified surface was occurred better during the PST process,
which was also agreed in the abovementioned changes of WCA values. In
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Progress in Natural Science: Materials International 32 (2022) 314–327
actual, a heterogeneous discharge was happened with numerous current
pulses at atmospheric pressure that was able to create an asymmetric
erosion on the surface of the polymeric membranes leading to eroding
and modifying the surface morphology, at same time that it could also
induce the differences in changes of chemical bonds, interactions and
orientations of molecules occurring on the surface of polymeric mem-
branes (Fig. 6G). These were obviously pointed in the increase in the
wettability of polymeric membranes after the PST process comparing to
the UST one, at same time that the wettability enhancement of treated
membranes was also agreed in relevant research of Toufik et al. [29].
3.2. FTIR and Raman spectroscopy of polymeric membranes
In general, it is truly necessary to determine possible changes on the
surface of polymeric membranes during the PST and UST processes, as
well as their mentioned chemical characterization. In addition to the
abovementioned morphological characterization of the polymeric
membranes with the treated surfaces, Fig. 7A and B showed the FTIR
spectra of polymeric membranes before and after the PST and UST
T.S. Vo, T.T.B.C. Vo Progress in Natural Science: Materials International 32 (2022) 314–327

Table 1 Table 3
FTIR and Raman characteristics and the corresponding chemical bonds of initial FTIR and Raman characteristics and the corresponding chemical bonds of PST-
PI and PET membranes (t ¼ 0 min). and UST-treated PET membrane (t ¼ 5 min).
FTIR, cm1 Chemical bonds of FTIR, cm1 Chemical bonds of PET FTIR, cm1 PST-treated PET FTIR, cm1 UST-treated PET
PI
3510–3250 Broader O–H 3510–3250 Broader O–H
3520–3180 CH2 (ethyl 3510–3250 O–H 3065 C–H (phenyl ring) 3065 C–H (phenyl ring)
groups) 2970 CH2 (ethyl groups) 2973 CH2 (ethyl groups)
2931–2895 C¼O (imide I 3065 C–H (phenyl ring) 2909 H–C¼O 2909 H–C¼O
linkage) 1721 C¼O (ester linkage) 1719 C¼O (ester linkage)
1705 C–H (ethyl groups) 2972 CH2 (ethyl groups) 1567 C–H (phenyl ring) 1577 C–H (phenyl ring)
1219 C–O (backbone) 2909 H–C¼O 1477 C–C (phenyl ring) 1505 C–C (phenyl ring)
1494–1347 C–N (imide II/III 1720 C¼O (ester linkage) 1361–1230 C–O (ester linkage) 1350–1227 C–O (ester linkage)
1186–899 linkages) 1151–900 C–H (ethyl groups) 1150–889 C–H (ethyl groups)
729 C–C (backbone) 1598 C–H (phenyl ring) 720 Sharper and larger 720 Sharper and larger
N–H 1508 C–C (phenyl ring) C–C (backbone) C–C (backbone)
1359–1228 C–O (ester linkage)
Raman, cm¡1 PST-treated PET Raman, cm¡1 UST-treated PET
1152–905 C–H (ethyl groups)
720 C–C (backbone) 3083 Benzene ring 3083 Benzene ring
skeleton skeleton
Raman, cm¡1 Chemical bonds of Raman, Chemical bonds of PET
1730 C¼O (ester linkage) 1730 C¼O (ester linkage)
PI cm¡1
1511 C¼C 1511 C¼C
1785 C¼O (imide I) 3083 Benzene ring skeleton 731–1351 C–O (ester linkage) 731–1351 C–O (ester linkage)
1509 C¼C 1730 C¼O (ester linkage) 1612 C–C (phenyl ring) 1612 C–C (phenyl ring)
1398 C–N–C axial (imide 1511 C¼C 1178–1186 C–C (phenyl ring) 1178–1186 C–C (phenyl ring)
II) <900 C–H 1089 Crystallinity degree of
