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R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com
ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45
www.ijera.com 41 | P a g e
Experimental Study of an Atmospheric Pressure Dielectric
Barrier Discharge and PET Surface Modification
R. Shrestha1,2,*
, D. P. Subedi1
1
Department of Natural Sciences, School of Science, Kathmandu University, Dhulikhel, Nepal
2
Department of physics, Basu college/Basu H.S.S, Bhaktapur, Nepal
ABSTRACT
A homogeneous dielectric barrier discharge (DBD) in argon was produced by applying high voltage A.C. source
of potential difference (0-20) kV operating at a frequency of 10-30 kHz across two parallel plate electrodes with
glass as dielectric barrier. The discharge was characterized by optical emission spectroscopy (OES) and
electrical measurement. Four argon emission lines from the discharge were analyzed and the electron
temperature was estimated by line intensity ratio method. The electron density in the discharge was estimated by
power balance method. An investigation of the effect of inter-electrode distance on the electron density was
made. The results showed that the electron temperature is less than 1 eV and the electron density is of the order
of 1011
cm-3
which varied with the inter electrode distance. Discharge was applied for surface modification of
polyethylene terepthalate (PET). Modified surfaces were studied by contact angle measurement and FTIR
spectroscopy.
Key words: Electron temperature, electron density, DBD, optical emission spectroscopy, power balance.
I. Introduction
Atmospheric pressure dielectric barrier
discharges (DBDs) are non thermal and non
equilibrium plasmas [1]. Atmospheric pressure non
equilibrium plasmas have been widely studied for
several emerging applications such as surface and
material processing biological and chemical
decontamination of media, light source, absorption
and reflection of electromagnetic radiation and
synthesis of nanomaterials [2]. This process can be
improved by a better understanding of basic plasma
phenomena and by knowing its properties. The
plasma properties depend on several parameters, such
as, the electrode geometry, cooling system, excitation
frequency, power injected, gas composition and type
of dielectric barrier [3].
The electron density and electron temperature
are the most fundamental parameter in gas discharges
and play a very important role in understanding the
discharge physics and optimization of the operation
of plasma [3, 4]. Different methods are employed to
measure the electron density and electron
temperature in plasma. In atmospheric-pressure
discharge system, both the probe and the microwave-
based methods are difficult to use due to the small
plasma dimension and strong collision process. The
OES based technique is suitable for measurement of
electron density and electron temperature. To
measure the electron temperature line intensity ratio
method is used, in which the intensity ratio of
emission lines is related to electron temperature and
electron density.
OES has been used for the measurement of
electron temperature and electron density in different
types of plasmas [5, 6, 7, 8]. Low temperature
plasmas are widely applied for the surface treatment
of polymers because of their several advantages over
other conventional methods. Jie-Rong, et al reported
wettability of Poly(ethylene Terephthalate) film
treated with low-temperature plasma and their
surface analysis by ESCA[9]. Novák et al also
studied the surface propertis of poly(ethylene
terephthalate) treated by low-temperature plasma
[10]. The present experiment uses a power supply
working at 27 kHz to produce the discharge at
atmospheric pressure. The discharge is found to
spread homogeneously over the whole area of the
electrode and known as the atmospheric pressure
glow discharge (APGD).
In this paper, electron temperature in
atmospheric pressure DBD in air/argon environment
is measured by line intensity ratio method and
electron density is determined by power balance
method. The relationship between the surface
wettability and the surface structure of PET is
investigated by FTIR spectroscopy. The change in
hydrophilic property of the sample has been studied.
II. Experimental
The experimental arrangement is shown in Fig.1.
The electrodes are made up of two brass discs, 7mm
thick and 51mm in diameter. A glass plate of
thickness 1.2mm was used as dielectric barrier
between the electrodes. A high voltage AC source (0-
RESEARCH ARTICLE OPEN ACCESS
R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com
ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45
www.ijera.com 42 | P a g e
13
7
9
11
1
2
3
4
5
6
10
8
14
12
20) kV and frequency (10-30) kHz was applied to
electrodes through a current limiting resister of 10k.
