Plasma Medicine, 7(4):395–406 (2017)

Surface Dielectric Barrier Discharge in

Closed-Volume Air
A. Dascalu,a A. Demeter,a F. Samoila,a V. Anita,a K. Shimizu,b & L. Sirghia,*
a
Iasi Plasma Advanced Research Center (IPARC), Faculty of Physics, Alexandru Ioan Cuza
University, Iasi, 700506, Romania; bOrganization for Innovation and Social Collaboration,
Shizuoka University, 3-5-1, Naka-ku, Johoku, Hamamatsu, Shizuoka 432-8561, Japan

*Address all correspondence to: L. Sirghi, Iasi Plasma Advanced Research Center (IPARC), Faculty of Physics,
Alexandru Ioan Cuza University, Iasi, 700506, Romania, E-mail: lsirghi@uaic.ro

ABSTRACT: The postdischarge kinetics of reactive species produced by a surface dielectric

barrier discharge (SDBD) ignited in closed-volume air for decomposition of organic mol-
ecules in aqueous solutions was investigated. A SDBD with surface of 6 cm2 was operated
in a closed volume (0.5 L) of air at atmospheric pressure. The voltage across the plasma gap,
the charge transferred through the plasma, and the dissipated power were computed from the
charge-voltage diagram to values of 3900V, 0.2 PC, and 6W, respectively. The reactive species
produced by the SDBD in a closed volume of air were active for decomposition of methylene
blue molecules in small volumes of aqueous solution for a relatively long period of time af-
WHUWKHGLVFKDUJHZDVFXWR൵7KHOLIHWLPHLQJDVHRXVSKDVHRIWKHVSHFLHVDFWLYHIRUGHFRP-
position of organic molecules was approximately 11 minutes. However, SDBD operation in
closed-volume air shortened the lifetime of polyimide dielectric of the discharge microelec-
trode system due to the increased humidity and reactivity of the active species generated by
plasma. Measurement of relative humidity revealed that the discharge enhanced water evapo-
ration. Atomic force microscopy investigations of dielectric surface in the discharge region
UHYHDOHGGUDVWLFPRGL¿FDWLRQVRIVXUIDFHPRUSKRORJ\ZLWKDQLPSRUWDQWLQFUHDVHRIVXUIDFH
roughness as the result of SDBD operation.

KEY WORDS: surface DBD, reactive species kinetics, methylene blue degradation, dielec-
tric degradation

I. INTRODUCTION

In recent years, interest in medical applications of atmospheric pressure plasmas has

JURZQVLJQL¿FDQWO\1 Among various atmospheric pressure plasmas, the surface dielec-
tric barrier discharge (SDBD) plasma has proven its potential as an important candi-
date for plasma treatments in wound healing,2 drug administration,3 sterilization,4,5 and
removal of contaminants from air6 or water.7 Most SDBD studies have been devoted
to discharges working in open air or in closed vessels through which air or rare gases
ÀRZHG87KHH൷XHQWVWKHQJHQHUDWHGE\SODVPDDUHWUDQVSRUWHGDQGXVHGIRUWUHDWPHQWV
Very few studies of SDBD plasma treatments have been performed in closed-volume
air.7,9 The present study is devoted to SDBD operated in closed-volume air at atmo-
spheric pressure for treatment of contaminant organic molecules in aqueous solution.
Oehmigen et al.7 studied the kinetic of chemical reactions taking place in liquid as result

1947-5764/17/$35.00 © 2017 by Begell House, Inc. www.begellhouse.com 395

396 Dascalu et al.

RI DFWLYH VSHFLHV SURGXFHG LQ WKH GLVFKDUJH SODVPD DQG WKHLU GL൵XVLRQ LQWR OLTXLG ,Q
their experimental arrangement, the plasma faced the liquid surface at a small distance
(5 mm) and the volume of air available for the discharge was very small (14 mL) com-
pared to the volume of treated liquid. In the present study, the plasma does not face the
liquid surface, and the volume of air enclosed in vessel is much larger (0.5 L) than the
volume of treated liquid (5 mL). Therefore, in the present study, the plasma treatment
can be considered totally indirect; the treatment is determined by the plasma-generated
DFWLYHVSHFLHVLQWKHJDVSKDVHDQGWKHLUIUHHGL൵XVLRQIURPWKHJDVSKDVHLQZDWHU7KH
active plasma species involved in treatment of water or aqueous solutions are reactive
oxygen species (ROS) and reactive nitrogen species (RNS).9 Among them, O3, OH-,
H2O2, NO2–, and NO3– are the most important active species, with important roles in
treatments for removal of organic contaminants from water, inactivation of bacteria, or

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for inducing biologic reactions in living tissue.10 Oh et al.11 showed that these species

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are generated immediately in water once the atmospheric-pressure plasma is ignited
and, if not consumed in reactions with organic molecules, they survive for long time.

