Journal of Electrostatics 69 (2011) 60e66

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Journal of Electrostatics
journal homepage: www.elsevier.com/locate/elstat

The effect of discharge power density on polyethylene terephthalate film surface

modification by dielectric barrier discharge in atmospheric air
Zhi Fang a, *, Xinguo Wang a, Ruping Shao a, Yuchang Qiu b, Kuffel Edmund c
a
School of Automation and Electrical Engineering, Nanjing University of Technology, Nanjing, Jiangsu 210009, China
b
State Key Laboratory of Electrical Insulation and Power Equipment, Xi’an Jiaotong University, Xi’an 710049, China
c
Department of Electrical and Computer Engineering, University of Manitoba, Winnipeg R3T 2N2, Canada

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

Article history: Polyethylene terephthalate (PET) films are modified using non-equilibrium plasma generated by DBD in
Received 7 January 2010 atmospheric air, and the effects of discharge power density on the surface modification are studied. It is
Received in revised form found that increasing discharge power density can induce more effective treatment of PET films, because
2 August 2010
this leads to a faster decrease in water contact angle and a faster increase in surface energy due to more
Accepted 1 November 2010
Available online 19 November 2010
creation of polar groups and more obvious etching occurring on the PET surface. So the treatment time
needed to achieve the same level of surface treatment can be reduced by increasing the discharge power
density.
Keywords:
Non-equilibrium plasma
Ó 2010 Published by Elsevier B.V.
Dielectric barrier discharge
Surface modification
Discharge power density
Treatment time

1. Introduction discharge current, preventing the transition of the discharge to an

PET film is widely used as an insulating material in the electrical
industry (used for making cables, capacitors etc.), and it is often
needed to be bonded with metals, alloys or ceramics. The low
surface energy of PET film results in weak joints with these high
surface energy solids. To meet the application requirements, PET
film surface modification is usually required to increase the overall
surface free energy without changing its bulk properties, thus
enhancing its wettability and the adhesive properties. In order to
extend the application range of PET films, methods have been
developed to modify its surface properties [1e7]. Among them,
surface modification by atmospheric non-thermal plasma treat-
ments has been proven as an attractive solution [8].
The dielectric barrier discharge (DBD) is one of the main ways
for generating non-equilibrium plasmas, and it has been exten-
sively studied and widely used for various industrial applications
due to its easy formation of stable plasma and its scalability [9e11].
DBD is usually generated between two metallic electrodes, of which
at least one is covered by a dielectric barrier, with an ac high voltage
applied to these electrodes. The dielectric barrier limits the
* Corresponding author. Tel.: þ86 25 84302153; fax: þ86 25 83587362.
E-mail address: myfz@263.net (Z. Fang).
arc discharge to ensure that stable non-equilibrium plasma can be
generated in the discharge regime, which is suitable for material
surface modification. DBD can operate under atmospheric pressure,
and numerous studies concerning surface treatment of materials
using DBD under atmospheric pressure have been undertaken.
These studies show that the highly reactive species in the discharge
regime of DBD can interact with the surfaces of materials and
induce some physical and chemical changes (oxidation, polymeri-
zation, crossing-linking, etching, etc.) on them, thus the surface
properties, such as wettability, printability, adhesion and conduc-
tivity are improved [12e19].
It is shown that the changes of surface properties induced by the
DBD treatments depend on the operation parameters of the DBD
system, such as gas gap distance, amplitude and frequency of
applied voltage, dielectric barrier thickness and treatment time etc.
[20,21]. Most of the results reported focus on studying on the effect
of DBD plasma to the treated surface at fixed operation parameters,
or focus on studying changes of the surface properties with treat-
ment time while keeping other operation parameters to be fixed.
While in on-line industrial applications of DBD for surface treat-
ment, in order to meet the requirements of improving the treat-
ment efficiency, it is needed to optimize the operation parameters
of DBD system to obtain optimum surface modification of poly-
mers. So it is of great interest to investigate the effects of operating

0304-3886/$ e see front matter Ó 2010 Published by Elsevier B.V.

