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División De Estudios De Posgrado E Investigación INSTITUTO TECNOLÓGICO DE CIUDAD MADERO DIVISIÓN DE ESTUDIOS DE POSGRADO E INVESTIGACIÓN DOCTORADO EN CIENCIAS EN MATERIALES TESIS “DISEÑO DE ELECTRO-CATALIZADORES BIMETÁLICOS SOBRE MATERIALES DE CARBONO NANOESTRUCTURADO PARA CELDAS DE COMBUSTIBLE” Para obtener el grado de Doctor en Ciencias en Materiales Presenta M.C. David Macias Ferrer Director de tesis Dr. José Aarón Melo Banda Co-director de tesis Dra. Rebeca Silva Rodrigo Altamira, Tamaulipas Junio 2018 ii Agradecimientos A mis padres, por su apoyo incondicional A mis hijos Irina Charity y David Mijhail Jesus A mis asesores, Dr. José Aarón Melo Banda y Dra. Rebeca Silva Rodrigo, por todo el apoyo y orientación que siempre me brindaron a lo largo de este proyecto Al personal académico de la División de Posgrado e Investigación, del Instituto Tecnológico de Ciudad Madero y del Instituto Tecnológico de Cancún que de una manera u otra contribuyeron a la caracterización de los materiales sintetizados Al CONACYT, por su valioso apoyo económico, que sin él, no hubiese sido posible la realización de este proyecto A mi compañera Dra. Mayda Lam Maldonado por su valiosa colaboración en la redacción de artículos científicos A todas aquellas amistades que me apoyaron incondicionalmente todo este tiempo iii Contenido Página Contenido .............................................................................................................................. iii Tablas y figuras .....................................................................................................................vii Resumen ..............................................................................................................................xvii Abstract ............................................................................................................................. xviii Símbolos y abreviaturas ...................................................................................................... xix Introducción ............................................................................................................................ 1 Capítulo I Marco Teórico 1.1. Celdas de combustible ....................................................................................................... 8 Historia de las celdas de combustible ................................................................................ 8 Celdas de combustible: Generalidades ............................................................................ 13 Las celdas de combustible como energía alternativa ....................................................... 17 1.2. Celdas de combustible de metanol directo ...................................................................... 18 El metanol ........................................................................................................................ 18 Configuración de una celda de combustible de metanol directo ..................................... 18 Reacciones electroquímicas ideales................................................................................. 20 1.3. Electrocatálisis y la electro-oxidación de metanol .......................................................... 20 Electrocatálisis ................................................................................................................. 20 El mecanismo de electro-oxidación de metanol .............................................................. 21 1.4. Electrocatalizadores para CCMD .................................................................................... 31 1.4.1. Generalidades ........................................................................................................ 31 1.4.2. La fase activa de un electrocatalizador .................................................................. 33 El platino................................................................................................................ 33 iv Los sistemas de nanopartículas metálicas como fase activa para ECAT’s ........... 34 1.4.3. Soporte catalítico de un electrocatalizador para CCMD ....................................... 35 Negro de carbón..................................................................................................... 36 Materiales de carbono mesoporoso ....................................................................... 37 Alótropos del carbono ........................................................................................... 38 Nanotubos de carbono (NTC)................................................................................ 39 Fabricación de nanotubos de carbono ................................................................... 40 Nanomoldeo........................................................................................................... 40 Materiales de carbono mesoporoso ordenado por nanomoldeo ............................ 41 Óxido de grafeno (GO) .......................................................................................... 45 Uso de los MCM como soporte catalítico en ECAT’s .......................................... 47 1.5. Síntesis de electro-catalizadores para CCMIP y CCMD ................................................. 48 Generalidades .................................................................................................................. 48 Funcionalización del soporte catalítico para nanopartículas metálicas en ECAT ........... 48 Sales precursoras de metales de transición en ECAT...................................................... 49 Agentes reductores y estabilizadores ............................................................................... 49 1.6. Mediciones electroquímicas en la electro-oxidación de metanol .................................... 50 Actividad electro-catalítica respecto de la oxidación del metanol .................................. 50 Voltametría cíclica ........................................................................................................... 51 Área electroquímicamente activa .................................................................................... 54 Corriente potenciostática. Pruebas de durabilidad .......................................................... 55 Estabilidad ....................................................................................................................... 55 Espectroscopía de impedancia electroquímica ................................................................ 56 1.7. Proyecto 5261.14-P ......................................................................................................... 58 1.7.1. Antecedentes .......................................................................................................... 58 1.7.2. Planteamiento del problema .................................................................................. 60 1.7.3. Propuesta tecnológica para el proyecto 5261-P ..................................................... 60 v 1.7.4. Hipótesis ............................................................................................................... 60 1.7.5. Objetivos ................................................................................................................ 61 1.7.5.1. Objetivo general ....................................................................................... 61 1.7.5.2. Objetivos específicos ................................................................................ 61 1.7.6. Metas ..................................................................................................................... 62 1.7.7. Justificación ........................................................................................................... 62 Bibliografía del Capítulo I ...................................................................................................... 64 Capítulo II Metodología 2.1. Síntesis y funcionalización de carbono micro/nano estructurado ................................... 75 2.2. Síntesis de óxido de grafeno (GO) .................................................................................. 78 2.3. Síntesis de los electro-catalizadores basados en Pt ......................................................... 78 2.3.1. Síntesis de los electro-catalizadores Pt/MNC y Pt/rGO ........................................ 79 2.3.2. Síntesis de PtCo/MNC, PtFe/MNC, PtCo/rGO y PtFe/rGO ................................. 79 2.4. Técnicas de caracterización ............................................................................................. 80 2.4.1. Espectroscopia infrarroja a través de la transformada de Fourier (FTIR) ............. 80 2.4.2. Espectroscopia Raman ........................................................................................... 81 2.4.3. Fisisorción de nitrógeno ........................................................................................ 81 2.4.4. Difracción de rayos X ............................................................................................ 81 2.4.5. Espectroscopía fotoelectrónica de rayos X (XPS) ................................................. 82 2.4.6. Microscopía electrónica de barrido de emisión de campo (FESEM) .................... 82 2.4.6.1. Espectrometría de dispersión de energía de rayos X (EDS) ..................... 83 2.4.7. Microscopía electrónica de transmisión de alta resolución (HRTEM) ................. 83 2.5. Mediciones electroquímicas ............................................................................................ 83 2.5.1.
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