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In the present study, kinetics of active species generated by SDBD operated in closed-
volume air is investigated indirectly by analyzing the decomposition rate of methylene
EOXH 0% PROHFXOHVLQDVPDOODPRXQWRIZDWHUH[SRVHGWRSODVPDH൷XHQWV0HWK\OHQH
blue is frequently used in studies of decomposition organic contaminant molecules in
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water.12 ROS such as O3, H2O2, and OH are the main active species for the degradation
process of MB molecules in water, while RNS such as NO, NO2, and NO3- are some-
how detrimental to the MB degradation process due to consumption of oxygen in their
generation processes.13 Therefore, exposure of small amounts of MB aqueous solution
WR6'%'SODVPDH൷XHQWVJHQHUDWHGLQFORVHGYROXPHDLUJLYHVLQIRUPDWLRQRQWKHFRQ-
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centration of ROS and their lifetime in postdischarge medium. These plasma-generated

species have a long lifetime (> 10 minutes), they were available for reactions in liquid
SKDVHIRUUHODWLYHO\ORQJSHULRG aPLQXWHV DIWHUWKHGLVFKDUJHKDGEHHQFXWR൵7KXV
FRPSDUHG ZLWK RSHUDWLRQ LQ RSHQ DLU RU JDV ÀRZ WKH RSHUDWLRQ RI 6'%' LQ FORVHG
ut

YROXPHDLULQFUHDVHVWKHH൶FLHQF\RIWUHDWPHQW+RZHYHUWKHRSHUDWLRQRIWKH6'%'LQ
closed-volume air has also drawbacks. Active plasma species promote water evapora-
tion, which results in a faster increase of water vapor in the air during the discharge. The
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high concentration of active species in gas phase and the increase of humidity determine
erosion of the dielectric polymer of the SDBD electrode system due to numerous reac-
tions of the reactive plasma species with the dielectric material.

II. EXPERIMENTAL SETUP

The SDBD was generated in atmospheric air in a glass vessel with the volume of 0.5
L. Figure 1 presents schematically the experimental setup. The SDBD microelectrodes
used in the present study had a sandwich structure (area = 2.3 u 3 cm2) formed by two
copper electrodes (18 Pm thickness) deposited on the two sides of a polyimide foil
(Kapton® with 14 Pm thickness and relative dielectric permittivity of 3.4). The upper
(hot) electrode was structured as 23 equidistant and parallel stripes (0.2 mm wide and 30

Plasma Medicine
Surface Dielectric Barrier Discharge 397

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FIG. 1: Schematic representation of the experimental setup
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mm long) with a gap width of 0.8 mm. In the glass vessel, side by side with the SDBD
electrodes, there was placed a Petri dish (40 mm in diameter) with a small volume (5mL
or 3 mL) of methylene blue (MB) solution (400 ppm) in deionized water. The SDBD
ZDVSRZHUHGE\DVLQXVRLGDOZDYHKLJKYROWDJHDPSOL¿HU7KHYROWDJHDQGLQWHQVLW\RI
discharge current signals were collected by specialized voltage probes and monitored by
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a digital oscilloscope (DPO 2024 from Tektronix, USA). The electric characterization of
the discharge is provided in the next section. Decomposition of MB in solution was de-
termined by measurements of optical absorbance in the region 400–800 nm (with a peak
in absorption at 664 nm) by a UV-VIS spectrophotometer (Evolution 300 from Thermo
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6FLHQWL¿F  7KH KXPLGLW\ LQ WKH JODVV YHVVHO KDV EHHQ PRQLWRUHG E\ D SUHFLVLRQ K\-
grometer (HM34C, Vaisala Oyj, Finland). The topography images and roughness of the
dielectric before and after operation of SDBD in open and closed-volume air have been
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obtained by atomic force microscopy (AFM) measurements performed by a commercial

AFM apparatus (XE 100 from Park, South Korea) working in noncontact mode. The
measurements were performed with a silicon AFM probe (HQ:NSG 35 from NT-MDT,
5XVVLD ZLWKDVKDUSHQHGWLS QRPLQDOFXUYDWXUHUDGLXVRIQP DQGDVWL൵FDQWLOHYHU
(nominal resonant frequency and force constant of 150 kHz and 5.4 N/m, respectively).