doi:10.1016/j.elstat.2010.11.003
 Z. Fang et al. / Journal of Electrostatics 69 (2011) 60e66
parameters on DBD plasma surface modification. Except for treat-
ment time, the discharge power density is another important
operation parameter for the DBD system, which has a significant
effect on DBD plasma surface modification [22,23]. Because the
change of other operation parameters, such as gas gap distance,
amplitude and frequency of applied voltage, dielectric barrier
thickness etc. can cause the changes of discharge power, and thus
can cause the changes of discharge power density. So the effects of
these operation parameters on DBD surface modification can be
represented by the effects of discharge power density, and it is of
great interest to investigate the effects of discharge power density
on DBD plasma surface modification. Despite the fact that DBD
plasma for surface modification are widely studied, there is
currently little published work on the effects of discharge power
density on the resultant surface treatment.
In our Previous work, we used the filamentary DBD in atmo-
spheric air and homogeneous DBD in medium pressure air at fixed
discharge power density to modify the surface properties of PP, PET
and PTFE films, and the changes of these polymer surface with
function of treatment time is studied [24e26]. In this work, the
filamentary DBD in atmospheric air is used to modified the surface
properties of PET films, and five different power densities are
adopted to study the effects of discharge power density on the PET
surface modification.
2. Experimental set-up
The experiments are performed in ambient air using the
experimental set-up shown in Fig. 1, which is similar to that used in
our earlier research work [24e26]. The discharge is created
between two circular plane-parallel brass electrodes, 50 mm in
diameter, and both of them are covered by a quartz glass plate with
a thickness of 2 mm and a diameter of 70 mm as dielectric barriers.
The air gap between the two dielectric plates is kept to 2 mm, and
the PET films to be treated are placed on the bottom glass plates.
The upper electrode is connected to an AC high voltage power
supply with the amplitude from 0 to 20 kV and the frequency from
1 to 15 kHz, while the lower electrode is connected to the ground
through a resistor or a capacitor. The voltage applied to the elec-
trodes is measured via a voltage probe (Tektronix P6015A), The
discharge current and transported charges are measured by placing
a 50 U non-inductance resistor (r) and a 100 nF capacitor (C0)
between the bottom electrodes and the ground, respectively. The
Lissajous figure can be obtained on the oscilloscope screen by
plotting the transported charge on the Y-axis and the applied
voltage on the X-axis. The voltage and current waveform, and the
Fig. 1. Schematic diagram of the experimental set-up and measurement connection: 1
high voltage electrode, 2 dielectric barrier (Quartz glass), 3 grounded electrode, 4 PET
film to be treated.
61
Lissajous figure are recorded by a digital oscilloscope Tek TDS2014
(100 MHz, 1 GS/s).
The materials for the treatment are the commercial PET films
with thickness of 0.15 mm. All samples are cleaned with detergent,
rinsed first with alcohol and then with distilled water to remove
surface contamination and dust, and finally dried at room temper-
ature for 2 h before the plasma treatments.
The surface properties of the PET films are characterized by
contact angle and surface energy measurement, XPS, SEM and
AFM. To determine the change of hydrophilicity of the PET surface,
static contact angle measurements are made immediately after
processing by dropping 2 ml deionized water and polyethylene
glycol on the surface and using the sessile drop method. The
measurements are performed at room temperature by using
the contact angle meter JC2000A (Zhongchen Company, China).
The values of the static contact angle shown in this paper are the
averages of nine measured values. The surface energy is calculated
with the measured contact angles of these two liquids by using the
OwenseWendt method [27e29]. The micrograph and topography
of the PET surface before and after the treatment is investigated by
using the SEM (JEOL JSM-5900) and AFM (Autoprobe CP-R, Veeco,
USA). The chemical composition of the PET surface is determined
by XPS, which is performed in a VG ESCALAB MK II system, using
non-monochromatic Mg Ka radiation (hn ¼ 1254.6 eV) operated at
20 kV and 20 mA. The pressure in the analyzing chamber is
maintained at 5  106 Pa or lower during analysis. The size of the
analyzed area is 10 mm  10 mm. Spectra are acquired at a take-off
angle of 90 , and all binding energies are in reference to carbon
(C1s) at 285 eV.
3. Discharge characteristics and treatment parameters
Fig. 2 shows the oscillograms of the applied voltage and
discharge current, and Lissajous figures of DBD in a 2 mm air gap.