The whole apparatus is enclosed in a cylindrical
chamber and argon is passed into it at a flow rate of
2l/m. The applied voltage and current were measured
by high voltage probe (Tektronics TDS2000). The
experiment were conducted with inter electrode
spacing varying between 1-3mm
Fig:1: Schematic diagram of the experimental set-
up.
1-Gas inlet, 2- power electrode, 3-Discharge, 4-
Glass plate , 5-Grounded electrode, 6- Plasma
reactor, 7- Resistance 10 k, 8- Linear Array
Spectrometer VS140, 9- Voltage probe, 10- Power
supply (A.C), 11-Osciloscope , 12-Computer, 13-
Resistance 10 M , 14- Teflon screw.
Optical emission spectra were recorded by liner
array optical spectrometer (Lynear VS140). Contact
angles were measured by rame hart goniometer. The
ATR-FTIR spectroscopy measurements of PET foils
were performed with IR Prestige-21, shimadzu, Japan
having a resolution of 4 cm-1
, a scan range was 4000
– 400 cm-1
, and a total of 50 scans per analysis.
III. Result and Discussion
3.1 Measurement of Electron Temperature by
Line Intensity Ratio Method:
Fig: 2 shows the OES of the discharge in the
range of 250nm-850nm. The applied voltage,
discharge current and spectrum are simultaneously
measured and analyzed for determination of electron
temperature. Using line intensity method, four
suitable lines (two for ArI and two for ArII are
chosen and electron temperatures is estimated using
the lines intensity ratio method. For the measurement
of electron temperature, equation (1) is used [5,6,7].
Where R is the ratio of intensity of two lines, I is
the intensity of spectral lines, Aij is the transition
probability of the transition ij, gi - The statistical
weight of the upper level,  - wave length of the
radiation, Ei - energy of the upper level, K -
Boltzmann constant and Te - electron temperature
Considering two Ar I lines of wavelength 696.54 nm,
and 751.034 nm and two Ar II lines with wavelength
314.13 nm and 378.75 nm and plot of R1/R2 against
Te has been made, the electron temperature has been
found to be 0.89eV. This result is in good agreement
with the results reported in previous work.
Electron temperature thus determined is used to
calculate the electron density by using the Eq. (2)
given below
The use of Eq. (2) is made for calculation of ne
from different lines and average values of ne=
3.47032×1011
cm-3
is obtained.
3.2 Determination of Electron Density by Power
Balance Method
The glow mode discharge is homogeneously
spread over the whole electrode area, so the plasma
density can be estimated from a power balance
method. In this method electron density is given by
[7].
(3)
2
e
b lost
p
n
Aev E
    
Where A - Area of each electrode=20.43cm2
, vb -
Bohm velocity = 2×105
cms-1
, Elost = 50eV (in our
3
2
1 21 1 2 2
2
2 2 1 1
2
2 [ ] (2)e e i
e
e
m kT E E EI A g
n Exp
I A g h KT


       
         
     
100 200 300 400 500 600 700 800 900
0
10000
20000
30000
wavelength (nm)
Intensity(Au)
Fig. 2 Optical emission lines of atmospheric
pressure discharge produced in Argon.
1 1 2
2 3 4
exp .....(1)
pq p xy p r x urs uv u
rs r pq xy x uv e
A g E E E EA gR I I
R I I A g A g kT

 
            
             
         
R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com
ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45
www.ijera.com 43 | P a g e
condition), Applied frequency = 27 kHz, Gas flow
rate 2l/min, Dielectric = 1.5mm thick glass.
By using Eq. (3) electron density was calculated
for different value of applied voltage and the
variation of electron density with applied voltage is
shown in Fig 4. It is evident that electron density
increases linearly with the applied voltage.
