Synthèse et étude de matériaux nanostructurés à base d'acétate de cellulose pour applications énergétiques.

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Fischer, Florent (2006) Synthèse et étude de matériaux nanostructurés à base d'acétate de cellulose pour applications énergétiques. Doctorat Energétique, ENSMP - CEP Centre Energétique et Procédés, ENSMP.

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Résumé

Les matériaux nanostructurés ont des propriétés remarquables (surfaces d'échanges élevées, effet de confinement...) issues de leurs très faibles dimensions caractéristiques. La démarche mise en place dans le cadre de ces travaux de thèse consiste à transposer les procédés classiques d'élaboration des matériaux nanostructurés de type aérogel (combinant synthèse sol-gel et extraction au CO2 supercritique) à des précurseurs cellulosiques.
Le travail a été subdivisé en quatre parties qui portent respectivement sur une étude approfondie de la bibliographie, la mise au point et l'étude des formulations chimiques conduisant à des aérogels à partir d'acétate de cellulose, les caractérisations (chimiques, structurales et thermiques) des matériaux nanostructurés élaborés, et finalement l'étude des premiers carbones obtenus par pyrolyse des matrices organiques.
Les formulations et le protocole sol-gel conduisent à des gels chimiques par réticulation de l'acétate de cellulose à l'aide d'un isocyanate polyfonctionnel. Les aérogels obtenus après extraction du solvant au CO2 supercritique sont nanostructurés et essentiellement mésoporeux. Les caractérisations structurales ont notamment permis de dégager des corrélations entre les paramètres chimiques de la synthèse (concentration en réactifs, taux de réticulation, degré de polymérisation) et les propriétés poreuses des matériaux (densité, porosité, distribution de taille des pores). Un aérogel ultraporeux de référence, avec une masse volumique égale à 0,245 g .cm-3 et un volume mésoporeux de 3,40 cm3 .g-1 a ainsi été élaboré. Une fois mis sous forme divisée, il présente une conductivité thermique de 0,029 W .m-1 .K-1. D'autre part, les carbones obtenus après pyrolyse du réseau solide organique puis broyage sont nanostructurés et nanoporeux, malgré les nombreuses modifications structurales intervenant lors de l'étape de carbonisation.
Les matériaux élaborés dans le cadre de cette thèse sont caractérisés et évalués pour des applications liées à l'énergétique telles que l'isolation thermique (aérogels organiques) mais également pour le stockage et la conversion d'énergie par voie électrochimique (aérogels de carbone).

Références Bibliographiques

[1]Roland E, Kleinschmit P., 1996, Zeolithes, Ullmann's Encyclopedia of Indutrial Chemistry, 5th ed. Wiley.
[2]Dauphin Y., 2006, Biomineralization, Encyclopedia of Inorganic Chemistry, 2nd ed. Wiley.
[3] Brinker CJ., Scherrer GW, 1990, Sol-gel science: The physics and chemistry of sol-gel processing, Academic Press.
[4]Hüsing N, Schubert U, 2002, Aerogels, Ullmann's Encyclopedia of Indutrial Chemistry, 6th ed. Wiley.
[5]Phalippou J, Kocon L, 2004, Elaboration des gels et des Aérogels, J2230, Techniques de l'ingénieur, Paris.
[6]Phalippou J, Kocon L, 2004, Aérogels: Aspects fondamentaux, AF 3609, Techniques de l'ingénieur, Paris.
[7]Kistler, S.S., 1932, Coherent Expanded aerogels, J. Phys. Chemistry 36, 52.
[8]Rouquérol J., Avnir D., Fairbridge C.W., Everett D.H., Haynes J.H., Pericone N., Ramsay J.D.F., Sing K.S.W., Unger K.K., 1994, Recommendation for the characterization of porous solids, Pure Appl. Chem. 66, 1739.
[9]Ayral, A., Phalippou, J., Woignier, T., 1992, Skeletal density of silica aerogels determined by helium pycnometry, Journal of materials science 27, 1166.
[10]Gregg S.J. and Sing K.S.W., 1982, Adsorption, Surface Area and Porosity, Academic Press, New York.
[11]Barrett E.P., Joyner L.G. and P.P.J. Halenda, 1951, The Determination of Pore Volume and Area Distributions in Porous Substances. I. Computations from Nitrogen Isotherms, J. Am. Chem. Soc. 73, 373.
[12]Dubinin M.M., 1960, The Potential Theory of Adsorption of Gases and Vapors for adsorbents with Energetically Non-uniform Surfaces, Chem. Rev. 60, 235.
[13]Scherer G.W., Smith D.M., Stein D., 1995, Deformation of aerogels during characterization, J. Non-Cryst. Solids 186 , 309.
[14]Reichenauer G., Scherer, G.W., 2001, Nitrogen sorption in aerogels, Journal of Non-Crystalline solids 285, 167.
[15]Washburn E. W., 1921, The dynamics of capillary flow, Phys. Rev. 17, 273.
[16]Duffours L., Woignier T., Phalippou J., 1996, Irreversible volume shrinkage of silica aerogels under isostatic pressure, J. Non-Cryst. Solids 194 , 283.
