On phenomena in ionized gases
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- 3. References
- Control methods of RONS in Dielectric Barrier Discharge
- 3. Experimental Results
- A novel non-invasive technique for detection and analysis of harmonics in Radio Frequency plasmas
- 3. Results and Conclusions
- Oscilloscope HDO4032 Ch1 Ch2 50 Ω 50 Ω
- Active and passive optical diagnostics in a model HV circuit breaker
- 1. Introduction and Experimental Set-Up
- 2. Results and Discussion
- O-atom (777nm) N-ion (568nm)
- Photoluminescence of plasma produced graphene quantum dots
1. General Although already more than two decades ago the feasibility of the deposition of nanocrystalline diamond (NCD) has been shown [1], the further development of this technology is still of great importance, in particular, as far the treatment of large substrates at relatively low temperatures is concerned. The physical properties of NCD are comparable to polycrystalline diamond (PCD), however, compared to PCD, NCD films are characterized by a very low roughness, which is independent on the thickness of the layers. A wider commercial use of NCD films has been limited so far (i) by insufficient adhesion properties to substrates and (ii) by the requirement of high substrate temperatures above 800 °C damaging sensitive substrates in the deposition process.
In 2007 Latrasse and co-workers developed a new approach to provide high density microwave plasma sources for large area depositions while ensuring relatively low substrate temperatures below 400 °C. This new concept to realize a planar reactor comprises a 2-dimensional matrix of several single microwave plasma source elements without using magnetic fields [2]. Based on this 2-dimensional matrix approach of microwave antennas a 4 x 4 configuration has been successfully used to deposit uniform NCD films with very low surface roughness between 5 – 10 nm and a grain size in the range of 10 – 20 nm on a 4 inch wafer in 2014 [3]. The deeper understanding of the complex chemistry in H 2 -CH
4 -CO
2 microwave plasmas will be a crucial step for the further improvement of large scale NCD deposition at low substrate temperatures. In the present contribution optical emission spectroscopy in the visible spectral range has been combined with absorption spectroscopy (AS) in the mid-infrared spectral. For the latter one two different radiation sources have been used. Firstly, traditional lead salt lasers, since several decades employed in tunable diode laser absorption spectroscopy. Secondly, a new laser class, external cavity quantum cascade lasers (EC-QCLs), which up to now have only been used in limited cases in plasma diagnostics. In contrast to lead salt lasers EC-QCLs can be tuned over a spectral range greater than 100 cm -1 with a mode-hop free tuning range of the order of 80 cm -1 . 3. Results Using AS the absolute concentrations of the methyl radical and of five stable molecules, CH 4 , CO 2 , CO, C 2 H 2 and C 2 H 6 , were monitored in the reactor. Reliable information about the neutral gas temperature is a crucial precondition for the determination of concentrations of molecular species. Monitoring a variety of CO lines in the ground state and in three hot bands enabled an extensive temperature analysis providing novel insights into energetic aspects of the multi component plasma. An additional target was to derive fragmentation rates of the CH 4 and CO 2
precursors and their conversion rates to the reaction products. The influence of the discharge parameters power and pressure on the molecular concentrations was another focus of interest.