1260 C–O–C backbone 731–1351 C–O (ester linkage) trans structure
1125 C–N–C transverse 1612 C–C (phenyl ring) 883 (weak) – –O–CH2CH2–O– <900 C–H
(imide III) 994 (strong) (gauche and trans)
865 Diamine ring 1178–1186 C–C (phenyl ring) 883 (weak) – –O–CH2CH2–O–
breathing 994 (strong) (gauche and trans)
739–826 C–H <900 C–H
640 C–O–C backbone 883–994 –O–CH2CH2–O– (gauche
orientations and trans) membrane relating to the C–H (phenyl ring) and H–C¼O vibrations,
1621–750 Dianhydride part respectively [39]. The typical peaks of the PI membranes were observed
at 1705 cm1, 1494–1347 cm1 and 1186–899 cm1 corresponding to
the C¼O (imide I linkage), C–O (backbone) and C–N (imide II and III
Table 2 linkages) stretching vibrations, while those of the PET membrane were
FTIR and Raman characteristics and the corresponding chemical bonds of PST- suggested at 1720 cm1, 1508 cm1 and 1359–1228 cm1 relating to the
and UST-treated PI membrane (t ¼ 5 min). C¼O (ester linkage), C–C (phenyl ring) and C–O (ester linkage) stretching
FTIR, cm1 PST-treated PI FTIR, cm1 UST-treated PI vibrations [39]. Concomitantly, the peaks at 729 cm1 (PI) and 720 cm1
3520–3180 Broader N–H 3520–3180 Broader N–H (PET) contributed to the C–C (backbone) bending vibration. Moreover,
2941–2900 CH2 (ethyl groups) 2952–2905 CH2 (ethyl groups) the peaks of C–H (ethyl groups) bending vibration were displayed at
1689 C¼O (imide I linkage) 1678 C¼O (imide I linkage) 1219 cm1 (PI) and 1152–905 cm1 (PET), at same time those of C–H
1720 C¼O (asymmetric 1718 C¼O (asymmetric
bending vibration containing in phenyl ring were observed at 1598 cm1
tension) tension)
1220–1249 C–H 1211–1240 C–H
in the FTIR spectrum of initial PET membrane [39]. In particular, the
1514–1359 C–O (backbone) 1526–1366 C–O (backbone) broad peak at 3520–3180 cm1 (PI) and 3510–3250 cm1 (PET) was
1186–899 Broader and larger C–N 1186–899 Broader and larger C–N characteristic to the N–H and O–H stretching vibrations, respectively
(imide II/III linkages) (imide II/III linkages) [39].
729 Sharper and larger 729 Sharper and larger
For the PST- and UST-treated PI membrane (t ¼ 5 min) (Fig. 7A and
C–C(backbone) C–C (backbone)
Table 2), it displayed the characteristic peak corresponding to the C¼O
Raman, PST-treated PI Raman, UST-treated PI
stretching vibration at 1689 cm1 (PST) and 1678 cm1 (UST), at same
cm¡1 cm¡1
time these treated PI membranes indicated another peak at 1720 cm1
1785 Broader C¼O (imide I) 1785 Sharper C¼O (imide I) (PST) and 1718 cm1 (UST) that also regarded to the C¼O vibration
1509 C¼C 1509 C¼C
1415 Broader C–N–C (imide 1411 C–N–C (imide II)
(asymmetric tension vibration) at lower intensities. Besides, the peaks
II) relating to the C–O stretching vibration moved to higher wavenumber
1260 C–O–C backbone 1260 C–O–C backbone regions (1514–1359 cm1/PST and 1526–1366 cm1/UST) and higher
1139 C–N–C (imide III) 1130 C–N–C (imide III) intensities comparing to the initial PI membrane (1494–1347 cm1). For
865 Diamine ring breathing 865 Diamine ring
the PST- and UST-treated PET membrane (t ¼ 5 min) (Fig. 7B and
breathing
739–826 C–H 739–826 C–H Table 3), the peaks of C¼O and C–O stretching vibrations almost un-
640 C–O–C backbone 640 C–O–C backbone changed much about the wavenumber regions, i.e., the C¼O stretching
orientations orientations vibration was observed at 1721 cm1 (PST) and 1719 cm1 (UST), while
