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Experimental Characterization of the Underwater Pulsed Electric Discharge Tetiana Tmenova

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Experimental Characterization of the Underwater Pulsed Electric Discharge Tetiana Tmenova Experimental characterization of the underwater pulsed electric discharge Tetiana Tmenova To cite this version: Tetiana Tmenova. Experimental characterization of the underwater pulsed electric discharge. Plas- mas. Université Paul Sabatier - Toulouse III, 2019. English. NNT : 2019TOU30248. tel-02651366 HAL Id: tel-02651366 https://tel.archives-ouvertes.fr/tel-02651366 Submitted on 29 May 2020 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. To my grandparents, parents, and Eduardo. Acknowledgements First and foremost, I thank my dissertation advisors, professors Yann Cressault and Anatoly Veklich, for bringing the idea of joint French- Ukrainian thesis supervision into life, for assigning me this pioneering role, and for their valuable guidance and support. I would like to express special gratitude to my French co-supervisor, M. Flavien Valensi, for his endless patience and motivation, direction and articulation throughout the course of this work. His interest in this work and his style of advising has motivated me to put in my best effort. I would also like to thank my committee members Prof. Pellerin, Prof. Anisimov, Mme Rond and M. Tsiolko for serving on my committee. I would also like to thank my Ukrainian co-supervisor, M. Viacheslav Boretskij, for his valuable practical inputs regarding the research, equipment and spectroscopy in general. Special thanks to all my colleagues from Kiev and Toulouse, both inside and outside the lab. Many of them have become much more than that. I would like to acknowledge the support of the Prof. Lopatko from the National University of Life and Environmental Sciences of Ukraine. I would never have gone this far without him teaching me how to run a synthesis reactor and sharing many of interesting ideas. Last but not the least, I want to thank my family and friends for supporting my PhD endeavor. Thanks to my parents, my sisters and my very special "new" family for their encouragement, motivation and support in the moments of need. 7 Abstract Although electric spark dispersion processes have been known for a while, the plasma created during this process is not well-studied and understood. The complexity of the phenomena occurring during the underwater electric discharges brings additional obstacles to experimental characterization of such plasmas imposed by as small sizes of plasma and their often-short duration, difficult environment of the discharge, its stochastic nature and poor reproducibility. The main objective of this thesis was set on the investigation of the plasma occurring during the synthesis of metal colloids by an electrospark dispersion generator. The first success of this work was simply to show the applicability of optical emission spectroscopy diagnostics to such discharges. The efforts made for the development of the effective experimental approach in order to meet this research objective have been well rewarded. The results obtained in this work allow to draw interesting conclusions about the physical properties of the underwater pulsed electric discharge plasma of the considered configuration. Discharge ignites from the short circuit and molten bridge mechanism. Ignition of the arc is characterized by formation of bubble resulting from a pressure shockwave. High-speed imaging allowed to distinguish two phases in the discharge lifetime: plasma in water, and plasma in bubble formed afterwards. From the vapor condensation point of view, these two phases presumably lead to different quenching conditions, and, consequently, to the different synthesis conditions. In the case of discharge generated between molybdenum electrodes, there is a slowly-decaying light emission after the end of the discharge which can be attributed to the ejection of eroded metallic particles. The energy dissipation on the electrodes was found to be different for copper and molybdenum: due to the lower thermal conductivity of molybdenum, smaller portion of energy transferred to the electrodes results in higher energy input into the arc column. Spectroscopic measurements allowed to establish that plasma density (~ 1017 cm−3) and moderate temperature (0.6 – 0.95 eV) correspond to a pressure greater than 1 bar. Moreover, plasma presents several non-ideal effects, such as broadening and the asymmetrical shape of the Hα line and absence of Hβ line. In general, plasma properties were found to be relatively insensitive to most of