[1] D. M. Gruen, X. Pan, A. R. Krauss, S. Liu, J. Luo, C.N. Foster, J. Vac. Sci. Technol. A 12 (1994) 1491. [2] L. Latrasse, A. Lacoste, J. Sirou, J. Pelletier, Plasma Sources Sci. Technol. 16 (2007) 7. [3] H.-A. Mehedi, J. Achard, D. Rats, O. Brinza, A. Tallaire, V. Mille, F. Silva, C. Provent, A. Gicquel, Diamond Rel. Mat. 47 (2014) 58. 14 69
XXXIII ICPIG, July 9-14, 2017, Estoril/Lisbon, Portugal
Control methods of RONS in Dielectric Barrier Discharge
Seungmin Ryu, Hyeongwon Jeon, Sangheum Eom, Jungwoo Yoon, Suk Jae Yoo and Seong Bong Kim
P
Plasma in natural air condition can produce reactive oxygen and nitrogen species (RONS) simultaneously but ROS (Reactive Oxygen Species) and RNS (Reactive Nitrogen Species) has different application in the field of postharvest. ROS is a powerful disinfectant and RNS is an inhibitor of agri-food ripening. Therefore the production rate control of RONS is important. Frequency and flowrate of air can be methods of RONS concentration control factor. Applied frequency range was from 0.1 to 8 kHz and atmospheric air flow rate was from 0 to 20 l/m. The generation rates of O 3 , NO and NO 2 were measured by the gas analysers. As external air flow rate was increased, the generation rate of O 3 was increased from 0 to 3.61 mg/min. In the contrary, the generation rate of NO was decreased from 0.21 to 0 μg/min. Frequency can control the production rate of RONS and optimum ozone and NO generation frequency was 3 and 8 kHz respectively. 1. Introduction 32% of all agri-food in the world was lost or wasted per year. The big two cause of food waste is rottenness by fungi and ripening by hormone. Ozone, OH radical, O radical, hydrogen peroxide are called as ROS and it is powerful disinfectant of fungi [1]. NO and NO 2 are called as RNS and considered as a key species in hormone-regulated processes [2]. Plasma discharge of air produces complex RONS but, only particular chemical reactive species might be useful to special purpose therefore, it is necessary to produce appropriate ROS or RNS. The flow rate and frequency was selected as affecting factors of RONS production rate.
Figure 1. Experimental Set-up Figure 1 shows the experimental set-up for measurements of electrical, optical and chemical properties of plasma discharge with different flow rate and frequencies. 3. Experimental Results Figure 2 shows the results of ozone and NO concentration changes with different flow rates. As external air flow rate was increased, the generation rate of O 3 was increased from 0 to 3.61 mg/min. In the contrary, the generation rate of NO was decreased from 0.21 to 0 μg/min. Figure 3 shows the optimum frequency for generating maximum ozone or NO generation. 3 kHz is best to produce ozone and 8 kHz to nitric oxide.
5 10 15 20 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 Species O 3 NO External Air Flow Rate (lpm) O 3 ( m g /m in ) 0.00 0.05 0.10 0.15 0.20 0.25 N O (m g /m in )
Figure 2. Generation rates of O 3 and NO by flow rates
Figure 3. Concentration of O 3 (a) and NO (b) according to the frequency
Frequency and air flow rate might be related to the plasma region bulk temperature. Temperature can be one key factor of RONS production and it is necessary to study further.
This work was supported by R&D Program of ‘Plasma Advanced Technology for Agriculture and Food (Plasma Farming)’ through the National Fusion Research Institute of Korea (NFRI) funded by the Government funds. 6. Reference [1] S. Horvitz, M. J. Cantalejo, Food Science and Nutrition , 54 (2014) 312-339 [2] Lili Deng et al., Postharvest Biology and
84 (2013) 9–15 -NO 17 70
XXXIII ICPIG, July 9-14, 2017, Estoril/Lisbon, Portugal
Topic number 6
A. Rawat, A. Ganguli, R. Narayanan, R. D. Tarey Centre for Energy Studies, Indian Institute of Technology, New Delhi 110016, India
In this work, a new plasma diagnostic technique is proposed to analyze the harmonics generated in Radio Frequency (RF) discharges accurately using a Dual Directional Coupler (DDC). A careful and complete analysis not only determines the harmonics present in plasma, but also yields accurately the power in the forward and reflected waves of the fundamental and each harmonic generated in the plasma, which makes it a valuable plasma diagnostic tool. Apart from this, one can estimate the complex impedance and reflection coefficient at the plasma end for each harmonic as well as the fundamental. This non-invasive, calibrated experimental technique may prove useful in formulating a systematic model which enhances understanding of RF plasma heating at low pressures. 1. Introduction In Radio Frequency (RF) discharges, two mechanisms of electron heating play crucial roles: (i) Ohmic heating at high pressures, due to electron- neutral collisions and (ii) Stochastic heating at low pressures, due to electron-sheath interaction [1, 2]. Due to the non-linear sheath behaviour, harmonics are generated in the plasma, which need to be considered for understanding how the RF power is coupled at low pressures. In this paper, a novel, non- invasive harmonic probe technique is presented that characterizes the plasma-generated-harmonics of a parallel-plate RF discharge using calibrated broadband Dual Directional Coupler (DDC). This technique determines the dominant harmonics produced by the plasma and yields accurately the forward and reflected power in the fundamental and harmonics.
