Patterning and Characterization of Graphene Nano-Ribbon by Electron Beam Induced Etching Sébastien Linas

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Patterning and Characterization of Graphene Nano-Ribbon by Electron Beam Induced Etching Sébastien Linas Patterning and characterization of graphene nano-ribbon by electron beam induced etching Sébastien Linas To cite this version: Sébastien Linas. Patterning and characterization of graphene nano-ribbon by electron beam induced etching. Materials Science [cond-mat.mtrl-sci]. Université Paul Sabatier - Toulouse III, 2012. English. NNT : 2012TOU30323. tel-01025043 HAL Id: tel-01025043 https://tel.archives-ouvertes.fr/tel-01025043 Submitted on 17 Jul 2014 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. 5)µ4& &OWVFEFMPCUFOUJPOEV %0$503"5%&-6/*7&34*5²%&506-064& %ÏMJWSÏQBS Université Toulouse 3 Paul Sabatier (UT3 Paul Sabatier) 1SÏTFOUÏFFUTPVUFOVFQBS LINAS Sébastien le mercredi 19 décembre 2012 5JUSF Fabrication et caractérisation de nano-rubans de graphène par gravure électronique directe. ²DPMF EPDUPSBMF et discipline ou spécialité ED SDM : Nano-physique, nano-composants, nano-mesures - COP 00 6OJUÏEFSFDIFSDIF Centre d'Elaboration de Matériaux et d'Etudes Structurales. CEMES CNRS UPR8011 %JSFDUFVS T EFʾÒTF DUJARDIN Erik Jury : BANHART Florian (IPCMS, Strasbourg), Rapporteur BOUCHIAT Vincent (Inst. Néel, Grenoble), Rapporteur SERP Philippe (LCC, Toulouse), Président MLAYAH Adnen (CEMES, Toulouse), Examinateur PAILLET Matthieu (L2C-UM2, Montpellier), Examinateur Remerciements. Mes premiers remerciements vont à mon amoureuse Céline et notre Paul qui ont sup‐ porté mes absences ces trois années durant. Je leur doit beaucoup, ce travail n’aurait pas abouti sans eux. Mes premiers remerciements professionnels vont à mon directeur de thèse, monsieur Dujardin Erik qui m’a permis d’effectuer cette thèse en me recrutant et en me fournissant tout au long de ce travail un soutien technique nécessaire à l’aboutissement de ce travail. Sous sa direction j’ai pu me familiariser avec de nombreuses techniques de caractérisation ainsi qu’acquérir rigueur et autonomie nécessaires au métier de chercheur. Je tiens à remercier chaleureusement les membres du jury qui ont évalué ce travail. Messieurs Banhart Florian et Bouchiat Vincent pour leur rapport, monsieur Serp philippe, président de ce jury ainsi que messieurs Mlayah Adnen et Paillet Matthieu en tant qu’examinateurs. Leur commentaires et remarques ont permis d’améliorer la qualité de ce manuscrit. Je souhaite également remercier toutes les personnes qui font tourner le laboratoire sans pour autant être mis en avant. Merci à tous les ingénieurs de recherche, d’étude et tech‐ niciens, et notamment les personnes qui m’ont assisté dans mon travail, Philippe Salles pour le FIB, Antoine Zwick, Frédéric Neumayer et Sébastien Moyano pour le service spectrosco‐ pie, Florent Houdellier et Sébastien Joulié pour la MET, Laure Noé pour le four, Christophe Deshayes pour le MEB, Christine Viala et bien sur Isabelle Labau, bibliothécaire émérite. Je tiens également à remercier ceux qui contribuent à l’entretien des locaux. 3 Remerciements. Je souhaite également remercier messieurs David Martrou (pour lll également) et Sé‐ bastien Gauthier qui m’ont aidé, six mois durant à me familiariser avec l’AFM non contact et l’ultra haut vide. Merci à monsieur Ondarçuhu Thierry pour son aide sur le mouillage en AFM. Je remercie également monsieur Gatel Cristophe pour ses routines de traitement d’images TEM. Je remercie spécialement Antoine Hinaut et Laure Fabié qui ont longuement partagé un bureau avec moi. Je remercie Gurunatha Kargal‐Laxminarayana dont j’ai beaucoup ap‐ précié les conversations. Merci également aux camarades Olivier Couturaud dont j’ai faillit boire les paroles et Miguel Rubio‐Roy. Je remercie Marc Nuñez que j’ai co‐encadré deux fois lors de ses stages et qui continue le travail au quel j’ai participé trois ans durant. Merci éga‐ lement à Alexandre ainsi qu’à toutes les personnes que j’ai rencontré au cours de mon séjour au laboratoire. Sébastien Linas 4 Acronyms. AFM Atomic force microscopy 2D Two dimensions A0 Free amplitude a‐C Amorphous carbon AGNR Armchair graphene nano‐ribbon (GNR with armchair edges) AM‐AFM Amplitude modulation atomic force microscopy ASP Amplitude set point CNT Carbon nano‐tube CVD Chemical vapor deposition DFT Density functional theory e‐beam Electron beam EBIE Electron beam induced etching FET Field‐emission transistor FIB Focused ion beam FLG Few layer graphene GIS Gas injection system GL Graphene layer GNR Graphene nano‐ribbon HBC Hexabenzocoronene 5 Acronyms. HRTEM High resolution transmission electron microscopy IPA Isopropanol MWCNT Multiwall carbon