III. ELECTRIC CHARACTERIZATION OF DISCHARGE

Figure 2a shows the typical waveforms of the applied voltage and intensity of the elec-
tric current through the SDBD during one oscillation period. The peak values of the
applied voltage and current intensity are approximately 1900 V and 35 mA, respec-
tively. As shown in Fig. 2b, the current intensity presents the typical pattern of a mul-

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398 Dascalu et al.

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FIG. 2: (a) Typical waveforms of voltage and current intensity during a period of SDBD. (b)
Detailed image showing current intensity variation at a smaller scale of time (1 μs).

WL¿ODPHQWDU\GLVFKDUJH14 with spikes with an amplitude of approximately 5 mA and a

lifetime of approximately 20 ns. The amplitude and number of current intensity spikes
are larger during the positive discharge than during the negative discharge. Several elec-
trical parameters of the discharge are important as the energy dissipates during one os-
cillation period: discharge power, electric charge transferred to dielectric surface during
one cycle of the discharge, Qdis, and the voltage across the gas gap, Ub. All of these can
be determined from charge-voltage Lissajous diagrams. Figure 3 shows a sketch of the
measuring circuit of SDBD that indicates the capacitances involved in the discharge

Plasma Medicine
Surface Dielectric Barrier Discharge 399

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FIG. 3: Sketch of the SDBD circuit. The current intensity, I, signal is collected on a 12 Ohms
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resistor and the discharge voltage, U, is collected by a high-voltage probe connected to the top
electrode. The bottom electrode has been grounded. Capacitance C0, C1, and Cg are shown sche-
matically.

mechanism. The capacitance C0 accounts for the capacitor formed by the dielectric be-
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tween the top and bottom electrodes and does not change during the discharge. The ca-
pacitance C1 accounts for the dielectric capacitor formed between the bottom electrode
and the bare surface of the dielectric. The gap capacitance accounts for the air capaci-
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tor formed between the top electrode and the bare surface of the dielectric. During the
PXOWL¿ODPHQWDU\GLVFKDUJHVWKHDLUJDSLVSDUWLDOO\VKRUWFXWE\WKHORZLPSHGDQFHRIDLU
plasma. If f is the fraction of bare dielectric area covered by plasma, the impedance of
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SDBD circuit during positive and negative discharge periods is approximately

Cd # C0  f ˜ C1 . (1)

:KLOHWKHGLVFKDUJHLVR൵WKHFDSDFLWDQFHRIWKH6'%'HOHFWURGHV\VWHPLV

C1 ˜ Cg . (2)
C 'd C0 
C1  Cg
The value of C0 has been determined to be approximately 309 pF using the plane capaci-
tor formula:

Volume 7, Issue 4, 2017

400 Dascalu et al.

H 0H r ˜ S
C0 , (3)
d

where S is the area of the upper electrode (S = 140 mm2), d the thickness of the dielec-
tric (d = 14 Pm), İr the relative electric permittivity of the dielectric (İr = 3.4), and İ0
the electric permittivity of vacuum (İ0 = 8.85 10-12 F/m). The same formula was used to
compute a value of 1324 pF for C1.
The changes in circuit capacitance from Cd’ to Cd during the discharge cycles deter-
mine the changes of the slope in the Q-U diagram, which typically have a parallelogram
shape. Figure 4 presents the Q-U diagram of the SDBD used in the present work. The

f
regions AB and CD show a smaller slope, which corresponds to capacitance Cd’ when

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WKHGLVFKDUJHLVR൵ZKLOHWKHUHJLRQV%&DQG'$VKRZDODUJHUVORSHZKLFKFRUUH-
sponds to capacitance Cd when the discharge is on. From the Q-U diagram, Cd‘ = 260

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pF and Cd = 390 pF. The values of Cd and C1 show that, on average, only 10% of the
bare dielectric surface is covered by conductive plasma. The value of Cd’ determined
from the Q-U diagram is close to the value of C0 computed using the plane capacitor
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formula. To determine the relevant parameters of the discharge, the Q-V diagram of the
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FIG. 4: Q-U diagram of SDBD showing typical parallelogram shape (ABCD) before (diagonal)
and after (horizontal) extraction of contribution of displacement current through the capacitance
Cd’. The slopes of quasi-linear parts of the diagram compute the capacitances Cd and Cd’.

Plasma Medicine
Surface Dielectric Barrier Discharge 401

discharge15 was computed by extracting the contribution of the displacement current Id

= Cd’dU/dtÀRZLQJWKURXJKWKHGLHOHFWULF FDSDFLWDQFHC’d). The Q-V diagram of the
discharge allows for determination of voltage across the plasma, Ub, and the charge
Qdis transferred through the plasma to values of 3900 V and 0.2 PC, respectively. These
values determine the energy dissipated in one cycle to be approximately 0.5 mJ and the
discharge power to be approximately 6 W.

