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TESIS DOCTORAL 2020 UTILIZACIÓN DE POLÍMEROS ISOTÓPICAMENTE MODIFICADOS PARA MISIONES CIENTÍFICAS ESPACIALES IN-SITU JULIO MORA NOGUÉS PROGRAMA DE DOCTORADO EN CIENCIAS DIRECTOR: Dr. RICARDO ATIENZA PASCUAL CODIRECTOR: Dr. AMADOR GARCÍA-SANCHO TUTOR: Dr. JESÚS ÁLVAREZ RODRÍGUEZ Programa de Doctorado en Ciencias Madrid, Marzo de 2020 UTILIZACIÓN DE POLÍMEROS ISOTÓPICAMENTE MODIFICADOS PARA MISIONES CIENTÍFICAS ESPACIALES IN-SITU JULIO MORA NOGUÉS Memoria para optar al grado de Doctor en Ciencias Dirigida por: Dr. RICARDO ATIENZA PASCUAL Dr. AMADOR GARCÍA-SANCHO Científico Titular de la Defensa Director de Tecnología Instituto Nacional de Técnica Instituto Tecnológico del Plástico Aeroespacial (INTA) (AIMPLAS) ii AGRADECIMIENTOS En primer lugar, quiero agradecer a mis Directores de Tesis, Ricardo y Amador, todos sus consejos, su guía, la libertad de acción que me han brindado y, sobre todo, su apoyo personal incondicional durante estos cuatro años, ¡muchas gracias! A mi tutor, el Dr. Jesús Álvarez Rodríguez, por su asesoramiento y sus buenos consejos para preservar la confidencialidad en los primeros compases del estudio, y al Coordinador del Programa de Doctorado de Ciencias, el Profesor José Luis Martínez Guitarte, por toda su colaboración. Muy especialmente a Guillermo López-Reyes que ha sido fundamental en que esta prueba de concepto tomase cuerpo, ha sido una guía y apoyo constante. A todos los compañeros que han participado en este trabajo: Margarita, José Antonio, Andoni, Rafa, Aurelio, Pepe, Pauline y sobre todo a mi compañero Alejandro. A mis Jefes por favorecer esta línea de investigación. En la parte personal no he podido sentirme más respaldado, animado y apoyado. Gracias a todos mis amigos de dentro y fuera de INTA por interesarse siempre y brindarme grandes consejos. Y como no, a mi familia, a los que siempre están a mi lado, y a los que sin estar ya, siempre llevo dentro, sois indispensables. A mi madre, pilar indiscutible en mi vida, apoyo incondicional y ejemplo personal y referente a seguir. Para acabar, gracias infinitas a Vero, Lucía y Carlos. Gracias por toda vuestra ayuda y paciencia en todos los momentos que esta tesis nos ha quitado, este trabajo es tan mío como vuestro. Sois mi mayor inspiración y todo lo que hago es para y por vosotros. iii iv ÍNDICE ABREVIATURAS UTILIZADAS ......................................................................................................... vii GLOSARIO DE FIGURAS, IMÁGENES, ESQUEMAS, TABLAS Y GRÁFICOS ....................................... xi RESUMEN ..................................................................................................................................... xvii PARTE I: ANTECEDENTES Y MARCO ................................................................................................ 1 1. CAPÍTULO 1: BÚSQUEDA DE VIDA EN EL ESPACIO Y PROTECCIÓN PLANETARIA .................. 1 1.1. Exploración espacial ........................................................................................................ 1 1.2. Misiones a Marte: ExoMars ............................................................................................ 6 1.3. Protección planetaria: contaminación bacteriana, molecular y de partículas ............ 18 2. CAPÍTULO 2: VALIDACIÓN DE MATERIALES POLIMÉRICOS PARA USO ESPACIAL ............... 39 3. CAPÍTULO 3: RADIOQUÍMICA Y MARCAJE ISOTÓPICO ......................................................... 55 3.1. Isótopos: características y abundancia natural ............................................................ 55 3.2. Marcaje isotópico y aplicaciones. Efecto isotópico ...................................................... 59 3.3. Análisis de isótopos ....................................................................................................... 62 4. CAPÍTULO 4: OBJETIVOS DE LA TESIS .................................................................................... 70 PARTE II: METODOLOGÍA .............................................................................................................. 75 5. CAPÍTULO 5: SÍNTESIS DE POLÍMEROS .................................................................................. 75 5.1. PET: Métodos de síntesis ............................................................................................... 75 5.2. Caracterización polimérica: TGA y DSC ......................................................................... 78 6. CAPÍTULO 6: CARACTERIZACIÓN ANALÍTICA MEDIANTE LAS MISMAS TÉCNICAS QUE SE EMPLEARAN EN LA MISIÓN EXOMARS ......................................................................................... 84 6.1. Espectroscopía Vibracional ........................................................................................... 