610 Benzene deformation 1629 (strong) Dianhydride part the C–O vibration was showed at 1361–1230 cm1 (PST) and
750(weak)
1350–1227 cm1 (UST), but their intensities were higher than those of
750 (weak) Dianhydride part

processes (t ¼ 5 min) to investigate the chemical characterization of their
treated surfaces. For the FTIR spectrums of initial PI and PET membranes
(t ¼ 0 min) (Fig. 7A and B and Table 1), all exhibited the characteristic
peaks at 2931–2895 cm1 (PI) and 2972 cm1 (PET) corresponding to
the –CH2 (ethyl groups) stretching vibrations, especially for the peaks at
3065 cm1 and 2909 cm1 appeared in the FTIR spectrum of initial PET
initial PET membrane. As such, these suggested the small surface changes
of polymeric membranes occurring in the wavenumber region of
carboxyl groups during the PST and UST processes [39], especially in the
PST process. Simultaneously, the other changes of N–H (PI) and O–H
(PET) stretching vibrations could be observed in the FTIR spectra of
treated polymeric membranes occurred in the very broad wavenumber
regions of 3520–3180 cm1 (PI) and 3510–3250 cm1 (PET) and higher

322
T.S. Vo, T.T.B.C. Vo
intensities (Fig. 7A and B). As abovementioned hydrophilic behaviors,
this investigation manifested a considerable quantity of polar functional
groups on the surface of treated polymeric membranes. Besides, the peak
of C–H beading vibration (1219 cm1) appeared in the treated PI
membranes (1220 cm1/PST and 1211 cm1/UST), another peak of C–H
vibration was also presented at 1249 cm1 and 1240 cm1 corresponding
to the PST- and UST-treated PI membranes (Fig. 7A and Table 2).
Whereas, the peaks of C–H bending vibration (1152–905 cm1) were
larger and sharper, at same time they moved slightly to lower wave-
number regions (1151–900 cm1/PST and 1150–889 cm1/UST) in the
treated PET membranes (Fig. 7B and Table 3). Furthermore, the treated
polymeric membranes have been found the C–C (backbone) bending
vibration (729 cm1/PI and 720 cm1/PET) at very sharp and large
peaks comparing to the initial polymeric membranes (Fig. 7A and B)
[39]. Notably, the intensities of C–H bending (1598 cm1) and C–C
stretching (1508 cm1) vibrations containing in phenyl ring decreased at
lower wavenumber regions occurring in the treated PET membranes
(Fig. 7B and Table 3), while the C–N stretching vibrations (1186–899
cm1) corresponding to the imide II and III linkages of treated PI mem-
branes reached at the broader and larger peaks (Fig. 7A and Table 2). As a
result, there were the obvious changes occurring on the surface of
polymeric membranes during the PST and UST processes. Thereby, the
bending and stretching vibrations were well determined consisting of
their relationships in the possible changes on the treated polymeric
surfaces, but researches in the low wavenumber range were uncommon
[40].
As known, there are some different principles between Raman and
FTIR spectra. Specifically, the FTIR spectroscopy bases on the changes of
molecular dipole moment, while the Raman spectrum involves to the
polarizations-induced molecules. In fact, both the FTIR and Raman
spectrums support mutually on the molecular structures. Indeed, the
peaks of stretching/bending vibrations can be strong in the Raman
spectra, and which cannot be specifically observed in the FTIR spectrum.
