Etude du stockage d'hydrogène par adsorption dans des carbones nanostructurés.

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Langohr, David (2004) Etude du stockage d'hydrogène par adsorption dans des carbones nanostructurés. Doctorat Energétique, ENSMP - CENERG, ENSMP.

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Résumé

Ce travail porte sur l'étude expérimentale du stockage d'hydrogène par adsorption dans des carbones nanostructurés. Il a été rédigé en trois parties: une étude approfondie de la bibliographie, la mise en place d'un banc d'essais destiné à quantifier le pourcentage gravimétrique d'hydrogène stocké par les carbones, et finalement la mesure du stockage d'hydrogène dans deux familles de carbones nanostructurés étudiées au sein du laboratoire.
L'étude bibliographique met en avant les différents moyens de stockage d'hydrogène actuellement disponibles (compression et liquéfaction) et se concentre essentiellement sur les techniques expérimentales de mesure du stockage d'hydrogène par adsorption et les problèmes qu'elles peuvent susciter. Un regard critique est également porté sur la forte variation des différents résultats publiés dans la littérature.
Le banc d'essais mis en place a été conçu pour mesurer la capacité de stockage d'hydrogène pour une masse importante de matière, de l'ordre de 10 grammes, et est basé sur le principe d'une mesure volumétrique de la quantité d'hydrogène désorbé par le carbone à la température de 25°C et une pression de 100 bars. Deux calculs ont été mis en place: un calcul détermine le pourcentage gravimétrique en comparaison à un système en compression et un autre le pourcentage gravimétrique intrinsèque des carbones. En parallèle à ces calculs, un calcul d'erreur a été fait, et le banc d'essais a été calibré grâce à trois moyens différents.
Les carbones nanostructurés étudiés sont issus de deux procédés: un procédé sol-gel permettant de produire des aérogels de carbone et un procédé plasma à haute température, permettant la synthèse de différentes variétés de nanostructure de carbone. Tous les échantillons, après avoir été préalablement caractérisés morphologiquement, ont été testés selon le même protocole expérimental mis en place et les résultats ont montré des valeurs de stockage d'hydrogène inférieures à 0,5 pour cent d'hydrogène en masse.