The measurement is performed with the PET films placed on the
lower glass plates during surface modification. It can be seen there
are a number of current pulses per half cycle of the applied voltage
(Fig. 2(a)), which suggests that the used DBD in this paper operates
in the filamentary mode. It is shown that the Lissajous figure is very
close to a parallelogram (Fig. 2(b)). With the measured Lissajous
figure, the energy consumed during one cycle of the discharge can
be calculated, which is equal to the enveloped area of the Lissajous
figure, and the discharge power coupled input to the reactor can
then be calculated by multiplying this area with the frequency f of
applied voltage [11,12].
In plasma surface modification, the discharge power density D is
usually used to weigh the action intensity of discharge plasma
[22,23], and it is defined as:
D ¼ P=V (1)
where P is the discharge power coupled input to the reactor, V is the
volume of the discharge space. When V is fixed, D is only controlled
by changing of discharge power P. In this paper, we fixed V to be
39.26 cm3 by fixing the air gap to be 2 mm and the area of elec-
trodes to be 19.63 cm2. With the fixed dielectric barriers and air gap
distance, the discharge power P is controlled by the frequency and
amplitude of applied voltage. The frequency of applied voltage is
fixed to be 8 kHz in this study, and the discharge power P, along
with the discharge power density D, is adjusted to five different
values by changing the amplitude of applied voltage. So in this
paper, we describe the changes of surface in the plasma processes
under five different discharge power densities as a function of
treatment time.
62 Z. Fang et al. / Journal of Electrostatics 69 (2011) 60e66
Fig. 2. Voltage and current waveform (a) and Lissajous figure (b) for the DBD measured
during surface modification.
4. Results and discussion
4.1. Change of contact angle and surface energy
Fig. 3 shows the changes of the static water contact angle on PET
film surface as a function of treatment times for five discharge
power densities of DBD. It is seen that an apparent decrease in
Fig. 3. Water contact angle as a function of treatment times for five discharge power
densities.
contact angles takes place with the treatment time up to 10 s for all
discharge power densities used, which suggests that a strong
increase of wettability in the PET surface induced by the DBD
plasma treatments. When the treatment time exceeds 10 s, the
measured static contact angles do not change anymore and reach
a saturation state, suggesting that the physical and chemical
changes induced by the plasmas on the PET surface are also in
saturation state when the plasma dose (treatment time and power
density) is in excess of some critical values. Regardless of the
discharge power density, the minimum values of static water
contact angle observed on the PET surface after the plasma treat-
ments is almost in the same value, which is found to change from
71 for the untreated samples to 32 after 10 s treatments. It can
also seen from Fig. 3 that increasing the discharge power density
leads to a faster decrease in water contact angle on the PET film
surface. After 1 s DBD treatment, the water contact angle on the PET
surface decreased to 45 , 43.5 , 41, 38 and 36 for discharge
power density of 10.2 W/m3, 15.3 W/m3, 20.4 W/m3, 25 W/m3 and
30.6 W/m3, respectively. In other words, the treatment time needed
to achieve the same level of surface treatment can be reduced by
increasing the discharge power density. As can be seen from Fig. 3
that the required treatment times for the reduction of water contact
angle to 36 are 1 s, 2 s, 3 s, 5 s, 8 s for the discharge power density
of 30.6 W/m3, 25 W/m3, 20.4 W/m3, 15.3 W/m3 and 10.2 W/m3,
respectively.
With the measured contact angles of deionized water and
polyethylene glycol, the surface energy on the PET film surface can
be calculated. Fig. 4 shows the changes of surface energy on PET
film surface as a function of treatment times for five discharge
power densities of DBD. The untreated PET film has a surface
energy of 33.8 mJ/m2. It can be seen that, at each discharge power
density, the surface energy increases with treatment time up to
10 s, and its values do not change significantly when the treatment
time is further increased and reaches the saturation state. The
maximum values of the surface energy after the plasma treatments
is 55 mJ/m2. As is also seen from Fig. 4 that increase in surface
energy on the PET film surface is faster at higher discharge power
density.
It is known that aging effect will occur on the plasma treated
polymer material surface. In order to study the aging effect, the
change of water contact angles with storage time in ambient air
after 10 s DBD plasma treatment under five discharge power
Fig. 4. Surface energy as a function of treatment time for five discharge power
densities.
 Z. Fang et al. / Journal of Electrostatics 69 (2011) 60e66 63

