Uniform Dielectric Barrier Discharge with Nanosecond Pulse Excitation for

Biomedical Applications



A Thesis
Submitted to the Faculty
of
Drexel University
by
Halim Ayan
in partial fulfillment of the
requirements for the degree
of
Doctor of Philosophy


July 2009



















© Copyright 2009 
Halim Ayan. All Rights Reserved. 






ii



DEDICATION








To my love, my best friend, my beautiful wife; EDA















iii

ACKNOWLEDGMENTS

I would like to express my sincere and deepest gratitude to my advisors Dr.
Gary Friedman and Dr. Alexander Fridman for their invaluable guidance, enduring
support, and for constantly educating me throughout my doctoral studies.
I would especially like to express my deep appreciation to Dr. Alexander
Gutsol for his guidance and patience, along with opening a whole different way of
thinking and perspective into the matters.
I would like to thank the members of my advisory committee including Dr.
Wei Sun, Dr. Young Cho, Dr. Adam Fontecchio, and Dr. Alexander Rabinovich for
their helpful and constructive comments to improve this thesis. I would also like to
thank Dr. Alan Lau for his advice and support over the last four years. I would also
like to acknowledge the help of Dr. Andrei Starikovskii, Dr. Victor Vasilets, and Dr.
Yuri Mukhin to my work.
I am thankful to all colleagues, co-workers, and friends at DPI and CATE
Lab. I would especially like to express my appreciation to Robert Chang, Tanvir
Farouk, Gregory Fridman, Shailesh Gangoli, Ondrej Hovorka, and David Staack, for
their friendship and for delightful discussions around science, politics, and
philosophy. I have been very privileged to have befriended you all.
Finally, I am grateful for the financial support from the Drexel Plasma
Institute and the Mechanical Engineering and Mechanics Department.




iv

TABLE OF CONTENTS



LIST OF FIGURES ..................................................................................................... vi
LIST OF TABLES .........................................................................................................x
ABSTRACT ................................................................................................................. xi
CHAPTER 1: INTRODUCTION AND BACKGROUND..........................................1
1.1 Plasma in Medicine ............................................................................................1
1.2 Dielectric Barrier Discharge Plasmas ................................................................4
1.3 Research Objectives and Approach ...................................................................9
1.4 Thesis Outline ....................................................................................................9
CHAPTER 2: DESIGN OF THE NANOSECOND-PULSED DIELECTRIC
BARRIER DISCHARGE DEVICE AND SYSTEM FOR BIOMEDICAL
APPLICATIONS .........................................................................................................10
2.1 Breakdown of Gas in DBD ..............................................................................10
2.2 Key Facts About the Nanosecond-pulsed Dielectric Barrier Discharge System
................................................................................................................................12
2.3 Power Supply ...................................................................................................14
2.4 Electrodes .........................................................................................................19
2.4.1 Planar electrode .......................................................................................19
2.4.2 Test tube electrode ..................................................................................20
CHAPTER 3: PLASMA AND DEVICE PHYSICAL CHARACTERIZATION .....22
3.1 Electrical Characterization ...............................................................................22
3.1.1 Voltage and current .................................................................................22
3.1.2 Power ......................................................................................................22
3.2 Characterization of the Uniformity of the Plasma ...........................................26
v

3.2.1 Side view imaging...................................................................................26
3.2.2 Lichtenberg figures .................................................................................30
3.3 Thermal Characterization of the Plasma ..........................................................35
3.3.1 Optical emission spectroscopy ................................................................35
3.3.2 Surface temperature ................................................................................46
3.4 Summary of Key Results and Conclusions ......................................................46
CHAPTER 4: STERILIZATION EFFICACY, BIOLOGICAL
CHARACTERIZATION AND QUANTIFICATION OF NANOSECOND-PULSED
DIELECTRIC BARRIER DISCHARGE ....................................................................48
4.1 Qualitative Demonstration of Sterilization ......................................................48
4.2 Qualitative Comparison of Conventional and Nanosecond-pulsed Dielectric
Barrier Discharge on Topographically Non-uniform Surfaces ........................48
4.3 Quantitative Comparison of Conventional and Nanosecond-pulsed Dielectric
Barrier Discharge on Topographically Non-uniform Surfaces ........................60
4.4 On the Mechanism of Sterilization ..................................................................65
4.5 Summary of Key Results and Conclusions ......................................................71
CHAPTER 5: SUMMARY AND CONCLUSIONS .................................................72
5.1 Summary of the Research and Conclusions.....................................................72
5.2 Research Contributions ....................................................................................73
LIST OF REFERENCES .............................................................................................76
VITA ............................................................................................................................89





vi

LIST OF FIGURES



Figure 1.1: Schematic representation of a typical APC setup and APC probe with the
plasma beam on the tissue (Raiser and Zenker 2006, Stoffels 2007) ............................3
Figure 1.2: Parallel and concentric configurations of Dielectric Barrier Discharge
(Kogelschatz 2003 and Kogelschatz 2004) ....................................................................6
Figure 1.3: Schematics of DBD operation .....................................................................7
Figure 1.4: Image of a typical DBD in air .....................................................................7
Figure 1.5: Microdischarges of a conventional dielectric barrier discharge striking on
the ridges of the skin (similar to lightning) ....................................................................8
Figure 2.1: Electron multiplication and avalanche growth (Raizer 1991) ...................11
Figure 2.2: Avalanche-to-streamer transition and streamer propagation (Raizer 1991)
......................................................................................................................................11
Figure 2.3: Schematic of double spark gap configuration external circuit ..................15
Figure 2.4: Pulse frequency (repetition) versus main spark gap distance for several
small spark gap distances (2.5 - 4.5 mm). Frequency values are average of 10
measurements and variance is ±10% ...........................................................................16
Figure 2.5: Pulse duration (FWHH) versus small spark gap distance for several main
spark gap distances (15 - 27 mm). Pulse duration values are average of 10
measurements and variance is ±10% ...........................................................................17
Figure 2.6: Peak voltage versus main spark gap distance for several small spark gap
distances (2.5 - 4.5 mm). Peak voltage values are average of 10 measurements and
variance is ±10% ..........................................................................................................17
Figure 2.7: Oscillogram of typical voltage and current signals (Main spark gap:
12mm, Secondary spark gap: 3 mm) ...........................................................................18
Figure 2.8: Superimposed voltage signals versus time (main spark gap: 15 mm and
secondary spark gap: 3mm) (a) Peak voltage: 15.6 kV, pulse length: 23 ns (b) 10
voltage signals superimposed ......................................................................................18
vii

Figure 2.9: Cylindrical electrode cross section ............................................................19
Figure 2.10: Glass test tube electrode ..........................................................................21
Figure 3.1: Schematic of calorimeter setup .................................................................24
Figure 3.2: Experimental data and curve fitting for ΔT. Electrical power
measurement: 5.02 ± 0.44 W (average of 10 measurements) ......................................25
Figure 3.3: Images of two discharges with plane-to-plane configuration: (a)
Sinusoidal waveform, (b) Microsecond-pulsed waveform ..........................................27
Figure 3.4: Spectroscopic measurement setup for single filament ..............................27
Figure 3.5: Locations of 21 cross sections on the images of two types of DBDs with
two test tube electrodes (1 mm gap). Exposure time of sinusoidal DBD is 50 msec
(600 cycles) and microsecond-pulsed DBD is 1 s (1000 cycles) .................................28
Figure 3.6: Contrast enhanced images of two types of DBDs with two test tube
electrodes (1 mm gap). Exposure time of sinusoidal DBD is 50 msec (600 cycles) and
microsecond-pulsed DBD is 1 s (1000 cycles) ............................................................28
Figure 3.7: Side view of nanosecond-pulsed DBD between test tube electrode and
ground metal electrode (a) with background light and (b) in a complete dark room for
the same exposure time (bottom halves of the images are due to reflection from the
ground plate electrode surface) ....................................................................................29
Figure 3.8: Schematic of experimental setup to acquire the Lichtenberg figures on
photo film .....................................................................................................................32
Figure 3.9: Lichtenberg figures of two different DBD systems on the emulsion of the
photo films: (a) nanosecond-pulsed DBD - b&w, (b) nanosecond-pulsed DBD - color,
(c) microsecond-pulsed DBD - b&w, (d) microsecond-pulsed DBD – color..............34
Figure 3.10: Oscillograms of (a) sinusoidal and (b) microsecond-pulsed DBDs ........36
Figure 3.11: Rotational temperature as a function of average power density for the
sinusoidal DBD and the microsecond-pulsed DBD.....................................................38
Figure 3.12: Vibrational temperatures as a function of average power density for the
sinusoidal DBD and the microsecond-pulsed DBD.....................................................39
viii

Figure 3.13: Spectra at various locations along the filament (cross sections : 1, 3, 5,
….17, 19, 21) ...............................................................................................................40
Figure 3.14: Spatial intensity versus wavelength (372.7 nm – 381.2 nm) ...................41
Figure 3.15: (a) Rotational and (b) Vibrational temperature distributions along the
microdischarges ...........................................................................................................42
Figure 3.16: Spectroscopic measurement setup for DBD ............................................43
Figure 3.17: Spectra of nanosecond-pulsed DBD for spectroscopic temperature
measurement. Rotational temperature: 313.5 ± 7.5 K and vibrational temperature:
3360 ± 50 K. (Model spectrum: Laux 2002, Staack et al. 2006) .................................45
Figure 3.18: Nanosecond-pulsed DBD igniting on finger (exposure time: 1 s) ..........45
Figure 4.1: Agar with skin flora treated by nanosecond-pulsed DBD (V
max
: 20 kV,
Repetition rate: 190 Hz) ...............................................................................................49
Figure 4.2: Patterned agar preparation .........................................................................50
Figure 4.3: Protocol for dilution assay .........................................................................51
Figure 4.4: Illustration of mesh on top of the agar to mimic the indentations (10 mm
diameter electrode with 0.66 mm quartz) ....................................................................54
Figure 4.5: Inactivation with nanosecond- (left-hand side) and microsecond- (right-
hand side) pulsed DBD through metal mesh and (b) schematic of the experimental
setup (schematic is not to scale; circles in (a) indicate the edge of the high voltage
electrode; brightness and contrast of the image are adjusted for clarity, no other
modifications done) .....................................................................................................55
Figure 4.6: Schematic of 3-level recess patterned agar ...............................................56
Figure 4.7: Uniform distribution of bacteria on patterned surface ..............................56
Figure 4.8: Side view of (a) high voltage electrode in light room with no plasma, (b)
conventional microsecond DBD and (c) nanosecond-pulsed DBD on the patterned
agar surface (three steps with 0.33 mm height and 2 mm width). Pictures of
discharges have been taken in a dark room with 0.5 s exposure time at 120 Hz
repetition (for both systems) ........................................................................................57
ix

Figure 4.9: 3-level recessed agar surface treated with (a) nanosecond-pulsed DBD
and (b) microsecond-pulsed DBD. Width of each step (distance between the
horizontal lines) is approximately 2 mm. For both plates treatment time: 30 s,
concentration: 10
8
CFU/ml .........................................................................................59
Figure 4.10: Four different agar patterns with different depth (dimensions in mm) ...60
Figure 4.11: Sterilization effect of two systems on valleys (dashed circles indicate the
active area of the electrode) .........................................................................................61
Figure 4.12: Flow chart for determining the log reduction in bacteria population after
plasma treatment on patterned agar .............................................................................63
Figure 4.13: CFU Log reductions on different patterns with 30 s plasma treatment
Statistics are collected by dividing the treated are into four equal sections (quarter
circle area) and performing a count in each area .........................................................64
Figure 4.14: CFU log reduction on Type 2 pattern (max depth: 0.78 mm) as a
function of plasma treatment time. Statistics are collected by dividing the treated area
into four equal sections (quarter circle area) and performing a count in each area .....65
Figure 4.15: Schematic of single recess (channel) patterned agar ...............................67
Figure 4.16: Diagram of the system for air flow through the channel on the agar plate .
......................................................................................................................................67
Figure 4.17: 30 s treatment with nanosecond-pulsed DBD (a) without air flow, (b)
with 0.3 SLPM air flow, (c) with 3 SLPM air flow on single level recessed agar.
Arrows indicate the direction of the flow. (Outer and inner circles represent quartz
and electrode active area, respectively) .......................................................................69
Figure 4.18: Plasma treatment through MgF
2
window ................................................70





x

LIST OF TABLES



Table 2.1: Typical microdischarge parameters in a 1-mm gap in atmospheric-pressure
air (Fridman et al. 2005, Kogelschatz 2007) ................................................................12

Table 2.2: Summary of nanosecond-pulsed DBD parameters .....................................14

Table 3.1 Comparison between calorimetric and electrical power measurements ......26

Table 3.2: Size of the filament versus voltage rise rates for different dielectric barrier
discharge systems.........................................................................................................30

Table 4.1: Summary of nanosecond- and microsecond-pulsed DBD parameters .......52












xi

Abstract
Uniform Dielectric Barrier Discharge with Nanosecond Pulse Excitation for
Biomedical Applications
Halim Ayan
Advisors: Dr. Gary Friedman and Dr. Alexander Fridman

For some period of time the use of plasma in medicine has been limited to
thermal discharges for cauterization and dissection. The effects of thermal plasma on
tissue are entirely related to local heating. Non-thermal plasma, on the other hand, can
have many different modes of interaction with tissue. It has been recently
demonstrated that direct treatment of smooth surfaces by non-thermal dielectric
barrier discharge (DBD) in air is highly effective in killing pathogens. Moreover,
DBD can create different sub-lethal and selective effects. These results hold
significant promise for medical applications such as sterilization of wound surfaces.
However, a typical DBD in air can be highly non-uniform, particularly on
topographically non-uniform surfaces such as in most living tissues. This creates
significant limitations for use of DBDs in wound care and other biomedical
applications. In this thesis, a novel non-thermal plasma system, namely nanosecond-
pulsed DBD, has been developed and investigated to address this important
limitation. Nanosecond-pulsed DBD is shown to be uniform in air at atmospheric
pressure and much more effective in killing bacteria than conventional DBDs,
particularly on topographically non-uniform surfaces. Thus, this new plasma system
is potentially convenient for in vivo and hospital sterilization cases.

xii










1



CHAPTER 1: INTRODUCTION AND BACKGROUND
1.1 Plasma in Medicine
For some period of time the use of plasma in medicine has been limited to
thermal discharges for cauterization and dissection (Vargo 2004, Sumiyama et al.
2006, and Watson et al. 2000). Plasma has been used for electro-surgery where it
desiccates tissue by passing electrical current through it (Pollack et al. 2000, Polousky
et al. 2000, Lord et al. 1991, Stalder et al. 2005). The argon plasma coagulator (APC)
is another early application of plasma for cauterization, tissue devitalization, and
removal which also causes local heating and burns due to elevated temperatures
(Raiser and Zenker 2006) (Figure 1.1). Some of the surgical applications of the argon
plasma coagulator are visceral surgery, skin surgery (Brand et al. 1998), urology,
gynecology, brain tumor surgery (Tirakotai et al. 2004), gastroenterology (Ginsberg
et al. 2002), breast surgery (Ridings et el. 1998) and bronchological endoscopy
(Reichle et al. 2000).
However, the aforementioned thermal plasma interacts with living tissue
mainly through temperature and heat. Non-thermal plasma, on the other hand, can
have many different modes of interaction where various plasma species can generate
different sub-lethal and selective effects (Fridman et al. 2008, Stoffels 2007,
Coulombe et al. 2006, Shekhter et al. 2005, Gostev 2008) as demonstrated in recent
studies. In non-equilibrium plasmas, electron energies are much higher than the heavy
particle (ions and neutral species) energies, resulting in enriched gas phase chemistry
without high temperature input through collisions and consecutive dissociation,
2



excitation, and ionization processes (Kunhardt 2000, Penetrante 1996). Non-
equilibrium plasmas, such as Dielectric Barrier Discharge (DBD), are very attractive
because of their non-thermal nature. They create new possibilities in biological and
medical fields where substances of interest are mostly heat-sensitive such as living
tissue, cells, and biomaterials (Laroussi 2009, Stoffels et al. 2008, Yonson et al. 2006,
Puac et al. 2006). Some of the recent research subjects of non-thermal plasma
applications are 1) inactivation of bacteria on living tissue, 2) accelerated blood
coagulation, 3) enhanced cell functions including attachment and proliferation, 4)
treatment of malignant tissue, and 5) wound healing (Stoffels 2006, Yildirim et al.
2008, and Kalghatgi et al. 2007).
Systems that employ afterglow from non-thermal plasma for medical
treatment and disinfection have been proposed and demonstrated within the last
decade (Sladek and Stoffels 2005, and Goree et al. 2006). Non-thermal treatment is
possible with thermal plasma if its afterglow is transported and cooled (Shimizu et al.
2008). Although this makes it possible to work with living tissue and heat-sensitive
surfaces (Weltmann et al. 2008, Foest et al. 2007), such treatment takes a relatively
long time and can’t employ many short-living active plasma species and charges.
Direct plasma created right on the tissue, on the other hand, can generate and bring
charges and short living active species directly to its surface.
3




Figure 1.1: Schematic representation of a typical APC setup and APC probe with the
plasma beam on the tissue (Raiser and Zenker 2006, Stoffels 2007)

Within the past few years it has been revealed that direct treatment of smooth
surfaces and living tissues by non-thermal Dielectric Barrier Discharge (DBD) in air
is highly effective in killing pathogens including bacteria and fungi (Fridman 2008a,
Birmingham and Hammerstrom 2000, Montie et al. 2000, Laroussi et al. 2002). DBD
generates several active species that are quite essential for sterilization and other
important biomedical processes. Some of the highly active oxygen-containing
species are ozone, atomic oxygen, electronically excited oxygen, and peroxide. In
general, oxygen is required to be part of the gas composition to generate the
4



aforementioned active species and consequently for effective sterilization (Fridman
2008b). It has been demonstrated recently that contact of living tissue with charges
from non-thermal atmospheric pressure plasma is the main reason for the observed
effects (Fridman et al. 2007 and Deng et al. 2006) and is much more effective for
sterilization compared to UV (ultraviolet) or long-living species such as ozone in the
plasma afterglow.
1.2 Dielectric Barrier Discharge Plasmas
Dielectric Barrier Discharges (DBDs) are significant among all types of non-
thermal plasmas because of their relative simplicity. DBDs offer a unique
combination of non-equilibrium and quasi-continuous behavior having high electron
mean energy with lower heavy particle (neutral, ion) temperatures. They produce
several chemically active species (electrons, radicals, metastables, and ions) with low
gas heating (Wagner et al. 2003). Because of these characteristics, DBDs are widely
used in gas cleaning (from NO
x
, SO
x
, VOC), thin film deposition (Salge 1996,
Williamson et al. 2006), ozone production, light sources (excimer UV sources)
(Motret et al. 2000), industrial processes of polymer films or fibers to increase
wettability and adhesion (Borcia et al. 2003, Massines et al. 1998), and many other
technologies (Fridman et al. 2005). In addition, DBDs enable various emerging novel
applications in biology and the medical field (Laroussi et al. 2000 and Stoffels et al.
2002). Several interesting medical possibilities have been demonstrated by Fridman
et al. in the past few years (Fridman et al. 2006).
DBDs are often applied at atmospheric pressure and in air. There are usually
two electrode configurations that have been employed for most of applications: 1)
5



parallel and 2) concentric configurations (Figure 1.2). Operating principals of DBD
are summarized with schematics shown in Figure 1.3 (a through d). In general, when
high voltage is applied between two electrodes that are without insulation, an arc
(high temperature plasma channel) develops given sufficient time (as short as few
milliseconds). A dielectric barrier layer placed in front of at least one of the
electrodes (Gibalov and Pietsch 2000) limits the current, avoiding the formation of an
arc. Instead, transient non-thermal plasma is generated in the gap. If the applied high
voltage remains constant, charge from plasma accumulates on the dielectric surface
and reduces the effective field in the discharge gap extinguishing the discharge (Xu
and Kushner 1998). In order to sustain the DBD plasma, the applied voltage needs to
change over time allowing the charges accumulating on the insulator surfaces to be
removed.
Although, it has been demonstrated that DBD can be ignited in the form of
homogenous plasma at atmospheric pressure in certain gas mixtures, pure nitrogen,
and some noble gases (Kanazawa et al. 1988, Yokoyama et al. 1990, Gherardi et al.
2000, Miralai et al. 2000, Massines and Gouda 1998, Rahel et al. 2007), in most
cases, DBD (particularly in oxygen-containing gases, e.g. air) results in a multi-
streamer mode of operation with formation of microdischarges (Kogelschatz 2003)
and subsequent filaments that are visible to the human eye (Figure 1.4). The filaments
typically have a diameter on the order of 100 μm (Fridman et al. 2005, Kogelschatz
2002) for discharge gaps that are few millimeters long.