[17]Pirard R., 2000, Etude de la texture des matériaux hyper poreux par porosimétrie au mercure, Thèse de doctorat, Université de Liège.
[18]Pirard, R., Blacher, S., Brouers, F., Pirard, J.P., 1995, Interpretation of mercury porosimetry applied to aerogels, Journal of material research 10, 2114.
[19]Pirard, R., Rigacci, A., Maréchal, J.C., Quenard, D., Chevalier, B., Achard, P., Pirard, J.P., 2003, Characterization of hyperporous polyurethane-based gels by non-intrusive mercury porosimetry, Polymer 44, 4881.
[20]Sing K.S.W., 1982, Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity, Pure and Appl. Chem. 54, 2201.
[21]Brunauer S., Emmett P.H. and Teller E., 1938, Adsorption of gases in multimolecular layers, Journal of the American Chemical Society 60, 309.
[22]Ponton A., Warlus S., Griesmar P., 2002, Rheological study of the sol-gel transition in silica alkoxides, J Colloid Interface Sci, 249, 209.
[23]Anglaret E., Hasmy A., Jullien R., 1995, Effect of container size on gelation time: experiments and simulations, Physical review letters 75, 4059.
[24]Stein D.J., Maskara A., Haereid S., Anderson J., Smith D.M., 1994, Contact angle measurement and its application to sol-gel processing, Better ceramics through chemistry VI, Materials Research Society: Pitttsburgh, PA, 643.
[25]Lide D.R., 2002, Handbook of chemistry physics, CRC press.
[26]Smith D.M., Scherer G.W. and Anderson J.M., 1995, Shrinkage during drying of silica gel, Journal of Non-Crystalline Solids 188, 191.
[27]Bisson A., Rigacci A., Lecomte D., Rodier E., Achard P., 2003, Drying of silica gels to obtain aerogels: phenomenology and basic techniques, Drying Technology 21, 593.
[28]Perrut M., 1999, Extraction par fluide supercritique, J 2270, Techniques de l'ingénieur, Paris.
[29]Pajonk G.M., 1989, Drying methods preserving the textural properties of gels, Revue de Physique appliquée 24, C4-13.
[30]Bommel M.J., Haan A.B., 1994, Drying of silica gels with supercritical carbon dioxide, Journal of Materials Science 29, 943.
[31]Francis A.W., 1954, Ternary systems of liquid carbon dioxide, J. Phys. Chem. 58, 1099.
[32]Scherer G.W., 1994, Stress in aerogel during depressurization of autoclave: I. Theory., J. Sol-Gel Sci. Techn, 3, 127.
[33]Woignier T., Scherer G.W., Alaoui A., 1994, Stress in aerogel during depressurization of autoclave: II. Silica gels. J. Sol-Gel Sci. and Techn., 3 ,141.
[34]Livage J., Henry M., Sanchez C., 1988, Sol-gel chemistry of transition metal oxides, Progress in solid-state chemistry 18, 259.
[35]Teichner S.J., Nicolaon G.A., Vicarini M.A., 1976, Inorganic oxide aerogel, Adv. Coll. Interf. Sci. 5, 245.
[36]Smith D.M., Ackerman W.C., Maskara A., 1999, Compositions and insulation bodies having low thermal conductivities, US Patent n° 5 877 100, Cabot Corporation.
[37]Bisson A., Rigacci A., Achard P., De Candido M., Florent P., Pouleyrn G., Bonnardel P., 2006, Preparation of silica xerogels, FR 2873677, Armines.
[38]Pope E.J.A., Mackenzie J.D., 1986, Sol-gel processing of silica II: the role of the catalyst, J. Non-Cryst. Solids 87, 185.
[39]Iler R.K., 1979, The chemistry of silica, John Wiley & Sons, 462.
[40]Scherer G.W., Swiatek R.M., 1989, Measurement of permeability II. Silica gel, Journal of Non-Crystalline Solids 113, 119.
[41]Hüsing N., Schubert U., 1998, Aerogels - Airy Materials: Chemistry, Structure, and Properties, Angewandte Chemie International Edition 37, 22.
[42]Scherer G.W., Hdach H., Phalippou J., 1991, Thermal expansion of gels: a novel method for measuring permeability, Journal of Non-Crystalline Solids 130, 157.
[43]Phalippou J., Woignier T., Prassas M., 1990, Glasses from aerogels. Part I: The synthesis of monolithic aerogels, J. Mater. Sci. 25, 3111.
[44]Pekala, R.W., 1989, Organic Aerogels from polycondensation of resorcinol with formaldehyde, J. Mater.Sci. 24, 3221.
[45]Pekala R.W., Kong F.M., 1989, A synthetic route to organic aerogels - Mechanism, structures and properties, Rev. Phys. Appl. 24, 33.
[46]Pekala, R.W., 1989, Low density resorcinol-formaldehyde aerogels, U.S. Patent 4 873 218, U.S. Department of Energy.
[47]Pekala R.W., 1991, Low density resorcinol-formaldehyde aerogels, U.S. Patent 4 997 804, U.S. Department of Energy.
[48]Biesmans, G., 1999, Polyisocyanate based aerogels, U.S. Patent 5 990 184, Imperial Chemical Industries.
