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Development of New Probes Based on Carbon Nanocones for Near-Field Microscopies Germercy Paredes Guerrero

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Development of New Probes Based on Carbon Nanocones for Near-Field Microscopies Germercy Paredes Guerrero Development of new probes based on carbon nanocones for near-field microscopies Germercy Paredes Guerrero To cite this version: Germercy Paredes Guerrero. Development of new probes based on carbon nanocones for near-field mi- croscopies. Materials. Université Paul Sabatier - Toulouse III, 2020. English. NNT : 2020TOU30206. tel-03193984 HAL Id: tel-03193984 https://tel.archives-ouvertes.fr/tel-03193984 Submitted on 9 Apr 2021 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. A la hermosa memoria de mis padres, Gregorio & Germania Estaré por siempre agradecida y orgullosa de su inspiración, confianza, apoyo, enseñanzas y legado. REMERCIEMENTS « La reconnaissance est la mémoire du cœur » Hans Crhistian Andersen Quisiera agradecer a la Pontificia Universidad Católica Madre y Maestra (PUCMM), particularmente, al “Programa de Formación Disciplinar” por financiar mi proyecto de investigación en el CEMES-CNRS; a la Vicerrectoría de Investigación e innovación, a la Facultad de Ciencias e Ingeniería y a la escuela de Ingeniería Industrial, por su receptividad y cooperación. Je voudrais aussi remercier le Centre d’Élaboration de Matériaux et d’Études Structurales (CEMES) et le Programme des Investissements d’Avenir (EUR grant NanoX n° ANR-17-EURE-0009) pour le financement partiel à ce projet en me donnant accès aux installations pour accomplir ce travail de recherche dans un cadre d’excellence internationale. Mes sincères remerciements vont également à mes directeurs de thèse Dr. Marc MONTHIOUX et Dr. Fabrice PIAZZA, pour leur support et la confiance qu’ils m’ont accordés pendant ces années. Merci pour l’inspiration, la compréhension et les encouragements que vous m’avez apportés dans les périodes très difficiles pour moi que ce soit dans le contexte personnel et/ou professionnel. I would like to thank all the jury members, M. Gérard VIGNOLES, Mme. Sophie MARSAUDON, M. Mauricio TERRONES, Mme. Christina VILLENEUVE-FAURE, and M. Thierry ONDARÇUHU; who have taken a valuable time for evaluating my work. Thanks for sharing your expertise with me and thus strengthening my research knowledge and experience. Je voudrais aussi remercier toutes les personnes des divers laboratoires de recherche avec qui j’ai eu l’opportunité de collaborer ici à Toulouse : o pour le CEMES : Pascal PUECH (qui parle peu, mais quand il parle, il donne toujours des bons conseils et PAS que sur le Raman !) ; Grégory SEINE (merci pour toute votre aide pour notre travail autour de l’AFM) ; Robin COURS (rebaptisé les “mains de fée”. Grand Merci à toi !) ; Laure NOE, David NEUMEYER, Cécile MARCELOT, Béatrice PECASSOU, Patrick, Mathieu DELMAS, Christophe DESHAYES, Renaud PECHOU, Erik DUJARDIN, et Mireille TRUPIN. I would like to thank also my “bestiole” Agnieszka, and my carbon gossip girls, Mariem and Divya. Thanks for all the time shared and for your support. But, as all was not “gossip-time” only, I have also to say thanks Mariem for the beautiful SEM images you have taken for this work. ii I cannot forget the most disciplined and organized guy I have ever met: Sir Abraao TORRES. Thank you for your patience to answer all my questions, for your help with SEM images, and for all our discussions about Latin-American education and socioeconomics issues. Gracias al grupo hispano-parlantes del CEMES, por todos los momentos compartidos literalmente alrededor de la mesa: Christophe, Daniela, Silvia, David, Amelia, Vero, Kathrin y tod@s.; o Pour le LPCNO-INSA- Etienne PALLEAU, Laurence RESSIER ; o Pour le LCC- Marine TASSE- et Gabor MOLNAR. Ainsi que Raúl Arenal de l’Instituto de Nanociencias de Aragon (INA-Sarragosse, Espagne) pour sa disponibilité et pour m’avoir accueilli pour les campagnes de caractérisations HRTEM. Gracias Raúl ! Un grand MERCI, à mon ami le Dr. Philippe Ouzilleau ! Merci pour ton écoute et pour tes bons conseils. Merci pour faire partie de mon réseau “graphénique” d’ aide. Quisiera agradecer a toda mi familia, elevo mi agradecimiento a Dios por los padres que me regaló. A mis padres por su amor incondicional y por su visión y ejemplo de vida. ¡Gracias a ellos, hoy por hoy el olor de las páginas de los libros de la biblioteca de la casa siguen siendo mi “magdalena de Proust”. ¡Ese recuerdo que con nostalgia me hace rememorar mis días de infancia, donde siempre había espacio para ser yo misma y soñar en grande! Gracias a mis hermanos Grecia, Fátima y Gregorio, por siempre estar. Gracias Grecia por tu optimismo y tu apoyo incondicional. Gracias