6




Figure 1.2: Parallel and concentric configurations of Dielectric Barrier Discharge
(Kogelschatz 2003 and Kogelschatz 2004)


As plasma density in the microdischarges is much higher than in the surrounding
space, these microdischarges can be considered as the only active locations of the
whole DBD volume, where all of the energy dissipates. Therefore, although average
temperature in the discharge volume is small, local temperature around the
microdischarge filaments can be relatively high. This temperature non-uniformity can
be very important, particularly when the microdischarges in DBD remain in the same
position for relatively long periods of time.


7





Figure 1.3: Schematics of DBD operation



Figure 1.4: Image of a typical DBD in air

8



Pinning of the microdischarges is more likely to occur on ridges of non-
uniform surfaces, like the surfaces of living tissues (Figure 1.5), which may
compromise effective treatment. The primary goal of the work reported here,
therefore, is to circumvent formation of discharge filaments in DBD and make the
discharge more uniform even on relatively non-uniform surfaces.


Figure 1.5: Microdischarges of a conventional dielectric barrier discharge striking on
the ridges of the skin (similar to lightning)


9



1.3 Research Objectives and Approach
This thesis rests on the hypothesis that ultra fast rising external voltage
enables generation of uniform plasma that will be effective and convenient for
treatment of non-uniform surfaces, e.g. living tissue. The objective of the research is
to retain the direct nature of the DBD plasma treatment, and to reduce the sensitivity
to topographical non-uniformities of the surface being treated. The scope this research
is 1) to develop and investigate non-thermal uniform DBD plasma system, and 2) to
demonstrate and assess its efficiency in applications requiring sterilization in air at
atmospheric pressure.

1.4 Thesis Outline
Chapter 2 explains the design of the nanosecond-pulsed dielectric barrier
discharge device and system for biomedical applications. The chapter starts with the
explanation of gas breakdown phenomenon in Dielectric Barrier Discharge and the
key facts of the nanosecond-pulsed dielectric barrier discharge system. Chapter 2 also
presents the details about the power supply circuit and the high voltage electrodes.
Chapter 3 focuses on the thermal, electrical, spectroscopic and uniformity
characterization of the novel nanosecond-pulsed system. Chapter 4 examines the
sterilization effect of the nanosecond-pulsed DBD plasma and presents a comparison
between it and conventional DBD. Finally, Chapter 5 summarizes the research
contributions.

10



CHAPTER 2: DESIGN OF THE NANOSECOND-PULSED DIELECTRIC
BARRIER DISCHARGE DEVICE AND SYSTEM FOR BIOMEDICAL
APPLICATIONS


2.1 Breakdown of Gas in DBD
It is important to revisit the breakdown mechanism of gas to understand the
operation of conventional DBD. When high voltage is first applied to the discharge
gap, free electrons gain energy and ionize the background gas by knocking out new
(secondary) electrons from heavy particles as they drift to the anode. Multiple
avalanches are formed and grow. This process is governed by the Townsend
ionization coefficient, α, which is a function of the reduced electric field, E/n (where
E is the electric field and n is the gas density).
Electron impact ionization dominates during the first phase of the breakdown
(Meek and Craggs 1978, Loeb 1960, and Bogdanov et al. 2004). During this phase,
many avalanches start. However, not all of them get a chance to develop equally. This
is due to the fact that, in the avalanche growth phase (Figure 2.1), usually the charge
density in the discharge gap grows non-uniformly. This results in non-uniform growth
of the electric field. If the external field grows slower than the non-uniform electric
field due to the space charge, it is possible for the field due to the space charge to
reach a critical level wherein it becomes comparable to the external field. This is
known as the Meek criterion. One of the effects of the high local electric field is that
it opposes the external field in some regions suppressing development of avalanches
there and enhancing ionization in other places. This effect is illustrated in Figure 2.2.
Some avalanches end up being ‘winners’, other become ‘losers’. In fact, the field of
11



the winning avalanches can be s strong that, in conjunction with the ionizing effects
of photons (photoionization), it creates a secondary fast ionization wave called a
streamer (Nikandrov et al. 2008, and Gouda and Massines 1999). Typical avalanche-
to-streamer transition and streamer propagation are presented in Figure 2.2. The front
of this secondary ionization wave actually propagates in the opposite direction.

Figure 2.1: Electron multiplication and avalanche growth (Raizer 1991)

Figure 2.2: Avalanche-to-streamer transition and streamer propagation (Raizer 1991)
12



When a streamer bridges the gap it forms a channel of weakly ionized plasma.
Eventually when the voltage polarity reverses, the residual negative charges from the
previous half-cycle contribute to the formation of new avalanches and streamers at (or
the vicinity of) the same spot. The outcome of the entire process from first electrons
to the streamer formation is called microdischarge. Typical microdischarge
parameters in a 1 mm gap in atmospheric-pressure air are presented in Table 2.1.

Table 2.1: Typical microdischarge parameters in a 1-mm gap in atmospheric-pressure
air (Fridman et al. 2005, Kogelschatz 2007)

Lifetime 1-20 (100) ns Filament radius 50 – 100 µm
Peak current 0.1 A Current density 0.1 – 1 kAcm
-2

Electron density 10
14
–10
15
cm
-3
Electron energy 1 – 10 eV
Total transported
charge
0.1 – 1 nC
Reduced electric
field
E/n = (1-2)(E/n)
Paschen

Total dissipated
energy
5 µJ Gas temperature ~ average, ~ 300 K
Overheating 5 K


2.2 Key Facts About the Nanosecond-pulsed Dielectric Barrier Discharge
System
Uniformity of the plasma could be improved in two ways: 1) increasing
uniform pre-ionization of the gas to initiate more avalanches or 2) shortening the
voltage rise time (Starikovskaia et al. 2001, Qi et al. 2006) to avoid growth of highly
inhomogeneous electric field that promotes growth of some avalanches at the expense
13



of others. If the number of primary avalanches is high enough before the
accumulation of the critical space charge, the discharge is likely to remain uniform
even if streamers do occur. The resulting discharge will resemble ‘pulsed avalanche’
regime (Levatter and Lin 1980). In addition, under these conditions, the shape of the
electrodes does not affect the location of the avalanches and streamers making the
discharge more independent of the topography. A fast rising driving voltage can also
shift electron energy distribution function to higher values (Gallagher et al. 1983).
Roughly, the criterion of the uniform discharge development could be
formulated with a simple relation:
τ
rise
< d / ν
d


where τ
rise
represents the excitation pulse rise time, d the discharge gap length,
and ν
d
the electron’s drift velocity in the critical electric field (Zatsepin et al. 1998).
Let us suppose that the discharge gap is about 1 mm. Let us also take the maximum
applied voltage, V
max
, for the DBD to be 16 kV. From this, the reduced electric field
(E/n) is found to be ~ 5.3 x 10
-15
V.cm
2
and, on average, the drift velocity (ν
d
) for an
electron in air is ~ 10
-7
cm/sec (tabulated value from Dutton 1975). Summary of the
parameters is given in Table 2.2. Accordingly, the time required for an avalanche to
travel the inter-electrode distance is ~ 10
-8
sec = 10 ns. This time is the characteristic
time of build-up of possible local non-uniformities in the electric field within the
discharge gap and, therefore, it is the goal of the proposed nanosecond-pulsed DBD
to achieve this rise time. The above estimate is consistent with other estimates of
dV/dt > 1 kV/ns (Raupassov et al. 2008). Tens of nanoseconds is considerably (at
14



least 2 orders of magnitude) shorter than rise time of microsecond-pulsed DBDs
which have been noted to be non-uniform.

Table 2.2: Summary of nanosecond-pulsed DBD parameters
Discharge
Gap
[mm]
Voltage
[kV]
Reduced
Electric
Field (E/n)
[ V.cm
2
]
Drift
Velocity

d
) [cm/s]
Time to
Bridge the
Gap [ns]
ns-DBD 1 16 5.3 x 10
-15
10
-7
10


2.3 Power Supply
A novel non-thermal nanosecond-pulsed DBD has been developed to generate
uniform plasma in air at atmospheric pressure. Rather than using expensive and often
unreliable semiconductor devices for creating nanosecond pulses (Miles et al. 2001
and Zhukov et al. 2007), a relatively simple double spark gap circuit has been built
for the generation of pulses with durations on the order of tens of nanoseconds (Ayan
et al. 2008).
The pulse generating circuit has been employed along with a current source to
obtain short duration high voltage pulses. The circuit with a double spark gap
configuration is shown in Figure 2.3.
15




Figure 2.3: Schematic of double spark gap configuration external circuit

The circuit produces repetitive short pulses. Voltage pulse starts when the
main spark gap is triggered. When the larger primary (main) spark gap breaks down,
charge initially stored in the main capacitor is transferred to the discharge as the
voltage across the plasma electrodes rises precipitously. The smaller (secondary)
spark gap starts to charge and eventually shorts out the DBD, resulting in a rapid
decay of the voltage across the DBD electrodes.
The size of the main spark gap determines the voltage that appears across the
discharge electrodes after the spark breakdown. The frequency of voltage pulses is
determined by the current source, main capacitor (how fast is the capacitor charged)
and is also affected by the peak voltage. The secondary spark gap affects mainly the
length of the voltage pulse that is maintained across the DBD electrodes. In the first
approximation, rise time of the voltage is independent of spark gaps.
16



The main spark gap was varied from 15 to 24 mm with at 3 mm intervals, and
repetition rates were measured between 250 and 100 Hz, respectively (for various
sizes of secondary spark gaps between 2.5 to 4.5 mm). The pulse frequency
(repetition) as a function of main spark gap distance is presented in Figure 2.4. Pulse
duration is linearly dependent on secondary spark gap length (Figure 2.5). For 2.5 and
4.5 mm gap distances, pulse durations are approximately 15 and 30 ns, respectively.
Peak voltage across the DBD is linearly dependant on the main spark gap distance
with approximately 1 kV per 1 mm for the above mentioned range (Figure 2.6). As
the main gap increases from 10 to 27 mm, peak voltage increases approximately from
10 kV to 27 kV. The rise time of approximately 3 kV/ns is obtained on the front of
the voltage pulse. A typical oscillogram of nanosecond-pulsed DBD with ultrafast
high voltage pulse is given in Figure 2.7. Additionally, both a single and 10-
consecutive (superimposed) voltage signals are presented in Figure 2.8.

Figure 2.4: Pulse frequency (repetition) versus main spark gap distance for several
small spark gap distances (2.5 - 4.5 mm). Frequency values are average of 10
measurements and variance is ±10%
0
50
100
150
200
250
300
15 18 21 24 27
F
r
e
q
u
e
n
c
y
 
[
H
z
]
Main Spark Gap [mm]
2.5 mm
3 mm
3.5 mm 
4 mm
4.5 mm
17




Figure 2.5: Pulse duration (FWHH) versus small spark gap distance for several main
spark gap distances (15 - 27 mm). Pulse duration values are average of 10
measurements and variance is ±10%


Figure 2.6: Peak voltage versus main spark gap distance for several small spark gap
distances (2.5 - 4.5 mm). Peak voltage values are average of 10 measurements and
variance is ±10%
0
5
10
15
20
25
30
35
2.5 3 3.5 4 4.5
P
u
l
s
e
 
D
u
r
a
t
i
o
n
 
[
n
s
]
Small Spark Gap [mm]
15 mm
18 mm
21 mm
24 mm
27 mm
0
5
10
15
20
25
30
15 18 21 24 27
P
e
a
k
 
V
o
l
t
a
g
e
 
[
k
V
]
Main Spark Gap [mm]
2.5 mm
3 mm
3.5 mm
4 mm
4.5 mm
18




Figure 2.7: Oscillogram of typical voltage and current signals
(Main spark gap: 12mm, Secondary spark gap: 3 mm)

Figure 2.8: Superimposed voltage signals versus time
(main spark gap: 15 mm and secondary spark gap: 3mm)
(a) Peak voltage: 15.6 kV, pulse length: 23 ns
(b) 10 voltage signals superimposed
19



2.4 Electrodes
Two electrodes are required in order to generate DBD: one electrode is
powered with high voltage and the other is grounded. There are two electrode
configurations with two different types of high voltage electrodes (powered) used.
The first configuration is plane-to-plane with flat surface electrode, and the second
configuration is sphere-to-plane with spherical electrode. In all cases, the grounded
electrode is either flat metal or agar.

2.4.1 Planar electrode
In the first configuration (plane-to-plane) the powered electrode is made out
of cylindrical copper and enclosed in Polyetherimide (Ultem®) for insulation (Figure-
2.9). The flat surface of the copper cylinder is covered with clear fused quartz
(Technical Glass Products, Painesville, OH) as a dielectric barrier. This configuration
was employed for characterization and sterilization experiments using with various
power densities.

Figure 2.9: Cylindrical electrode cross section
20




The flat surface electrode is made in two sizes for several different
experiments. The larger size cylindrical copper has 25 mm diameter and the thickness
of the clear fused quartz is 1 mm. The smaller size electrode cylindrical copper is 10
mm in diameter and covered by 0.66 mm thick quartz.

2.4.2 Test tube electrode
In the second configuration (sphere-to-plane), the high voltage electrode
(Figure 2.10) consists of a borosilicate glass (Pyrex®) test tube (cat.# 60825-902,
VWR Scientific, San Francisco, CA) with a conductive silver paste (SPI West
Chester, PA) filling inside. The thickness of the glass of the test tube is approximately
0.75 mm with a radius of curvature of 5 mm. It should be noted that in some cases,
this test tube electrode was positioned to be in contact near its tip with the grounded
plane metal electrode.






21




Figure 2.10: Glass test tube electrode









22



CHAPTER 3: PLASMA AND DEVICE PHYSICAL CHARACTERIZATION


3.1 Electrical Characterization
3.1.1 Voltage and current
Electrical measurements have been conducted by using a high frequency high
voltage probe (#PVM-4, 110 MHz, 1000:1, North Star High Voltage, Marana, AZ)
connected in parallel with the discharge and a high frequency current transformer
(#CM-10-L, Ion Physics Corporation, 0.1 V/Amp, 45 MHz bandwidth) around the
high voltage electrode wire. Electrical schematics with voltage and current probes at
positions have been shown previously in Figure 2.3. The probe signals were acquired
and recorded using a high speed oscilloscope (500 MHz bandwidth, 5 Gsample/s,
TDS5052B Digital Phosphor Oscilloscope, Tektronix, Inc., Richardson, TX). Power
dissipation in the discharge was analyzed by measuring instantaneous current and
voltage in the gap. Recorded data was processed using customized MATLAB code
which integrates the instantaneous power (V∗I) over many cycles to determine an
average energy per cycle and average power.

3.1.2 Power
Current signal of a typical DBD has many spikes in the oscillograms and they
are associated with individual microdischarges. These current spikes are
characteristically very short in duration and questions arise regarding the validity of
using the measured current to calculate the discharge power (Ayan et al. 2009a). The
bandwidth of the current probe and the inverse of the microdischarge duration are
23



comparable, and some loss of information about the actual discharge current may
occur. For this reason, the electrical measurements for average power were verified
with custom made calorimetric setup (Figure 3.1). Calorimeter is composed of a
peristaltic pump (model # 3386, Control Company, TX), two mercury thermometers
(model # 112C, -1 - 51˚C, 1/10˚C div., Palmer Instruments, Inc., NC), a copper
chamber and an insulation casing. Water is pumped at a controllable flow rate
through the copper tube that surrounds the chamber and encloses the DBD electrodes.
One thermometer is placed upstream to the chamber to measure the inlet temperature
of the water. A second thermometer is located downstream from the chamber to
measure the outlet temperature of the water. The system is insulated to ensure that the
only heat loss is attributed to the flowing water. The insulation is minimum 10 cm
thick around the system.
When the plasma ignites, dissipated energy in the chamber is taken away by
copper chamber and copper tube surrounding the chamber and transferred to the
running water. Temperature measurements from both thermometers are recorded
every minute throughout the experiments. Since the heat transfer to the water is a
rather slow process, it took typically more than 100 minutes to reach the steady-state
conditions in most cases. After reaching the steady state, the heat transferred from the
discharge (thus the average power dissipation in the discharge gap) can be calculated
by using flow rate, water specific heat capacity, and a constant water temperature
difference between inlet and outlet:

0

= m C
p
∆I
24



where 0

is heat, m is the mass flow rate, C
p
is the specific heat capacity of water, and
ΔT is the temperature difference between inlet and outlet ports.


Figure 3.1: Schematic of calorimeter setup

Additionally, a curve with double exponential term is fit to the experimental
data to ensure that the converged value is accurate. The double exponential term
curve is as follows:
∆I = c
1
+c
2
(1 -c
-c
3
t
) +c
4
(1 -c
-c
S
t
)

25



Here t is time, and c
1
, c
2
, c
3
, c
4
, and c
5
are arbitrary coefficients. A sample set
of data with curve fitting is given in Figure 3.2. It is found that the electrical and
calorimetric power measurements agree to within less than 10% indicating that the
bandwidth of the current transformer is at least sufficient for these measurements
(Table 2.1).


Figure 3.2: Experimental data and curve fitting for ΔT.
Electrical power measurement: 5.02 ± 0.44 W (average of 10 measurements)




ΔT(t∞) = 4.06 C
R2: 0.998365
0
0.5
1
1.5
2
2.5
3
3.5
4
4.5
0 50 100 150 200 250
Δ
T
e
m
p
e
r
a
t
u
r
e
 
[
C
]
Time [min]
Calorimetric measurement
Exp.
Fit
26




Table 3.1 Comparison between calorimetric and electrical power measurements
Parameter [unit] Value
Flow [ml/min] 16.55
Specific heat capacity (@ 25 °C) [J/g.°C] 4.1855
ΔT (fit) [°C] 4.0613
Power (calorimetry) [W] 4.689
Power (electrical) [W] 5.02
Difference % 6.6


3.2 Characterization of the Uniformity of the Plasma
3.2.1 Side view imaging
Along with nanosecond-pulsed DBD, a few other DBD systems are also
assessed visually for uniformity analysis. Initially, side view pictures of discharges
are taken by a digital camera (Nikon D70). Side view images of two conventional
type DBDs with plane-to-plane configuration are given in Figure 3.3 with 25 mm
diameter active area. In Figure 3.3, filaments are clearly visible for both types in the 1
mm discharge gap between the high voltage electrode (top) and the grounded
electrode (bottom). Detailed short time exposure images of filaments are captured
with a CCD camera on the spectrometer (Figure 3.4). A concave mirror with 5 cm
focal length is used to focus the light emitted from the plasma onto the slit of the
spectrometer. In order to facilitate spatially resolved measurements, the plasma image
is magnified approximately five times. Figures 3.5 and 3.6 illustrate the real and
contrast enhanced images of the filaments (microdischarges) of conventional
27



discharges created between two test tube electrodes (cross section lines on Figure 3.5
will be explained in the next chapter). In this electrode configuration (Kozlov et al.
2001, Kozlov and Wagner 2007), the filaments are localize at the opposing tips of the
electrodes and do not laterally wander as they would in the case of planar electrodes.
Arrows on Figure 3.6 identify the location of the electrodes (Figure 3.6 images are
contrast enhanced for clarity).