[49]Biesmans G., Randall D., Francais E., Perrut M., 1998, Polyurethane-based organic aerogels' thermal performance, Journal of Non-Crystalline Solids 225, 36.
[50]Rigacci A., Marechal J.C., Repoux M., Moreno M., Achard P., 2004, Preparation of polyurethane-based aerogels and xerogels for thermal superinsulation, Journal of non-crystalline solids 350, 372.
[51]Woods G., 1990, The ICI Polyurethanes book, 2th ed. Wiley.
[52]Dieterich D., Uhlig K., 2000, Polyurethanes, Ullmann's Encyclopedia of Indutrial Chemistry, 5th ed. Wiley.
[53]Marotel Y., 2000, Polyuréthannes, AM3425, Techniques de l'ingénieur, Paris.
[54]Luo S.G., Tan H.M., Zhang J.G., Wu Y.J., Pei F.K., Meng X.H., 1997, Catalytic mechanisms of triphenyl bismuth, dibutyltin dilaurate and their combination in polyurethane-forming reaction, Journal of applied polymer science 65, 1217.
[55]Frisch K.C., Reegen S.L., Floutz W.V., Olivier J.P., 1967, Complex formation between catalysts, alcohols, and isocyanates in the preparation of urethanes, Journal of applied polymer science part A: polymer chemistry 5, 35.
[56]Reegen S.L., Frisch K.C., 1970, Isocyanate-catalyst and hydroxyl-catalyst complex formation, Journal of applied polymer science part A: polymer chemistry 8, 2883.
[57]Abbate F.W., Ulrich H., 1969, Urethane: organometallic catalysis of the reaction of alcohols with isocyanates, Journal of applied polymer science 13, 1929.
[58]Baker W.B, Gaunt J., 1949, The mechanism of the aryl isocyanates with alcohols and amines. Part III. The base-catalysed reaction of phenyl isocyanate with alcohols, Journal of the chemical society, 9.
[59]Baker W.B, Davies M.M., Gaunt J., 1949, The mechanism of the aryl isocyanates with alcohols and amines. Part IV. The evidence of infra red absorption spectra regarding alcohol-amine association in the base-catalysed reaction of phenyl isocyanate with alcohols, Journal of the chemical society, 24.
[60]Flynn K.G., Nenortas D.R., 1963, Kinetics and mechanism of the reaction between phenyl isocyanate and alcohols. Strong base catalysis and deuterium effects, Journal of Organic Chemistry 28, 3527.
[61]Farkas A., Strohm P.F., 1965, Mechanism of Amine-Catalyzed Reaction of Isocyanates with Hydroxyl Compounds, Ind. Eng. Chem. Fundam. 4, 32.
[62]Borsus J.M., Merckaert P., Jérôme R., Teyssier Ph., 1982, Catalysis of the reaction between isocyanates and protonic substrates. II Kinetic study of the polyurea foaming processcatalysed by a series of amino compounds, Journal of applied polymer science 27, 4029.
[63] Alfred D., Bertoniere R., Brown R. M., Chanzy H., Gray D., Hattori K., Glasser W., 2003, Cellulose, Encyclopedia of Polymer Science and Technology, Wiley.
[64]Krassig H., Schurz J., 2002, Cellulose, Ullmann's Encyclopedia of Industrial Chemistry, 6th ed, Wiley.
[65]Payen A., 1838, Mémoire sur la composition du tissu propre des plantes et du ligneux, Compt. Rend. 7, 1052.
[66]Klemm D., Philipp B., Heinze T., Heinze U., Wagenknecht W., 1998, Comprehensive Cellulose Chemistry, volume 1, Fundamentals and analytical methods, Wiley.
[67]Lesec J., 1996, Masses molaires moyennes, A3060, Techniques de l'ingénieur, Paris.
[68]Lesec J., 1994, Chromatographie par perméation de gel/ chromatographie par exclusion stérique, P1465, Techniques de l'ingénieur, Paris.
[69]Kroon-Batenburg LMJ., Kroon J., Nordholt MG, 1986, Chain modulus and intramolecular hydrogen bonding in native and regenerated cellulose fibres, Polym. Commun. 27, 290.
[70]Attala, R.H., 1984, Native cellulose: a composite of two distinct crystalline forms, Science, 223.
[71]Attala, R.H., 1985, Studies of polymorphy in native cellulose, Papermaking raw materials, 59.
[72]Lapointe R. E., 2000, Précis de chimie de la cellulose, 2nd edition, CCDMD.
[73]Davidson G. F., 1934, The dissolution of chemically modified cotton cellulose in alkaline solutions Part 1- In solutions of sodium hydroxide at temperature below the normal, Journal of the textile institute 25, T174.
[74]Davidson G. F., 1936, The dissolution of chemically modified cotton cellulose in alkaline solutions Part 2- A comparison of the solvent action of solutions of lithium, sodium, potassium and tetramethylammonium hydroxides, Journal of the textile institute 27, T112.
[75]Hinterholzer P., 1993, Cellulose solution in water and NMMO, US Patent 5 189 152.
[76]Cuculo J.A., Hudson S.M., 1983, Preparation of cellulose films or fibers from cellulose solutions, US Patent 4 367 191.