Fig. 5. Post-exposure change of the static water contact angle with storage time in
ambient air after the DBD treatments.

densities is monitored, and results are shown in Fig. 5. For the

treatments at each discharge power density, the contact angles are
seen to increase rapidly during the first 3 days, and at longer
storage times, contact angles change a little. There is little differ-
ence for the angles after 3 days and after 5 days of storage, sug-
gesting that the recovery happens mainly in the three day. It is also
important to mention that the maximal water contact angle after
storage in air (54 ) is still lower than that of the untreated PET
surfaces (71 ), which means that a part of the surface wettability is
kept after the plasma treatment. This phenomenon is in agreement
with the findings reported elsewhere, which may result from the
continuous chemical reactions of the remaining active radicals on
the PET surface with oxygen or moisture in ambient air, or from free
rotation of the oxygen-containing hydrophilic polar groups into the
inside of PET film [16,17,30,31].

4.2. Change of surface physical and chemical characteristics

Fig. 6 shows the SEM micrographs of the PET surface before and
after the DBD treatments for different discharge power densities of
DBD. As shown in Fig. 6(a), the untreated PET surface is relatively
smooth and defects-free, without specific morphological aspects. A
modified morphology after the plasma treatments is observed in
Fig. 6(b)e(d). It can be seen that the surface is etched and the
surface roughness is increased in all cases, and these images are
dominated by random and irregular protuberances round in shape.
With the same treatment time of 10 s, the surface roughness
increases with the increase of discharge power density. As shown in
Fig. 6(b) and (c), the size of irregular protuberances after higher
discharge power density treatment is larger than that of the lower
one. But excess discharge power density will cause damage to the
treated surface. It can be seen from Fig. 6(d) some random and
irregular concavities are located on the treated surface, which
suggests the injury or ablate of surface structure of PET film
induced by the plasma treatment.
Apart from SEM observation, the PET surface is analyzed by AFM
technique to detect the 3D surface topography and to calculate the
changes in surface roughness. Fig. 7 shows the 3D images of PET
surface before and after the treatments for different discharge
power densities. As shown in Fig. 7(a), the surface of untreated PET
film is relatively smooth with conical protuberances and moderate Fig. 6. SEM observations of the PET surface before and after DBD plasma treatments:
roughness. It can be seen form Fig. 7(b) and (c) that, after the (a) untreated, (b) after 10 s DBD treatment in 10.2 W/cm3, (c) after 10 s DBD treatment
plasma treatments, the surface of PET film shows rough in 20.4 W/cm3, (d) after 10 s DBD treatment in 30.6 W/cm3.
64 Z. Fang et al. / Journal of Electrostatics 69 (2011) 60e66
Fig. 7. Three-dimensional AFM images of the PET surface before and after DBD plasma
treatments: (a) untreated, (b) after 10 s DBD treatment in 10.2 W/cm3, (c) after 10 s
DBD treatment in 20.4 W/cm3.
morphology, and the size of the conical protuberances increases.
The surface roughness of PET films increase with the increase
of discharge power density. The values of root mean square
roughness, Rrms, is calculated from 1 mm  1 mm AFM images. The
Rrms of untreated PET is 0.37 nm, and it increases to 5.6 nm for
discharge power density of 10.2 W/cm3 and 7.2 nm for discharge
power density of 20.4 W/cm3.
Surface modification by using plasma is a process of interaction
between the plasma and surface for treatment. This process occurs
at the plasmaepolymer interface, and it includes several concurrent
physical and chemical actions, such as etching, grafting and poly-
merization etc. In the discharge regimes of DBD, there are many
active species [11,12]. The energetic active species (e.g. ions, elec-
trons, excited atoms and molecules, UV photons, etc.) present in the