One of the most notable features of Raman spectroscopy is regarded to
the photonic probe that can be seen as a nondestructive detection
approach. Previously, both the FTIR and Raman spectrums utilized
models of variable calibration for morphology characterization of poly-
meric materials, but the molecular orientations in a polymeric material
regarding its available composition can considerably affect to the con-
tained band shapes and intensities. Herein, the Raman spectrum was also
used to evaluate the nature of chemical bonds, interactions and orien-
tations of molecules in the polymeric membranes. Specific Raman spec-
trums of initial and treated polymeric membranes’ surfaces were
displayed in Fig. 7C and D. For the Raman spectra of initial PI membrane
(t ¼ 0 min) (Fig. 7C and Table 1), the characteristic peaks were exhibited
at 1785 cm1, 1398 cm1 and 1125 cm1 corresponding to the stretching
vibrations of imide I (C¼O stretching vibration), imide II (C–N–C axial
stretching vibration) and imide III (C–N–C transverse stretching vibra-
tion) [41,42]. Besides, the C–O–C backbone orientations involved to the
aromatic imide ring at 1260 cm1 (stretching vibration) and 640 cm1
(bending), at same time that those of aromatic imide ring in di-anhydride
part were indicated at 1621 cm1 (strong) and 750 cm1 (weak) [41,42].
The peaks at 1509 cm1, 865 cm1 and 739–826 cm1 belonged to the
C¼C, diamine ring breathing and C–H vibrations, respectively. For the
initial PET membrane spectra (t ¼ 0 min) (Fig. 7D and Table 1), it
indicated that the main peak intensities were larger, which could be due
to the PET molecules included the high Raman scattering intensity
benzene ring. The typical peaks were displayed at 1730 cm1 (sharp and
large peak) and 731–1351 cm1 regarding to the C¼O (ester linkage) and
C–O (ester linkage) stretching vibrations, while the peaks of C–C (phenyl
ring) vibrations were seen at 1178–1186 cm1 (anti-symmetric stretch-
ing vibration) and 1612 cm1 [43,44]. Especially, the bending vibration
peak of C–H with isolated adjacent hydrogen and hydrogen bond on
323
Progress in Natural Science: Materials International 32 (2022) 314–327
benzene ring was at <900 cm1 [45], and the C¼C vibration related to
the peak at 1511 cm1. The notable peaks at 883 cm1 (weak) and 994
cm1 (strong) were attributed to the gauche and trans structures in the
ethylene glycol segments (–O–CH2CH2–O–) regarding to the orientation
and crystallinity degree of the PET membrane [43,46]; moreover, the
weak peak at 3083 cm1 was yielded on the benzene ring skeleton
vibration.
There were some changes of chemical bonds, interactions and ori-
entations of molecules in the Raman spectrums of PST- and UST-treated
polymeric membranes (t ¼ 5 min) (Fig. 7C and D). Notably, all intensities
lowered after the PST and UST processes, maybe due to the chain length
reduction regarding to the chain breakage, i.e., the C–H and C–C groups
would be fractured by the yielded free radicals on the membranes' sur-
faces leading to combining with the species (PST and UST) and producing
the polar groups on these treated surfaces, at same time the molecular
chains and planes were also rearranged and reoriented [47]. Conse-
quently, these peaks were also moved to the lower Raman shifts' regions
comparing with the initial membranes. The peak of mono-substituted
benzene deformation (610 cm1) in the PI membrane spectrum
(Fig. 7C and Table 2) also changed for the intensity and the region of
Raman shift after the PST process; simultaneously, the characteristic
peaks of the initial PI membrane at 1621 cm1, 1398 cm1 and 1125
cm1 shifted to other regions of Raman shift in the PST- and UST-treated
PI membrane (i.e., PST: those at 1632 cm1, 1415 cm1 and 1139 cm1;
and UST: those at 1629 cm1, 1411 cm1 and 1130 cm1). Thereby,
these differences manifested that the aromatic imide ring and C–N–C
groups (imide II and III) were much affected through these treatment
processes, especially for the PST process [48]. In another word, the