[77]Jacobasch B., 1984, Oberflächen faserbildender polymere, Berlin: Akademieverlag.
[78]Fink H.P., Phillip B., Zschunke C., Hayn M., 1992, Structural changes of LODP cellulose in the original and mercerized state during enzymatic hydrolysis, Acta Polym. 43, 270.
[79]Fink H.P., Walenta E., 1994, Papier(Darmstadt) 48, 739.
[80]Balser K., Hope L., Eeicher T., Wandel M., Astheimer HJ., Steinmeir H., 2000, Cellulose Esters, Ullmann's Encyclopedia of Industrial Chemistry, Editions Wiley.
[81]Rustemeyer P., 2003, Cellulose acetates: properties and applications, Macromolecular symposia 208, Wiley.
[82]Groupe français d'étude et d'application des polymères (GFP), 2000, Initiation à la chimie et à la physico-chimie macromoléculaire Vol 13: Les polymères naturels: structures, modifications, applications, Edition Strasbourg.
[83]Gedon S., Fengi R., 2000, Cellulose esters (organic esters), Kirk-Othmer Encyclopedia of Chemical Technology, Editions Wiley.
[84]Norme ASTM D1343, 2000, Test method for viscosity of cellulose derivatives by ball-drop method.
[85]Norme ASTM D5897-96, 2001, Determination of percent hydroxyl on cellulose esters by potentiometric titration - alternative method.
[86]Goebel K.D., Berry G.C., Tanner D.W., 1978, Properties of cellulose acetate. III. Light scattering from concentrated solutions and films. Tensile creep and desalination studies on films, Journal of polymer science: polymer physics edition 17, 917.
[87]Schulz L., Seger B., Burchard W., Structures of cellulose in solution, Macromolecular chemistry and physics 201, 2008.
[88]Flory P.J., 1974, Gels and gelling processes, Disc. Faraday Soc. 57, 7.
[89]Flory P.J., 1953, Principles of polymer chemistry, Cornell University Press, Ihaca, New York.
[90]Stockmayer W.H., 1943, Theory of molecular size distribution and gel formation in branched-chain polymers, J. Chem. Phys. 11, 45.
[91]Kavanagh G.M. and Ross-Murphy S.B., 1998, Rheological characterisation of polymer gels, Progress in Polymer Science 23, 533.
[92]De Gennes P.G, 1979, Scaling concepts in polymer physics, Cornell University Press, Ithaca New York.
[93]Stockmayer W.H., 1944, Theory of molecular size distribution and gel formation in branched-chain polymers. II. General cross linking, J. Chem. Phys. 12, 125.
[94]Verdu J., 1993, Structures macromoléculaires tridimensionnelles, A3045, Techniques de l'ingénieur, Paris.
[95]Tanaka T, 1981, Gels, Sci. Am. 244,124.
[96]Roy C., Budtova T., Navard P., 2003, Rheological Properties and Gelation of Aqueous Cellulose - NaOH Solutions, Biomacromolecules 4, 259.
[97]Fink H.P., Weigel P., Purz H.J., Ganster J., 2001, Structure formation of regenerated cellulose materials from NMMO solutions, Prog. Polym. Sci. 26, 1473.
[98]Dubose, A. 1905, Bull Soc Ind Rouen 33, 318.
[99]Kuga S., 1980, The porous structure of cellulose gel regenerated from calcium thiocyanate solution, Journal of colloid and interface science 77, 413.
[100]Jin H., Nishiyama Y., Wada M., Kuga S., 2004, Nanofibrillar cellulose aerogels, Colloids and surfaces A 240, 63.
[101]Frey M.W., Cuculo J.A., Khan S.A., 1996, Rheology and gelation of cellulose/ammonia/ammonium thiocyanate solutions, Journal of polymer science part B: Polymer physics 34, 2375.
[102]Altena F.W., Shroder J.S, Van de Huls R., Smolders C.A, 1986, Thermoreversible gelation of cellulose acetate solutions studied by differential scanning calorimetry, Journal of polymer science part B: Polymer physics 24, 1725.
[103]Reuvers A.J., Altena F.W., Smolders C.A., 1986, Demixing and gelation behavior of ternary cellulose acetate solutions, Journal of polymer science part B: Polymer physics 24, 1725.
[104]Pimenov V.G., Drozhzhin V.S., Sakharov A. M., 2003, Ultra-low density microcellular aerogels based on cellulose acetate, Polymer science, Ser. B, 45,4.
[105]Takahashi M., Shimazaki M., Yamamoto J., 2000, Thermoreversible gelation and phase separation in aqueous methyl cellulose solutions, Journal of polymer science part B: Polymer physics 24, 1725.
[106]Desbrières J., Hirrien M., Rinaudo M., 1998, A calorimetric study of methylcellulose gelation, Carbohydrate polymers 37, 145.
[107]Haque A., Morris E.R., 1993, Thermogelation of methylcellulose. Part I: Molecular structures and processes, Carbohydrates Polymers 22, 161.
[108]Sarkar N., 1995, Kinetics of thermal gelation of methylcellulose and hydroxypropylmethylcellulose in aqueous solutions, Carbohydrate Polymers 26, 195.