IV. RESULTS AND DISCUSSION

A. Degradation of Methylene Blue Solution

Figure 5 shows the variation of MB concentration in the solution exposed to the action

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of reactive species produced by SDBD plasma. Due to dielectric failure, the SDBD

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electrodes could not be operated more than 10 minutes in closed-volume air (Fig. 5,
discharge on plot). The discharge was then operated for only 4 minutes, and the time

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evolution of MB concentration in the solution exposed to active species generated by
6'%'SODVPDZDVLQYHVWLJDWHGGXULQJWKHGLVFKDUJHDQGDIWHUWKHGLVFKDUJHZDVFXWR൵
As explained in the introductive section, ROS are the main active species for the deg-
radation process of MB molecules in water, while RNS are more or less detrimental to
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the degradation process. The degradation of MB molecules in small volumes of aqueous
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FIG. 5: Time variation of concentration of MB in water during SDBD plasma operation and after
6'%'KDVEHHQFXWR൵

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402 Dascalu et al.

VROXWLRQ P/ H[SRVHGWRSODVPDH൷XHQWVLQDUHODWLYHO\ODUJHYROXPHRIDLU P/ 

yields information on the concentration of ROS in the gas phase. The decay of MB con-
centration in the solution shows that the ROS generated by SDBD plasma have a long
lifetime and decompose MB molecules for approximately 30 minutes after the SDBD is
FXWR൵7KHUHDIWHUQRIXUWKHUGHFRPSRVLWLRQRI0%RFFXUV7KHWLPHYDULDWLRQVRI0%
concentration show that, for smaller amounts of solution (less than 3 mL), the amount of
the decomposed MB molecules is independent of the volume of the solution used in the
H[SHULPHQWV7KLV¿QGLQJLQGLFDWHVWKDWWKHGHFRPSRVLWLRQSURFHVVLVOLPLWHGE\WKHÀX[
of active species coming from air and dissolved in solution. Therefore, the time evolu-
tion of the decomposition rate of MB molecules in aqueous solution is an indicator of
WKHWLPHYDULDWLRQRIWKHFRQFHQWUDWLRQRIDFWLYHVSHFLHVLQWKHJDVHRXVSKDVH7KH¿WRI
the time variation of MB concentration with the exponential decay (Fig. 5) determines

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the decay time for the active species in the closed-volume air, which is approximately

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11 minutes. This decay time may depend on the volume and surface of the glass vessel
WKDWFRQWDLQWKHGLVFKDUJHJDV$OVRWKHDLUKXPLGLW\PD\D൵HFWWKHSURGXFWLRQDQGFRQ-

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sumption of ROS. Therefore, we monitored the relative humidity (RH) of the air during
the discharge and found that the SDBD enhances the evaporation of water from the MB
solution, probably due to the contribution of radical species generated by plasma and the
ultrasound produced by the SDBD dielectric.
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Figure 6 shows the comparative increase of RH in the closed-volume air without and
with SDBD. The evaporation of water under a closed-volume air condition raises the RH
from the initial value of ambient air toward saturation. This process is relatively slow
in the absence of SDBD plasma and faster in its presence. Therefore, SDBD enhanced
the evaporation of the liquid water exposed to active plasma species. When SDBD is
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operated for relatively long time (10 minutes), this may contribute to the electric failure
of the dielectric material because water is absorbed on the dielectric surface and modify
its electric properties. Also, the content of water vapor in the discharge gas has a great
impact on the discharge current and ultimately on the discharge power.16
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B. Degradation of the Dielectric Material

The dielectric materials used in surface dielectric barrier discharge (SDBD) devices are
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LQHYLWDEO\H[SRVHGWRSODVPDRIWKHGLVFKDUJH¿ODPHQWVIRUPLQJDWWKHLUVXUIDFH7KHVH
discharges determine the erosion and degradation of dielectric material because the ac-
tion of active high-energy plasma species (i.e., electrons, ions, UV photons, and radical
and metastable molecules) can cause dielectric failure. The increase in humidity during
SDBD may also contribute to the degradation of the dielectric material.
,Q6'%'SODVPD¿ODPHQWVIRUPRQWKHEDUHGLHOHFWULFVXUIDFHDWWKHHGJHRIWKH
hot electrode. Therefore, we investigated the evolution of dielectric surface topography
at this position using atomic force microscopy (AFM). We expected the operation of
SDBD in open air to degrade the dielectric less because in this case the active species
formed in plasma are diluted and transported in the environmental air. Therefore, we
compared the changes of the dielectric surface morphology during SDBD operation