3.3 Measurement of Contact Angle and Surface
Energy
Contact angles were measured on PET surface
treated with APPJ in argon for exposure time 0–60
seconds. The measurements of the contact angles
were performed by contact goniometer using distilled
water and glycerol on different positions of the
treated sample. Surface energy was calculated using
the Owens-Wendt Kaelble method. In this method, it
is possible to determine the solid surface energy (γ)
as the sum of polar (γp
) and dispersive (γd
)
contribution using at least two different test liquids
(water and glycerin) [9, 10, 11,12]
The dependence of contact angle and surface
energy on exposure time for PET is shown in Fig: (5
and 6). The images of water drops on the surface of
untreated and plasma treated PET sample are shown
in the inset of Fig 5. The value of contact angle
decreases and consequently the surface energy
increases with the treatment time. The increase in
surface free energy is attributed to the
functionalization of the polymer surface with
hydrophilic groups.
3.4 Surface Analysis of PET
The wettability of the sample is related to the
presence of a particular functional group that resides
on the outermost surface layer. The relationship
2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6
1.5
2.0
2.5
3.0
3.5
4.0
Electrondensity(10
11
)/cm
3
Applied Voltage (kV)
Fig 4: Electron density as a function of applied voltage.
 
1 1
2 21 cos 2 2 (4)d d p p
l l s l s              
Fig 5: Water contact angle on PET as function of
treatment time in Argon plasma
0 10 20 30 40 50 60
30
35
40
45
50
55
60
65
70
Treatment Time (Sec)
Surfaceenergyoftreatedpolymer(PET)
Fig 6: Surface energy of PET as function of
treatment time in Argon plasma
0 10 20 30 40 50 60
20
30
40
50
60
70
80
ContactAngle
Treatment Time (Sec)
Fig.3: Voltage and current waveforms of
discharge.
-60.0µ -40.0µ -20.0µ 0.0 20.0µ 40.0µ 60.0µ
-6
-4
-2
0
2
4
6
voltage
Current(mA)
Time(s)
voltage(kv)
-30
-20
-10
0
10
20
30
current
R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com
ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45
www.ijera.com 44 | P a g e
between the surface chemical structure and surface
wettability of plasma treated PET was characterized
by Fourier Transform Infrared (FTIR) Spectroscopy.
.
The chemical changes in surface properties of
plasma-treated polymer are analyzed using ATR-
FTIR spectroscopy. Fig.7 shows the ATR-FTIR
spectra of unmodified PET. FTIR spectra for PET
treated in atmospheric pressure plasma in Ar gas is
shown in Fig 8 for comparison.
It is also observed from the FTIR spectra (Fig.
7and 8) that there is a change in intensity of
absorption peaks corresponding to certain functional
groups. The wave number region: from 3600 to 2500
cm−1
, where the C–H and O–H stretching vibrations
of different types of H-bonds occur.
Spectrum of PET has the characteristic
absorption peaks at 1714 cm-1
(C=O bonds), 1410,
1018, and 872 cm-1
(vibration of aromatic ring), 1340
and 1177 cm-1
(bending vibration of -CH2 groups),
1244 and 964 cm-1
(stretching vibration of C-O
bonds), 690 cm-1
and 750 cm-1
phenyl group ( =C-H
& C=C ) 1124 and 1100 cm-1
(stretching vibration of
C-O bonds due to amorphous and crystalline
structure of PET respectively) [12,13,14].
For PET treated in APPJ, the broadening of the
C=O stretch at 1714 cm-1
has appeared due to
creation of oxygen-containing sites .
The information from the FTIR spectra indicates
that the carbon content decreases and the oxygen
content increases in the surface of PET, and a large
amount of oxygen polar functional groups are
introduced into the surface of plasma-treated PET.
This is responsible for improving the wettability of
PET.
IV. Conclusion
Atmospheric pressure argon plasma has been
produced and characterized by optical and electrical
methods. Electron density (ne) and Electron
temperature (Te) were found to be 3.361011
cm-3
and
0.786eV respectively with the electrode gap of 2mm.
Electron density and electron temperature were found
to be dependent on the applied voltage for constant
inter electrode distance.
Atmospheric pressure argon plasma treatment of
PET surface resulted an improvement on
hydrophilicity. It is mainly due to the increase in the
polar component of the surface free energy after
plasma treatment which indicates the formation of
polar functional groups on the surface. The
improvement of wettability of PET strongly depends
on the treatment time. This system can be very useful
for the treatment of thermally sensitive materials and
also for the treatment of biological samples.