[109]Li L., Thangamathesvaran P.M., Yue C.Y., Tam K.C., Hu X., Lam Y.C., 2001, Gel network structure of methylcellulose in water, Langmuir 17, 8062.
[110]Kundu P.P., Kundu M., 2001, Effect of salt and surfactant and their doses on the gelation of extremely dilute solutions of methyl cellulose, Polymer 42, 2015.
[111]Werbowyj R.S., Derek G.G., 1980, Ordered phase formation in concentrated Hydroxypropylcellulose solutions, Macromolecules 13, 69.
[112]Gao J., Haidar G., Lu X., Hu Z., 2001, Self-association of Hydroxypropylcellulose in water, Macromolecules 34, 2242.
[113]Klemm D., Philipp B., Heinze T., Heinze U., Wagenknecht W., 1998, Comprehensive Cellulose Chemistry, volume 2: Functionalization of cellulose, Wiley.
[114]Pierce A.G. (Jr.), Frick J.G. (Jr), 1967, Crosslinking cotton with formaldehyde in phosphoric acid, Journal of applied polymer science 11, 2577.
[115]Rowland S.P., Post A.W., 1966, A measure of effective crosslinks in formaldehyde-modified cotton celluloses, Journal of applied polymer science 10, 1751.
[116] Weatherwax R. C., Caufield D.F., 1978, The pore structure of papers wet stiffened by formaldehyde crosslinking, Journal of colloid and interface science 67, 498.
[117]Yang C.Q., Andrews B.A.K., 1991, Infrared spectroscopic studies of the nonformaldehyde durable press finishing of cotton fabrics by use of polycarboxylic acids, Journal of applied polymer science 43, 1609.
[118]Chen D., Yang C.Q., Qiu X., 2005, Aqueous polymerization of maleic acid and cross-Linking of cotton cellulose by poly(maleic acid), Ind. Eng. Chem. Res. 44, 7921.
[119]Zhou Y.J., Luner P., Caluwe P., 1995, Mechanism of Crosslinking of papers with polyfunctionnal carboxylic acids, Journal of applied polymer science 58, 1523.
[120]Yang C.Q., Hu C., Lickfield G.C., 2002, Crosslinking cotton with poly(itaconic acid) and in situ polymerisation of itaconic acid: fabric mechanical strength retention, Journal of applied polymer science 87, 2023.
[121]Yang C.Q., 1993, Infrared spectroscopic studies of the effects of the catalyst on the ester Crosslinking of cellulose by polycarboxylic acids, Journal of applied polymer science 50, 2047.
[122]Luby P., Kuniak T., Fanter C., 1979, Crosslinking statistics, 3. Relation between relative reactivity and accessibility of cellulose hydroxyl groups, Die Makromolekulare chemie 180, 2379.
[123]Bai Y.X., Li Y-F., 2006, Preparation and characterization of crosslinked porous cellulose beads, Carbohydrate polymers 64, 402.
[124] Chelbli C., Cartillier L., 1998, Cross-linked cellulose as tablet excipient: a binding / disintegrating agent, International journal of Pharmaceutics 171, 1001.
[125]Rivera-Armenta J.L., Heinze Th., Mendoza-Martinez A.M, 2004, New polyurethane foams modified with cellulose derivatives, European polymer journal 41, 2803.
[126]Hatakeyama H., Hirose S., Nakamura K., Hatakeyama T., 1993, New types of polyurethanes derived from lignocellulose and saccharides in Cellulosics: Chemical, Biochemical and material aspects, Ellis Horwood Series in Polymer Science and Technology.
[127]Kamath M., Mandal B. K., 1996, Crosslinked copolymers of cyanoethylated cellulose, European polymer journal 32, 285.
[128]Tan C., Fung B. M., Newman J. K., Vu C., 2001, Organic aerogels with very high impact strength, Advanced materials 13, 644.
[129]Anbergen U., Oppermann W., 1990, Elasticity and swelling behaviour of chemically crosslinked cellulose ethers in aqueous systems, Polymer 31, 1854.
[130 Espositio F., Del Nobile M.A., Mensitieri, Nicolais L., 1996, Water sorption in cellulose-based hydrogels, Journal of applied polymer science 60, 2403.
[131]Durand B., 1980, Kerogen: Insoluble organic matter from sedimentary rocks, Edition technip, Paris.
[132]Marsh H., Rodriguez-Reinoso F. (Editors), 2000, Science of Carbon Materials, Publicaciones de la Universidad de Alicante, Alicante.
[133]Edison, 1879, Electric lamp, US Patent 223 898.
[134]Burshell T.D., 1999, Carbon materials for advanced technologies, Elesevier.
[135]Treusch O., Hofenauer A., Tröger F., Fromm J., Wegener G., 2004, Basic properties of specific wood-based materials carbonised in a nitrogen atmosphere, Wood science and technology 38, 323.
[136]Shafizadeh F., 1984, The chemistry of pyrolysis and combustion in the Chemistry of solid wood, American chemical society, Washington DC.
[137]Byrne C.E., Nagle D.C., 1997, Carbonization of wood for advanced materials applications, Carbon 35, 259.