dipole C¼O moment containing in the aromatic imide ring could vibrate
much more in the electric direction comparing to the UV LED field, which
led to moving the molecular segments and orientating the dipole in the
cases of the corresponding vectors. On the other hand, this moment could
also vibrate according to the opposite direction in the aromatic imide
ring. As such, the changes of chemical bonds, interactions and orienta-
tions of molecules, specifically in the aromatic imide ring, which would
occur and be much impacted leading to the Raman shifts moving to larger
regions compared to other groups on a basic of repeated vibrations in the
two directions [48]. Furthermore, it could be also found in the rela-
tionship of amide-imide linkages and the orientations of imide linkages
occurred in the PI membrane after the PST and UST processes, especially
in the PST process (Fig. 7C) [49]. Basically, the peak at 1621 cm1 (ar-
omatic imide ring) was selected as a reference peak, and which could
allow manifesting the orientations of various availably functional groups
regarding to the imide phenyl ring, i.e., the C–O–C backbone (1260
cm1) orientation was corresponded to the aromatic imide ring and the
C¼O group (1785 cm1, imide I). As a result, the intensity of C–O–C
backbone lowered and the C¼O group was more stretched during the PST
and UST processes, which could be due to the effects of the radiation and
the alternating electric field respectively, especially for the C¼O
stretching occurred in the PST process [49,50]. This phenomenon could
probably induce the possible chemical bond fractures, the formation of
free radicals and the PI molecular degradation on the basic of PST process
[50]; instead of the reorientations and reversion of the chemical bonds in
the PI molecules basing on the UST process. Also, this was occurred
similarly with the C–N–C backbone orientation (1398 cm1/imide II and
1125 cm1/imide III), which led to stretching the C–N–C vibrations more
during the PST process [50]. For the PST- and UST-treated PET mem-
brane (Fig. 7D and Table 3), in addition to the abovementioned main
chain length reductions, the molecular chain rearrangements and plane
reorientations occurred during the PST and UST processes, the phenyl
ring contributions to the Raman spectra were sited at 1612 cm1 (C–C
stretching vibrations), 1178–1186 cm1 (anti-symmetric stretching vi-
bration) and 1511 cm1 (C¼C vibration), which were almost unchanged
T.S. Vo, T.T.B.C. Vo
Fig. 8. Schematic diagram of membrane under a 90
peel test (A). Peel Force-Length curves of PI (B, D) and PET (C, E) membranes before and after PST (B, C) and UST
(D, E).
much during the PST and UST processes that could be due to possible
strength of phenyl ring [43,44,46,51]. This approach was similar with
the carbonyl stretching peaks (C¼O and C–O groups, ester linkages),
which did not also appear on the changes of intensity and Raman shift
regions [40]. Notably, the peak at 994 cm1 (trans) was observed clearly
more than that at 883 cm1 (gauche) (–O–CH2CH2–O– segments) in both
the PST- and UST-treated PET membrane relating to the amorphous
phase of the treated PET membrane, main due to the reorientation and
rearrangement of these segments under the effects of electric and UV LED
fields, especially in the PST process [43,46]. However, the new peak
appeared at 1089 cm1 in the UST-treated PET membrane, which was a
probe of crystallinity degree and a conformation of the trans structure
[52]. Obviously, there were the changes occurred on the membranes’
surface during the PST and UST processes, which were based on the
chemical bonds, interactions and orientations of molecules through the
FTIR and Raman spectroscopy, and it can significantly support to the
324
Progress in Natural Science: Materials International 32 (2022) 314–327
abovementioned hydrophilic behaviors, more specially for the apparition
and insertion of polar functional groups (C¼O and –OH) after the surface
treatments.