Figure 3.3: Images of two discharges with plane-to-plane configuration:
(a) Sinusoidal waveform, (b) Microsecond-pulsed waveform


Figure 3.4: Spectroscopic measurement setup for single filament
28




Figure 3.5: Locations of 21 cross sections on the images of two types of DBDs with
two test tube electrodes (1 mm gap). Exposure time of sinusoidal DBD is 50 msec
(600 cycles) and microsecond-pulsed DBD is 1 s (1000 cycles)

Figure 3.6: Contrast enhanced images of two types of DBDs with two test tube
electrodes (1 mm gap). Exposure time of sinusoidal DBD is 50 msec (600 cycles) and
microsecond-pulsed DBD is 1 s (1000 cycles)
29




On the other hand, nanosecond-pulsed DBD with glass test tube electrode is
shown in Figure 3.7. This discharge typically appears dim. Nevertheless, it can be
seen in Figure 3.7(a-b) that plasma is spread all over the spherical tip of the electrode.
Figure 3.7a is taken in the presence of background light and Figure 3.7b is taken in a
dark room. Both images are taken under the same conditions, i.e., repetition rate is
approximately 190 Hz and exposure time of the photography is 0.62 s. Table 3.2
provides a comparison of the size of the filament and voltage rise rates for different
dielectric barrier discharge systems.


Figure 3.7: Side view of nanosecond-pulsed DBD between test tube electrode and
ground metal electrode (a) with background light and (b) in a complete dark room for
the same exposure time (bottom halves of the images are due to reflection from the
ground plate electrode surface)
30



Table 3.2: Size of the filament versus voltage rise rates for different dielectric barrier
discharge systems
Plasma system Voltage rise Filament size Remarks
Sinusoidal 0.5 V/ns ~ 0.18 mm Fig. 3.6
Microsecond-
pulsed
20 V/ns ~ 0.1 mm Fig. 3.6
Nanosecond-
pulsed
3000 V/ns
(3kV/ns)
- Fig 3.7 & Fig. 3.9


Side view images of the nanosecond-pulsed DBD show that it is “filament-
free” and much more uniform than the conventional DBDs (microsecond-pulsed and
sinusoidal). Here, it should be highlighted that in Figure 3.3 the inter-electrode
distance is a constant 1 mm in the entire plasma gap. On the other hand, it can be seen
in Figure 3.7 that the plasma gap varies from 0 mm to approximately 4 mm for
nanosecond-pulsed DBD with a test tube electrode. Despite the large gap range,
nanosecond-pulsed DBD presents a uniform glow-like appearance, whereas despite
the constant 1 mm gap, conventional discharges exhibit a filamentary non-uniform
structure.

3.2.2 Lichtenberg figures
Although long exposure imaging is helpful to demonstrate distinction between
nanosecond-pulsed DBD and the conventional DBDs, a new experimental setup is
designed and built for qualitative yet more rigorous uniformity analysis. Qualitative
31



uniformity measurements of the various discharges have previously been done by
simply exposing a commercial photo film to the plasma. If conventional plasma is
generated on a dielectric surface, microdischarges create a "branching" form as soon
as they strike on the surface. Optical emission from the plasma can be registered if the
surface is a photo film. Images on the photo film provide information about the size
and the number of the microdischarges, and they are referred to as Lichtenberg
figures (Chirokov et al. 2004). A schematic of the setup is presented in Figure 3.8.
The photo film is placed between the insulated test tube electrode and the grounded
metal electrode. A roll-to-roll setup driven by an electric motor is engaged to advance
the photo film with a rate of about 1 m/s, where pulses of DBD plasma were being
ignited. The speed of the photo film is selected so that Lichtenberg figures of each
single pulse (cycle) of DBDs plasma could be resolved. Lichtenberg figures are
developed on black & white and color photo films. Black & white photo films
possess two different sensitivities, i.e. ISO100 and ISO3200. The experiment is
carried out in a dark room.
To analyze the distinction in uniformity more profoundly, Lichtenberg figures
of the nanosecond-pulsed DBD are compared with those of a conventional discharge,
i.e. microsecond-pulsed DBD. For microsecond-pulsed DBD, charge patterns are
obtained for 10 kV peak voltage pulses with a maximum 10 kV/μs rise with 2-5μs
pulse width. In the case of nanosecond-pulsed DBD, voltage rise and pulse duration
are approximately 3 kV/ns and 20 ns, respectively. Thus, both voltage rise and pulse
duration are at least two orders of magnitude longer for the microsecond-pulsed DBD
compared to its nanosecond DBD counterpart. Microsecond-pulsed DBD is operated
32



at a 120 Hz repetition rate, its lowest repetition rate, in order to facilitate capture of
consecutive pulses.
Both plasma systems are operated with the same test tube electrode. The
photo film is situated between the grounded plane metal electrode and the test tube
electrode near its tip.


Figure 3.8: Schematic of experimental setup to acquire the Lichtenberg figures on
photo film

As evident from the Figure 3.9, Lichtenberg figures show significant
differences between the two discharges. The nanosecond-pulsed discharge displays a
round pattern that is approximately equivalent in size to the diameter of the high
voltage electrode without any bright spot or irregular pattern distribution. The contact
point of the electrode appears as a dark point at the center of Figure 3.9a. Rays-type
33



pattern at the edge of the spot appears likely due to the secondary surface discharge
being driven by the lateral component of electric field. Figure 3.9(a-b) also verifies
that nanosecond-pulsed DBD ignites uniformly over a relatively large range of
electrode gap distances (0 - 4 mm). It is worth noting that 0 – 4 mm inter-electrode
gap range is due to the curvature of the glass covered high voltage electrode as it is in
contact near its tip with the grounded plane metal electrode. On the other hand,
discharge patterns of microsecond-pulsed DBD in Figure 3.9(c-d) clearly shows the
filamentary structure (microdischarges) when used with the same electrode under the
same conditions.


34





Figure 3.9: Lichtenberg figures of two different DBD systems on the emulsion of the
photo films: (a) nanosecond-pulsed DBD - b&w, (b) nanosecond-pulsed DBD - color,
(c) microsecond-pulsed DBD - b&w, (d) microsecond-pulsed DBD - color





35



3.3 Thermal Characterization of the Plasma
3.3.1 Optical emission spectroscopy
Optical emission spectroscopy (OES) is employed to measure the vibrational
and rotational temperatures of the DBDs in the plasma volume using 375.4 nm and
380.4 nm vibrational lines and rotational structure at this region of the second positive
system of molecular nitrogen
,
N
2
(C
3
Π-B
3
Π). The experimental spectrum is compared
to the simulated spectrum with T
vib
and T
rot
determined by the best fit (minimum
RMSE) between the modeled and experimental spectrum detailed in the literature
(Yalin et al. 2002, Laux et al. 2003, Packan et al. 2003, Staack et al. 2006, and Staack
et al. 2007).
Prior to the investigation of nanosecond-pulsed DBD, in order to set a
benchmark for the rest of the study, two conventional non-uniform DBD systems are
characterized. The features of the two power supplies that have been employed to
generate plasma are as follows: 1) Microsecond-pulsed DBD system can generate up
to 35 kV peak-to-peak voltage with 120 Hz to 1 kHz repetition rate, and 1.5 to 5 μs
pulse width at the half maximum of the voltage pulse, 2) Sinusoidal DBD system can
generate up to 35 kV peak-to-peak voltage with 12 kHz frequency. Typical
waveforms of two power supplies are given in Figure 3.10 where peak-to-peak
voltage is 17 kV for sinusoidal and 18 kV for microsecond-pulsed systems. Multiple
current peaks in the oscillograms (Figure 3.10) reflect a characteristic non-uniform
DBD discharge.
36





Figure 3.10: Oscillograms of (a) sinusoidal and (b) microsecond-pulsed DBDs

Optical emission spectroscopy show that the rotational temperatures are
between 340 and 400 K for both types of DBD. For DBD plasmas, rotational
37



temperature is essentially equal to the translational (gas) temperature (Nozaki et al.
2001, Nozaki et al. 2002). Here, one important point should be clarified. To be more
precise, there can be 2 different temperatures defined for conventional DBDs: 1)
temperature of the microdischarges (maximum temperature) and 2) average
temperature of discharge gap (taking the entire gap into account). OES measures the
maximum temperature, namely temperature of the microdischarge. Since rotational
temperature (gas temperature) has been obtained via spectroscopy, and the lifetime of
the upper state of N
2
is very short (Chelouah et al. 1994) compared to the shortest
voltage pulse duration (microsecond-pulsed DBD), it means that the collected light
and measured temperature correspond to the plasma state during the time of the
microdischarge.
The rotational and vibrational temperatures of the two conventional DBDs are
measured at different power levels. Power densities are calculated based on the power
input and the size of the active area of the electrode. Given in Figure 3.11 & 3.12 are
the averages of 3 measurements under the same conditions and the error bars shown
representing the deviation of those three measurements.
As might be expected, Figure 3.11 shows a near linear increase in rotational
(gas) temperature with average power density. Moreover, the two distinct type of
voltage waveforms seem to fit to the same slope (although no overlap is seen within
their respective operating ranges due to power supply limitations). This demonstrates
that the power-temperature relation is largely independent of voltage waveform shape
for the power range studied here. Thus, although sterilization effects may be different
38



for different discharges, i.e., dependant on several physical and chemical factors, it
appears that gas temperature depends only on average power.
In Figure 3.12, vibrational temperatures are plotted for different average
power densities. Even though, it looks like there exists a trend of a decrement in
vibrational temperature as the power increases, this is not really clear because of the
relatively low sensitivity of the calculation method for the vibrational temperature,
and therefore all values can be considered to be roughly the same (3300 – 3400 K).
Nonetheless, a slight increase in vibrational temperature accompanying a decrease
rotational temperature has been observed before and is not unexpected as the rates of
vibrational to translational energy transfer decrease with decreasing translational
temperature (Staack et al. 2006).


Figure 3.11: Rotational temperature as a function of average power density for the
sinusoidal DBD and the microsecond-pulsed DBD

39




Figure 3.12: Vibrational temperatures as a function of average power density for the
sinusoidal DBD and the microsecond-pulsed DBD

In addition to the volume discharge temperatures, spatial temperature
distribution along a single filament has also been measured in order to investigate the
effect of energy dissipation in the volume onto near-surface locations. A double glass
test tube electrode configuration with a 1 mm distance between electrodes is used to
obtain a single filament. Temperatures for the two different types of DBD filaments
have been measured over 20 equally divided intervals (at 21 cross sections) along the
axial direction of single filaments shown in Figure 3.5. Spectra at each cross section
have been acquired simultaneously and temperature calculations have been conducted
on each spectrum for different locations (of the axial position). A sample of set of
spectra at various locations along the filament is presented in Figure 3.13 (discrete).
40



Also Figure 3.14 illustrates spatial intensity for the wavelength range of interest
(continuous).
The radial thickness of the microsecond-pulsed DBD is clearly seen to be
thinner than that of the sinusoidal DBD. This may be due to the fact that the
volumetric ‘memory’ effect (Eliasson et al. 1987) is stronger for sinusoidal DBD
which has a much higher current pulsing frequency, and therefore each streamer has
better marked “road” that is formed by the diffuse decay of the previous streamer.


Figure 3.13: Spectra at various locations along the filament
(cross sections : 1, 3, 5, ….17, 19, 21)
41




Figure 3.14: Spatial intensity versus wavelength (372.7 nm – 381.2 nm)

The aforementioned results of temperature measurements along the axis of
single filaments are plotted in Figure 3.15. These measurements do not reveal any
significant differences in rotational and vibrational temperatures along the discharge
channel (except possibly very near the electrodes). Rotational temperature
distributions are uniform along filament for both types of discharges, thus power
appears to dissipate more or less evenly.
Along the central axis, emission intensity (for the region of interest of the
spectrum) from the single filament is minimal in the middle and increases towards the
electrode surfaces, roughly doubling for both types of discharges. However, as seen
in Figure 3.15, an increase in the emission intensity does not necessarily imply that
the temperature is higher. Also, a slight increase in the light intensity at the electrodes
might be due to inevitable reflection from the glass test tube surfaces. In summary,
42



Figure 3.15(a-b) indicates that the rotational and vibrational temperatures can be
considered constant along the channel. In general, vibrational temperatures are one
order of magnitude higher than rotational temperatures and this indicates the non-
equilibrium nature of the discharge.


Figure 3.15: (a) Rotational and (b) Vibrational temperature distributions along the
microdischarges
43




A different setup is used to measure temperature of the nanosecond-pulsed
DBD. A fiber-optic bundle (Princeton Instruments-Acton, 10 fibers – 200 μm core) is
utilized to acquire the optical emission from the discharge and to transmit it to the
spectrometer (Acton Research SpectraPro 500i with Roper Scientific model 7430
CCD camera or Princeton Instruments – Acton Research, TriVista TR555
spectrometer system with PIMAX digital ICCD camera, Trenton, NJ) and spectra are
digitally acquired with approximately 0.6 nm resolution (Figure 3.16). The
temperature of the camera is set at -25°C in all experiments.


Figure 3.16: Spectroscopic measurement setup for DBD

The background noise obtained for the same exposure time is subtracted from
the discharge emission spectrum prior to the temperature estimation. Low pressure
mercury lamp is used to determine the slit function and calibrate the spectrometer.
The ambient room temperature is 22°C throughout the spectroscopic measurements.
44



Curve fitting of model spectra (Laux 2002) to experimental data is carried out.
The second positive system spectrum of nanosecond-pulsed DBD and best fit
simulated spectrum are given in Figure 3.17. Rotational and vibrational temperatures
are measured to be 313.5 ± 7.5 K and 3360 ± 50 K, respectively, for the power range
that has been used for the experiments explained below. These ‘temperatures’
describe the relative population of different vibrational and rotational levels of the C
3

state of molecular nitrogen. Rotational distribution of the C
3
state under the pulsed
excitation at high overvoltage reflects the rotational population of the ground state
and gives information regarding the temperature of the gas. Vibrational spectra of the
second positive reflect the interplay between the population by electron impact from
different lower states and depopulation due to the collisional quenching and radiative
processes. Thus the vibrational distribution is an indicator of the electron’s
temperature in the discharge region. Thus, it is demonstrated that the nanosecond-
pulsed DBD does not heat the gas but provides strong excitation of the gas due to the
high energy of the electrons. Figure 3.18 shows nanosecond-pulsed DBD igniting on
a finger without causing any damage or even discomfort.


Figure 3
measureme
33
Figure 3.
3.17: Spectra
ent. Rotation
360 ± 50 K.
.18: Nanosec
a of nanosec
nal temperatu
(Model spec
cond-pulsed

cond-pulsed D
ure: 313.5 ±
ctrum: Laux


d DBD ignitin
DBD for spe
7.5 K and v
x 2002, Staac
ng on finger
ectroscopic t
vibrational te
ck et al. 2006
r (exposure t
4
temperature
emperature:
6)

time: 1 s)
45

46



3.3.2 Surface temperature
In addition to the spectroscopic temperature measurements, surface
temperature on the grounded electrode is measured in the presence of the discharge
using a reversible liquid crystal temperature indicator (model 4002B, Accuracy: ±
1°C, LCR Hallcrest L.L.C., IL). A sheet of the temperature indicator is placed over
the grounded copper electrode and acts as the secondary electrode in the discharge
(Goree et al. 2006). The room temperature is 22°C during the surface temperature
measurements. Surface temperature due to plasma is measured at 25°C, while the
temperature of the ground electrode surface without the discharge is also measured to
be 22°C.

3.4 Summary of Key Results and Conclusions
Several characterizations have been conducted to explore the feasibility of
using nanosecond-pulsed DBD for living tissue treatment. Electrical measurements
for average power are verified with a custom-made calorimeter.
Two conventional DBD systems have been analyzed spectroscopically and
single filament measurements show that there is no significant change in gas
temperature along the channel.
Volume discharge measurements demonstrate that microdischarges within the
volume for different types of discharges have the same gas temperature for the same
power. A power-temperature relation is found to be somewhat linear and largely
independent of voltage waveform shape.
47



Nanosecond-pulsed DBD and other DBD systems are assessed visually for
uniformity analysis. Side view long exposure images of the nanosecond-pulsed DBD
show that it is “filament-free” and much more uniform than the conventional DBDs.
Some other qualitative experiments with photo films verify that nanosecond-pulsed
DBD is completely uniform.
Also it is found that with spherical electrode nanosecond-pulsed DBD can
ignite and be sustained over a wide range of inter-electrode gap.
Optical emission spectroscopy measurements reveal that nanosecond-pulsed
DBD is almost at room temperature with 313.5 ± 7.5 K and 3360 ± 50 K for
rotational and vibrational temperatures, respectively. Surface temperature increases of
3°C are observed after 5 minutes of plasma exposure with typical power density.











48



CHAPTER 4: STERILIZATION EFFICACY, BIOLOGICAL
CHARACTERIZATION AND QUANTIFICATION OF NANOSECOND-
PULSED DIELECTRIC BARRIER DISCHARGE


4.1 Qualitative Demonstration of Sterilization
Nanosecond-pulsed DBD has been tested for demonstration of sterilization by
treating bacteria culture on agar. Skin flora bacteria, a mix of Staphylococcus,
Streptococcus, and yeast, are transferred onto a blood agar plate (Trypticase Soy Agar
with 5% Sheep Blood; Cardinal Health, Dublin, OH) for a sterilization demonstration
(Fridman et al. 2006). Figure 4.1 shows the image of an agar surface covered with
skin flora (dark red area covering most of the surface) being sterilized (light red area)
with nanosecond-pulsed DBD treatment for 15 s. This result does show both the
sterilization ability of the discharge as well as its efficiency. Treatment with power as
low as a few tens of mW for 15 s, with an average power density of approximately 1
mW/mm
2
(discharge diameter equal to electrode diameter) can sterilize. This power
density is one order of magnitude lower than typical conventional DBD power
densities. For the same duration, complete sterilization can be attained with
nanosecond-pulsed DBD at a significantly lower power density.

4.2 Qualitative Comparison of Conventional and Nanosecond-pulsed
Dielectric Barrier Discharge on Topographically Non-uniform Surfaces

In addition to a typical sterilization experiment, effectiveness of the DBD
excited by nanosecond rise and fall time voltage pulses has been tested for
inactivation of the bacteria located within indentations on surfaces (Ayan et al.
49



2009b). It is vital for the discharge to produce uniform plasma independent of the
uniformity of the bacteria covering surface that serves as one of the DBD electrodes,
so the discharge can sterilize irregular surfaces completely.


Figure 4.1: Agar with skin flora treated by nanosecond-pulsed DBD (V
max
: 20 kV,
Repetition rate: 190 Hz)

The agar used for bacteria culture in this study is made out of a broth (Difco
Brain Heart Infusion Agar powder, Fisher Scientific, PA) mixture that solidifies
shortly after it is poured in the petri dish. In general, two different sorts of agar plates
are fashioned and used for topographically non-uniform (uneven) surface sterilization
experiments. The first type is characterized by a flat planar surface which is used in
50



studies of non-uniform surfaces by placing meshes over them, as well as for control
samples.
The second type of agar plates which are specifically prepared to have non-
uniform surfaces (with ridges and indentations) on the agar to mimic the real case for
living skin tissue. The agar ridges are molded by placing a polymer form at the
bottom of the dish. Then, agar is poured on top of the mold and left to dry. After the
agar is solidified, it is removed and inverted and placed into the new (final) dish.
Different steps of patterned agar preparation are presented in Figure 4.2.