por ser mi “community manager” J . Fátima, sin ti nada de esto hubiese sido posible, gracias por tu generosidad y entrega para toda la familia. Je voudrais également remercier mi novio Julien, pour son encouragement, pour son soutien et amour. Merci pour avoir supporté mon caractère, bien qu’il ne soit pas facile de nature, et qui s’est souvent empiré à cause des nuits blanches passées lors de la rédaction de ce manuscrit. Grand merci pour ta compréhension ! Merci également à madame Jacqueline et monsieur Gérard, ainsi qu’à Émilie, Sébastien et Aurore (merci pour tes bisous du haut de tes 2 ans), pour votre intérêt à mon travail et votre encouragement pendant tout ce temps-là. Agradezco además a mis tías Miledy, Leocadia; a mis primas Dennis, Eléxida, Carmen, Fanny, Karina, Elvia, Jenny, Idalma por entender mi “weirdness” y apoyarme. Así como mis entrañables amigas Miosotis, Melissa y Dayelin, que me han demostrado que los verdaderos amigos no conocen de distancias, y que el cariño y la amistad pueden atravesar el atlántico y a veces un poco más… Thanks to my super team -supporters, either as my life-coaching, hiking, or sharing some beers: Orlando (love you Orly), Néstor (el españolete), Geoffrey, Yves, Misael, Néstor (le Grec), Dinesh, Anthony, Joanna, Delphine. iii Summary Introduction 1 Chapter 1: Graphene-based carbon (nano)cones: a review 5 1. Introduction 7 2. The various ways to generate carbon conical morphologies 9 2.1 Structure-driven conical forms 9 2.1.1 Wedge disclination (introducing pentagon defects) 2.1.2 Screw dislocation (the "cone-helix" model) 2.1.3 Radial edge dislocation 2.2. Texture-driven conical forms 27 2.2.1. Graphene oBlique with respect to the cone axis 2.2.2 Graphenes parallel to the cone axis 2.2.3 Graphene perpendicular with respect to the cone axis: 2.3 Morphology-driven (process-driven) conical forms 37 2.3.1. During growth 2.3.2. Post-growth 3. Property and applications of conical carbon morphologies 43 3.1. Properties 43 3.1.1. Electronic properties 3.1.2. Mechanical properties 3.2. Applications 45 3.2.1. Electron field-emission 3.2.2. Scanning proBe microscopies (SPM) 3.2.3. Electrodes 3.2.4. Adsorption-Based applications 4. Conclusions 54 References Chapter 2: Synthesis process and formation mechanisms of carbon nanocones by CVD 65 1. Summary of the previous work (Allouche's thesis) 67 1.1. The basis of synthesis process 67 1.2. Description of the morphologies obtained 70 iv 1.3. Pyrolysis conditions vs morphology type 73 1.4. Detailed description of the conical sub-morphology: the Spiky-Bead case (SB) 75 1.5. Growth mechanisms 81 1.6 Questions and remarks 85 2. The synthesis of carbon-cone-bearing morphologies at CEMES 86 2.1. Introduction 86 2.2. Description of the process 87 2.2.1. Furnace description 2.2.2. Preparation of suBstrate 2.2.3. Process conditions 2.3. Towards the synthesis of Spiky Short-Fibers (SSF) 91 2.3.1 Reference conditions (1390°C, CH4/H2 = 1/2, total flow rate = FLOW3) 2.3.2. Decreasing CH4/H2 By decreasing CH4 and leaving H2 unchanged (hence reducing the total flow rate) 2.3.3. Decreasing CH4/H2 By increasing H2 and leaving CH4 unchanged (hence increasing the total flow rate) 2.3.4. Defining the conditions for the synthesis of the SSF morphology 2.4. Understanding further the growth mechanisms 100 2.4.1. The deposition process 2.4 2. The cone description (SEM, TEM, Raman) and growth 3. Conclusions 114 References Chapter 3: Fabrication and mounting process of carbon cones as scanning microscopy probes 121 1. Scanning Probe Microscopy (SPM) techniques 123 2. Fabrication and mounting process of SPM probes 124 2.1. Top-down micromachining process 125 2.2. Bottom up manufacturing process 126 3. Carbon nanocones as SPM probes 129 3.1. SSF carbon nanocone tips: description and characteristics 130 3.2. Mounting process 131 3.2.1. Cantilever specifications 3.2.2. Gluing process 3.2.3. Welding Process 4 Characterization of the carbon nanocone probes 137 4.1. Resonance frequency 137 4.2. Tip geometry 138 4.3. Tip alignment 140 4.4. Structural integrity of the carbon probe once mounted as a probe 142 v 4.4.1. High Resolution Transmission Electron Microscopy (HRTEM) 4.4.2. Raman spectrometry 5. Conclusions 147 References Chapter 4: Application tests of nanocone probes for various SPM modes 151 1. Introduction 153 2. Non-electrical modes 153 2.1. Atomic Force Microscopy (AFM) – Topography 154 2.1.1. Principle and notions 2.1.2. Imaging quality and performances 2.1.3. CapaBility of the carBon nanocones as AFM probes 2.1.4. Sample description and imaging protocol and performances a) Au nanoparticles deposited on Si wafer b) Highly-Oriented Pyrolytic Graphite (HOPG) c) Single silicon crystal surface (wafer) 2.1.5.
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