the discharge parameters, such as the discharge current or the type of liquid 8 with the main differences being associated to the used electrodes material. Key words: electric discharge, plasma in liquid, emission spectroscopy 9 Résumé Bien que le procède de dispersion par arc électrique soit connu depuis un certain temps, le plasma formé durant ce procédé est encore peu étudié et compris. La complexité des phénomènes se produisant durant les décharges immergées génèrent de nouveaux obstacles à la caractérisation de tels plasmas, du fait de la faible taille et de la durée souvent très courte, les difficultés liées à l’environnement de la décharge, leur nature stochastique et la faible reproductibilité. Le principal objectif de cette thèse est l’étude du plasma se formant lors de la synthèse de colloïdes métalliques par un générateur de dispersion par étincelle électrique. Le premier résultat concluant de ce travail a été de démontrer la faisabilité de la spectroscopie optique d’émission pour le diagnostic de telles décharges. Les efforts réalisés pour le développement d’une approche expérimentale ont permis d’atteindre les objectifs de recherche. Les résultats obtenus au cours de ce travail permettent de tirer des conclusions intéressantes sur les propriétés physiques des plasmas de décharge électrique pulsée dans la configuration étudiée. La décharge est créée à partir d’un court-circuit et d’un amorçage par pont fondu. L’allumage de l’arc est caractérisé par la formation d’une bulle causée par une onde de choc de pression. L’imagerie rapide a permis de distinguer deux phases dans la durée de vie de la décharge : d’abord un plasma dans l’eau, puis un plasma à l’intérieur d’une bulle de gaz formée par la suite. Du point de vue de la condensation de la matière vaporisée, on peut s’attendre à ce que ces deux phases conduisent à des conditions de trempe différentes, et en conséquence des conditions de synthèse différentes. Dans le cas d’une décharge générée entre des électrodes en molybdène, une émission de lumière décroissant lentement après la fin de la décharge se produit, ce qui peut être attribué à l’éjection de particules métalliques érodées. La dissipation de l’énergie aux électrodes s’est avérée être différente pour le cuivre et le molybdène : du fait d’une conductivité thermique plus faible pour le molybdène, une part plus faible de l’énergie transférée aux électrodes conduit à une part plus importante de l’énergie fournie à la colonne d’arc. Les mesure par spectroscopie optique d’émission ont permis d’établir que la densité (~ 1017 cm−3) et la température modérée (0.6 – 0.95 eV) du plasma correspondent à une pression supérieure à 1 bar. Il présente donc 10 quelques effets non-idéaux, tels que l’élargissement et la forme asymétrique de la raie Hα et l’absence de la raie Hβ. En général, les paramètres du plasma se sont avérés être relativement insensibles à la plupart des paramètres de la décharge, tels que le courant de décharge ou le type d’eau, les principales différences étant liées aux matériaux des électrodes utilisées. Mots-clés : décharge électrique, plasma immergé, spectroscopie d’émission 11 Table of Contents Acknowledgements 7 Abstract 8 Résumé 10 List of figures 14 List of tables 19 1. Introduction 23 1.1 Context and motivation 23 1.2 Objectives and structure of the thesis 27 References to chapter I 30 2. Discharges in liquid: state of the art 35 2.1 Introduction 35 2.2 The wide variety of plasma-liquid reactors 35 2.3 Plasma generation in liquid for nanomaterial synthesis 38 2.4 Direct in-liquid discharge between two electrodes 39 2.5 Plasma diagnostics of electric discharges in water 44 2.5.1 Electric Discharge Machining (EDM) – a perfect case of a low- voltage underwater electric discharge plasma 45 2.5.2 EDM discharge plasma imaging and visualization 48 2.5.3 EDM discharge plasma diagnostics 53 2.6 Conclusions 62 References to chapter II 65 3. Experimental setups and methodology 73 3.1 Introduction 73 3.2 Experimental setup for multiple-pulse underwater electric discharge investigation 75 3.2.1 Electric spark dispersion of metals 75 3.2.2 Experimental setup description 75 3.2.3 Plasma emission registration 80 3.3 Experimental setup for single-pulse underwater electrical discharge investigation 83 3.3.1 General description 83 3.3.2 Impulse generator and electrical measurements 84 12 3.3.3 Optical characterization: high-speed imaging and spectroscopy 88 3.3.4 Electrodes and liquid media 91 3.4 Optical emission spectroscopy of the underwater electric discharge plasma 92 3.4.1 Sensitivity calibration 92 3.4.2 Abel inversion 94 3.4.3 Determination of plasma parameters 97
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