Figure 4.2: Patterned agar preparation
51



Escherichia coli bacteria (E.coli K12 strain, Ward's Natural Science,
Rochester, NY) are plated onto the surface of agar with concentrations of up to 10
8

10
9
CFUs/ml (colony forming units/ml). The suspension volume (water and bacteria)
is enough to completely cover the surface of the agar. Concentrations were measured
and calculated on flat agar plates with a dilution assay which is a common technique
in microbiology (Singleton and Sainsbury 2002, Silverthorn et al. 2004). The dilution
assay protocol is presented in Figure 4.3.

Figure 4.3: Protocol for dilution assay

52



Before plasma treatment, bacteria seeded plates are left to dry in the laminar
flow hood (Labconco, Class-II, Kansas City, MO) for 1 hr along with the control
plates. After plasma treatment, treated and untreated (control) samples are cultured
for 12 hrs in the incubator (VWR, Sheldon Manuf. Inc., Model#1545, OR) at 37 ºC.
Sterilization results are evaluated by visually examining the resulting colonies after
incubation. Samples are also observed up to a 48 hrs incubation period in which
delayed recovery is not found in the plasma treated regions.
The sterilization effectiveness of nanosecond-pulsed DBD on non-uniform
surface is proved by comparing with conventional DBD. For nanosecond-pulsed
DBD applying 20 ns long, 16 kV pulses with approximately 3kV/ns rise/fall times
and for microsecond-pulsed DBD applying 1.5 μs long, 10 kV pulses with 20V/ns
rise time both are produced at 120 Hz to maintain the comparable power. In all
experiments, power density for the active area of the electrode is maintained at 100
mW/cm
2
(approximately 75 mW for 1 cm electrode diameter). Parameters for both
systems are summarized in Table 4.1.

Table 4.1: Summary of nanosecond- and microsecond-pulsed DBD parameters
Pulse
Length
[ns]
Voltage
[kV]
Front
[ V/ns]
Frequency
[Hz]
Power
[mW/cm
2
]
ns-DBD 20 16 3000 120 100
µs-DBD 1500 10 20 120 100


53



The first part of the non-uniform surface sterilization experiments is done by
placing a stainless steel mesh over the flat surface agar as shown in Figure 4.4. In this
case, a metal mesh simulates the effects of ridges and indentations; i.e. surface non-
uniformities. The opening between the wires of the mesh is 1.5 mm, the wires are
0.25 mm in diameter, and total thickness of the mesh is 0.5 mm. The gap between the
bottom of the high voltage electrode and the top of the mesh is 1 mm.
A typical sterilization result comparing both nanosecond-pulsed and
microsecond-pulsed DBD systems is shown in Figure 4.5. Light color areas in this
figure are the locations on the agar that are completely sterilized by plasma treatment
and the rest of the agar with a darker color is E.coli covered. On the left-hand side of
Figure 4.5, sterilization is achieved at the ‘valleys’ with a slightly larger diameter
than the active area of the electrode in 30 s. In contrast, conventional DBD affects a
significantly smaller area (on the right-hand side of Figure 4.5). The concentration of
sterilization effect to the middle part for microsecond-pulsed DBD can be due to
possible occurrence of surface discharges following the extinction of the
microdischarges. These preliminary results from the sterilization experiments clearly
indicate that the nanosecond-pulsed discharge is much more effective and faster than
the conventional microsecond DBD in killing E.coli bacteria.

54




Figure 4.4: Illustration of mesh on top of the agar to mimic the indentations
(10 mm diameter electrode with 0.66 mm quartz)


55




Figure 4.5: Inactivation with nanosecond- (left-hand side) and microsecond- (right-
hand side) pulsed DBD through metal mesh and (b) schematic of the experimental
setup (schematic is not to scale; circles in (a) indicate the edge of the high voltage
electrode; brightness and contrast of the image are adjusted for clarity, no other
modifications done)

In the second group of experiments, the sterilization effect of novel DBD
system has been tested and also compared with that of a conventional DBD system.
For this experiment, the agar is patterned with a 3-level recess with 2 mm width and
0.33 mm depth at every stage. Dimensions are shown on a schematic in Figure 4.6.
56



It should be also noted that prior to these experiments, uniform distribution of
bacteria on the patterned surfaces are verified by seeding low enough concentrations
(10
3
– 10
4
CFU/ml) to get a countable number of colonies on the surface (Figure 4.7).


Figure 4.6: Schematic of 3-level recess patterned agar






Figure 4.7: Uniform distribution of bacteria on patterned surface
57




A two-piece spacer with 0.5 mm thickness is placed between the high voltage
electrode and the top surface of the agar. In Figure 4.8, the side view of electrode on
patterned agar surface (Figure 4.8a), and the typical appearance of a conventional
microsecond-pulsed DBD (Figure 4.8b) and a nanosecond-pulsed DBD (Figure 4.8c)
are given.



Figure 4.8: Side view of (a) high voltage electrode in light room with no plasma, (b)
conventional microsecond DBD and (c) nanosecond-pulsed DBD on the patterned
agar surface (three steps with 0.33 mm height and 2 mm width). Pictures of
discharges have been taken in a dark room with 0.5 s exposure time at 120 Hz
repetition (for both systems)

58



As it can be easily seen from Figure 4.8b, the conventional microsecond-
pulsed DBD produces microdischarges (filaments) that are often terminated on the
top of asperities and irregularities (mostly at smaller gaps or corner of the surface
features) whereas the nanosecond-pulsed DBD exhibits a rather diffuse structure in
Figure 4.8c. Although the latter is also slightly more intense on the corners, it is fully
covering the entire gap.
The exclusive features of nanosecond-pulsed DBD can also be easily seen in
Figure 4.9 with the distinction in sterilization performance. This figure shows a top
view of a treated 3-level recess patterned agar that is given in Figure 4.8 previously.
In the case of nanosecond-pulsed DBD, all three steps are uniformly treated and
sterilized (Figure 4.9a) whereas in the case of conventional microsecond-pulsed
DBD, only partial sterilization is achieved in the vicinity of the edge of the first step
where the discharge gap is minimal (Figure 4.9b).


59





Figure 4.9: 3-level recessed agar surface treated with (a) nanosecond-pulsed DBD
and (b) microsecond-pulsed DBD. Width of each step (distance between the
horizontal lines) is approximately 2 mm. For both plates treatment time: 30 s.,
concentration: 10
8
CFU/ml



60



4.3 Quantitative Comparison of Conventional and Nanosecond-pulsed
Dielectric Barrier Discharge on Topographically Non-uniform Surfaces

Sterilization efficacies of nanosecond-pulsed DBD and conventional DBD
have also been compared quantitatively. E.coli suspensions with different
concentrations are seeded on the patterned agar plates. Four different patterns are
used to assess the sterilization as a function of surface pattern depth. The preparation
method of patterned agar is described in the previous chapter. Drawings of the
patterns with dimensions are given in Figure 4.10.


Figure 4.10: Four different agar patterns with different depth (dimensions in mm)

Figure 4.11 shows the typical difference between uniform nanosecond-pulsed
DBD and conventional DBD. Arrows on each pictures show the lowest level of the
pattern (Type 2). When nanosecond-pulsed DBD is applied, all surfaces at different
levels are sterilized. In contrast, microsecond DBD sterilizes only the highest level
Type 1 Type 0
Type 2 Type 3
61



while it can partially affect the bacteria at the bottom of the valleys and cannot fully
sterilize.


Figure 4.11: Sterilization effect of two systems on valleys (dashed circles indicate the
active area of the electrode)

In this experiment, an electrode with 10 mm diameter active area is used.
After plasma treatment, bacteria quantification is done by counting the colony
forming units on the treated surface within the 10 mm diameter circle. Initial seeding
concentrations are determined by a standard dilution assay method (Figure 4.3).
Following the plasma treatment, agar plates are placed into the incubator for 12 hrs.
62



Bacteria colonies are then counted (after-treatment). At some higher seeding
concentrations, plasma treatment resulted in partial sterilization wherein it is not
possible to quantify the CFUs after treatment. In those cases, quantification is carried
on with the next lower dilution. In every case, the highest countable seeding
concentration is taken into account and the CFU log reduction is calculated from the
difference between initial seeding and post-treatment counts. The protocol for
determining the log reduction is given in Figure 4.12.
63





Figure 4.12: Flow chart for determining the log reduction in bacteria population after
plasma treatment on patterned agar


64



Results for log reduction of bacteria colonies after a 30 s treatment are
presented in Figure 4.13. As expected, data shows that the sterilization effect
diminishes as the pattern depth increases. In addition, in most cases nanosecond-
pulsed DBD is found to be inactivating more than 1 order of magnitude more bacteria
than with conventional DBD. Also, the E.coli CFU log reduction on the Type 2
pattern as a function of plasma treatment time is presented in Figure 4.14.


Figure 4.13: CFU Log reductions on different patterns with 30 s plasma treatment
Statistics are collected by dividing the treated are into four equal sections (quarter
circle area) and performing a count in each area

In the literature, there exists a widely used kinetics measurement parameter to
characterize the sterilization efficacy in a broader perspective. The parameter is often
referred to as a D-value and is essentially equal to the time required to reduce the
1
2
3
4
5
6
1 2 3 4
L
o
g
 
R
e
d
u
c
t
i
o
n
 
Pattern Type / Max Depth
Type 0                      Type 1                      Type 2                      Type 3
0.34 mm                  0.56mm                    0.78mm                  1mm
ns‐DBD
Conventional 
DBD
65



original concentration by 1 log (Laroussi 2005). In Figure 4.14, the shortest treatment
time is 5 s reductions in bacteria population are already more than 1 log for both DBD
systems. Therefore, these results set the D-value at a few seconds which is a relatively
shorter time compared to the other studies (Laroussi et al. 1999 and Herrmann et al.
1999).


Figure 4.14: CFU log reduction on Type 2 pattern (max depth: 0.78 mm) as a
function of plasma treatment time. Statistics are collected by dividing the treated area
into four equal sections (quarter circle area) and performing a count in each area


4.4 On the Mechanism of Sterilization
Plasma is a chemically active medium including thermal, electric, radiative
energy forms and they interact with background gas and substances being exposed.
0
1
2
3
4
5
1 2 3
L
o
g
 
R
e
d
u
c
t
i
o
n
 
Treatment time
5 s                                    15 s                                  30 s
ns‐DBD
Conventional DBD
66



There are several factors in the plasma that can cause inactivation of bacteria (Stoffels
2007, Gaunt et al. 2006, Lerouge et al. 2000); namely heat, UV radiation, ozone, and
charged particles (electrons and positive and negative ions).
In order to help understand the basic mechanism of sterilization with
nanosecond-pulsed DBD, some experiments are designed and implemented. In the
first experiment, plasma treatment applied on the bacteria seeded surface in the
presence of air flow in the single recess (channel) agar. A schematic of the single
recess pattern is shown in Figure 4.15. A diagram of the system is presented in Figure
4.16. Air was supplied from a tank and flow rate regulated with a digital flow
controller (Omega Engineering, Inc., Model#: FMA-2620A & FMA-2607A).
Additionally, a top view of the single step recessed agar that is used for this
experiment is given in Figure 4.17. The depth and the width of the recess are 1 mm
and 10 mm, respectively. In the first case (Figure 4.17a), the surface of the agar plates
are treated for 30 s in a regular fashion. In the second and third cases (Figure 4.17b
and Figure 4.17c), air is blown through the gap between the quartz and the bottom of
the recess with 0.3 and 3 SLPM flow, yielding 0.5 m/s and 5 m/s air velocity in this
cross section, respectively.
67




Figure 4.15: Schematic of single recess (channel) patterned agar


Figure 4.16: Diagram of the system for air flow through the channel on the agar plate

In terms of sterilization, the results are similar to each other except for slight
size differences in the size of the sterilized area. However there is no qualitative
difference between the air flow and no flow cases, i.e. there is no partial sterilization
due to the plasma afterglow downstream of the flow (to the right hand side of the
figure). The lack of major differences in the figures indicates that the sterilization
68



occurs through direct contact with the plasma. The sterilizing agents cannot be blown
or translated away from the electrode location with air flow.
Additionally, another experiment is conducted to assess the effect of UV in
nanosecond-pulsed DBD. A VUV (vacuum UV) grade MgF
2
window (Crystran
Limited, UK) has been placed on the E.coli seeded flat agar surface. The area covered
by the MgF
2
window receives only UV and the rest of the treated area is exposed to
whole plasma products. As presented in Figure 4.18, the area covered (exposed to
only UV) is not sterilized whereas the rest of the treated area is sterilized. This result
suggests that UV, by itself, is not the major bactericidal factor in the plasma.




Figure 4.17
with 0.3 S
Arrows ind
: 30 s treatm
LPM air flow
dicate the dire
an
ment with nan
w, (c) with 3
ection of the
nd electrode


nosecond-pu
3 SLPM air f
e flow. (Oute
active area,
ulsed DBD (
flow on sing
er and inner
respectively
(a) without a
gle level rece
circles repre
y)
6

air flow, (b)
essed agar.
esent quartz
69
70





Figure 4.18: Plasma treatment through MgF
2
window


Taking the last two experiments together in to consideration: 1) the afterglow
of the plasma contains only neutral atoms, radicals and molecules, some of which are
in an excited state (Deng et al. 2006 and Moisan et al. 2002), and most of the charged
particles remain in the plasma region (lifetime of charged particles at atmospheric
pressures is very short) and 2) UV is not playing a major role in those experiments.
The conclusion drawn from these results is that sterilization by nanosecond-pulsed
DBD is mostly due to the charged particles.





71



4.5 Summary of Key Results and Conclusions
Sterilization capability of nanosecond-pulsed DBD has been first
demonstrated on plain agar with skin flora. Then sterilization effectiveness of
nanosecond-pulsed DBD on topographically non-uniform surfaces has been tested
and proven with a series of experiments.
Sterilization efficacy of nanosecond-pulsed DBD and conventional DBD
have also been compared quantitatively where nanosecond-pulsed DBD is found to
be inactivating 1 to 1.5 orders of magnitude more bacteria than with conventional
DBD.
As it is shown in the previous chapter, the temperature of nanosecond-pulsed
DBD is measured to be at room temperature level. Therefore, ‘temperature of the
plasma’ cannot be the factor that causes sterilization. Additionally, experiments in
this chapter on mechanism of the sterilization rules out ozone and UV, and concluded
that charged particles are the most important factors in the plasma.










72



CHAPTER 5: SUMMARY AND CONCLUSIONS


5.1 Summary of the Research and Conclusions
A novel uniform non-thermal plasma system was developed in this work for
living tissue sterilization and other medical applications. Experiments on non-uniform
surfaces using meshes and patterned agar revealed that the nanosecond-pulsed DBD
can penetrate valleys (indentations between ridges), whereas the microsecond-pulsed
DBD fails to do so as well. The nanosecond-pulsed DBD with short rise time and
high overvoltage is insensitive to the surface non-uniformities of the agar and does
not require uniform discharge gaps as it can ignite and be sustained over a wide gap
range. Thus, DBDs with nanosecond rise times are potentially more convenient for in
vivo and real sterilization cases with non-uniform profile surfaces.
It should be emphasized that the technique employed to generate a few tens of
nanosecond long pulses is relatively simple and inexpensive. This method may be
easily used for a variety of applications.
The uniformity of this nanosecond-pulsed DBD is proven qualitatively with a
new technique for such high frequency discharge, using high speed photosensitive
film exposure. Lichtenberg figures of nanosecond-pulsed DBD show clearly that few
tens of nanosecond pulse duration avoids streamer formation and generates uniform
discharge in atmospheric pressure air.
The ability of the nanosecond-pulsed discharge to sterilize has been
demonstrated, quantified, and compared with that of a conventional discharge. This
novel DBD is proven to be much more effective in killing bacteria on surfaces than
with conventional DBD. Experiments that have been conducted in order to
73



understand the basic mechanism of sterilization by comparing direct and indirect
plasma effects indicate that charges (electrons and ions) play a major role in
sterilization with nanosecond-pulsed DBD.

5.2 Research Contributions
The main research contribution in this work has been developing a novel
dielectric barrier discharge system that enables uniform plasma treatment for living
tissue sterilization in atmospheric pressure air. This system can also be used in other
biological studies and non-uniform surface treatment applications. The thesis research
and activities will help to develop knowledge and novel solutions in the Plasma
Medicine field.
The specific contributions of this research are summarized as follows.
• Development of a uniform dielectric barrier discharge system with
nanosecond pulse excitation for the first time in air and at atmospheric
pressure.
• Demonstration of uniform plasma on topographically non-uniform
surfaces for the first time in air at atmospheric pressure.
• Demonstration and quantification of sterilization on non-uniform surfaces
with nanosecond-pulsed DBD treatment. The nanosecond plasma works
significantly better than conventional DBD on non-uniform surfaces. This
makes it a promising tool for medicine.
74



• Confirmation that the mechanism of sterilization in nanosecond DBD is
associated with charges.
• Elimination of microdischarges, therefore offering a safer treatment
without possible local heating.