V. Acknowledgement
This work was supported by the National
Academy of Sciences NAST Nepal. Authors would
like to thank Dr. Rajani Sakya and Dr. Aswani
Kumar Shrestha, Department of Pharmacy, School of
Science, Kathmandu University for FTIR analysis of
the samples.
Reference
[1] A. Lonascut-Nedelcescu, C. Carlone, U.
Kogelschatz, D.V.Gravelle and M.I.Boulos,
Calculation of the gas temperature in a
through flow atmospheric pressure dielectric
barrier discharge torch by spectral line shape
analysis, Journal of applied physics, 103,
2008
[2] U Kogelschatz, Dielectric-barrier
Discharges: their history, discharge
physics, and industrial applications, Plasma
Chem. and Plasma process 23, 2003
Fig.8 Furrier Transform Infrared (FTIR)
Spectroscopy of plasma treated PET
4000 3500 3000 2500 2000 1500 1000 500
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Absorbance
Wave number [cm
-1
]
Fig.7 Furrier Transform infrared (FTIR)
Spectroscopy control sample
4000 3500 3000 2500 2000 1500 1000 500
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Absorbance
Wave number [cm-1]
R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com
ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45
www.ijera.com 45 | P a g e
[3] U. Fantz, Basics of plasma spectroscopy,
Plasma Source Science Technol. 15, 2006,
137-147
[4] N. Balcon, A. Aanesland and R. Boswell.,
Pulsed RF discharges, glow and filamentary
mode at atmospheric pressure in argon,
Plasma Source Science. Technol.16, 2007,
217-225,
[5] X. M. Zhu., W. Cong-Che. and Y.K. Pu.,
Gas temperature, electron density and
electron temperature measurement in a
microwave excited microplasma, J. Phy.D:
Appl. Phys. 41, 2008.
[6]. N. Ohno, M. A. Razzak H.Ukai, S
Takamura and Y.Uesugi, Validity of
electron temperature measurement by using
boltzmann plot method in radio frequency
inductive discharge in the atmospheric
pressure range, Plasma and fusion research,
1, 2006.
[7]. R. B. Tyata, D. P. Subedi, R. Shrestha and
C.S.Wong, Generation of uniform
atmospheric pressure argon glow plasma by
dielectric barrier discharge, Pramana
Journal of Physics Indian Academy of
Sciences 80, 2013
[8] Z. Buntat, J .E. Harryand I. R. Smith,
Generation of a homogeneous glow
discharge in air at atmospheric pressure,
ELECTRIKA, 9, 2007, 60-65
[9] C. Jie-Rong, W. Xue-Yan, W. Tomiji,
Wettability of Poly(ethylene Terephthalate)
Film Treatedwith Low-Temperature Plasma
and Their Surface Analysis by ESCA,
Journal of Applied Polymer Science,72,
1999, 1327–1333
[10] I. Novák, I. Chodák, J. Sedlia_Ik, M.
Števiar, A. Popelka, J. Kopný, Investigation
of poly(ethylene terephthalate) treated by
low-temperature plasma. Annals of Warsaw
University of Life Sciences – SGGW
Forestry and Wood Technology 72, 2010,
83-89
[11] M Żenkiewicz, Methods for the calculation
of surface free energy of solids, Journal of
Achievements in Materials and
Manufacturing Engineering. 24, 2007.
[12] U.M.Joshi and D.P.Subedi, Surface
Treatement Of High Density Polyethylene
In Air And Argon/Air Mixture At
Atmospheric Pressure, International Iournal
of Engineering Research and Application, 5,
2015
[13] S. J. Park and H.Y. Lee, Effect of
atmospheric-pressure plasma on adhesion
characteristics of polyimide film, Journal of
Colloid and Interface Science 285, 2005,
267- 272.
[14] M. Drobota, M. Aflori, V. Barboiu,
Immobilization on poly(ethylene
terephthalate) films modified by plasma and
chemical treatments. Digest Journal of
Nanomaterials and Biostructures 5,(1),
2010, 35 - 42.
[15] Yu. S. Akishev, M.E. Grushin, A.I.