nano‐tube NC‐AFM Non contact atomic force microscopy NEMS Nanoelectro‐mechanical system PMMA Polymethyl methacrylate PmPV Poly(m‐phenylenevinylene‐co‐2,5‐dioctoxy‐p‐phenylenevinylene) RH Relative humidity RMS Root mean square RT Room temperature SACTEM Spherical aberration corrected transmission electron microscopy SAED Selected area electron diffraction SEM Scanning electron microscopy STM Scanning tunneling spectroscopy SWCNT Single walled carbon nano‐tube TEM Transmission electron microscopy UHV Ultra high vacuum VLSI Very large scale integration ZGNR Zig‐zag graphene nano‐ribbon (GNR with Zig‐zag edges) 6 Table of content. Remerciements.............................................................................................................................................. 3 Acronyms....................................................................................................................................................... 5 Table of contents........................................................................................................................................... 7 11 Introduction......................................................................................................................................... 21 Chapter 1: Properties, production, and patterning of graphene............. 1.1 ...Properties of graphene........................................................................................ 24 1.1.1 ..........Graphene, a no gap semi conductor.................................................................... 24 1.1.2 ..........Electronic properties............................................................................................. 26 1.1.3 ..........Graphene nanoribbons......................................................................................... 27 1.2 ...Identification of graphene.................................................................................... 29 1.2.1 ..........Optical characterization........................................................................................ 29 1.2.2 ..........Raman spectroscopy............................................................................................ 29 1.2.3 ..........Atomic force microscopy characterization. .......................................................... 31 1.2.4 ..........Transmission electron microscopy....................................................................... 32 1.3 ...Graphene production............................................................................................ 33 1.3.1 ..........Micromechanical exfoliation of graphite................................................................ 33 1.3.2 ..........Epitaxial graphene................................................................................................ 34 1.3.3 ..........Molecular approaches.......................................................................................... 36 1.4 ...Graphene patterning techniques...................................................................... 36 1.4.1 ..........Ion based patterning............................................................................................. 37 1.4.2 ..........Direct electron beam patterning of graphene....................................................... 40 1.4.3 ..........Catalytic patterning of graphene by metal nanoparticles...................................... 46 1.5 ...Perspectives........................................................................................................... 49 1.6 ...References.............................................................................................................. 51 Chapter 2 : Materials, techniques and instruments............................................ 59 2.1 ...Materials and techniques.................................................................................... 60 2.1.1 ..........Chemicals, solvent and gases.............................................................................. 60 2.1.2 ..........Si/SiO2 substrates................................................................................................. 60 2.1.3 ..........Si/SiO2 substrates cleaning.................................................................................. 61 2.1.4 ..........Annealing and storage.......................................................................................... 61 2.1.5 ..........Mechanical exfoliation deposition of graphene..................................................... 61 2.1.6 ..........Graphene on TEM grid........................................................................................
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