75




















76



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89


VITA 
 
EDUCATION  Ph.D. Candidate, Mechanical Engineering                                           October 2005 – July 2009   
Department of Mechanical Engineering and Mechanics 
Drexel University, Philadelphia, PA 
 
B.Sc., Mechanical Engineering                                                           September 1997 – July 2001
Department of Mechanical Engineering 
Ege University, Izmir, Turkey   
(valedictorian and summa cum laude) 
 
PROFESSIONAL 
EXPERIENCE 
Graduate Research Assistant / Teaching Assistant                            October 2005 – July 2009
Department of Mechanical Engineering and Mechanics 
Drexel Plasma Institute  
Drexel University  
 
Gas Turbines Supervisor                                                                                  July 2001 – July 2005 
Bechtel‐Enka Joint Venture  
(Kazakhstan, The Netherlands, and Turkey)                           
 
JOURNAL 
PUBLICATIONS 
1. Application  of  nanosecond‐pulsed  dielectric  barrier  discharge  for  biomedical 
treatment  of  topographically  non‐uniform  surfaces,  H  Ayan,  D  Staack,  G  Fridman,  A 
Gutsol,  Y  Mukhin, A  Starikovskii,  A  Fridman  and  G Friedman,  J.  Phys.  D: Appl.  Phys.  42, 
(2009) 125202 
 
2. Heating  Effect  of  Dielectric  Barrier  Discharges  for  Direct  Medical  Treatment,  H.  Ayan, 
G.  Fridman,  D.  Staack,  A.F.  Gutsol,  V.N.  Vasilets,  A.A.  Fridman,  G.  Friedman,  IEEE 
Transactions on Plasma Science, 37 (2009), 1, 113‐120   
 
3. Nanosecond  Pulsed  Uniform  Dielectric  Barrier  Discharge,  H.  Ayan,  G.  Fridman,  A.F. 
Gutsol, V.N. Vasilets, A. Fridman, G. Friedman, IEEE Transactions on Plasma Science, 36 
(2008), 2, 504‐508 
 
4. Effect  of  Dielectric  Barrier  Discharge  Plasma  on  the  Attachment  and  Proliferation  of 
Osteoblasts Cultured over Poly(ε‐caprolactone) Scaffolds, Eda D. Yildirim, Halim Ayan, 
Victor  N.  Vasilets,  Alexander  Fridman,  Selcuk  Guceri,  Gary  Friedman,  Wei  Sun,    Plasma 
Process. Polym. (2008), 5(1), 58–66 
 
5. Comparison  of  Direct  and  Indirect  Effects  of  Non‐Thermal  Atmospheric  Pressure 
Plasma  on  Bacteria,  G.  Fridman,  A.D.  Brooks,  M.  Balasubramanian,  A.  Fridman,  A. 
Gutsol, V.N. Vasilets, H. Ayan, G. Friedman, Plasma Process. Polym., (2007), 4, 370‐375 
 
6. Blood  Coagulation  and  Living  Tissue  Sterilization  by  Floating‐Electrode  Dielectric 
Barrier  Discharge  in  Air,  G.  Fridman,  M.  Peddinghaus,  H.  Ayan,  A.  Fridman,  M. 
Balasubramanian,  A.  Gutsol,  A.  Brooks,  G.  Friedman,  Plasma  Chemistry  and  Plasma 
Processing, 26, 425‐442 (2006) 
 
SELECTED 
AWARDS AND 
HONORS  
• Drexel University Graduate Student Teaching Award – Winner, 2009  
• Drexel University Graduate Student Research Award – Highly Commended, 2009 
• IEEE – ICOPS Student Travel Grant, 2009 
• NSF – GRC Travel Fellowship, 2008 
• Laurence A. Baiada Center for Entrepreneurship Business Plan Competition 
Second Place, 2008 
• Laurence A. Baiada Center for Entrepreneurship Business Concept Competition  
Winner, 2008 
• NSF – NATO‐ASI Travel Fellowship, 2007 
• NSF – GRC Travel Fellowship, 2006 
• Gold Medal for Graduating Ranked 1
st
 in class ‘01, 2001 
 
 
90


 

© Copyright 2009  Halim Ayan. All Rights Reserved. 

ii

DEDICATION

To my love, my best friend, my beautiful wife; EDA

Victor Vasilets. Dr. I would especially like to express my appreciation to Robert Chang. and Dr. Finally. and friends at DPI and CATE Lab. Andrei Starikovskii. Adam Fontecchio. Young Cho. Ondrej Hovorka. Wei Sun. Gary Friedman and Dr.iii ACKNOWLEDGMENTS I would like to express my sincere and deepest gratitude to my advisors Dr. for their friendship and for delightful discussions around science. and for constantly educating me throughout my doctoral studies. I am grateful for the financial support from the Drexel Plasma Institute and the Mechanical Engineering and Mechanics Department. . Shailesh Gangoli. and Dr. Dr. Alexander Rabinovich for their helpful and constructive comments to improve this thesis. Yuri Mukhin to my work. co-workers. I would also like to thank Dr. Tanvir Farouk. I am thankful to all colleagues. Alexander Gutsol for his guidance and patience. I would also like to acknowledge the help of Dr. and David Staack. I would like to thank the members of my advisory committee including Dr. Alexander Fridman for their invaluable guidance. enduring support. Alan Lau for his advice and support over the last four years. I have been very privileged to have befriended you all. Dr. and philosophy. I would especially like to express my deep appreciation to Dr. Gregory Fridman. along with opening a whole different way of thinking and perspective into the matters. politics.

.....1 Voltage and current ..........1 Breakdown of Gas in DBD ............1 1.............................19 2.....4 Electrodes ................4......................................................1 Electrical Characterization ...............iv TABLE OF CONTENTS LIST OF FIGURES ............................................................................. vi LIST OF TABLES ...........................................................................4 1.........................................1 Planar electrode........................................1 Plasma in Medicine .................................................................2 Characterization of the Uniformity of the Plasma ..9 1..............................................................22 3.....26 ...............................................10 2....................2 Power .....................................................................................................20 CHAPTER 3: PLASMA AND DEVICE PHYSICAL CHARACTERIZATION ...............................................................................................................................9 CHAPTER 2: DESIGN OF THE NANOSECOND-PULSED DIELECTRIC BARRIER DISCHARGE DEVICE AND SYSTEM FOR BIOMEDICAL APPLICATIONS ..............................................................................................................22 3........... xi CHAPTER 1: INTRODUCTION AND BACKGROUND..............................................x ABSTRACT ....................................................................2 Dielectric Barrier Discharge Plasmas ................2 Key Facts About the Nanosecond-pulsed Dielectric Barrier Discharge System .....................14 2....................2 Test tube electrode ........22 3...............1.............................................................1 1.........................................4 Thesis Outline ....................................................................3 Power Supply .............................................................................3 Research Objectives and Approach ......19 2....4.................................................................................................................22 3..............................12 2...1................................................10 2...........................................................................................................................

.................................3......................v 3................35 3.....2 Lichtenberg figures ....................................26 3.......................3 Thermal Characterization of the Plasma ...........................46 CHAPTER 4: STERILIZATION EFFICACY...........................................................65 4.......................................................................................................................1 Optical emission spectroscopy ........................................................................46 3............................2 Qualitative Comparison of Conventional and Nanosecond-pulsed Dielectric Barrier Discharge on Topographically Non-uniform Surfaces ..........1 Side view imaging.....................89 .... BIOLOGICAL CHARACTERIZATION AND QUANTIFICATION OF NANOSECOND-PULSED DIELECTRIC BARRIER DISCHARGE ...2.....76 VITA .....72 5.....73 LIST OF REFERENCES .......35 3...............48 4........................4 On the Mechanism of Sterilization ....................48 4....................................................................2 Research Contributions .................................................3.....................71 CHAPTER 5: SUMMARY AND CONCLUSIONS ..................................................2....3 Quantitative Comparison of Conventional and Nanosecond-pulsed Dielectric Barrier Discharge on Topographically Non-uniform Surfaces ............................................................2 Surface temperature ......................1 Qualitative Demonstration of Sterilization ....................................................................................5 Summary of Key Results and Conclusions.............4 Summary of Key Results and Conclusions...........................................................................48 4...1 Summary of the Research and Conclusions...72 5........60 4................................30 3.................................................................................

..........................................3: Schematic of double spark gap configuration external circuit .....................6: Peak voltage versus main spark gap distance for several small spark gap distances (2...18 ............1: Schematic representation of a typical APC setup and APC probe with the plasma beam on the tissue (Raiser and Zenker 2006................................2: Parallel and concentric configurations of Dielectric Barrier Discharge (Kogelschatz 2003 and Kogelschatz 2004).....................................3: Schematics of DBD operation .....................17 Figure 2.........7: Oscillogram of typical voltage and current signals (Main spark gap: 12mm.............................16 Figure 2..................................15 Figure 2......5: Pulse duration (FWHH) versus small spark gap distance for several main spark gap distances (15 ..........................7 Figure 1.............................................6 Figure 1.11 Figure 2................4: Image of a typical DBD in air .. Stoffels 2007) ..7 Figure 1....................... pulse length: 23 ns (b) 10 voltage signals superimposed ...............3 Figure 1..............................................8 Figure 2..........................................27 mm). Pulse duration values are average of 10 measurements and variance is ±10% .......... Frequency values are average of 10 measurements and variance is ±10% ...............2: Avalanche-to-streamer transition and streamer propagation (Raizer 1991) ......4: Pulse frequency (repetition) versus main spark gap distance for several small spark gap distances (2.............................18 Figure 2...........1: Electron multiplication and avalanche growth (Raizer 1991) ..................... Peak voltage values are average of 10 measurements and variance is ±10% ........................ Secondary spark gap: 3 mm) .........................5 mm).....8: Superimposed voltage signals versus time (main spark gap: 15 mm and secondary spark gap: 3mm) (a) Peak voltage: 15....4.............................................................5 mm)...........5 ...........................5 .............vi LIST OF FIGURES Figure 1.....................................4...........................................................................5: Microdischarges of a conventional dielectric barrier discharge striking on the ridges of the skin (similar to lightning)......................6 kV.................................17 Figure 2.......11 Figure 2.................

....................... (b) nanosecond-pulsed DBD ................. Electrical power measurement: 5........10: Oscillograms of (a) sinusoidal and (b) microsecond-pulsed DBDs ...............36 Figure 3....7: Side view of nanosecond-pulsed DBD between test tube electrode and ground metal electrode (a) with background light and (b) in a complete dark room for the same exposure time (bottom halves of the images are due to reflection from the ground plate electrode surface) .......12: Vibrational temperatures as a function of average power density for the sinusoidal DBD and the microsecond-pulsed DBD....27 Figure 3............ (c) microsecond-pulsed DBD ..........................9: Lichtenberg figures of two different DBD systems on the emulsion of the photo films: (a) nanosecond-pulsed DBD ..........38 Figure 3.....................................11: Rotational temperature as a function of average power density for the sinusoidal DBD and the microsecond-pulsed DBD..........................3: Images of two discharges with plane-to-plane configuration: (a) Sinusoidal waveform.... Exposure time of sinusoidal DBD is 50 msec (600 cycles) and microsecond-pulsed DBD is 1 s (1000 cycles)...................39 .....................................10: Glass test tube electrode .........................................................................27 Figure 3...............9: Cylindrical electrode cross section .............................................................44 W (average of 10 measurements) ................................ (b) Microsecond-pulsed waveform ..................................4: Spectroscopic measurement setup for single filament ...... Exposure time of sinusoidal DBD is 50 msec (600 cycles) and microsecond-pulsed DBD is 1 s (1000 cycles) ..................................... (d) microsecond-pulsed DBD – color............color..............8: Schematic of experimental setup to acquire the Lichtenberg figures on photo film .........b&w.2: Experimental data and curve fitting for ΔT...vii Figure 2.29 Figure 3...............19 Figure 2.5: Locations of 21 cross sections on the images of two types of DBDs with two test tube electrodes (1 mm gap)...28 Figure 3.........1: Schematic of calorimeter setup .....28 Figure 3.....24 Figure 3.....32 Figure 3......25 Figure 3...................21 Figure 3........................34 Figure 3..............................02 ± 0.b&w....6: Contrast enhanced images of two types of DBDs with two test tube electrodes (1 mm gap)....................................................................................

..................... (b) conventional microsecond DBD and (c) nanosecond-pulsed DBD on the patterned agar surface (three steps with 0.......................................... 19........................56 Figure 4......57 ..................... brightness and contrast of the image are adjusted for clarity.......................6: Schematic of 3-level recess patterned agar .17.....43 Figure 3..........5: Inactivation with nanosecond........56 Figure 4..........................2 nm)...........17: Spectra of nanosecond-pulsed DBD for spectroscopic temperature measurement........................54 Figure 4....................................16: Spectroscopic measurement setup for DBD...33 mm height and 2 mm width)................................................................. 21) ............................. Rotational temperature: 313................ Staack et al................5 ± 7.......5 K and vibrational temperature: 3360 ± 50 K.50 Figure 4...........7: Uniform distribution of bacteria on patterned surface ................. 2006) ........................ 3.45 Figure 3....42 Figure 3.......51 Figure 4......................1: Agar with skin flora treated by nanosecond-pulsed DBD (Vmax: 20 kV................ …......7 nm – 381..................8: Side view of (a) high voltage electrode in light room with no plasma...................................... Pictures of discharges have been taken in a dark room with 0.............. circles in (a) indicate the edge of the high voltage electrode.........................................................41 Figure 3.........................45 Figure 4..........2: Patterned agar preparation .....(righthand side) pulsed DBD through metal mesh and (b) schematic of the experimental setup (schematic is not to scale................ (Model spectrum: Laux 2002......... no other modifications done) .........18: Nanosecond-pulsed DBD igniting on finger (exposure time: 1 s) ............ Repetition rate: 190 Hz) ................................3: Protocol for dilution assay ..................................40 Figure 3......49 Figure 4............14: Spatial intensity versus wavelength (372....................15: (a) Rotational and (b) Vibrational temperature distributions along the microdischarges ...........................4: Illustration of mesh on top of the agar to mimic the indentations (10 mm diameter electrode with 0...........................13: Spectra at various locations along the filament (cross sections : 1..... 5....................55 Figure 4........66 mm quartz) ......(left-hand side) and microsecond...viii Figure 3.....5 s exposure time at 120 Hz repetition (for both systems) ..................

........................... Statistics are collected by dividing the treated area into four equal sections (quarter circle area) and performing a count in each area ..67 Figure 4......17: 30 s treatment with nanosecond-pulsed DBD (a) without air flow...18: Plasma treatment through MgF2 window ......................................................ix Figure 4.15: Schematic of single recess (channel) patterned agar .................... Arrows indicate the direction of the flow........... concentration: 108 CFU/ml .. (b) with 0.............16: Diagram of the system for air flow through the channel on the agar plate ................... .......9: 3-level recessed agar surface treated with (a) nanosecond-pulsed DBD and (b) microsecond-pulsed DBD.64 Figure 4.................59 Figure 4..70 ...... (Outer and inner circles represent quartz and electrode active area......................13: CFU Log reductions on different patterns with 30 s plasma treatment Statistics are collected by dividing the treated are into four equal sections (quarter circle area) and performing a count in each area .................................................... (c) with 3 SLPM air flow on single level recessed agar.......11: Sterilization effect of two systems on valleys (dashed circles indicate the active area of the electrode) .........................................10: Four different agar patterns with different depth (dimensions in mm) ............................................................61 Figure 4.65 Figure 4..........67 Figure 4..............60 Figure 4................................... For both plates treatment time: 30 s......63 Figure 4........................................... respectively) .......12: Flow chart for determining the log reduction in bacteria population after plasma treatment on patterned agar ................. Width of each step (distance between the horizontal lines) is approximately 2 mm...............69 Figure 4..............3 SLPM air flow......................78 mm) as a function of plasma treatment time...............14: CFU log reduction on Type 2 pattern (max depth: 0.......................................................

x LIST OF TABLES

Table 2.1: Typical microdischarge parameters in a 1-mm gap in atmospheric-pressure air (Fridman et al. 2005, Kogelschatz 2007)................................................................12 Table 2.2: Summary of nanosecond-pulsed DBD parameters .....................................14 Table 3.1 Comparison between calorimetric and electrical power measurements ......26 Table 3.2: Size of the filament versus voltage rise rates for different dielectric barrier discharge systems.........................................................................................................30 Table 4.1: Summary of nanosecond- and microsecond-pulsed DBD parameters .......52

xi Abstract Uniform Dielectric Barrier Discharge with Nanosecond Pulse Excitation for Biomedical Applications Halim Ayan Advisors: Dr. Gary Friedman and Dr. Alexander Fridman

For some period of time the use of plasma in medicine has been limited to thermal discharges for cauterization and dissection. The effects of thermal plasma on tissue are entirely related to local heating. Non-thermal plasma, on the other hand, can have many different modes of interaction with tissue. It has been recently demonstrated that direct treatment of smooth surfaces by non-thermal dielectric barrier discharge (DBD) in air is highly effective in killing pathogens. Moreover, DBD can create different sub-lethal and selective effects. These results hold significant promise for medical applications such as sterilization of wound surfaces. However, a typical DBD in air can be highly non-uniform, particularly on topographically non-uniform surfaces such as in most living tissues. This creates significant limitations for use of DBDs in wound care and other biomedical applications. In this thesis, a novel non-thermal plasma system, namely nanosecondpulsed DBD, has been developed and investigated to address this important limitation. Nanosecond-pulsed DBD is shown to be uniform in air at atmospheric pressure and much more effective in killing bacteria than conventional DBDs, particularly on topographically non-uniform surfaces. Thus, this new plasma system is potentially convenient for in vivo and hospital sterilization cases.

xii

and removal which also causes local heating and burns due to elevated temperatures (Raiser and Zenker 2006) (Figure 1. In non-equilibrium plasmas. can have many different modes of interaction where various plasma species can generate different sub-lethal and selective effects (Fridman et al. 2008. Plasma has been used for electro-surgery where it desiccates tissue by passing electrical current through it (Pollack et al. Shekhter et al. 2004). Coulombe et al. on the other hand. 1998) and bronchological endoscopy (Reichle et al. gynecology. resulting in enriched gas phase chemistry without high temperature input through collisions and consecutive dissociation. 2005.1 CHAPTER 1: INTRODUCTION AND BACKGROUND 1. 1998). 2005). Sumiyama et al. tissue devitalization. . 2006. and Watson et al. Stoffels 2007. 2000. Some of the surgical applications of the argon plasma coagulator are visceral surgery. the aforementioned thermal plasma interacts with living tissue mainly through temperature and heat. However. 2006. breast surgery (Ridings et el. electron energies are much higher than the heavy particle (ions and neutral species) energies. Lord et al. 2000).1). gastroenterology (Ginsberg et al. Polousky et al. 2000). Non-thermal plasma. urology. skin surgery (Brand et al. brain tumor surgery (Tirakotai et al. 2000. Gostev 2008) as demonstrated in recent studies.1 Plasma in Medicine For some period of time the use of plasma in medicine has been limited to thermal discharges for cauterization and dissection (Vargo 2004. The argon plasma coagulator (APC) is another early application of plasma for cauterization. Stalder et al. 1991. 2002).

Stoffels et al. 2008. Non-thermal treatment is possible with thermal plasma if its afterglow is transported and cooled (Shimizu et al. 2007). 2006). 2008). Yildirim et al. on the other hand. 2008. 3) enhanced cell functions including attachment and proliferation. 2008. Although this makes it possible to work with living tissue and heat-sensitive surfaces (Weltmann et al. cells. Penetrante 1996).2 excitation. and biomaterials (Laroussi 2009. such as Dielectric Barrier Discharge (DBD). 2006. Yonson et al. and 5) wound healing (Stoffels 2006. and ionization processes (Kunhardt 2000. and Kalghatgi et al. 2) accelerated blood coagulation. are very attractive because of their non-thermal nature. Puac et al. and Goree et al. They create new possibilities in biological and medical fields where substances of interest are mostly heat-sensitive such as living tissue. 4) treatment of malignant tissue. Some of the recent research subjects of non-thermal plasma applications are 1) inactivation of bacteria on living tissue. Systems that employ afterglow from non-thermal plasma for medical treatment and disinfection have been proposed and demonstrated within the last decade (Sladek and Stoffels 2005. Foest et al. Nonequilibrium plasmas. can generate and bring charges and short living active species directly to its surface. such treatment takes a relatively long time and can’t employ many short-living active plasma species and charges. Direct plasma created right on the tissue. 2007). . 2006).

Montie et al. oxygen is required to be part of the gas composition to generate the . atomic oxygen. Laroussi et al. 2000. Birmingham and Hammerstrom 2000.3 Figure 1. Some of the highly active oxygen-containing species are ozone. DBD generates several active species that are quite essential for sterilization and other important biomedical processes. Stoffels 2007) Within the past few years it has been revealed that direct treatment of smooth surfaces and living tissues by non-thermal Dielectric Barrier Discharge (DBD) in air is highly effective in killing pathogens including bacteria and fungi (Fridman 2008a. electronically excited oxygen.1: Schematic representation of a typical APC setup and APC probe with the plasma beam on the tissue (Raiser and Zenker 2006. 2002). and peroxide. In general.