Drachev, V.B. Karalnik, A.V. Petryakov
And N.I. Trushkin, On Hydrophilicity
Ageing of PP and PET Films Induced by
Ultraviolet Radiation and Hydrogen Atoms,
The Open Plasma Physics Journal, 6,2013,
19-29.

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Experimental Study of an Atmospheric Pressure Dielectric Barrier Discharge and PET Surface Modification

  • 1. R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45 www.ijera.com 41 | P a g e Experimental Study of an Atmospheric Pressure Dielectric Barrier Discharge and PET Surface Modification R. Shrestha1,2,* , D. P. Subedi1 1 Department of Natural Sciences, School of Science, Kathmandu University, Dhulikhel, Nepal 2 Department of physics, Basu college/Basu H.S.S, Bhaktapur, Nepal ABSTRACT A homogeneous dielectric barrier discharge (DBD) in argon was produced by applying high voltage A.C. source of potential difference (0-20) kV operating at a frequency of 10-30 kHz across two parallel plate electrodes with glass as dielectric barrier. The discharge was characterized by optical emission spectroscopy (OES) and electrical measurement. Four argon emission lines from the discharge were analyzed and the electron temperature was estimated by line intensity ratio method. The electron density in the discharge was estimated by power balance method. An investigation of the effect of inter-electrode distance on the electron density was made. The results showed that the electron temperature is less than 1 eV and the electron density is of the order of 1011 cm-3 which varied with the inter electrode distance. Discharge was applied for surface modification of polyethylene terepthalate (PET). Modified surfaces were studied by contact angle measurement and FTIR spectroscopy. Key words: Electron temperature, electron density, DBD, optical emission spectroscopy, power balance. I. Introduction Atmospheric pressure dielectric barrier discharges (DBDs) are non thermal and non equilibrium plasmas [1]. Atmospheric pressure non equilibrium plasmas have been widely studied for several emerging applications such as surface and material processing biological and chemical decontamination of media, light source, absorption and reflection of electromagnetic radiation and synthesis of nanomaterials [2]. This process can be improved by a better understanding of basic plasma phenomena and by knowing its properties. The plasma properties depend on several parameters, such as, the electrode geometry, cooling system, excitation frequency, power injected, gas composition and type of dielectric barrier [3]. The electron density and electron temperature are the most fundamental parameter in gas discharges and play a very important role in understanding the discharge physics and optimization of the operation of plasma [3, 4]. Different methods are employed to measure the electron density and electron temperature in plasma. In atmospheric-pressure discharge system, both the probe and the microwave- based methods are difficult to use due to the small plasma dimension and strong collision process. The OES based technique is suitable for measurement of electron density and electron temperature. To measure the electron temperature line intensity ratio method is used, in which the intensity ratio of emission lines is related to electron temperature and electron density. OES has been used for the measurement of electron temperature and electron density in different types of plasmas [5, 6, 7, 8]. Low temperature plasmas are widely applied for the surface treatment of polymers because of their several advantages over other conventional methods. Jie-Rong, et al reported wettability of Poly(ethylene Terephthalate) film treated with low-temperature plasma and their surface analysis by ESCA[9]. Novák et al also studied the surface propertis of poly(ethylene terephthalate) treated by low-temperature plasma [10]. The present experiment uses a power supply working at 27 kHz to produce the discharge at atmospheric pressure. The discharge is found to spread homogeneously over the whole area of the electrode and known as the atmospheric pressure glow discharge (APGD). In this paper, electron temperature in atmospheric pressure DBD in air/argon environment is measured by line intensity ratio method and electron density is determined by power balance method. The relationship between the surface wettability and the surface structure of PET is investigated by FTIR spectroscopy. The change in hydrophilic property of the sample has been studied. II. Experimental The experimental arrangement is shown in Fig.1. The electrodes are made up of two brass discs, 7mm thick and 51mm in diameter. A glass plate of thickness 1.2mm was used as dielectric barrier between the electrodes. A high voltage AC source (0- RESEARCH ARTICLE OPEN ACCESS