3.3. Peel strength behavior of polymeric membranes
For a surface-treated membrane, the adhesive behavior is an impor-
tant factor to assess performances of the surface modification. The most
usual way is used to investigate the bonding and interaction happened
between the surfaces (or layers), named “peel test”. Tape will be manu-
ally applied to the testing surface, which is then quickly removed. In this
work, a 90
peel test was conducted to evaluate the adhesive perfor-
mances on the treated surface of these membranes, as described in
Fig. 8A. For the initial membranes (t ¼ 0 min), the tape was peeled with a
calculated average force of 2.99  0.35 N and 2.79  0.31 N, while a
maximum force obtained at 3.09  0.31 N and 2.89  0.33 N
T.S. Vo, T.T.B.C. Vo Progress in Natural Science: Materials International 32 (2022) 314–327

Table 4 calculated average force almost unchanged significantly). Generally,

The peel force values of all samples. these peel forces of initial PI membrane were greater than those of initial
Samples Maximum Force Average Force Calculated Average PET one (Table 4), maybe due to the hydrophilic behavior of the mem-
(N) (N) Force (N) brane surface and the chemical bonds/interactions between the tape and
PST-treated PI – 0 3.09  0.31 3.00  0.32 2.99  0.35 these membranes [53–55]. After performing the PST and UST processes,
min the peel forces exhibited an increase comparing to the initial membranes,
PST-treated PI – 2 3.28  0.33 3.01  0.34 3.07  0.34 especially in the PST process (Fig. 8B–E). The adhesive behavior
min mentioned in this study was characterized by a delamination of the tape
PST-treated PI – 5 3.67  0.35 3.21  0.39 3.25  0.38
min
from these membranes without any tearing, which was demonstrative in
PST-treated PI – 3.56  0.40 3.34  0.29 3.39  0.32 reversible bonds and interactions (Fig. 9B and C). Specifically, it
10 min described three stages taking place during the 90
peel process, such as:
PST-treated PET – 2.89  0.33 2.78  0.31 2.79  0.31 (1) the tape would begin peeling from the surface of polymeric mem-
0 min branes, (2) which continued then partial peel from this surface consisting
PST-treated PET – 3.11  0.36 2.99  0.38 2.97  0.35 of extra elongation and bending of the tape layer. Resulting that the local
2 min peel angle was able to be variable leading to more complexing and so-
PST-treated PET – 3.28  0.38 2.98  0.37 2.94  0.32
5 min
phisticating in this stage, and then (3) the tape was completely peeled
PST-treated PET – 3.44  0.34 3.20  0.32 3.22  0.38 from this surface [53–55]. Actually, the case of low peel forces shows that
10 min the chemical bonding and interactions do not happen or were weak in
UST-treated PI – 0 3.09  0.31 3.00  0.32 3.05  0.33 order to probably couple the tape onto the polymeric membranes. Based
min on a comparison of the initial and treated membranes, the adhesive
UST-treated PI – 2 3.07  0.42 3.11  0.36 3.16  0.37 behavior favored the treated specimens more, including the tape onto the
min PST- and UST-treated membranes.
UST-treated PI – 5 3.23  0.41 3.13  0.38 3.20  0.35
min
In the case of increasing treated durations (t ¼ 2; 5; 10 min), the tape
UST-treated PI – 3.28  0.39 3.20  0.39 3.24  0.42 was still delaminated from the treated membranes during testing,
10 min meaning that the maximum and calculated average forces significantly
UST-treated PET – 2.89  0.33 2.78  0.31 2.82  0.33 improved with the treated durations (Fig. 8B–E). Besides, the adhesive
0 min behavior favored the PST-treated specimens more through their high
UST-treated PET – 3.31  0.39 3.09  0.38 3.02  0.32 peel forces (Table 4). The adhesion behavior of both PST- and UST-
2 min treated processes was happened well through the delamination of tape
UST-treated PET – 1.98  0.32 3.10  0.37 3.09  0.35
5 min
onto these membrane surfaces that was main due to the reversible bonds
UST-treated PET – 2.72  0.33 3.18  0.32 3.15  0.39 and interactions [53–55]; however, changing the treatment method from
10 min the UST to PST process improved significantly the regarding peel forces
(Table 4). Similarly, the PST of low-density polyethylene and PET also
resulted in adhesion enhancement by up to a factor of two to ten [56].