2006). ion) temperatures. Williamson et al. 2006). Several interesting medical possibilities have been demonstrated by Fridman et al. In addition. It has been demonstrated recently that contact of living tissue with charges from non-thermal atmospheric pressure plasma is the main reason for the observed effects (Fridman et al. light sources (excimer UV sources) (Motret et al. DBDs enable various emerging novel applications in biology and the medical field (Laroussi et al. SOx. and ions) with low gas heating (Wagner et al. DBDs are often applied at atmospheric pressure and in air. metastables. and many other technologies (Fridman et al. 2002). VOC). 2007 and Deng et al. 2006) and is much more effective for sterilization compared to UV (ultraviolet) or long-living species such as ozone in the plasma afterglow. 2003. ozone production. 2003).4 aforementioned active species and consequently for effective sterilization (Fridman 2008b). thin film deposition (Salge 1996. 2000). Massines et al. industrial processes of polymer films or fibers to increase wettability and adhesion (Borcia et al. There are usually two electrode configurations that have been employed for most of applications: 1) . in the past few years (Fridman et al. 1998). 2005). 1. 2000 and Stoffels et al. They produce several chemically active species (electrons.2 Dielectric Barrier Discharge Plasmas Dielectric Barrier Discharges (DBDs) are significant among all types of nonthermal plasmas because of their relative simplicity. Because of these characteristics. DBDs are widely used in gas cleaning (from NOx. DBDs offer a unique combination of non-equilibrium and quasi-continuous behavior having high electron mean energy with lower heavy particle (neutral. radicals.

avoiding the formation of an arc. when high voltage is applied between two electrodes that are without insulation. 1988. the applied voltage needs to change over time allowing the charges accumulating on the insulator surfaces to be removed. 2000. air) results in a multistreamer mode of operation with formation of microdischarges (Kogelschatz 2003) and subsequent filaments that are visible to the human eye (Figure 1. .g. in most cases. Rahel et al. Gherardi et al. In order to sustain the DBD plasma. Miralai et al. The filaments typically have a diameter on the order of 100 μm (Fridman et al. 1990. In general. transient non-thermal plasma is generated in the gap. it has been demonstrated that DBD can be ignited in the form of homogenous plasma at atmospheric pressure in certain gas mixtures. DBD (particularly in oxygen-containing gases. Kogelschatz 2002) for discharge gaps that are few millimeters long. Massines and Gouda 1998.4). Operating principals of DBD are summarized with schematics shown in Figure 1.3 (a through d). pure nitrogen. e. Although.5 parallel and 2) concentric configurations (Figure 1. 2000. an arc (high temperature plasma channel) develops given sufficient time (as short as few milliseconds).2). If the applied high voltage remains constant. Yokoyama et al. 2007). Instead. A dielectric barrier layer placed in front of at least one of the electrodes (Gibalov and Pietsch 2000) limits the current. charge from plasma accumulates on the dielectric surface and reduces the effective field in the discharge gap extinguishing the discharge (Xu and Kushner 1998). and some noble gases (Kanazawa et al. 2005.

these microdischarges can be considered as the only active locations of the whole DBD volume.6 Figure 1. . This temperature non-uniformity can be very important. local temperature around the microdischarge filaments can be relatively high. where all of the energy dissipates.2: Parallel and concentric configurations of Dielectric Barrier Discharge (Kogelschatz 2003 and Kogelschatz 2004) As plasma density in the microdischarges is much higher than in the surrounding space. although average temperature in the discharge volume is small. Therefore. particularly when the microdischarges in DBD remain in the same position for relatively long periods of time.

7 Figure 1.3: Schematics of DBD operation Figure 1.4: Image of a typical DBD in air .

is to circumvent formation of discharge filaments in DBD and make the discharge more uniform even on relatively non-uniform surfaces. like the surfaces of living tissues (Figure 1. which may compromise effective treatment. therefore.5). Figure 1.5: Microdischarges of a conventional dielectric barrier discharge striking on the ridges of the skin (similar to lightning) .8 Pinning of the microdischarges is more likely to occur on ridges of nonuniform surfaces. The primary goal of the work reported here.

living tissue. and to reduce the sensitivity to topographical non-uniformities of the surface being treated. Chapter 5 summarizes the contributions.3 Research Objectives and Approach This thesis rests on the hypothesis that ultra fast rising external voltage enables generation of uniform plasma that will be effective and convenient for treatment of non-uniform surfaces. Chapter 3 focuses on the thermal. 1. The objective of the research is to retain the direct nature of the DBD plasma treatment. The scope this research is 1) to develop and investigate non-thermal uniform DBD plasma system. research . electrical.4 Thesis Outline Chapter 2 explains the design of the nanosecond-pulsed dielectric barrier discharge device and system for biomedical applications.g. and 2) to demonstrate and assess its efficiency in applications requiring sterilization in air at atmospheric pressure.9 1. spectroscopic and uniformity characterization of the novel nanosecond-pulsed system. Chapter 4 examines the sterilization effect of the nanosecond-pulsed DBD plasma and presents a comparison between it and conventional DBD. Chapter 2 also presents the details about the power supply circuit and the high voltage electrodes. The chapter starts with the explanation of gas breakdown phenomenon in Dielectric Barrier Discharge and the key facts of the nanosecond-pulsed dielectric barrier discharge system. e. Finally.

it is possible for the field due to the space charge to reach a critical level wherein it becomes comparable to the external field. not all of them get a chance to develop equally. α.2. During this phase.1). This process is governed by the Townsend ionization coefficient. This is due to the fact that. However. Multiple avalanches are formed and grow. Loeb 1960. This is known as the Meek criterion. many avalanches start. If the external field grows slower than the non-uniform electric field due to the space charge.10 CHAPTER 2: DESIGN OF THE NANOSECOND-PULSED DIELECTRIC BARRIER DISCHARGE DEVICE AND SYSTEM FOR BIOMEDICAL APPLICATIONS 2. E/n (where E is the electric field and n is the gas density). which is a function of the reduced electric field. Electron impact ionization dominates during the first phase of the breakdown (Meek and Craggs 1978.1 Breakdown of Gas in DBD It is important to revisit the breakdown mechanism of gas to understand the operation of conventional DBD. usually the charge density in the discharge gap grows non-uniformly. This effect is illustrated in Figure 2. This results in non-uniform growth of the electric field. When high voltage is first applied to the discharge gap. 2004). One of the effects of the high local electric field is that it opposes the external field in some regions suppressing development of avalanches there and enhancing ionization in other places. free electrons gain energy and ionize the background gas by knocking out new (secondary) electrons from heavy particles as they drift to the anode. other become ‘losers’. In fact. in the avalanche growth phase (Figure 2. and Bogdanov et al. the field of . Some avalanches end up being ‘winners’.

2. Figure 2. in conjunction with the ionizing effects of photons (photoionization). it creates a secondary fast ionization wave called a streamer (Nikandrov et al. The front of this secondary ionization wave actually propagates in the opposite direction.1: Electron multiplication and avalanche growth (Raizer 1991) Figure 2. 2008. and Gouda and Massines 1999).2: Avalanche-to-streamer transition and streamer propagation (Raizer 1991) .11 the winning avalanches can be s strong that. Typical avalancheto-streamer transition and streamer propagation are presented in Figure 2.

Table 2.2 Key Facts About the Nanosecond-pulsed Dielectric Barrier Discharge System Uniformity of the plasma could be improved in two ways: 1) increasing uniform pre-ionization of the gas to initiate more avalanches or 2) shortening the voltage rise time (Starikovskaia et al.1 – 1 kAcm-2 1 – 10 eV E/n = (1-2)(E/n)Paschen ~ average. Kogelschatz 2007) Lifetime Peak current Electron density Total transported charge Total dissipated energy Overheating 1-20 (100) ns 0. 2005.1. 2001. the residual negative charges from the previous half-cycle contribute to the formation of new avalanches and streamers at (or the vicinity of) the same spot. Typical microdischarge parameters in a 1 mm gap in atmospheric-pressure air are presented in Table 2. Qi et al.12 When a streamer bridges the gap it forms a channel of weakly ionized plasma.1: Typical microdischarge parameters in a 1-mm gap in atmospheric-pressure air (Fridman et al. 2006) to avoid growth of highly inhomogeneous electric field that promotes growth of some avalanches at the expense . ~ 300 K 2. Eventually when the voltage polarity reverses. The outcome of the entire process from first electrons to the streamer formation is called microdischarge.1 – 1 nC 5 µJ 5K Filament radius Current density Electron energy Reduced electric field Gas temperature 50 – 100 µm 0.1 A 1014–1015 cm-3 0.

the reduced electric field (E/n) is found to be ~ 5. A fast rising driving voltage can also shift electron energy distribution function to higher values (Gallagher et al. the time required for an avalanche to travel the inter-electrode distance is ~ 10-8 sec = 10 ns.13 of others. If the number of primary avalanches is high enough before the accumulation of the critical space charge. the criterion of the uniform discharge development could be formulated with a simple relation: τrise < d / νd where τrise represents the excitation pulse rise time. Roughly. Summary of the parameters is given in Table 2. In addition. From this.3 x 10-15 V. Let us also take the maximum applied voltage. for the DBD to be 16 kV. the discharge is likely to remain uniform even if streamers do occur. on average. Let us suppose that the discharge gap is about 1 mm. This time is the characteristic time of build-up of possible local non-uniformities in the electric field within the discharge gap and. 2008). 1983). 1998). therefore. The above estimate is consistent with other estimates of dV/dt > 1 kV/ns (Raupassov et al. and νd the electron’s drift velocity in the critical electric field (Zatsepin et al. Accordingly. Tens of nanoseconds is considerably (at . the drift velocity (νd) for an electron in air is ~ 10-7 cm/sec (tabulated value from Dutton 1975). Vmax. it is the goal of the proposed nanosecond-pulsed DBD to achieve this rise time. the shape of the electrodes does not affect the location of the avalanches and streamers making the discharge more independent of the topography.cm2 and.2. The resulting discharge will resemble ‘pulsed avalanche’ regime (Levatter and Lin 1980). d the discharge gap length. under these conditions.

2008).2: Summary of nanosecond-pulsed DBD parameters Discharge Gap [mm] Voltage [kV] Reduced Electric Field (E/n) [ V. .3 Power Supply A novel non-thermal nanosecond-pulsed DBD has been developed to generate uniform plasma in air at atmospheric pressure. 2007).3 x 10-15 10-7 10 2. The circuit with a double spark gap configuration is shown in Figure 2.14 least 2 orders of magnitude) shorter than rise time of microsecond-pulsed DBDs which have been noted to be non-uniform. 2001 and Zhukov et al. a relatively simple double spark gap circuit has been built for the generation of pulses with durations on the order of tens of nanoseconds (Ayan et al.cm2] Drift Velocity (νd) [cm/s] Time to Bridge the Gap [ns] ns-DBD 1 16 5. Table 2. The pulse generating circuit has been employed along with a current source to obtain short duration high voltage pulses. Rather than using expensive and often unreliable semiconductor devices for creating nanosecond pulses (Miles et al.3.

3: Schematic of double spark gap configuration external circuit The circuit produces repetitive short pulses. Voltage pulse starts when the main spark gap is triggered. resulting in a rapid decay of the voltage across the DBD electrodes. charge initially stored in the main capacitor is transferred to the discharge as the voltage across the plasma electrodes rises precipitously. The size of the main spark gap determines the voltage that appears across the discharge electrodes after the spark breakdown. The frequency of voltage pulses is determined by the current source. . The secondary spark gap affects mainly the length of the voltage pulse that is maintained across the DBD electrodes. main capacitor (how fast is the capacitor charged) and is also affected by the peak voltage. rise time of the voltage is independent of spark gaps. When the larger primary (main) spark gap breaks down.15 Figure 2. The smaller (secondary) spark gap starts to charge and eventually shorts out the DBD. In the first approximation.

Frequency values are average of 10 measurements and variance is ±10% . The pulse frequency (repetition) as a function of main spark gap distance is presented in Figure 2. Pulse duration is linearly dependent on secondary spark gap length (Figure 2. Peak voltage across the DBD is linearly dependant on the main spark gap distance with approximately 1 kV per 1 mm for the above mentioned range (Figure 2.5 mm).5 to 4. As the main gap increases from 10 to 27 mm. respectively.4.5).6).5 mm gap distances. 300 250 Frequency [Hz] 200 150 100 50 0 15 18 21 24 27 2.4: Pulse frequency (repetition) versus main spark gap distance for several small spark gap distances (2. peak voltage increases approximately from 10 kV to 27 kV. Additionally.5 and 4.5 mm 3 mm 3.16 The main spark gap was varied from 15 to 24 mm with at 3 mm intervals.5 mm  4 mm 4. respectively (for various sizes of secondary spark gaps between 2. both a single and 10consecutive (superimposed) voltage signals are presented in Figure 2. and repetition rates were measured between 250 and 100 Hz.5 mm).5 mm Main Spark Gap [mm] Figure 2. The rise time of approximately 3 kV/ns is obtained on the front of the voltage pulse. A typical oscillogram of nanosecond-pulsed DBD with ultrafast high voltage pulse is given in Figure 2.4.8.5 .7. pulse durations are approximately 15 and 30 ns. For 2.

5: Pulse duration (FWHH) versus small spark gap distance for several main spark gap distances (15 .4.5 mm).27 mm).5 .5 mm 15 10 5 0 15 18 21 24 27 3 mm 3. Peak voltage values are average of 10 measurements and variance is ±10% .5 4 4. Pulse duration values are average of 10 measurements and variance is ±10% 30 25 Peak Voltage [kV] 20 2.5 15 mm 18 mm 21 mm 24 mm 27 mm Small Spark Gap [mm] Figure 2.5 mm 4 mm 4.5 3 3.17 35 30 Pulse Duration [ns] 25 20 15 10 5 0 2.6: Peak voltage versus main spark gap distance for several small spark gap distances (2.5 mm Main Spark Gap [mm] Figure 2.

8: Superimposed voltage signals versus time (main spark gap: 15 mm and secondary spark gap: 3mm) (a) Peak voltage: 15. Secondary spark gap: 3 mm) Figure 2.18 Figure 2.6 kV.7: Oscillogram of typical voltage and current signals (Main spark gap: 12mm. pulse length: 23 ns (b) 10 voltage signals superimposed .

OH) as a dielectric barrier. 2. The first configuration is plane-to-plane with flat surface electrode.1 Planar electrode In the first configuration (plane-to-plane) the powered electrode is made out of cylindrical copper and enclosed in Polyetherimide (Ultem®) for insulation (Figure2. In all cases. This configuration was employed for characterization and sterilization experiments using with various power densities.9: Cylindrical electrode cross section . Figure 2.9). Painesville.19 2. and the second configuration is sphere-to-plane with spherical electrode.4 Electrodes Two electrodes are required in order to generate DBD: one electrode is powered with high voltage and the other is grounded.4. the grounded electrode is either flat metal or agar. The flat surface of the copper cylinder is covered with clear fused quartz (Technical Glass Products. There are two electrode configurations with two different types of high voltage electrodes (powered) used.

# 60825-902. The smaller size electrode cylindrical copper is 10 mm in diameter and covered by 0. this test tube electrode was positioned to be in contact near its tip with the grounded plane metal electrode. The thickness of the glass of the test tube is approximately 0. CA) with a conductive silver paste (SPI West Chester. PA) filling inside. VWR Scientific. It should be noted that in some cases. . The larger size cylindrical copper has 25 mm diameter and the thickness of the clear fused quartz is 1 mm.75 mm with a radius of curvature of 5 mm.66 mm thick quartz.4. the high voltage electrode (Figure 2.20 The flat surface electrode is made in two sizes for several different experiments.10) consists of a borosilicate glass (Pyrex®) test tube (cat. 2.2 Test tube electrode In the second configuration (sphere-to-plane). San Francisco.

10: Glass test tube electrode .21 Figure 2.

TX). 110 MHz. Tektronix.1. 45 MHz bandwidth) around the high voltage electrode wire.1 V/Amp. AZ) connected in parallel with the discharge and a high frequency current transformer (#CM-10-L.1.2 Power Current signal of a typical DBD has many spikes in the oscillograms and they are associated with individual microdischarges. These current spikes are characteristically very short in duration and questions arise regarding the validity of using the measured current to calculate the discharge power (Ayan et al. TDS5052B Digital Phosphor Oscilloscope. The probe signals were acquired and recorded using a high speed oscilloscope (500 MHz bandwidth. Recorded data was processed using customized MATLAB code which integrates the instantaneous power (V∗I) over many cycles to determine an average energy per cycle and average power. 0. The bandwidth of the current probe and the inverse of the microdischarge duration are . North Star High Voltage. Inc. 3.. Marana.1 Electrical Characterization Voltage and current Electrical measurements have been conducted by using a high frequency high voltage probe (#PVM-4. Ion Physics Corporation. 1000:1.22 CHAPTER 3: PLASMA AND DEVICE PHYSICAL CHARACTERIZATION 3.3. Richardson. Electrical schematics with voltage and current probes at positions have been shown previously in Figure 2.1 3. 2009a). 5 Gsample/s. Power dissipation in the discharge was analyzed by measuring instantaneous current and voltage in the gap.

TX). Palmer Instruments. When the plasma ignites. Calorimeter is composed of a peristaltic pump (model # 3386. The system is insulated to ensure that the only heat loss is attributed to the flowing water.1). the electrical measurements for average power were verified with custom made calorimetric setup (Figure 3. water specific heat capacity. -1 . Water is pumped at a controllable flow rate through the copper tube that surrounds the chamber and encloses the DBD electrodes. two mercury thermometers (model # 112C. Inc. and a constant water temperature difference between inlet and outlet: ∆ .51˚C. 1/10˚C div. Control Company.. For this reason.. the heat transferred from the discharge (thus the average power dissipation in the discharge gap) can be calculated by using flow rate.23 comparable. it took typically more than 100 minutes to reach the steady-state conditions in most cases. A second thermometer is located downstream from the chamber to measure the outlet temperature of the water. After reaching the steady state. One thermometer is placed upstream to the chamber to measure the inlet temperature of the water. Since the heat transfer to the water is a rather slow process. and some loss of information about the actual discharge current may occur. a copper chamber and an insulation casing. NC). The insulation is minimum 10 cm thick around the system. dissipated energy in the chamber is taken away by copper chamber and copper tube surrounding the chamber and transferred to the running water. Temperature measurements from both thermometers are recorded every minute throughout the experiments.

Cp is the specific heat capacity of water.24 where is heat. a curve with double exponential term is fit to the experimental data to ensure that the converged value is accurate.1: Schematic of calorimeter setup Additionally. is the mass flow rate. and ΔT is the temperature difference between inlet and outlet ports. Figure 3. The double exponential term curve is as follows: ∆ 1 1 .

5 2 1. c3.2. c2. Calorimetric measurement 4.2: Experimental data and curve fitting for ΔT.5 4 3.5 1 0.44 W (average of 10 measurements) . and c1. It is found that the electrical and calorimetric power measurements agree to within less than 10% indicating that the bandwidth of the current transformer is at least sufficient for these measurements (Table 2. Fit Time [min] Figure 3.998365 Exp.5 Δ Temperature [C] 3 2.06 C R2: 0.1). Electrical power measurement: 5.02 ± 0. and c5 are arbitrary coefficients.25 Here t is time. c4.5 0 0 50 100 150 200 250 ΔT(t∞) = 4. A sample set of data with curve fitting is given in Figure 3.

Figures 3. In order to facilitate spatially resolved measurements. Side view images of two conventional type DBDs with plane-to-plane configuration are given in Figure 3. a few other DBD systems are also assessed visually for uniformity analysis.°C] ΔT (fit) [°C] Value 16.55 4. Initially.26 Table 3.3 with 25 mm diameter active area.1 Characterization of the Uniformity of the Plasma Side view imaging Along with nanosecond-pulsed DBD.2.0613 4. Detailed short time exposure images of filaments are captured with a CCD camera on the spectrometer (Figure 3. filaments are clearly visible for both types in the 1 mm discharge gap between the high voltage electrode (top) and the grounded electrode (bottom). the plasma image is magnified approximately five times.1855 4.5 and 3. side view pictures of discharges are taken by a digital camera (Nikon D70).2 3. In Figure 3.02 % 6.1 Comparison between calorimetric and electrical power measurements Parameter [unit] Flow [ml/min] Specific heat capacity (@ 25 °C) [J/g. A concave mirror with 5 cm focal length is used to focus the light emitted from the plasma onto the slit of the spectrometer.6 illustrate the real and contrast enhanced images of the filaments (microdischarges) of conventional .689 5.3.6 Power (calorimetry) [W] Power (electrical) [W] Difference 3.4).