  • 2. R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45 www.ijera.com 42 | P a g e 13 7 9 11 1 2 3 4 5 6 10 8 14 12 20) kV and frequency (10-30) kHz was applied to electrodes through a current limiting resister of 10k. The whole apparatus is enclosed in a cylindrical chamber and argon is passed into it at a flow rate of 2l/m. The applied voltage and current were measured by high voltage probe (Tektronics TDS2000). The experiment were conducted with inter electrode spacing varying between 1-3mm Fig:1: Schematic diagram of the experimental set- up. 1-Gas inlet, 2- power electrode, 3-Discharge, 4- Glass plate , 5-Grounded electrode, 6- Plasma reactor, 7- Resistance 10 k, 8- Linear Array Spectrometer VS140, 9- Voltage probe, 10- Power supply (A.C), 11-Osciloscope , 12-Computer, 13- Resistance 10 M , 14- Teflon screw. Optical emission spectra were recorded by liner array optical spectrometer (Lynear VS140). Contact angles were measured by rame hart goniometer. The ATR-FTIR spectroscopy measurements of PET foils were performed with IR Prestige-21, shimadzu, Japan having a resolution of 4 cm-1 , a scan range was 4000 – 400 cm-1 , and a total of 50 scans per analysis. III. Result and Discussion 3.1 Measurement of Electron Temperature by Line Intensity Ratio Method: Fig: 2 shows the OES of the discharge in the range of 250nm-850nm. The applied voltage, discharge current and spectrum are simultaneously measured and analyzed for determination of electron temperature. Using line intensity method, four suitable lines (two for ArI and two for ArII are chosen and electron temperatures is estimated using the lines intensity ratio method. For the measurement of electron temperature, equation (1) is used [5,6,7]. Where R is the ratio of intensity of two lines, I is the intensity of spectral lines, Aij is the transition probability of the transition ij, gi - The statistical weight of the upper level,  - wave length of the radiation, Ei - energy of the upper level, K - Boltzmann constant and Te - electron temperature Considering two Ar I lines of wavelength 696.54 nm, and 751.034 nm and two Ar II lines with wavelength 314.13 nm and 378.75 nm and plot of R1/R2 against Te has been made, the electron temperature has been found to be 0.89eV. This result is in good agreement with the results reported in previous work. Electron temperature thus determined is used to calculate the electron density by using the Eq. (2) given below The use of Eq. (2) is made for calculation of ne from different lines and average values of ne= 3.47032×1011 cm-3 is obtained. 3.2 Determination of Electron Density by Power Balance Method The glow mode discharge is homogeneously spread over the whole electrode area, so the plasma density can be estimated from a power balance method. In this method electron density is given by [7]. (3) 2 e b lost p n Aev E      Where A - Area of each electrode=20.43cm2 , vb - Bohm velocity = 2×105 cms-1 , Elost = 50eV (in our 3 2 1 21 1 2 2 2 2 2 1 1 2 2 [ ] (2)e e i e e m kT E E EI A g n Exp I A g h KT                           100 200 300 400 500 600 700 800 900 0 10000 20000 30000 wavelength (nm) Intensity(Au) Fig. 2 Optical emission lines of atmospheric pressure discharge produced in Argon. 1 1 2 2 3 4 exp .....(1) pq p xy p r x urs uv u rs r pq xy x uv e A g E E E EA gR I I R I I A g A g kT                                        