discharge regimes of DBD can bombard the PET surface under
treatment and break the chemical bonds (CeC bond or CeH bond)
on the surface, and this leads to the formation of radicals on the PET
surface and the removal of molecules fragments from the PET
surface. The physical removal of molecules fragments and the
breaking of chemical bonds cause plasma etching on the surface,
resulting in the change of surface morphology. It is shown by SEM
and AFM (Figs 6 and 7) results that the surface roughness on PET is
increased and the surface morphology is changed after the DBD
plasma treatments due to plasma etching. The increase in surface
roughness causes an increase in surface area of the PET film, and this
is helpful for H2O molecules to be adsorbed on the surface easily by
capillary effect. Therefore the hydrophilicity on PET surface is
enhanced. Similar results were also reported by other authors. Esena
et al. [32] found an increasing of Rrms on PET films after DBD plasma
treatment at atmospheric air by AFM, and Upadhyay et al. [33]
reported the results of induced increase in the surface roughness
of the PET films by the DBD plasma treatment at atmospheric air.
Also Shenton et al. [34] found an increasing roughness on PET films
due to plasma etching after DBD treatment in atmospheric nitrogen.
Fig. 8 shows the C1s spectra of the PET samples before and after
10 s DBD treatments at discharge power density of 10.2 W/cm3 and
20.4 W/cm3. The concentration of each chemical component with
C1s can be calculated by deconvolution using GaussianeLorentzian
fit, and the results are summarized in Table 1. As shown in Fig. 8(a),
the C1s spectrum of the untreated PET sample can be decomposed
into four components: a component at binding energy of 285.0 eV
due to the CeC(H) bonds (component C1), a component at binding
energy of 286.5 eV due to CeO(H) bonds (component C2) and
a component at binding energy of 289.0 eV due to the O]CeO(H)
bonds (component C3) [35,36]. The C1s spectrum of plasma treated
PET films reveals the significant chemical changes produced by the
treatments. It is seen from Fig. 8(b) and (c) that after the treat-
ments, the intensity of C1 peak decreases, while the intensities of
both C2 and C3 peaks increase. This suggests that a number of
oxygen-containing polar groups are introduced into PET surface.
The concentration of C2 is found to change from 19.84% for the
untreated samples to the values of 23.73% after 10 s DBD treatment
at discharge power density of 10.2 W/cm3 and 26.51% after 10 s DBD
treatment at discharge power density of 20.4 W/cm3, respectively,
and the concentration of C3 is found to change from 15.34% for the
untreated samples to the values of 18.40% after 10 s DBD treatment
at discharge power density of 10.2 W/cm3 and 21.7% after 10 s DBD
treatment at discharge power density of 20.4 W/cm3, respectively.
The results in Fig. 8 and Table 1 show that after the plasma treat-
ments, the CeC(H) groups decrease, while CeO(H) and O]CeO(H)
groups increase at the same time. The above analysis indicates that
the DBD plasma treatments have the function of surface oxidation
by introducing oxygen-containing polar functional groups into the
molecular chain of PET surface, which contributes to the
improvement (decrease in water contact angle and increase in
surface energy) of the PET surface properties, and the treatment at
higher discharge power density yielded higher hydrophilicity than
the lower one due to more polar functional groups are introduced
into the PET surface at this case.
Some of radicals generated on the PET surface induced by the DBD
plasma can react with the active species (mainly oxygen-containing
species) in the discharge regime, resulting in the creation of oxygen-
containing polar groups on the PET surface. These oxygen-containing
polar groups let much more H2O molecules bond to them easily, and
 Z. Fang et al. / Journal of Electrostatics 69 (2011) 60e66 65

Table 1
High-resolution XPS of C1s peak deconvolution and possible groups after 10 s DBD
treatments at discharge power density of 10.2 W/cm3 and 20.4 W/cm3.