2001. Figure 3.4: Spectroscopic measurement setup for single filament . In this electrode configuration (Kozlov et al. (b) Microsecond-pulsed waveform Figure 3. Arrows on Figure 3.6 images are contrast enhanced for clarity).3: Images of two discharges with plane-to-plane configuration: (a) Sinusoidal waveform. Kozlov and Wagner 2007). the filaments are localize at the opposing tips of the electrodes and do not laterally wander as they would in the case of planar electrodes.6 identify the location of the electrodes (Figure 3.5 will be explained in the next chapter).27 discharges created between two test tube electrodes (cross section lines on Figure 3.

Exposure time of sinusoidal DBD is 50 msec (600 cycles) and microsecond-pulsed DBD is 1 s (1000 cycles) .28 Figure 3. Exposure time of sinusoidal DBD is 50 msec (600 cycles) and microsecond-pulsed DBD is 1 s (1000 cycles) Figure 3.5: Locations of 21 cross sections on the images of two types of DBDs with two test tube electrodes (1 mm gap).6: Contrast enhanced images of two types of DBDs with two test tube electrodes (1 mm gap).

it can be seen in Figure 3. repetition rate is approximately 190 Hz and exposure time of the photography is 0.. i. nanosecond-pulsed DBD with glass test tube electrode is shown in Figure 3.2 provides a comparison of the size of the filament and voltage rise rates for different dielectric barrier discharge systems.7.7b is taken in a dark room. Figure 3. Figure 3.29 On the other hand.7: Side view of nanosecond-pulsed DBD between test tube electrode and ground metal electrode (a) with background light and (b) in a complete dark room for the same exposure time (bottom halves of the images are due to reflection from the ground plate electrode surface) . Table 3.e.62 s.7(a-b) that plasma is spread all over the spherical tip of the electrode.7a is taken in the presence of background light and Figure 3. Nevertheless. Both images are taken under the same conditions. This discharge typically appears dim.

3. whereas despite the constant 1 mm gap.5 V/ns 20 V/ns 3000 V/ns (3kV/ns) Filament size ~ 0. Here. On the other hand. 3.3 the inter-electrode distance is a constant 1 mm in the entire plasma gap. 3. it should be highlighted that in Figure 3.6 Fig.6 Fig 3.30 Table 3. conventional discharges exhibit a filamentary non-uniform structure. a new experimental setup is designed and built for qualitative yet more rigorous uniformity analysis.2 Lichtenberg figures Although long exposure imaging is helpful to demonstrate distinction between nanosecond-pulsed DBD and the conventional DBDs. Qualitative .18 mm ~ 0. Despite the large gap range. nanosecond-pulsed DBD presents a uniform glow-like appearance.1 mm Remarks Fig.7 & Fig.9 Side view images of the nanosecond-pulsed DBD show that it is “filamentfree” and much more uniform than the conventional DBDs (microsecond-pulsed and sinusoidal).7 that the plasma gap varies from 0 mm to approximately 4 mm for nanosecond-pulsed DBD with a test tube electrode.2: Size of the filament versus voltage rise rates for different dielectric barrier discharge systems Plasma system Sinusoidal Microsecondpulsed Nanosecondpulsed Voltage rise 0. it can be seen in Figure 3. 3.2.

i.e. microdischarges create a "branching" form as soon as they strike on the surface. The experiment is carried out in a dark room.31 uniformity measurements of the various discharges have previously been done by simply exposing a commercial photo film to the plasma. Microsecond-pulsed DBD is operated . voltage rise and pulse duration are approximately 3 kV/ns and 20 ns. Lichtenberg figures of the nanosecond-pulsed DBD are compared with those of a conventional discharge. A schematic of the setup is presented in Figure 3. In the case of nanosecond-pulsed DBD. charge patterns are obtained for 10 kV peak voltage pulses with a maximum 10 kV/μs rise with 2-5μs pulse width. microsecond-pulsed DBD. If conventional plasma is generated on a dielectric surface. and they are referred to as Lichtenberg figures (Chirokov et al. Lichtenberg figures are developed on black & white and color photo films. where pulses of DBD plasma were being ignited. ISO100 and ISO3200. Images on the photo film provide information about the size and the number of the microdischarges. The speed of the photo film is selected so that Lichtenberg figures of each single pulse (cycle) of DBDs plasma could be resolved. Thus. To analyze the distinction in uniformity more profoundly.e. 2004). For microsecond-pulsed DBD.8. A roll-to-roll setup driven by an electric motor is engaged to advance the photo film with a rate of about 1 m/s. Optical emission from the plasma can be registered if the surface is a photo film. The photo film is placed between the insulated test tube electrode and the grounded metal electrode. both voltage rise and pulse duration are at least two orders of magnitude longer for the microsecond-pulsed DBD compared to its nanosecond DBD counterpart. Black & white photo films possess two different sensitivities. respectively. i.

Figure 3. Lichtenberg figures show significant differences between the two discharges. Rays-type . Both plasma systems are operated with the same test tube electrode. its lowest repetition rate.9a. in order to facilitate capture of consecutive pulses. The nanosecond-pulsed discharge displays a round pattern that is approximately equivalent in size to the diameter of the high voltage electrode without any bright spot or irregular pattern distribution.32 at a 120 Hz repetition rate. The contact point of the electrode appears as a dark point at the center of Figure 3.9. The photo film is situated between the grounded plane metal electrode and the test tube electrode near its tip.8: Schematic of experimental setup to acquire the Lichtenberg figures on photo film As evident from the Figure 3.

9(c-d) clearly shows the filamentary structure (microdischarges) when used with the same electrode under the same conditions. It is worth noting that 0 – 4 mm inter-electrode gap range is due to the curvature of the glass covered high voltage electrode as it is in contact near its tip with the grounded plane metal electrode.9(a-b) also verifies that nanosecond-pulsed DBD ignites uniformly over a relatively large range of electrode gap distances (0 . On the other hand. Figure 3. discharge patterns of microsecond-pulsed DBD in Figure 3.4 mm). .33 pattern at the edge of the spot appears likely due to the secondary surface discharge being driven by the lateral component of electric field.

(b) nanosecond-pulsed DBD . (c) microsecond-pulsed DBD .color. (d) microsecond-pulsed DBD .b&w.9: Lichtenberg figures of two different DBD systems on the emulsion of the photo films: (a) nanosecond-pulsed DBD .color .34 Figure 3.b&w.

5 to 5 μs pulse width at the half maximum of the voltage pulse. 2003.3.35 3. Typical waveforms of two power supplies are given in Figure 3. and Staack et al.4 nm and 380. 2006.10 where peak-to-peak voltage is 17 kV for sinusoidal and 18 kV for microsecond-pulsed systems.10) reflect a characteristic non-uniform DBD discharge. Multiple current peaks in the oscillograms (Figure 3. Packan et al.4 nm vibrational lines and rotational structure at this region of the second positive system of molecular nitrogen. two conventional non-uniform DBD systems are characterized.3 3. N2 (C3Π-B3Π).1 Thermal Characterization of the Plasma Optical emission spectroscopy Optical emission spectroscopy (OES) is employed to measure the vibrational and rotational temperatures of the DBDs in the plasma volume using 375. 2007). The features of the two power supplies that have been employed to generate plasma are as follows: 1) Microsecond-pulsed DBD system can generate up to 35 kV peak-to-peak voltage with 120 Hz to 1 kHz repetition rate. 2) Sinusoidal DBD system can generate up to 35 kV peak-to-peak voltage with 12 kHz frequency. The experimental spectrum is compared to the simulated spectrum with Tvib and Trot determined by the best fit (minimum RMSE) between the modeled and experimental spectrum detailed in the literature (Yalin et al. Prior to the investigation of nanosecond-pulsed DBD. 2002. . Staack et al. in order to set a benchmark for the rest of the study. Laux et al. and 1. 2003.

36 Figure 3. For DBD plasmas.10: Oscillograms of (a) sinusoidal and (b) microsecond-pulsed DBDs Optical emission spectroscopy show that the rotational temperatures are between 340 and 400 K for both types of DBD. rotational .

although sterilization effects may be different . there can be 2 different temperatures defined for conventional DBDs: 1) temperature of the microdischarges (maximum temperature) and 2) average temperature of discharge gap (taking the entire gap into account).11 shows a near linear increase in rotational (gas) temperature with average power density. This demonstrates that the power-temperature relation is largely independent of voltage waveform shape for the power range studied here. The rotational and vibrational temperatures of the two conventional DBDs are measured at different power levels. OES measures the maximum temperature. Since rotational temperature (gas temperature) has been obtained via spectroscopy. As might be expected. and the lifetime of the upper state of N2 is very short (Chelouah et al. it means that the collected light and measured temperature correspond to the plasma state during the time of the microdischarge. To be more precise. Moreover. one important point should be clarified. Figure 3. Thus.12 are the averages of 3 measurements under the same conditions and the error bars shown representing the deviation of those three measurements.11 & 3. 2001. namely temperature of the microdischarge. 1994) compared to the shortest voltage pulse duration (microsecond-pulsed DBD). the two distinct type of voltage waveforms seem to fit to the same slope (although no overlap is seen within their respective operating ranges due to power supply limitations). Given in Figure 3.37 temperature is essentially equal to the translational (gas) temperature (Nozaki et al. Power densities are calculated based on the power input and the size of the active area of the electrode. 2002). Here. Nozaki et al.

and therefore all values can be considered to be roughly the same (3300 – 3400 K).. Figure 3. In Figure 3. Nonetheless. vibrational temperatures are plotted for different average power densities. it appears that gas temperature depends only on average power. it looks like there exists a trend of a decrement in vibrational temperature as the power increases. i. a slight increase in vibrational temperature accompanying a decrease rotational temperature has been observed before and is not unexpected as the rates of vibrational to translational energy transfer decrease with decreasing translational temperature (Staack et al.12.11: Rotational temperature as a function of average power density for the sinusoidal DBD and the microsecond-pulsed DBD . this is not really clear because of the relatively low sensitivity of the calculation method for the vibrational temperature. dependant on several physical and chemical factors. 2006).e. Even though.38 for different discharges.

.12: Vibrational temperatures as a function of average power density for the sinusoidal DBD and the microsecond-pulsed DBD In addition to the volume discharge temperatures. Spectra at each cross section have been acquired simultaneously and temperature calculations have been conducted on each spectrum for different locations (of the axial position).5. A sample of set of spectra at various locations along the filament is presented in Figure 3. spatial temperature distribution along a single filament has also been measured in order to investigate the effect of energy dissipation in the volume onto near-surface locations. A double glass test tube electrode configuration with a 1 mm distance between electrodes is used to obtain a single filament. Temperatures for the two different types of DBD filaments have been measured over 20 equally divided intervals (at 21 cross sections) along the axial direction of single filaments shown in Figure 3.13 (discrete).39 Figure 3.

40 Also Figure 3. 19. 21) . This may be due to the fact that the volumetric ‘memory’ effect (Eliasson et al. 1987) is stronger for sinusoidal DBD which has a much higher current pulsing frequency. …. 5. Figure 3. The radial thickness of the microsecond-pulsed DBD is clearly seen to be thinner than that of the sinusoidal DBD. 3.17. and therefore each streamer has better marked “road” that is formed by the diffuse decay of the previous streamer.13: Spectra at various locations along the filament (cross sections : 1.14 illustrates spatial intensity for the wavelength range of interest (continuous).

roughly doubling for both types of discharges. a slight increase in the light intensity at the electrodes might be due to inevitable reflection from the glass test tube surfaces. emission intensity (for the region of interest of the spectrum) from the single filament is minimal in the middle and increases towards the electrode surfaces.15. Along the central axis. . as seen in Figure 3. Also.14: Spatial intensity versus wavelength (372.7 nm – 381. However.41 Figure 3. In summary. Rotational temperature distributions are uniform along filament for both types of discharges. These measurements do not reveal any significant differences in rotational and vibrational temperatures along the discharge channel (except possibly very near the electrodes).2 nm) The aforementioned results of temperature measurements along the axis of single filaments are plotted in Figure 3. thus power appears to dissipate more or less evenly. an increase in the emission intensity does not necessarily imply that the temperature is higher.15.

Figure 3. vibrational temperatures are one order of magnitude higher than rotational temperatures and this indicates the nonequilibrium nature of the discharge.15: (a) Rotational and (b) Vibrational temperature distributions along the microdischarges .42 Figure 3. In general.15(a-b) indicates that the rotational and vibrational temperatures can be considered constant along the channel.

16). 10 fibers – 200 μm core) is utilized to acquire the optical emission from the discharge and to transmit it to the spectrometer (Acton Research SpectraPro 500i with Roper Scientific model 7430 CCD camera or Princeton Instruments – Acton Research. . The temperature of the camera is set at -25°C in all experiments.43 A different setup is used to measure temperature of the nanosecond-pulsed DBD. Trenton. NJ) and spectra are digitally acquired with approximately 0.6 nm resolution (Figure 3.16: Spectroscopic measurement setup for DBD The background noise obtained for the same exposure time is subtracted from the discharge emission spectrum prior to the temperature estimation. A fiber-optic bundle (Princeton Instruments-Acton. The ambient room temperature is 22°C throughout the spectroscopic measurements. Figure 3. TriVista TR555 spectrometer system with PIMAX digital ICCD camera. Low pressure mercury lamp is used to determine the slit function and calibrate the spectrometer.

44 Curve fitting of model spectra (Laux 2002) to experimental data is carried out. Figure 3. .5 K and 3360 ± 50 K. for the power range that has been used for the experiments explained below. Vibrational spectra of the second positive reflect the interplay between the population by electron impact from different lower states and depopulation due to the collisional quenching and radiative processes.17. respectively. These ‘temperatures’ describe the relative population of different vibrational and rotational levels of the C3 state of molecular nitrogen. it is demonstrated that the nanosecondpulsed DBD does not heat the gas but provides strong excitation of the gas due to the high energy of the electrons. Thus.5 ± 7. Rotational and vibrational temperatures are measured to be 313. Thus the vibrational distribution is an indicator of the electron’s temperature in the discharge region. Rotational distribution of the C3 state under the pulsed excitation at high overvoltage reflects the rotational population of the ground state and gives information regarding the temperature of the gas.18 shows nanosecond-pulsed DBD igniting on a finger without causing any damage or even discomfort. The second positive system spectrum of nanosecond-pulsed DBD and best fit simulated spectrum are given in Figure 3.

(Model spec 360 ctrum: Laux 2002. . nal ure: vibrational te emperature: 33 ± 50 K.45 4 Figure 3. 2006 x ck 6) Figure 3.5 K and v ent.18: Nanosec cond-pulsed DBD ignitin on finger (exposure t d ng r time: 1 s) .17: Spectra of nanosec 3 a cond-pulsed D DBD for spe ectroscopic t temperature measureme Rotation temperatu 313. Staac et al.5 ± 7.

. IL).3.46 3. Surface temperature due to plasma is measured at 25°C. surface temperature on the grounded electrode is measured in the presence of the discharge using a reversible liquid crystal temperature indicator (model 4002B. Electrical measurements for average power are verified with a custom-made calorimeter. Two conventional DBD systems have been analyzed spectroscopically and single filament measurements show that there is no significant change in gas temperature along the channel.L.4 Summary of Key Results and Conclusions Several characterizations have been conducted to explore the feasibility of using nanosecond-pulsed DBD for living tissue treatment. Volume discharge measurements demonstrate that microdischarges within the volume for different types of discharges have the same gas temperature for the same power. 3. Accuracy: ± 1°C. The room temperature is 22°C during the surface temperature measurements.2 Surface temperature In addition to the spectroscopic temperature measurements. LCR Hallcrest L. A power-temperature relation is found to be somewhat linear and largely independent of voltage waveform shape. while the temperature of the ground electrode surface without the discharge is also measured to be 22°C. A sheet of the temperature indicator is placed over the grounded copper electrode and acts as the secondary electrode in the discharge (Goree et al..C. 2006).

respectively.5 ± 7. Side view long exposure images of the nanosecond-pulsed DBD show that it is “filament-free” and much more uniform than the conventional DBDs. Some other qualitative experiments with photo films verify that nanosecond-pulsed DBD is completely uniform. . Also it is found that with spherical electrode nanosecond-pulsed DBD can ignite and be sustained over a wide range of inter-electrode gap.5 K and 3360 ± 50 K for rotational and vibrational temperatures.47 Nanosecond-pulsed DBD and other DBD systems are assessed visually for uniformity analysis. Surface temperature increases of 3°C are observed after 5 minutes of plasma exposure with typical power density. Optical emission spectroscopy measurements reveal that nanosecond-pulsed DBD is almost at room temperature with 313.

Treatment with power as low as a few tens of mW for 15 s. 4. Figure 4. are transferred onto a blood agar plate (Trypticase Soy Agar with 5% Sheep Blood. Skin flora bacteria. Cardinal Health. a mix of Staphylococcus. This result does show both the sterilization ability of the discharge as well as its efficiency. Dublin. with an average power density of approximately 1 mW/mm2 (discharge diameter equal to electrode diameter) can sterilize. complete sterilization can be attained with nanosecond-pulsed DBD at a significantly lower power density. Streptococcus. This power density is one order of magnitude lower than typical conventional DBD power densities. For the same duration. BIOLOGICAL CHARACTERIZATION AND QUANTIFICATION OF NANOSECONDPULSED DIELECTRIC BARRIER DISCHARGE 4.1 Qualitative Demonstration of Sterilization Nanosecond-pulsed DBD has been tested for demonstration of sterilization by treating bacteria culture on agar. and yeast.2 Qualitative Comparison of Conventional and Nanosecond-pulsed Dielectric Barrier Discharge on Topographically Non-uniform Surfaces In addition to a typical sterilization experiment.1 shows the image of an agar surface covered with skin flora (dark red area covering most of the surface) being sterilized (light red area) with nanosecond-pulsed DBD treatment for 15 s. . OH) for a sterilization demonstration (Fridman et al. effectiveness of the DBD excited by nanosecond rise and fall time voltage pulses has been tested for inactivation of the bacteria located within indentations on surfaces (Ayan et al. 2006).48 CHAPTER 4: STERILIZATION EFFICACY.

Fisher Scientific.1: Agar with skin flora treated by nanosecond-pulsed DBD (Vmax: 20 kV. so the discharge can sterilize irregular surfaces completely. two different sorts of agar plates are fashioned and used for topographically non-uniform (uneven) surface sterilization experiments.49 2009b). Repetition rate: 190 Hz) The agar used for bacteria culture in this study is made out of a broth (Difco Brain Heart Infusion Agar powder. It is vital for the discharge to produce uniform plasma independent of the uniformity of the bacteria covering surface that serves as one of the DBD electrodes. In general. PA) mixture that solidifies shortly after it is poured in the petri dish. Figure 4. The first type is characterized by a flat planar surface which is used in .

as well as for control samples. Figure 4. The second type of agar plates which are specifically prepared to have nonuniform surfaces (with ridges and indentations) on the agar to mimic the real case for living skin tissue.2. Then.50 studies of non-uniform surfaces by placing meshes over them. After the agar is solidified. Different steps of patterned agar preparation are presented in Figure 4. agar is poured on top of the mold and left to dry.2: Patterned agar preparation . it is removed and inverted and placed into the new (final) dish. The agar ridges are molded by placing a polymer form at the bottom of the dish.

Concentrations were measured and calculated on flat agar plates with a dilution assay which is a common technique in microbiology (Singleton and Sainsbury 2002. 2004). Silverthorn et al. The dilution assay protocol is presented in Figure 4.51 Escherichia coli bacteria (E.3. The suspension volume (water and bacteria) is enough to completely cover the surface of the agar. Rochester.3: Protocol for dilution assay . NY) are plated onto the surface of agar with concentrations of up to 108 – 109 CFUs/ml (colony forming units/ml).coli K12 strain. Figure 4. Ward's Natural Science.