  • 3. R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45 www.ijera.com 43 | P a g e condition), Applied frequency = 27 kHz, Gas flow rate 2l/min, Dielectric = 1.5mm thick glass. By using Eq. (3) electron density was calculated for different value of applied voltage and the variation of electron density with applied voltage is shown in Fig 4. It is evident that electron density increases linearly with the applied voltage. 3.3 Measurement of Contact Angle and Surface Energy Contact angles were measured on PET surface treated with APPJ in argon for exposure time 0–60 seconds. The measurements of the contact angles were performed by contact goniometer using distilled water and glycerol on different positions of the treated sample. Surface energy was calculated using the Owens-Wendt Kaelble method. In this method, it is possible to determine the solid surface energy (γ) as the sum of polar (γp ) and dispersive (γd ) contribution using at least two different test liquids (water and glycerin) [9, 10, 11,12] The dependence of contact angle and surface energy on exposure time for PET is shown in Fig: (5 and 6). The images of water drops on the surface of untreated and plasma treated PET sample are shown in the inset of Fig 5. The value of contact angle decreases and consequently the surface energy increases with the treatment time. The increase in surface free energy is attributed to the functionalization of the polymer surface with hydrophilic groups. 3.4 Surface Analysis of PET The wettability of the sample is related to the presence of a particular functional group that resides on the outermost surface layer. The relationship 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 1.5 2.0 2.5 3.0 3.5 4.0 Electrondensity(10 11 )/cm 3 Applied Voltage (kV) Fig 4: Electron density as a function of applied voltage.   1 1 2 21 cos 2 2 (4)d d p p l l s l s               Fig 5: Water contact angle on PET as function of treatment time in Argon plasma 0 10 20 30 40 50 60 30 35 40 45 50 55 60 65 70 Treatment Time (Sec) Surfaceenergyoftreatedpolymer(PET) Fig 6: Surface energy of PET as function of treatment time in Argon plasma 0 10 20 30 40 50 60 20 30 40 50 60 70 80 ContactAngle Treatment Time (Sec) Fig.3: Voltage and current waveforms of discharge. -60.0µ -40.0µ -20.0µ 0.0 20.0µ 40.0µ 60.0µ -6 -4 -2 0 2 4 6 voltage Current(mA) Time(s) voltage(kv) -30 -20 -10 0 10 20 30 current
  • 4. R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45 www.ijera.com 44 | P a g e between the surface chemical structure and surface wettability of plasma treated PET was characterized by Fourier Transform Infrared (FTIR) Spectroscopy. . The chemical changes in surface properties of plasma-treated polymer are analyzed using ATR- FTIR spectroscopy. Fig.7 shows the ATR-FTIR spectra of unmodified PET. FTIR spectra for PET treated in atmospheric pressure plasma in Ar gas is shown in Fig 8 for comparison. It is also observed from the FTIR spectra (Fig. 7and 8) that there is a change in intensity of absorption peaks corresponding to certain functional groups. The wave number region: from 3600 to 2500 cm−1 , where the C–H and O–H stretching vibrations of different types of H-bonds occur. Spectrum of PET has the characteristic absorption peaks at 1714 cm-1 (C=O bonds), 1410, 1018, and 872 cm-1 (vibration of aromatic ring), 1340 and 1177 cm-1 (bending vibration of -CH2 groups), 1244 and 964 cm-1 (stretching vibration of C-O bonds), 690 cm-1 and 750 cm-1 phenyl group ( =C-H & C=C ) 1124 and 1100 cm-1 (stretching vibration of C-O bonds due to amorphous and crystalline structure of PET respectively) [12,13,14]. For PET treated in APPJ, the broadening of the C=O stretch at 1714 cm-1 has appeared due to creation of oxygen-containing sites . The information from the FTIR spectra indicates that the carbon content decreases and the oxygen content increases in the surface of PET, and a large amount of oxygen polar functional groups are introduced into the surface of plasma-treated PET. This is responsible for improving the wettability of PET. IV. Conclusion Atmospheric pressure argon plasma has been produced and characterized by optical and electrical methods. Electron density (ne) and Electron temperature (Te) were found to be 3.361011 cm-3 and 0.786eV respectively with the electrode gap of 2mm. Electron density and electron temperature were found to be dependent on the applied voltage for constant inter electrode distance. Atmospheric pressure argon plasma