Peak no. Center (eV) Possible groups At. %

Untreated 10.2 W/cm3 20.4 W/cm3

C1 285 CeC(H) 64.82 57.87 51.79
C2 286.6 CeO(H) 19.84 23.73 26.51
C3 289.3 (H)OeC]O 15.34 18.40 21.70

this is also beneficial for hydrophilicity enhancement. The DBD can

generate a wide range of active species including atomic oxygen,
ozone, nitrogen oxides, neutral and metastable molecules, radicals
and ultraviolet radiation, which can change surface chemistry
[10,12,24e26,30]. For the oxygen inclusion into the PET surface, it is
known that atomic oxygen including that dissociated from O3 is the
main reactive species, and the radicals (like OH, HO2 etc) may also
have some contributions [24e26,31,37,38]. It is shown by XPS results
that air DBD plasma increases the surface energy of PET films by
introducing CeO and OeC]O groups onto the polymer surface. This
observation was also done by several authors. Borcia et al [39,40] and
De Geyter et al [37,38] et al studied DBDs operating in air at atmo-
spheric pressure and medium pressure for the surface treatment of
PET films. It is shown by XPS results that the decrease in water contact
angle is due to the incorporation of oxygen-containing groups, such
CeO and OeC]O groups for both pressure conditions. Upadhyay et al.
[33] used a DBD at atmospheric pressure air to modify a PET film and
found the same oxygen-containing groups. So the increase in wetta-
bility in PET surface is due to both the introduction of oxygen-con-
taining functional groups to the surface and the etched of the surface.

4.3. Discussion about the effect of discharge power density

As shown by the results of contact angle and surface energy

measurements (Figs. 3 and 4), increasing the discharge power
density leads to a faster decrease in water contact angle and a faster
increase in surface energy. This can be attributed to more creation
of oxygen-containing polar groups and more obvious etching
occurring on the PPT surface, as is shown in the AFM observation
and XPS analysis results in Fig. 8, suggesting that more active
species interact with the PET surface at higher discharge power
density. This may be explained as follow: the DBD used in this
paper operates in atmospheric air, and it manifests as filamentary
streamer discharge, with a large number of discharge filaments
(also named microdischarges), which have a nanosecond duration
being randomly distributed in the discharge region. The micro-
discharge channels of the DBD bridges the air gap from the anode to
the cathode, so the active species are generated along the fila-
mentary channels and spatially distributed in the discharge regime.
Increasing the discharge power density results in the presence of
more microdischarge in the DBD discharge regime, thus results in
the presence of a higher amount of active species, as is confirmed
by the researches [41,42]. So more active species in the DBD
discharge regime can interact with the PET surface, and this results
in more formation of radicals on the surface and more removal of
molecules fragments from the PET surface. This leads to a faster
incorporation of oxygen-containing polar groups and larger etching
on the PET surface, and therefore results in a very efficient modi-
fication of the PET film.

5. Conclusions
Fig. 8. High-resolution XPS of C1s spectra before and after the plasma treatments: (a)
untreated, (b) after 10 s filamentary DBD treatment in 10.2 W/cm3 (c) after 10 s fila- Modification of the PET film surface with the plasma generated
mentary DBD treatment in 20.4 W/cm3. by DBD are conducted in air at atmospheric pressure, and the
66 Z. Fang et al. / Journal of Electrostatics 69 (2011) 60e66
effects of discharge power density on the surface modification are
studied. It is demonstrated in this paper that the increase in surface
roughness and oxygen-containing polar groups on the PET surface
contribute to the significant reduction of contact angle and signif-
icant increase of surface energy. It is found that the power density
has a significant effect on the surface modification. Increasing
discharge power density can induce more effective treatment of
PET films, as this leads to a faster decrease in water contact angle
and a faster increase in surface energy due to more creation of
oxygen-containing polar groups and more obvious etching occur-
ring on the PET surface. The treatment time needed to achieve the
same level of surface treatment can be reduced by increasing the
discharge power density. The test results of aging in ambient air
after the treatments show that the treated PET surface has good
stability with aging time.
Acknowledgements
This work is supported by the National Natural Science Foun-
dation of China under Grant No. 50707012 and is sponsored by
“Qing Lan Project” in Jiangsu Province of China.
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