Sterilization results are evaluated by visually examining the resulting colonies after incubation. In all experiments. 10 kV pulses with 20V/ns rise time both are produced at 120 Hz to maintain the comparable power. Sheldon Manuf. Table 4. Inc. treated and untreated (control) samples are cultured for 12 hrs in the incubator (VWR. Class-II. The sterilization effectiveness of nanosecond-pulsed DBD on non-uniform surface is proved by comparing with conventional DBD.and microsecond-pulsed DBD parameters Pulse Length [ns] Voltage [kV] Front [ V/ns] Frequency [Hz] Power [mW/cm2] ns-DBD µs-DBD 20 1500 16 10 3000 20 120 120 100 100 . power density for the active area of the electrode is maintained at 100 mW/cm2 (approximately 75 mW for 1 cm electrode diameter). For nanosecond-pulsed DBD applying 20 ns long.52 Before plasma treatment. Model#1545. Samples are also observed up to a 48 hrs incubation period in which delayed recovery is not found in the plasma treated regions.5 μs long. Kansas City.1: Summary of nanosecond. OR) at 37 ºC. 16 kV pulses with approximately 3kV/ns rise/fall times and for microsecond-pulsed DBD applying 1. MO) for 1 hr along with the control plates.1. After plasma treatment. Parameters for both systems are summarized in Table 4. bacteria seeded plates are left to dry in the laminar flow hood (Labconco..

sterilization is achieved at the ‘valleys’ with a slightly larger diameter than the active area of the electrode in 30 s.25 mm in diameter. On the left-hand side of Figure 4.5.e.5 mm. i. The opening between the wires of the mesh is 1. In contrast.5). surface nonuniformities. . a metal mesh simulates the effects of ridges and indentations. and total thickness of the mesh is 0.5.coli covered. In this case. A typical sterilization result comparing both nanosecond-pulsed and microsecond-pulsed DBD systems is shown in Figure 4. the wires are 0.coli bacteria. The gap between the bottom of the high voltage electrode and the top of the mesh is 1 mm.5 mm.53 The first part of the non-uniform surface sterilization experiments is done by placing a stainless steel mesh over the flat surface agar as shown in Figure 4. These preliminary results from the sterilization experiments clearly indicate that the nanosecond-pulsed discharge is much more effective and faster than the conventional microsecond DBD in killing E. The concentration of sterilization effect to the middle part for microsecond-pulsed DBD can be due to possible occurrence of surface discharges following the extinction of the microdischarges. Light color areas in this figure are the locations on the agar that are completely sterilized by plasma treatment and the rest of the agar with a darker color is E.4. conventional DBD affects a significantly smaller area (on the right-hand side of Figure 4.

54 Figure 4.4: Illustration of mesh on top of the agar to mimic the indentations (10 mm diameter electrode with 0.66 mm quartz) .

Dimensions are shown on a schematic in Figure 4.55 Figure 4. .6. For this experiment.(left-hand side) and microsecond.33 mm depth at every stage.5: Inactivation with nanosecond. circles in (a) indicate the edge of the high voltage electrode. no other modifications done) In the second group of experiments.(righthand side) pulsed DBD through metal mesh and (b) schematic of the experimental setup (schematic is not to scale. the agar is patterned with a 3-level recess with 2 mm width and 0. the sterilization effect of novel DBD system has been tested and also compared with that of a conventional DBD system. brightness and contrast of the image are adjusted for clarity.

7: Uniform distribution of bacteria on patterned surface .7). Figure 4.6: Schematic of 3-level recess patterned agar Figure 4. uniform distribution of bacteria on the patterned surfaces are verified by seeding low enough concentrations (103 – 104 CFU/ml) to get a countable number of colonies on the surface (Figure 4.56 It should be also noted that prior to these experiments.

the side view of electrode on patterned agar surface (Figure 4.8b) and a nanosecond-pulsed DBD (Figure 4. Pictures of discharges have been taken in a dark room with 0. Figure 4. (b) conventional microsecond DBD and (c) nanosecond-pulsed DBD on the patterned agar surface (three steps with 0.5 mm thickness is placed between the high voltage electrode and the top surface of the agar. and the typical appearance of a conventional microsecond-pulsed DBD (Figure 4.5 s exposure time at 120 Hz repetition (for both systems) . In Figure 4.57 A two-piece spacer with 0.33 mm height and 2 mm width).8.8c) are given.8: Side view of (a) high voltage electrode in light room with no plasma.8a).

8 previously. This figure shows a top view of a treated 3-level recess patterned agar that is given in Figure 4. In the case of nanosecond-pulsed DBD.8b.8c. .9 with the distinction in sterilization performance. all three steps are uniformly treated and sterilized (Figure 4.58 As it can be easily seen from Figure 4.9b). only partial sterilization is achieved in the vicinity of the edge of the first step where the discharge gap is minimal (Figure 4. The exclusive features of nanosecond-pulsed DBD can also be easily seen in Figure 4. Although the latter is also slightly more intense on the corners. it is fully covering the entire gap.9a) whereas in the case of conventional microsecond-pulsed DBD. the conventional microsecondpulsed DBD produces microdischarges (filaments) that are often terminated on the top of asperities and irregularities (mostly at smaller gaps or corner of the surface features) whereas the nanosecond-pulsed DBD exhibits a rather diffuse structure in Figure 4.

For both plates treatment time: 30 s..9: 3-level recessed agar surface treated with (a) nanosecond-pulsed DBD and (b) microsecond-pulsed DBD.59 Figure 4. Width of each step (distance between the horizontal lines) is approximately 2 mm. concentration: 108 CFU/ml .

microsecond DBD sterilizes only the highest level . In contrast. When nanosecond-pulsed DBD is applied. Drawings of the patterns with dimensions are given in Figure 4. Type 0 Type 1 Type 2 Type 3 Figure 4. The preparation method of patterned agar is described in the previous chapter.60 4. Four different patterns are used to assess the sterilization as a function of surface pattern depth. E.3 Quantitative Comparison of Conventional and Nanosecond-pulsed Dielectric Barrier Discharge on Topographically Non-uniform Surfaces Sterilization efficacies of nanosecond-pulsed DBD and conventional DBD have also been compared quantitatively.11 shows the typical difference between uniform nanosecond-pulsed DBD and conventional DBD.coli suspensions with different concentrations are seeded on the patterned agar plates. all surfaces at different levels are sterilized. Arrows on each pictures show the lowest level of the pattern (Type 2).10.10: Four different agar patterns with different depth (dimensions in mm) Figure 4.

. After plasma treatment.11: Sterilization effect of two systems on valleys (dashed circles indicate the active area of the electrode) In this experiment. agar plates are placed into the incubator for 12 hrs.61 while it can partially affect the bacteria at the bottom of the valleys and cannot fully sterilize. Following the plasma treatment. Figure 4.3). bacteria quantification is done by counting the colony forming units on the treated surface within the 10 mm diameter circle. an electrode with 10 mm diameter active area is used. Initial seeding concentrations are determined by a standard dilution assay method (Figure 4.

In every case. plasma treatment resulted in partial sterilization wherein it is not possible to quantify the CFUs after treatment.12.62 Bacteria colonies are then counted (after-treatment). At some higher seeding concentrations. The protocol for determining the log reduction is given in Figure 4. . quantification is carried on with the next lower dilution. In those cases. the highest countable seeding concentration is taken into account and the CFU log reduction is calculated from the difference between initial seeding and post-treatment counts.

12: Flow chart for determining the log reduction in bacteria population after plasma treatment on patterned agar .63 Figure 4.

64 Results for log reduction of bacteria colonies after a 30 s treatment are presented in Figure 4.13. As expected, data shows that the sterilization effect diminishes as the pattern depth increases. In addition, in most cases nanosecondpulsed DBD is found to be inactivating more than 1 order of magnitude more bacteria than with conventional DBD. Also, the E.coli CFU log reduction on the Type 2 pattern as a function of plasma treatment time is presented in Figure 4.14.

6 5

Log Reduction 

4 3
ns‐DBD

2
Conventional  DBD

1
Type 0                      Type 1                      Type 2                      Type 3 1 2 3 4 0.34 mm                  0.56mm                    0.78mm                  1mm

Pattern Type / Max Depth Figure 4.13: CFU Log reductions on different patterns with 30 s plasma treatment Statistics are collected by dividing the treated are into four equal sections (quarter circle area) and performing a count in each area

In the literature, there exists a widely used kinetics measurement parameter to characterize the sterilization efficacy in a broader perspective. The parameter is often referred to as a D-value and is essentially equal to the time required to reduce the

65 original concentration by 1 log (Laroussi 2005). In Figure 4.14, the shortest treatment time is 5 s reductions in bacteria population are already more than 1 log for both DBD systems. Therefore, these results set the D-value at a few seconds which is a relatively shorter time compared to the other studies (Laroussi et al. 1999 and Herrmann et al. 1999).

5 4

Log Reduction 

3 2 1 0
1 2 3 5 s                                    15 s                                  30 s ns‐DBD Conventional DBD

Treatment time

Figure 4.14: CFU log reduction on Type 2 pattern (max depth: 0.78 mm) as a function of plasma treatment time. Statistics are collected by dividing the treated area into four equal sections (quarter circle area) and performing a count in each area

4.4

On the Mechanism of Sterilization Plasma is a chemically active medium including thermal, electric, radiative

energy forms and they interact with background gas and substances being exposed.

66 There are several factors in the plasma that can cause inactivation of bacteria (Stoffels 2007, Gaunt et al. 2006, Lerouge et al. 2000); namely heat, UV radiation, ozone, and charged particles (electrons and positive and negative ions). In order to help understand the basic mechanism of sterilization with nanosecond-pulsed DBD, some experiments are designed and implemented. In the first experiment, plasma treatment applied on the bacteria seeded surface in the presence of air flow in the single recess (channel) agar. A schematic of the single recess pattern is shown in Figure 4.15. A diagram of the system is presented in Figure 4.16. Air was supplied from a tank and flow rate regulated with a digital flow controller (Omega Engineering, Inc., Model#: FMA-2620A & FMA-2607A). Additionally, a top view of the single step recessed agar that is used for this experiment is given in Figure 4.17. The depth and the width of the recess are 1 mm and 10 mm, respectively. In the first case (Figure 4.17a), the surface of the agar plates are treated for 30 s in a regular fashion. In the second and third cases (Figure 4.17b and Figure 4.17c), air is blown through the gap between the quartz and the bottom of the recess with 0.3 and 3 SLPM flow, yielding 0.5 m/s and 5 m/s air velocity in this cross section, respectively.

15: Schematic of single recess (channel) patterned agar Figure 4.16: Diagram of the system for air flow through the channel on the agar plate In terms of sterilization.e. there is no partial sterilization due to the plasma afterglow downstream of the flow (to the right hand side of the figure). The lack of major differences in the figures indicates that the sterilization .67 Figure 4. the results are similar to each other except for slight size differences in the size of the sterilized area. i. However there is no qualitative difference between the air flow and no flow cases.

by itself. Additionally. is not the major bactericidal factor in the plasma. The sterilizing agents cannot be blown or translated away from the electrode location with air flow.coli seeded flat agar surface. . The area covered by the MgF2 window receives only UV and the rest of the treated area is exposed to whole plasma products. This result suggests that UV. the area covered (exposed to only UV) is not sterilized whereas the rest of the treated area is sterilized.68 occurs through direct contact with the plasma. another experiment is conducted to assess the effect of UV in nanosecond-pulsed DBD. As presented in Figure 4.18. UK) has been placed on the E. A VUV (vacuum UV) grade MgF2 window (Crystran Limited.

respectively nd y) .3 SLPM air flow (c) with 3 SLPM air f Arrows ind dicate the dire ection of the flow. (Oute and inner circles repre e er esent quartz an electrode active area. (b) (a) air Figure 4.69 6 ment nosecond-pu ulsed DBD ( without a flow. flow on sing level rece gle essed agar. with 0.17: 30 s treatm with nan w.

The conclusion drawn from these results is that sterilization by nanosecond-pulsed DBD is mostly due to the charged particles. 2006 and Moisan et al. and most of the charged particles remain in the plasma region (lifetime of charged particles at atmospheric pressures is very short) and 2) UV is not playing a major role in those experiments. radicals and molecules. some of which are in an excited state (Deng et al. .18: Plasma treatment through MgF 2 window Taking the last two experiments together in to consideration: 1) the afterglow of the plasma contains only neutral atoms.70 Figure 4. 2002).

71 4. the temperature of nanosecond-pulsed DBD is measured to be at room temperature level. and concluded that charged particles are the most important factors in the plasma. experiments in this chapter on mechanism of the sterilization rules out ozone and UV. Additionally.5 orders of magnitude more bacteria than with conventional DBD. Therefore. Then sterilization effectiveness of nanosecond-pulsed DBD on topographically non-uniform surfaces has been tested and proven with a series of experiments. Sterilization efficacy of nanosecond-pulsed DBD and conventional DBD have also been compared quantitatively where nanosecond-pulsed DBD is found to be inactivating 1 to 1. ‘temperature of the plasma’ cannot be the factor that causes sterilization. As it is shown in the previous chapter.5 Summary of Key Results and Conclusions Sterilization capability of nanosecond-pulsed DBD has been first demonstrated on plain agar with skin flora. .

This method may be easily used for a variety of applications.72 CHAPTER 5: SUMMARY AND CONCLUSIONS 5. quantified. and compared with that of a conventional discharge. It should be emphasized that the technique employed to generate a few tens of nanosecond long pulses is relatively simple and inexpensive. whereas the microsecond-pulsed DBD fails to do so as well. Experiments that have been conducted in order to .1 Summary of the Research and Conclusions A novel uniform non-thermal plasma system was developed in this work for living tissue sterilization and other medical applications. using high speed photosensitive film exposure. Lichtenberg figures of nanosecond-pulsed DBD show clearly that few tens of nanosecond pulse duration avoids streamer formation and generates uniform discharge in atmospheric pressure air. The uniformity of this nanosecond-pulsed DBD is proven qualitatively with a new technique for such high frequency discharge. DBDs with nanosecond rise times are potentially more convenient for in vivo and real sterilization cases with non-uniform profile surfaces. This novel DBD is proven to be much more effective in killing bacteria on surfaces than with conventional DBD. The ability of the nanosecond-pulsed discharge to sterilize has been demonstrated. Thus. Experiments on non-uniform surfaces using meshes and patterned agar revealed that the nanosecond-pulsed DBD can penetrate valleys (indentations between ridges). The nanosecond-pulsed DBD with short rise time and high overvoltage is insensitive to the surface non-uniformities of the agar and does not require uniform discharge gaps as it can ignite and be sustained over a wide gap range.

This makes it a promising tool for medicine. The specific contributions of this research are summarized as follows. • Demonstration and quantification of sterilization on non-uniform surfaces with nanosecond-pulsed DBD treatment. 5.73 understand the basic mechanism of sterilization by comparing direct and indirect plasma effects indicate that charges (electrons and ions) play a major role in sterilization with nanosecond-pulsed DBD. . The thesis research and activities will help to develop knowledge and novel solutions in the Plasma Medicine field.2 Research Contributions The main research contribution in this work has been developing a novel dielectric barrier discharge system that enables uniform plasma treatment for living tissue sterilization in atmospheric pressure air. This system can also be used in other biological studies and non-uniform surface treatment applications. The nanosecond plasma works significantly better than conventional DBD on non-uniform surfaces. • Demonstration of uniform plasma on topographically non-uniform surfaces for the first time in air at atmospheric pressure. • Development of a uniform dielectric barrier discharge system with nanosecond pulse excitation for the first time in air and at atmospheric pressure.

• Elimination of microdischarges.74 • Confirmation that the mechanism of sterilization in nanosecond DBD is associated with charges. . therefore offering a safer treatment without possible local heating.

75 .

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 425‐442 (2006)    SELECTED  AWARDS AND  HONORS   • • • • • • • • • Drexel University Graduate Student Teaching Award – Winner.  A.A. Fridman.  Ayan.F..  Brooks.Sc.  M.  A.  H.  G. 2009  IEEE – ICOPS Student Travel Grant.D.N. 4.  M.  Fridman. 58–66    5.  G  Fridman.  Plasma  Chemistry  and  Plasma  Processing. V.  Victor N. Mechanical Engineering                                           October 2005 – July 2009    Department of Mechanical Engineering and Mechanics  Drexel University.  A.  A. and Turkey)                              JOURNAL  1.  Gutsol.  Ayan. (2008). Baiada Center for Entrepreneurship Business Plan Competition  Second Place. 37 (2009). H. Polym. Gary Friedman. (2007). Vasilets. Phys. Effect  of  Dielectric  Barrier  Discharge  Plasma  on  the  Attachment  and  Proliferation  of  Osteoblasts Cultured over Poly(ε‐caprolactone) Scaffolds. V.  D  Staack. G. 2009  NSF – GRC Travel Fellowship.  G.  A. Blood  Coagulation  and  Living  Tissue  Sterilization  by  Floating‐Electrode  Dielectric  Barrier  Discharge  in  Air.  Gutsol.  Fridman. Baiada Center for Entrepreneurship Business Concept Competition   Winner.  Vasilets.  Fridman.  Friedman.  M. Philadelphia. 113‐120      3. Heating Effect of Dielectric Barrier Discharges for Direct Medical Treatment.  Brooks.89 VITA    EDUCATION  Ph. J. 42.D. Turkey    (valedictorian and summa cum laude)    PROFESSIONAL  Graduate Research Assistant / Teaching Assistant                            October 2005 – July 2009 EXPERIENCE  Department of Mechanical Engineering and Mechanics  Drexel Plasma Institute   Drexel University     Gas Turbines Supervisor                                                                                  July 2001 – July 2005  Bechtel‐Enka Joint Venture   (Kazakhstan.  Staack. Phys. The Netherlands. Candidate.  (2009) 125202    2. 2. IEEE Transactions on Plasma Science. Application  of  nanosecond‐pulsed  dielectric  barrier  discharge  for  biomedical  PUBLICATIONS  treatment  of  topographically  non‐uniform  surfaces. Vasilets.F.N. 2001      . 36  (2008). 1. 504‐508    4. Y Mukhin. G. Friedman.  H. A Fridman and G Friedman.  G. 2007  NSF – GRC Travel Fellowship. 2006  Gold Medal for Graduating Ranked 1st in class ‘01.  D. 2008  NSF – NATO‐ASI Travel Fellowship. A. Friedman. A Starikovskii.  H  Ayan.  G. Selcuk Guceri.  A.  Plasma  Process. Izmir..  A.  A. 370‐375    6.N. Comparison  of  Direct  and  Indirect  Effects  of  Non‐Thermal  Atmospheric  Pressure  Plasma  on  Bacteria.  A  Gutsol.  Fridman.  G. Alexander Fridman. 2008  Laurence A. Ayan.  Gutsol. Yildirim. Vasilets.  Gutsol.  IEEE  Transactions on Plasma Science. Nanosecond  Pulsed  Uniform  Dielectric  Barrier  Discharge. Plasma Process.  G. Eda D.  Fridman. 2009   Drexel University Graduate Student Research Award – Highly Commended.  Friedman.  Fridman.  Balasubramanian. H. Mechanical Engineering                                                           September 1997 – July 2001 Department of Mechanical Engineering  Ege University. Polym.  Balasubramanian. Halim Ayan. Ayan. Wei Sun.  Peddinghaus.  A. 2008  Laurence A. 26. PA    B. 5(1). D: Appl.  V.  Fridman.

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