corresponding to the initial PI and PET membrane (Fig. 8B–E and
These adhesion enhancement measurements were also associated to
Table 4) (the maximum and calculated average peel forces of each
relevantly previous researches of Shenton et al. [56,57], where the
specimen were determined as in Fig. 9A, the average force and the

Fig. 9. Peel Force-Length profile of a membrane under 90
peel test (A, B). Schematic diagram of membrane under a 90
peel test with various peeling steps (C).
Stress-Strain curve of initial membranes (D).

325
T.S. Vo, T.T.B.C. Vo
surface energy of polymers could be altered and surface oxygen content
increased by exposure to the approaches of these surface treatments. In
our opinion, the effect of membrane surface and in the gap of the treated
surfaces could form a possibly binding matrix to enhance the adhesion
occurring between the tape and the membrane surface by forming the
possible chemical bonds and interactions, at same time that this surface
treatment cannot reach sufficient bond strength between the treated
membranes and the tape layer in the case of lower treated durations [55],
the discharge electrode and UV LED were not enough time to be probably
conducted for achieving polarity reversal interface on the treated mem-
brane surface. Concomitantly, the tensile stress-strain curve of each
initial polymeric membrane was presented in Fig. 9D, indicating that the
PET membrane was stiffer than the PI membrane relating to the stress at
break and Young's modulus of PET membrane higher than those of PI
membrane. Overall, the peel forces of the treated membranes exhibited
an increase comparing to the initial membranes, characteristically for
enhancing their adhesion behavior. Moreover, under the conditions of
this study, the enhancement of adhesion behavior was readily achievable
by the PST and UST methods, more especially for the PST. Although this
corresponding enhancement by the UST was not as large as that
achievable by the PST, it is still significant as in many cases only small
changes in adhesion are necessary. Also, we hope that by process opti-
mization, the degree of adhesion enhancement for the UST can be
improved.
4. Conclusion
In summary, the various approaches of the PST and UST were applied
successfully on the PI and PET membranes, indicating that the changes
occurred on the surface of these membranes. Their hydrophilic behavior
significantly improved through the WCA investigation, as well as there
were the changes in the chemical bonds, interactions and orientations of
molecules based on the FTIR and Raman spectroscopy. In another word,
these spectrums confirmed the apparition and insertion of polar func-
tional groups (C¼O and –OH) after the surface treatments, accordingly,
their wettability enhanced significantly. Besides, the SEM and OM im-
ages also displayed the direct impactions on these membranes' surface
and the evidence of slight surface aging/damage by the strange streaks’
presentation on the PST- and UST-treated surfaces. Moreover, their peel
strength behavior exhibited an increase comparing to the initial mem-
branes, characteristically for enhancing their adhesion behavior. A
comparison between the PST and UST methods, the performance of PST
reached better than that of UST, owing to special characteristics of PST
system. Besides, the physical and chemical surface changes in the PI
membrane (an aromatic thermoplastic and thermosetting polymer) were
more effective than those of PET one (a thermoplastic polymer) that was
attributed to its availably chemical features of structure. These results
were needful for enhancing surface characterization, and reaching better
adhesion behavior on the membrane-like materials and recycling poly-
mer materials. Concomitantly, this work also gave an overview on
various approaches of the surface treatment performed on different
polymeric materials.
Authors’ contributions
T.S. Vo: Conceptualization, Methodology, Formal analysis, Investi-
gation, Data curation, Visualization, Writing – original draft & review &
editing. T.T.B.C. Vo: Writing – review & editing.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
326
Progress in Natural Science: Materials International 32 (2022) 314–327
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