The experiment is carried out in a 13.56 MHz, RF discharge system with parallel plate electrode geometry as shown in Fig. 1. The measured plasma densities are in the range 10 9 - 10 10 cm
-3 and electron temperatures in the range 1 - 2.5 eV. The experimental parameters varied are the RF power (25 - 60 W) and Argon gas pressure (10 - 80 mTorr).
Figure 1 Experimental set up for harmonics analysis using DDC and Capacitive Probe.
A matching network was not used in the present experiments as its coupling capacitance allows the (plasma) load to develop a high DC self-bias voltage that can damage the DDC. However, an isolator has to be used to isolate the generator from the power flowing from the load to the generator. The two DDC output signals yield the total forward (from the generator to the load) and reverse (from the load to the generator) power flow in the fundamental and the harmonics. The two output signals of the DDC are actually a superposition of the fundamental and harmonics produced by the plasma. The contribution of each frequency to the total signal is carried out by Fast Fourier Transform (FFT), from which other data like forward and reflected power, complex impedance at load etc. may also be determined for each frequency.
While detailed results will be presented during the conference, the results indicate that among all the harmonics generated in the plasma, power content of the third harmonic (40.68 MHz) dominates in the present experiments. Since RF isolator absorbs all the harmonics generated from the plasma, this diagnostic gives way to characterize the different harmonics in a non-invasive manner. This precise information can be used to develop a better model for understanding power coupling in the low pressure regime.
[1] M. A. Lieberman and A. J. Lichtenberg, Principles of Plasma Discharges and Materials Processing, Wiley, New York, (1994). [2] J. Schulze, Z. Donko, D. Luggenholscher and U. Czarnetzki, Plasma Sources Sci. Technol. , 18, (2009) 034011.
DDC3001
Langmuir Probe Capacitive Probe 40dB, 0.1 – 1000 MHz P4 (reflected) Oscilloscope HDO4032 Ch1 Ch2 50 Ω 50 Ω RF Generator 13.56MHz RF Isolator 71
XXXIII ICPIG, July 9-14, 2017, Estoril/Lisbon, Portugal
Active and passive optical diagnostics in a model HV circuit breaker
E.Panousis 1 , P. Stoller 1 , J.Carstensen 1 , V.Teppati 1 , R.Methling 2 , St.Franke 2 , S.Gortschakow 2
1 ABB Corporate Research Center, ABB Schweiz AG, Baden - Switzerland 2 Leibniz Institute for Plasma Science and Technology (INP), Greifswald - Germany
We present results on the probing of an air arc in a HV circuit breaker model geometry using two distinct experimental techniques. First we apply Speckle imaging, an active refractive index based technique that yields quantitative information on the radial temperature distribution T(r) via a generalization of the Gladstone-Dale law [1]. Second, in a passive technique we use high speed video imaging of selected atomic (O-I) and ionic species (N-II) using appropriate narrow band filters. Post-processing the videos also allows to obtain T(r) based on the Fowler-Milner method [3] for the atomic emission. The results of the two techniques are found to be in good agreement.