treatment of PET surface resulted an improvement on hydrophilicity. It is mainly due to the increase in the polar component of the surface free energy after plasma treatment which indicates the formation of polar functional groups on the surface. The improvement of wettability of PET strongly depends on the treatment time. This system can be very useful for the treatment of thermally sensitive materials and also for the treatment of biological samples. V. Acknowledgement This work was supported by the National Academy of Sciences NAST Nepal. Authors would like to thank Dr. Rajani Sakya and Dr. Aswani Kumar Shrestha, Department of Pharmacy, School of Science, Kathmandu University for FTIR analysis of the samples. Reference [1] A. Lonascut-Nedelcescu, C. Carlone, U. Kogelschatz, D.V.Gravelle and M.I.Boulos, Calculation of the gas temperature in a through flow atmospheric pressure dielectric barrier discharge torch by spectral line shape analysis, Journal of applied physics, 103, 2008 [2] U Kogelschatz, Dielectric-barrier Discharges: their history, discharge physics, and industrial applications, Plasma Chem. and Plasma process 23, 2003 Fig.8 Furrier Transform Infrared (FTIR) Spectroscopy of plasma treated PET 4000 3500 3000 2500 2000 1500 1000 500 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 Absorbance Wave number [cm -1 ] Fig.7 Furrier Transform infrared (FTIR) Spectroscopy control sample 4000 3500 3000 2500 2000 1500 1000 500 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 Absorbance Wave number [cm-1]
  • 5. R. Shrestha Int. Journal of Engineering Research and Applications www.ijera.com ISSN : 2248-9622, Vol. 5, Issue 5, ( Part -6) May 2015, pp.41-45 www.ijera.com 45 | P a g e [3] U. Fantz, Basics of plasma spectroscopy, Plasma Source Science Technol. 15, 2006, 137-147 [4] N. Balcon, A. Aanesland and R. Boswell., Pulsed RF discharges, glow and filamentary mode at atmospheric pressure in argon, Plasma Source Science. Technol.16, 2007, 217-225, [5] X. M. Zhu., W. Cong-Che. and Y.K. Pu., Gas temperature, electron density and electron temperature measurement in a microwave excited microplasma, J. Phy.D: Appl. Phys. 41, 2008. [6]. N. Ohno, M. A. Razzak H.Ukai, S Takamura and Y.Uesugi, Validity of electron temperature measurement by using boltzmann plot method in radio frequency inductive discharge in the atmospheric pressure range, Plasma and fusion research, 1, 2006. [7]. R. B. Tyata, D. P. Subedi, R. Shrestha and C.S.Wong, Generation of uniform atmospheric pressure argon glow plasma by dielectric barrier discharge, Pramana Journal of Physics Indian Academy of Sciences 80, 2013 [8] Z. Buntat, J .E. Harryand I. R. Smith, Generation of a homogeneous glow discharge in air at atmospheric pressure, ELECTRIKA, 9, 2007, 60-65 [9] C. Jie-Rong, W. Xue-Yan, W. Tomiji, Wettability of Poly(ethylene Terephthalate) Film Treatedwith Low-Temperature Plasma and Their Surface Analysis by ESCA, Journal of Applied Polymer Science,72, 1999, 1327–1333 [10] I. Novák, I. Chodák, J. Sedlia_Ik, M. Števiar, A. Popelka, J. Kopný, Investigation of poly(ethylene terephthalate) treated by low-temperature plasma. Annals of Warsaw University of Life Sciences – SGGW Forestry and Wood Technology 72, 2010, 83-89 [11] M Żenkiewicz, Methods for the calculation of surface free energy of solids, Journal of Achievements in Materials and Manufacturing Engineering. 24, 2007. [12] U.M.Joshi and D.P.Subedi, Surface Treatement Of High Density Polyethylene In Air And Argon/Air Mixture At Atmospheric Pressure, International Iournal of Engineering Research and Application, 5, 2015 [13] S. J. Park and H.Y. Lee, Effect of atmospheric-pressure plasma on adhesion characteristics of polyimide film, Journal of Colloid and Interface Science 285, 2005, 267- 272. [14] M. Drobota, M. Aflori, V. Barboiu, Immobilization on poly(ethylene terephthalate) films modified by plasma and chemical treatments. Digest Journal of Nanomaterials and Biostructures 5,(1), 2010, 35 - 42. [15] Yu. S. Akishev, M.E. Grushin, A.I. Drachev, V.B. Karalnik, A.V. Petryakov And N.I. Trushkin, On Hydrophilicity Ageing of PP and PET Films Induced by Ultraviolet Radiation and Hydrogen Atoms, The Open Plasma Physics Journal, 6,2013, 19-29.