Study of the micro-discharges / metallic surfaces interactions for a better understanding of the growth mechanisms within the PEO process Vitalios Ntomprougkidis To cite this version: Vitalios Ntomprougkidis. Study of the micro-discharges / metallic surfaces interactions for a better understanding of the growth mechanisms within the PEO process. Plasma Physics [physics.plasm-ph]. Université de Lorraine, 2020. English. NNT : 2020LORR0077. tel-02961871 HAL Id: tel-02961871 https://hal.univ-lorraine.fr/tel-02961871 Submitted on 8 Oct 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. AVERTISSEMENT Ce document est le fruit d'un long travail approuvé par le jury de soutenance et mis à disposition de l'ensemble de la communauté universitaire élargie. Il est soumis à la propriété intellectuelle de l'auteur. Ceci implique une obligation de citation et de référencement lors de l’utilisation de ce document. D'autre part, toute contrefaçon, plagiat, reproduction illicite encourt une poursuite pénale. Contact : [email protected] LIENS Code de la Propriété Intellectuelle. articles L 122. 4 Code de la Propriété Intellectuelle. articles L 335.2- L 335.10 http://www.cfcopies.com/V2/leg/leg_droi.php http://www.culture.gouv.fr/culture/infos-pratiques/droits/protection.htm UNIVERSITE DE LORRAINE Ecole Doctorale : Chimie – Mécanique – Matériaux - Physique Institut Jean Lamour Département Chimie et Physique des Solides et des Surface THESE Soutenue le 15 Juillet 2020 Pour obtenir le grade de Docteur de l’Université de Lorraine Spécialité : Physique – Physique des plasmas et applications par Vitalios NTOMPROUGKIDIS Etude de l'interaction micro-décharges / surfaces métalliques pour une meilleure compréhension des mécanismes de croissance lors du procédé PEO (Titre en anglais) Study of the micro-discharges / metallic surfaces interactions for a better understanding of the growth mechanisms within the PEO process Jury Rapporteurs ARURAULT Laurent Professeur, CIRIMAT, Université de Toulouse LAVISSE Luc Maître de conférences, ICB, Université de Bourgogne Examinateurs CHAMPEAUX Corinne Professeure, IRCER, Université de Limoges BESLAND Marie-Paule Directrice de recherche, IMN, Université de Nantes VEYS-RENAUX Delphine Maître de conférences, IJL, Université de Lorraine Directeur de thèse HENRION Gérard Directeur de recherche, IJL, Université de Lorraine Co-directeur MARTIN Julien Maître de conférences, IJL, Université de Lorraine Acknowledgements Acknowledgements First of all, I would like to express my sincere gratitude to my supervisor, Gérard Henrion, for accepting me in this project, for putting his trust and belief in my capability to carry out this research. I am grateful for his guidance, mentorship and support during these three years, from which I have learned a lot. One could not ask for a better supervisor. Thank you very much. I would also like to thank my co-supervisor, Julien Martin, with whom we had an excellent collaboration conducting all the experiments of this work. For his guidance and tutoring on experimental procedures, for all our discussions analysing our results and all the advices he provided on multiple occasions. A very special thanks to Alexandre Nominé for all the work we have done together, particularly for the discussions we had and his scientific advices and help. It was a real pleasure to share an office in a very friendly and enjoying environment both professionally and personally. I would like to acknowledge the members of the CC3M competence cluster for their contributions in this work. I am thankful to Sandrine Mathieu and Christine Gendarme for their tutoring and their advices on the SEM microscope, to Stéphanie Bruyère and Sylvie Migot for their contributions with the TEM analysis, Erwan Etienne for his help in metallurgical post-treatments. For their help and advices on XRD measurements and analysis, I would like also to thank Pascal Boulet and Sebastien Diliberto from the x-gamma competence cluster. I would like to thank Ilya Bardin from MISIS university of Moscow, with whom I had the pleasure to work in person, discuss and learn from. A great amount of this work involved people from within the Institute Jean Lamour as well as outside the laboratory. I would like to thank Pauline Haraux, Komlan Akoda, Alexandre Bastien, Pascal Brenot, Guillaume Ezo’o, A. Maizeray, O. Ferry and Julien Jourdan for their contributions in this thesis. Charles Roux-Pertus for his help in thickness and porosity calculations. I would very much like to thank all the colleagues of the laboratory for their help, each one in their own way. Vincent Guigoz, Stephane Cuynet, Thierry Czerwiec, Mohammed Belmahi, Maike Thal for their input in my work with occasional discussions to resolve some of the problematics concerning this research. A great thanks to Cédric Noël for his tutoring, support and constant availability on spectroscopic measurements and analysis methods and to Régis Reigner for his technical support. I would like to express my appreciation to Christine Sartori, Georges Billant, Martine Tailleur, Nathalie Niclas, Valerie Frank and Anne-Marie Airault for their help in administrative procedures. I Acknowledgements These three years would have not been the same without the friends I met and from whom I received a warm welcome in and outside the laboratory. Fahad, Joseph, Christophe, Alejandro, Claudia at first and later on Alexis, Marianna, Feriel, Agathe, Shantanu. Thank you guys for all the wonderful moments we have spent. I would like also to thank the Greek community of Nancy, Katerina Cael, Ortho Salomon, Alexandros Petrelis, for their help and support from the very moment of my arrival to Nancy. I am grateful to LabEx DAMAS (Laboratoire d’ Exellence Design of Alloy Metals for low-mAs Structures) for financing this doctoral scholarship. Finally, I would like to thank my family in Greece, my brother and particularly my parents. Their constant support, encouragement, love and care was invaluable during all this period. II Table of Contents Table of Contents General Introduction ......................................................................................................................... 1 Chapter I - State of the art ................................................................................................................ 5 I.1 Introduction .............................................................................................................................................. 5 I.2 Plasma Electrolytic Oxidation .................................................................................................................. 5 I.2.1 Historical development of PEO ......................................................................................................... 5 I.2.2 Processing principle .......................................................................................................................... 6 I.2.3 Supplying modes ............................................................................................................................... 7 I.2.4 Influence of PEO processing parameters .......................................................................................... 8 I.2.4a Effect of the electrolyte ................................................................................................................. 9 I.2.4b Influence of the electrical parameters ......................................................................................... 12 I.3 “Soft” regime ......................................................................................................................................... 14 I.4 Properties of micro-discharges ............................................................................................................... 16 I.4.1 Spatial characteristics ...................................................................................................................... 17 I.4.2 Temporal characteristics ................................................................................................................. 17 I.4.3 Physical properties of the micro-discharges .................................................................................... 19 I.5 Structural properties of PEO oxide coatings .......................................................................................... 21 I.6 Growth mechanisms ............................................................................................................................... 24 I.7 Conclusions of Chapter I ........................................................................................................................ 26 Chapter II - Experimental considerations ..................................................................................... 29 II.1 Introduction of the chapter II ................................................................................................................ 29 II.2 Experimental installation .....................................................................................................................