[138]Byrne C.E., Nagle D.C., 1997, Carbonization wood monoliths - characterization, Carbon 35, 267.
[139]Fang M.X., Shen D.K., Li Y.X., Yu C.J., Luo Z.Y., Cen K.F., 2006, Kinetic study on pyrolysis and combustion of wood under different oxygen concentrations by using TG-FTIR analysis, Journal of analytical and applied pyrolysis 77, 22.
[140]Pekala R.W., Alviso C.T., LeMay J.D., 1990, Organic aerogels: microstructural dependence of mechanical properties in compression, Journal of non-crystalline solids 125, 67.
[141]Biesmans G., Mertens A., Duffours L., Woignier T., Phalippou J., 1998, Polyurethane based organic aerogels and their transformation into carbon aerogels, Journal of non-crystalline solids 225, 64.
[142]Yamashita J., Ojima T., Shioya M., Hatori H., Yamada Y., 2003, Organic and carbon aerogels derived from poly(vinyl chloride), Carbon 41, 285.
[143]Zhang R., Lu Y., Zhan L., Liang X., Wu G., Ling L., 2003, Monolithic carbon aerogels from sol-gel polymerization of phenolic resoles and methylolated melamine, Carbon 41, 1660.
[144]Pekala R.W., Farmer J.C., Alviso C.T., Tran T.D., Mayer S.T., Miller J.M., Dunn B., 1998, Carbon aerogels for electrochemical applications, Journal of non-crystalline solids 225, 74.
[145]Simon B., Hilaire M., Jehoulet C., Cousseau J-F., 2005, Electrochemical cell having a carbon aerogel cathode, US Patent application publication 0287421 A1.
[146]Langohr D., 2004, A study on hydrogen storage through adsorption in nanostructured carbons, thesis, ENSMP.
[147]Fitzer E., Schafer W., Yamada S., 1968, The formation of glasslike by pyrolyis of nonmelting resins, Carbon 6, 217.
[148]Tamon H., Ishizaka H., Mikami M., Okazaki M., 1997, Porous structure of organic and carbon aerogels synthesized by sol-gel polycondensation of resorcinol with formaldehyde, Carbon 35, 791.
[149]Bock V., Emmerling A., Fricke J., 1998, Influence of monomer and catalyst concentration on RF and carbon aerogel structure, Journal of non-crystalline solids 225, 69.
[150]Reichenauer G., Emmerling A., Fricke J., Pekala R.W., 1998, Microporosity in carbon aerogels, Journal of non-crystalline solids 225, 210.
[151]Fitzer E., Schafer W., Yamada S., 1969, The formation of glasslike by pyrolyis of polyfurfuryl alcohol and phenolic resin, Carbon 7, 643.
[152]Hanzawa Y., Hatori H., Yoshizawa N., Yamada Y., 2002, Structural changes in carbon aerogels with high temperature treatment, Carbon 40, 575.
[153]Fung A.W.P., Reynolds G.A.M., Wang Z.H., Dresselhaus M.S., Dresselhaus G., Pekala R.W., 1995, Relationship between particle size and magnetoresistance in carbon aerogels prepared under different catalyst conditions, Journal of non-crystalline solids 186, 200.
[154]Pekala R.W., Alviso C.T., 1992, Carbon aerogels and xerogels, in Material Research Society Symposium Proceedings 270, National Laboratory.
[155]Schwob Y., Bois et charbon de bois, Produit Chimique Ugine Kuhlmann.
[156]Gille B., 1966, Histoire de la métallurgie, Que sais-je.
[157]Donnet J.B., Wang T.K., Peng J.C.M. (editors), 1998, Carbon fibers, 3th edition, Marcel Dekker.
[158]Hatakeyama T., Hatakeyama H., 2004, Thermal properties of green polymers and biocomposites, Kluwer Academic Publishers.
[159]Duffy J.V., 1970, Pyrolysis of treated rayon fiber, Journal of applied polymer science 15, 715.
[160]Ishida O., Kim D.Y, Kuga S., Nishiyama Y., Brown R.M, 2004, Microfibrillar carbon from native cellulose, Cellulose 11, 475.
[161]Meier D., Faix O., 1999, State of the art of applied fast pyrolysis of lignocellulosic materials- a review, Bioresource technology 68, 71.
[162]Bridgwater A.V., 1999, Principles and practice of biomass fast pyrolysis process for liquids, Journal of analytical and applied pyrolysis 51, 3.
[163]Graham R.G., Mok L.K., Bergougnou M.A., De Lasa H.I., Freel B.A., 1984, Fast pyrolysis (ultrapyrolysis) of cellulose, Journal of analytical and applied pyrolysis 6, 363.
[164]Tang M.M., Bacon R., 1964, Carbonization of cellulose fibers - I. Low temperature pyrolysis, Carbon 2, 211.
[165]Higgins H.G., 1958, The degradation of cellulose in air at 250°C as shown by infrared spectroscopic examination, Journal of polymer science 28, 645.
[166]Konkin A.A., 1985, Production of cellulose based carbon fibrous materials, chap VIII of Handbook of composites volume 1 Strong fiber, Elsevier.