Optical diagnostics are a non-invasive means of probing the spatio-temporal evolution of key quantities (e.g. temperature) in the understanding of the phenomena in HV switching arcs: such experimental data are important for the benchmarking of CFD simulations that are used in the development of HV gas circuit breakers. The goal of the present work is to provide such validated data by employing two distinct optical diagnostic techniques and comparing their findings. On the one hand we apply the Speckle interferometric technique [1] which probes the spatial derivative of the refractive index by illuminating the arc with a pulsed (20ns, 60kHz) Nd:YAG laser at 532nm. On the other hand we record the emissions of selected atomic and ionic lines with the use of a high speed video camera (1μs integration time, 20kfps) [2]. In both cases we record side-on images that are used for deriving 2D information by Abel inversion based on a rotational symmetry assumption. Furthermore, the temperature is estimated under an LTE assumption, that should be valid in the conditions here investigated. The aforementioned methods are employed for the probing of a switching arc in a simplified circuit breaker model suitable for such optical diagnostic measurements [1]. The test object was operated in air at an exhaust pressure of 1 bar, while the arc was blown with quasi-constant pressure in the range of 3.5 to 8 bar. Sonic flow conditions in the arcing zone are thus ensured, while the interaction of the gaseous arc with the surrounding PTFE nozzle walls and CuW electrodes is negligible. 2. Results and Discussion Fig. 1 shows the evolution of arc mantle and arc core diameters as a function of arc current (I) under a a constant blowing pressure of 8 bar. These are estimated both from Speckle measurements [1] as well as from measuring the luminous lateral extent of the corresponding video frames 0 1 2 3 4 5 0.4
0.6 0.8
1.0 1.2
0 1 2 3 4 5 Speckle (0.5
cold
) Camera (O - I) Speckle (10kK) Camera (N-II) Mant le
Cor e [mm] arc current [kA] Speckle
Speckle Video (O-I) O-atom (777nm) N-ion (568nm) Video (N-II)
diameters. The dashed eye-guides correspond to a √I law. Fig. 2 shows the radial distribution of temperature as estimated by the Speckle technique and the O-I emission intensity using the method [3]. 0 .0
0.5 1 .0
1.5 2 .0
2 .5 3.0
0 5 1 0 1 5 2 0
2 5 O -I em ission S peck le T e mp er a tur e [ k K ] rad iu s [m m ]
1kA air arc at 3.5 bar blowing pressure. We observe in both figures a good agreement between the two measurement techniques: validated measurements of a switching arc are thus obtained. 3. References [1] P.C. Stoller et al, J. Phys. D: Appl. Phys., vol. 48, 015501, 2015 [2] R. Methling et al, Plasma Phys. Technol., vol. 2, 167-170, 2015 [3]
R. H. Fowler, E. A. Milner, Roy. Astron.Soc. vol. 83, 403, 1923
Topic #6 72 XXXIII ICPIG, July 9-14, 2017, Estoril/Lisbon, Portugal
Photoluminescence of plasma produced graphene quantum dots
S. Espinho PP , N. Bundaleska, J. Henriques, F. M. Dias and E. Tatarova
P
Free-standing graphene sheets were synthesized using surface wave driven microwave plasmas, operating at 2.45 GHz stimulating frequency and at atmospheric pressure. A chemical treatment has been applied to cut the sheets and obtain small size, less than 10 nm particles, i.e. graphene quantum dots (GQDs) in an aqueous solution. The obtained suspension was then irradiated with soft UV light emitted by a commercial blue LED ( = 410 nm). The photoluminescence of GQDs was evidenced by the rise of a broad peak at 510 nm, following the main one radiated by the LED. SEM and Raman analysis further confirmed the presence of GQDs in the suspension.
Graphene quantum dots are nanometer sized fragments (< 10 nm) of graphene that demonstrate unique properties and show significant potential for many applications, ranging from energy storage and conversion, to optoelectronics and nano-medicine [1]. Their photoluminescence is one of their most promising properties for applications. However, the mechanism behind this phenomenon is not yet fully understood [2]. In the present work, free-standing graphene sheets were synthesized using microwave plasmas driven by surface waves at 2.45 GHz stimulating frequency and at atmospheric pressure as described in detail in [3, 4]. A chemical route has been applied to cut and reduce the size of the graphene sheets, so as to obtain GQDs in an aqueous solution. 450
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