84 6.1.1. Espectroscopía Raman........................................................................................... 84 6.1.2. Espectroscopía FTIR (Fourier-Transform InfraRed) .............................................. 86 6.2. Cromatografía de gases con espectrometría de masas (GC/MS) ................................ 88 7. CAPÍTULO 7: ENSAYOS DE VALIDACIÓN ESPACIAL ............................................................... 93 7.1. Desgasificación según ECSS-Q-ST-70-02C, Thermal vacuum Outgassing test for the screening of space materials ..................................................................................................... 94 7.2. Desgasificación dinámica según ECSS-Q-TM-70-52A Kinetic Outgassing of materials for space ..................................................................................................................................... 99 PARTE III: DISCUSIÓN DE RESULTADOS ...................................................................................... 101 8. CAPÍTULO 8: RESULTADOS. DISCUSIÓN .............................................................................. 101 v 8.1. RESULTADOS DE OBJETIVO 1: SÍNTESIS DE UN MATERIAL FUNCIONAL INTEGRA O PARCIALMENTE MARCADO ISOTÓPICAMENTE ...................................................................... 102 8.1.1. Proceso de síntesis y purificación ....................................................................... 102 8.1.2. Ensayos de caracterización de polímeros sintetizados mediante TGA y DSC ... 106 8.1.3. Resumen de resultados y adecuación al objetivo 1 ........................................... 109 8.2. RESULTADOS DE OBJETIVO 2: ESTUDIO DE LAS DIFERENCIAS ISOTÓPICAS INTRODUCIDAS MEDIANTE TÉCNICAS ESPECTROSCÓPICAS Y ESPECTROMÉTRICAS ............ 111 8.2.1. Estudio de precursores monoméricos mediante Raman, FTIR y GC/MS ........... 111 8.2.2. Caracterización por espectroscopía vibracional: Raman y FTIR de los polímeros sintetizados .......................................................................................................................... 131 8.2.3. Caracterización por espectrometría de masas de los polímeros sintetizados .. 149 8.2.4. Estudio de contaminación forzada mediante desgasificación en polímeros sin desgasificación térmica ....................................................................................................... 157 8.2.5. Resumen de resultados y adecuación al objetivo 2 ........................................... 162 8.3. RESULTADOS DE OBJETIVO 3: ENSAYOS DE VALIDACIÓN ESPACIAL PARA LOS POLÍMEROS PROPUESTOS ....................................................................................................... 166 8.3.1. Ensayo de desgasificación de los polímeros sintetizados .................................. 166 8.3.2. Resumen de resultados y adecuación al objetivo 3 ........................................... 172 9. CAPÍTULO 9: CONCLUSIONES .............................................................................................. 175 TRABAJOS FUTUROS .................................................................................................................... 179 BIBLIOGRAFÍA .............................................................................................................................. 181 vi ABREVIATURAS UTILIZADAS AE Activation Energy AIV Assembly, Integration and Verification ALD Analytical Laboratory Drawer ASTM American Society for Testing and Materials ATOX Atomic Oxygen ATR Attenuated total reflection CAP Cold Atmospheric Plasma CARS Coherent anti-Stokes Raman spectroscopy CCD Charge Coupled Device CETEX Committee on the Exploration of Extraterrestrial Space CI Chemical Ionization CNES Centre National d'Études Spatiales COSPAR Committee on space research COSY Correlation spectroscopy CVCM Collected Volatile Condensable Material DHMR Dry Heat Microbiological Reduction DMT Dimetiltereftalato DOP Dioctyl Phthalate - Dioctilftalato DSC Differential scanning calorimetry ECSS European Cooperation for Space Standardization EI Electronic Impact EIC Efecto Isotópico Cinético EIE Efecto isotópico de Equilibrio END Ensayos no destructivos EMC Electromagnetic compatibility ESA European Space Agency ESI Electrospray ionization ExoMars Exobiology on Mars EXSY Exchange spectroscopy FAB Fast atom bombardment FD Field desorption FTIR Fourier-Transform Infrared Spectroscopy GC/FID Gas chromatography/Flame ionization detector GC/MS Gas chromatography/mass spectrometry HabCat Catalog of Nearby Habitable Systems HMBC Heteronuclear multiple Bond Correlation HMQC Heteronuclear multiple quantum coherence HR Humedad relativa HSQC Heteronuclear single quantum coherence vii ICP-MS Inductively coupled plasma mass spectrometry IPA Isopropilyc alcohol – Alcohol isopropílico
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