[167]Salvetat-Delmotte J-P., Rubio A., 2002, Mechanical properties of carbon nanotubes: a fiber digest for beginners, Carbon 40, 1729.
[168]Plaisantin H., 1999, Etude de la carbonisation de fibres cellulosiques, thèse de doctorat, Université Bordeaux I.
[169]Delhaes P., Orly P., 2006, Fibres de carbone et matériaux composites dans Les matériaux carbonés, L'actualité chimique 295, 42.
[170]Bansal R.C., Donnet J-B., Stoeckli F., 1988, Active carbon, Marcel Dekker, New York.
[171]Cagnon B., 2002, Elaboration de charbons actifs à texture contrôlée, Thèse de doctorat, Université de Perpignan.
[172]Roskill information services, 2003, The economics of activated carbons, Londres, 183.
[173]Norme ASTM D871-96, Standard test methods of testing cellulose acetate.
[174]Pouchert C.J., 1985, The aldrich library of FT-IR spectra.
[175]Philipp H.J., Bjork C.F., 1951, Viscosity-molecular weight relationship for cellulose acetate in acetone, Journal of polymer science 6, 549.
[176]Richter R.H., Priester R.D., 1995, Isocyanates, Organic, Kirk-Othmer Encyclopedia of chemical technology.
[177]Norme ASTM D5155-96 Standard Test Methods for Polyurethane Raw Materials Determination of the Isocyanate Content of Aromatic Isocyanates.
[178]Wurtz A., 1848, Compt. Rend. 27, 242.
[179]Bayer O., 1947, Angew. Chem A59, 257.
[180]Wilson R.B., Roxy B., Chen Y., Paul I.C., Curtin D.Y., 1983, Crystal structure and solid-state reactivity of 4,4'-methylenediphenyl isocyanate (MDI), J. Am. Chem. Soc. 105, 1672.
[181]Goidssedet P.E.C., 1920, Manufacture of new products derived from cellulose, US Patent 1 357 450.
[182]Malm C.J., Nadeau G.F., 1935, Cellulose acetate carbamate, US Patent 1 991 107.
[183]Hearon W.M., Hiatt D., Fordyce C.R., 1943, Carbamates of Cellulose and Cellulose Acetate. I. Preparation, J. Am. Chem. Soc. 65, 829.
[184]Donnelly M.J., Stanford J.L., Still R.H., 1991, The conversion of polysaccharides into polyurethanes: a review, Carbohydrate polymers 14, 221.
[185]Mormann W., Michel U., 2002, Improved synthesis of cellulose carbamate without by-products, Carbohydrate polymers 50, 201.
[186]Anzuino G., Pirro A., Rossi O., Polo Friz L., 1975, Reaction of diisocyanates with alcohols I - Uncatalysed reactions, Journal of polymer science 13, 1657.
[187]Anzuino G., Pirro A., Rossi O., Polo Friz L., 1975, Reaction of diisocyanates with alcohols II - Catalysed reactions, Journal of polymer science 13, 1667.
[188]Adkins R.L., Miller W.E., 2003, Allophanates of polymeric MDI, US Patent 6 528 609.
[189]Masmoudi Y., 2006, Thèse ENSMP, Etude du séchage au CO2 supercritique pour l'élaboration de matériaux nanostructurés: Application aux aérogels de silice monolithiques.
[190]Chang C.J., Day C.Y., Ko C.M. Chiu K.L., 1997, Densities and P-x-y diagrams for carbon dioxide dissolution in methanol, ethanol, and acetone mixtures, Fluid Phase Equilib131, 243.
[191]Pierre A.C., Pajonk G.M., 2002, Chemistry of aerogels and their applications, Chemical Reviews 102, 4243.
[192]Van Bommel M.J., De Haan A.B., 1994, Drying of silica gels with supercritical carbon dioxide, Journal of materials science 29, 943.
[193] Barton A.F.M., 1991, Handbook of solubility parameters and other cohesion parameters (2nd ed.), CRC Press, chapter 14.
[194]Brandrup, E.H. Immergut, E.A. Grulke, 1999, Polymer handbook 4th ed., Wiley, chapter 8.
[195]Takahashi S., 1983, Determination of cohesive energy densities of unsaturated polyester resins from swelling measurements, Journal of applied polymer science 28, 2847.
[196]Errede L.A., 1986, Polymer swelling 5. Correlations of relative swelling of poly(styrene-co-divinylbenzene) with the Hildebrand solubility parameter of the swelling liquid, Macromolecules 19, 1522.
[197]Bisson A., 2004, Synthèse et étude de matériaux nanostructurés à base de silice pour la super isolation thermique, Thèse ENSMP.
[198]Scherer G.W., 1998, Adsorption in aerogel networks, Journal of Non-Crystalline solids 225, 192.
[199]Hay B., Filtz J.R., Batsale J-C., 2004, Mesure de la diffusion thermique par la méthode flash, R2955 Techniques de l'ingénieur, Paris.
[200]Rigacci A., 1998, Elaboration d'aérogels de silice monolithiques et étude des relations entre leur structure et leur conductivité thermique équivalente, Thèse de doctorat, Ecole des Mines de Paris.