Plasma Medicine
Surface Dielectric Barrier Discharge 403

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FIG. 6: Variation of relative humidity in closed-volume air during SDBD operation (squares)
and without SDBD (dots)

in open and closed-volume (0.5 L) air. Figure 7 shows the comparative AFM topogra-
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phy images of the dielectric surface before operation (a) and after 4 minutes of SDBD
operation in open (b) and closed-volume air (c). The AFM topography image of the
dielectric surface before operation shows a relatively smooth surface (root mean square
[RMS] roughness of ~20 nm). The AFM topography images of the dielectric surface
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after 4 minutes of operation revealed drastic changes consisting of surface buckling at

the nanoscale. After 4 minutes of SDBD operation, the RMS roughness of the dielectric
surfaces was 73 nm for operation in open air and 95 nm for operation in closed-volume
air. Figure 8 shows the evolution of RMS roughness of dielectric surface as result of
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6'%'RSHUDWLRQ7KHGL൵HUHQFHEHWZHHQ506URXJKQHVVYDOXHVREVHUYHGLQWKHVHWZR
cases is not very large for operation times less than 7 minutes. However, at longer opera-
WLRQWLPHVWKHGL൵HUHQFHLQFUHDVHVVLJQL¿FDQWO\SUREDEO\GXHWRWKHH൵HFWRILQFUHDVHG
humidity in the closed-volume air.

V. CONCLUSION

In summary, we investigated the postdischarge kinetics of reactive species produced by

SDBD plasma ignited in closed-volume air at atmospheric pressure to determine the
decomposition of methylene blue molecules in aqueous solutions. The SDBD electrode
system consisted of a dielectric foil of polyimide covered on one face with a planar cop-

Volume 7, Issue 4, 2017

404 Dascalu et al.

FIG. 7: Atomic force microscopy images of the dielectric surface before (a) and after 4 minutes
of operation of SDBD in open air (b) and closed-volume air (c)

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FIG. 8: Changes of root mean square (RMS) roughness of the dielectric surface during SDBD
operation in open and closed-volume air

per electrode (grounded) and on the other face with a striped cooper electrode (connected
WRDQKLJKYROWDJHDPSOL¿HU 7KHYROWDJHDFURVVWKHSODVPDJDSWKHFKDUJHWUDQVIHUUHG
through the plasma, and the dissipated power were determined from the charge-voltage
/LVVDMRXVGLDJUDPV$IWHURSHUDWLRQIRUPLQXWHVWKHGLVFKDUJHZDVWXUQHGR൵+RZ-
ever, the decomposition of methylene blue molecules continued for approximately 30
minutes, which indicates that the reactive species produced by SDBD were active for a
relatively long period of time. The decomposition rate of methylene blue molecules in
VROXWLRQDIWHUWKHGLVFKDUJHZDVFXWR൵GHWHUPLQHGWKHOLIHWLPHRIDFWLYHVSHFLHVLQJDV-

Plasma Medicine
Surface Dielectric Barrier Discharge 405

eous phase to be approximately 11 minutes. The operation of SDBD in closed-volume

air in the presence of water shortened the lifetime of the polyimide dielectric of the dis-
charge microelectrode system due to increased humidity and reactivity of the active spe-
cies generated by the plasma. Atomic force microscopy was used to observe the changes
in the surface morphology of the dielectric material during the discharge operation. The
AFM topography images of the dielectric surface revealed drastic changes consisting
in surface buckling at nanoscale, with formation of grains after only 4 minutes of op-
eration. These surface-morphology transformations were indicated by the surface RMS
roughness, which increased from approximately 20 nm for the dielectric surface before
operation to approximately 90 nm for the dielectric surface after 4 minutes of operation.
2SHUDWLRQRI6'%'LQFORVHGYROXPHDLUUHVXOWHGLQODUJHUPRGL¿FDWLRQVRIGLHOHFWULF
surface morphology, especially for long operation times (compared with operation in

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RSHQDLU 7KLVH൵HFWLVSUREDEO\GXHWRWKHLQFUHDVHGKXPLGLW\REVHUYHGGXULQJ6'%'

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operation in closed-volume air.

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ACKNOWLEDGMENT

7KLVZRUNZDVVXSSRUWHGE\WKH1DWLRQDO&RXQFLORI6FLHQWL¿F5HVHDUFKLQ+LJKHU(GX-
cation (CNCSIS), IDEI Research Program of Romanian Research, Development and
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Integration National Plan II (Grant No. 267/2011).

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