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Table des Matières

I GENERAL INTRODUCTION
II LITERATURE REVIEW ON HYDROGEN STORAGE AND ON THE CARBONS USED FOR HYDROGEN ADSORPTION
1 Introduction
2 Hydrogen and various means to store it
2.1 Hydrogen
2.1.1 Hydrogen properties
2.1.2 Hydrogen production
2.1.3 The issues of hydrogen storage
2.2 Compressed hydrogen
2.2.1 Types of vessels for compression
2.2.2 Conformable vessels
2.3 Liquefied hydrogen (LH2)
2.3.1 The liquefaction process
2.3.2 The cylinders used for LH2
2.3.3 Actors and applications
2.4 Metal hydrides
2.4.1 The hydriding and dehydriding process
2.4.2 Different types of metal hydrides
2.5 Other storage techniques
2.6 Summary of hydrogen storage technologies
2.7 Physical adsorption in carbons
2.7.1 A few definitions
2.7.2 Gas on Solid adsorption
2.7.3 The specific case of carbon
3 Carbon materials used for hydrogen storage
3.1 Graphitic carbon
3.2 Carbon black and activated carbon
3.2.1 The main elaboration processes
3.2.2 Growth and texture of carbon blacks
3.2.3 Activated carbon
3.3 Carbon nanofibres
3.4 Carbon fullerenes
3.5 Carbon nanotubes
3.5.1 Presentation of the Carbon nanotubes
3.5.2 Producing carbon nanotubes
3.5.3 Various theories on the nucleation and growth of carbon nanotubes
3.5.4 Influence of various parameters
4 Methods available to measure the hydrogen storage
4.1 Expressing the amount of hydrogen stored
4.2 The experimental techniques to measure the hydrogen storage
4.2.1 Gravimetric method
4.2.2 Volumetric method
4.2.3 Temperature programmed desorption (TPD)
4.2.4 Electrochemical measurements
4.3 Classical pitfalls on measuring hydrogen storage
4.3.1 The sample
4.3.2 The pressure vessel
4.3.3 Experimental protocol
4.3.4 Measurement techniques
4.4 The experimental calibration
5 Hydrogen storage in nanostructured carbon materials
5.1 Graphite, carbon black and activated carbons
5.1.1 Preliminary results
5.1.2 The influence of the experimental conditions
5.1.3 Carbon treatment effect
5.2 Carbon nanofibres
5.2.1 Catalytic hydrogen transfer
5.2.2 High temperature heat treatment
5.3 Carbon nanotubes
5.3.1 Alkali-doped nanotubes
5.3.2 Purification by chemical and/or heat treatment
5.3.3 The sonication of nanotubes
5.3.4 Multi Wall carbon nanotube
5.3.5 Electrochemical storage of hydrogen in carbon nanotubes
5.4 The chemical adsorption of hydrogen in fullerenes
6 Conclusion
III CHARACTERISATION OF HYDROGEN STORAGE THANKS TO A VOLUMETRIC METHOD - EXPERIMENTAL TEST BENCH DEVELOPED
1 Introduction
2 Presentation of the experimental set-up
2.1 Presentation and instrumentation of the test bench
2.1.1 Presentation of the set-up
2.1.2 Acquisition unit
2.2 Measuring range
2.3 Advantages of such a process
3 Calculating the weight percent stored and the errors generated
3.1 The volumetric method
3.2 Desorbing the empty pressure vessel
3.2.1 The determination of the equation for the empty pressure vessel
3.2.2 Calculating the volume of the pressure vessel
3.3 The gravimetric percentage - a comparison to pure compression
3.4 Calculating the intrinsic gravimetric percentage of our materials
3.4.1 Configuration of the carbon in the vessel
3.4.2 Defining the intrinsic weight percent
3.5 Calculation of the errors
3.5.1 Wt% calculated compared to compression
3.5.2 The intrinsic weight percent
3.6 The limits of the test bench
4 Experimental protocol and calibration of the experimental set-up
4.1 Experimental protocol
4.1.1 The outgassing of the sample
4.1.2 The pressurisation of the pressure vessel
4.1.3 The desorption process
4.2 Calibration of the measuring device
4.2.1 Leak proof tests
4.2.2 Reproducibility of an empty measurement
4.3 Calibration with a non adsorbing material
4.3.1 Experimental protocol
4.3.2 Measurements and errors
4.3.3 Conclusions on this measurement
4.4 Calibration with a metal hydride
4.5 Testing our materials in a different laboratory
5 Conclusion
IV THE NANOSTRUCTURED CARBON MATERIALS ELABORATED AND INVESTIGATED
1 Introduction
2 Carbon aerogels
2.1 The elaboration process of Carbon aerogels
2.1.1 The sol-gel reaction
2.1.2 The CO2 supercritical drying
2.1.3 The pyrolysis
2.1.4 Experimental procedure
2.2 The influence of the chemistry on the microstructure
2.2.1 Representation of a carbon aerogel
2.2.2 The influence of the R/C ratio and the solid percent
2.2.3 The influence of the heat treatment: pyrolysis and activation
2.3 Properties and applications of carbon aerogels
2.3.1 Properties of carbon aerogels
2.3.2 Applications of carbon aerogels
2.3.3 Hydrogen storage
3 The high temperature plasma process
3.1 Production of carbon blacks
3.1.1 Presentation of the initial technology
3.1.2 The operating principle
3.1.3 Numerical modelling
3.2 Adaptation of the plasma technology
3.2.1 Production of carbon fullerenes
3.2.2 Production of carbon nanotubes
3.3 Advantages of the plasma process
4 Conclusion
V CHARACTERISATION AND EXPERIMENTAL RESULTS OF HYDROGEN STORAGE ON THE CARBON MATERIALS ELABORATED
1 Introduction
2 Characterisation of the two families of samples
2.1 Characterisation of the carbon aerogels
2.1.1 Mercury pycnometry
2.1.2 Elemental analysis
2.1.3 Raman spectroscopy
2.1.4 Helium pycnometry
2.1.5 TEM analysis
2.1.6 Nitrogen adsorption
2.1.7 SAXS analysis
2.2 The samples produced by the high temperature plasma process
2.2.1 Carbon black
2.2.2 Fullerene rich soots
2.2.3 Nanotube rich soots
2.2.4 Conclusion on the carbons from the plasma process
3 The experimental results with the carbon aerogels
3.1 Presentation of the results
3.2 Microstructural effect on the hydrogen storage
3.2.1 Influence of the specific surface area
3.2.2 Influence of the porosity
3.2.3 The surface area
3.2.4 The gaseous chord length and the particle size
3.2.5 Conclusions
4 Results with the carbons coming from the plasma process
4.1 Three families of carbons tested
4.2 The problem of the intrinsic weight percent
4.2.1 The skeleton density
4.2.2 The weight percent of nanotubes
4.3 Analysing the hydrogen weight percent compared to compression
5 Carbon nanofibres
6 Conclusions
VI GENERAL CONCLUSIONS AND PERSPECTIVES
VII RÉSUMÉ DE LA THÈSE EN FRANÇAIS
VIII APPENDICES
1 Appendix 1: The experimental protocol for hydrogen storage measurements and security issues
2 Appendix 2: The estimation of the experimental technical errors
3 Appendix 3: Experimental techniques for the characterisation of materials
3.1 Nitrogen adsorption
3.1.1 Classification of the isotherms
3.1.2 The BET treatment
3.1.3 Pore size distribution
3.2 Small Angle X-Ray Scattering
3.2.1 Basic principles of X-Ray scattering
3.2.2 The Porod regime
3.2.3 The Guinier regime
3.2.4 Fractal diffusion
3.2.5 Calculating the specific surface area
3.2.6 The two phase media model
3.3 Mercury pycnometry
3.4 Helium pycnometry
3.5 Elemental analysis
3.6 Raman Spectroscopy
3.7 Electron microscopy
IX REFERENCES

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