[201]Isover, 2004, Catalogue des produits et solutions d'isolation, p 92.
[202]Norme ASTM D 4164-03, Standard Test Method for Mechanically Tapped Packing Density of Formed Catalyst and Catalyst Carriers.
[203]Melka S., 1996, Etude théorique et expérimentale des transferts thermiques dans les milieux poreux granulaires pour l'isolation thermique, Thèse de doctorat, Ecole des Mines de Paris.
[204]Fricke J., Hummer E., Morper H-J, Scheuerpflug P., 1989, Thermal properties of silica aerogels, Proceedings of the 2nd International symposium on aerogels, Montpellier, p87.
[205]Daudon J-L., 2001, Thermogravimétrie, P1260, Techniques de l'ingénieur, Paris.
[206]Teyssedre G., Lacabanne C., 1996, Caractérisation des polymères par analyse thermique, P3770, Techniques de l'ingénieur, Paris.
[207]Job N., Théry A., Pirard R., Marien J., Kocon L., Rouzaud J-N., Béguin F., Pirard J-L., 2005, Carbon aerogels cryogels and xerogels: Influence of the drying method on the textural properties of porous carbon materials, Carbon 43, 2381.
[208]Sarrazin C., 2002, Piles électriques: piles au lithium, D3322, Techniques de l'ingénieur, Paris.
[209]Antoine O., Durand R. 2000, RRDE study of oxygen reduction on Pt nanoparticles inside Nafion: H2O2 production in PEMFC cathode conditions, Journal of Applied Electrochemistry 30, 839.
[210]Marie J., Berthon-Fabry S., Achard P., Chatenet M., Pradourat A., Chainet E., 2004, Highly dispersed platinum on carbon aerogels as supported catalysts for PEM fuel cell-electrodes: comparison of two different synthesis paths, Journal of Non-Crystalline solids 350, 88.
[211]Rouquerol F., Luciani L., Llewellyn P., Denoyel R., Rouquerol J., 2003, Texture des matériaux pulvérulents et poreux, P1050, Techniques de l'ingénieur, Paris.

Table des Matières

Introduction générale
I- Etat de l'art
I-1 Les aérogels
1.1 Introduction
1.2 Synthèse sol-gel et séchage supercritique
1.3 Les aérogels de silice
1.4 Les aérogels organiques
I-2 La cellulose et l'acétate de cellulose
2.1 Introduction
2.2 La cellulose
2.3 L'acétate de cellulose
I-3 Vers des matériaux nanostructurés à base de cellulose
3.1 Définitions et nomenclature des gels
3.2 Gels physiques
3.3 Gels chimiques et réticulation
I-4 Carbonisation
4.1 Généralités sur la carbonisation par pyrolyse
4.2 Les aérogels de carbone 39
4.3 Les matériaux carbonés ex-cellulose 42
II- Synthèse chimique et séchage de gels nanostructurés organiques à base d'acétate de cellulose
II-1 Introduction
II-2 Description du système
2.1 Composition chimique du système
2.2 Réactions chimiques
III-3 Etude de la gélification
3.1 Conditions de l'étude
3.2 Résultats expérimentaux
3.3 Discussions
3.4 Conclusions sur la gélification
III-4 Séchage par extraction supercritique
4.1 Introduction
4.2 Résultats expérimentaux
4.3 Conclusions sur le séchage des gels chimiques d'acétate de cellulose
III- Caractérisations des aérogels organiques
III-1 Introduction
III-2 Analyses chimiques
2.1 Proportion du catalyseur piégé dans l'aérogel
2.2 Comparaison des compositions mesurées et calculées
III-3 Propriétés structurales
3.1 Etude du réseau solide
3.2 Etude du réseau poreux
3.3 Conclusions structurales
III-4 Propriétés thermiques et hydriques
4.1 Conductivité thermique d'un aérogel monolithique
4.2 Conductivité thermique d'un lit granulaire d'aérogel
4.3 Adsorption d'eau en atmosphère contrôlée
4.3 Conclusions
IV- Etude de la carbonisation et des carbones élaborés: Evaluations en tant que matériaux d'électrodes
IV-1 Introduction
IV-2 Etude de la carbonisation
2.1 Analyses thermiques
2.2 Protocole expérimental de pyrolyse
2.3 Influence du profil de pyrolyse sur les pertes de masse
2.4 Influence du taux de réticulation
2.5 Analyses élémentaires des carbones élaborés
IV-3 Caractérisations structurales
3.1 Etude du réseau solide
3.2 Etude du réseau poreux
IV-4 Caractérisations électrochimiques
4.1 Evaluation des carbones élaborés pour piles primaires Li/SOCl2
4.2 Evaluation des carbones élaborés pour piles à combustible de type PEM
V- Conclusions et perspectives
V-1 Conclusions générales
V-2 Perspectives
Annexes
A-1 Séchage par extraction supercritique
A-2 Méthodes expérimentales de caractérisation structurale des matériaux
A-3 Evaluation expérimentale de la constante de flambement (kf)
A-4 Caractérisation thermique des matériaux
A-5 Communication pour le 7th European Symposium on Electrochemical Engineering
Références bibliographiques

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