Ce travail de thèse porte sur l’étude d’oxydes (ZnO et SiO2) fabriqués par voie sol-gel. Dans un premier temps, nous avons étudié la cinétique de croissance des nanoparticules de ZnO en milieu aqueux. L’étude in-situ de la croissance d’oxyde de zinc par la technique de croissance en milieu aqueux (ACG) a été réalisée grâce à la radiation synchrotron de l’ESRF sur la ligne ID10B. Nous avons réalisé la diffraction de rayons X en incidence rasante sur un substrat plongé dans une solution constituée de nitrate de zinc hexahydraté [Zn(NO3)2,6H2O], d’hexamethylenetetramine (HMT) (C6H12N4) et de l’eau dé-ionisée comme solvant. Nous avons réussi à mettre en évidence l’existence de nanoparticules de ZnO dans la solution et suivre la cinétique de formation. La deuxième partie de ce travail est consacrée à l’étude des films minces de silice mésoporeux structurés par un tensioactif connu sous l’acronyme Brij58. Nous avons commencépar établir le diagramme de phase du Brij58 par la diffusion centrale des rayons X (SAXS), complété par l’établissement d’un diagramme d’état solide-liquide par la rhéologie. Grâce à ce diagramme de phase nous avons pu fabriquer des films minces de silice. L’étude de la structuration des films a été réalisée par la diffusion des rayons X en incidence rasante (GISAXS) et la réflectivité des rayons X. Nous avons finalisé ce travail par l’utilisation des films mésoporeux comme matrice hôte à deux fluides : l’eau et le CO2, et par l’insertion de nanocristaux de ZnO dans les pores de la matrice mésoporeuse. / This thesis presents the study of oxides (ZnO and SiO2) synthesized by sol-gel method. Firstly, we study the kinectics growth of ZnO nanoparticles in aqueous medium. The aqueous chemical growth of ZnO was done at the ESRF (ID10 beamline) for using the synchrotron radiation (22 Kev). The in-situ monitoring by synchrotron radiation on a substrate placed in solution made up from zinc nitrate hexahydrate [Zn(NO3)2,6H2O, 98%, Acros Organics] and hexamethylenetetramine (HMT, C6H12N4, 99%, Acros Organics) precursors dissolved in equimolar concentration in deionized water (MilliQ, 18.2Mo), allowed us to highlight the presence of ZnO nanoparticles in solution and permit to follow the kinetics of the formation of zinc oxide. In the second part, we have synthesized and analysed mesoporous silica thin films templated by a non-ionic surfactant, the Brij58. This work required to establish the binary phase diagramm Water/Brij58 by Small Angle X-rays Scattering (SAXS) at room temperature. The SAXS study is complemented by the determination of the liquid-solid transition of binary system Water/Brij58 by rheolgy. The study of well structured films was carried out by Grazing Incidence Small Angle X-rays Scattering (GISAXS) and by X-rays reflectivity. Lastly, our aim was then to combine the synthesis of porous thin film with the inclusion of zinc oxide nanocrystals in the pores. We completed this work by using these films as porous host matrix for two fluids, water and CO2.

The removal of trace amounts of acetylene in ethylene streams is a high-volume industrial process that must possess high selectivity of alkyne hydrogenation over hydrogenation of alkenes. Current technology uses metallic nanoparticles, typically palladium or platinum, for acetylene removal. However, problems arise due to the deactivation of the catalysts at high temperatures as well as low selectivities at high conversions. Pore expanded MCM-41 is synthesized via a two-step strategy in which MCM-41 was prepared via cetyltrimethylammonium bromide (CTMABr) followed by the hydrothermal treatment with N,N-dimethyldecylamine (DMDA). This material was washed with ethanol to remove DMDA, or calcined to remove both surfactants. PE-MCM-41 based materials were impregnated with palladium, gold, and palladium-gold nanoparticles. The removal of DMDA had an effect on both the conversion and selectivity, in which they were found to drop significantly. However, by using the bimetallic PdAu catalysts, higher selectivity could be achieved due to increased electron density.

Orientador: Claudio Airoldi / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Quimica / Made available in DSpace on 2018-08-14T14:21:13Z (GMT). No. of bitstreams: 1 Moscofian_AndreaSalesdeOliveira_D.pdf: 1968679 bytes, checksum: b66014bf3fdc4c05b9755eac5d6d6ef0 (MD5) Previous issue date: 2009 / Resumo: Filossilicatos de magnésio e sílicas mesoporosas, com grupos orgânicos ligados às estruturas poliméricas inorgânicas, foram estudados na remoção de corantes. Para a síntese dos materiais nanoestruturados organofuncionalizados foram empregados agentes sililantes, (H3CO)3Si-R1, em que R1 é a cadeia carbônica contendo grupos funcionais: 3-aminopropiltrimetoxissilano, cloreto de octadecildimetil(3-trimetoxissilil-propil)amônio, 3-mercaptopropiltrimetoxissilano, 3-etilenodiaminopropiltrimetoxissilano e 3-dietilenotriaminopropiltrimetoxissilano. Através do processo sol-gel foram obtidos filossilicatos com estruturas inorgânicas similares àquelas dos silicatos lamelares naturais e sílicas mesoporosas empregando-se o surfatante CTAB como direcionador da estrutura inorgânica. As moléculas pendentes nos poros dos novos materiais com cargas positivas ou protonadas interagiram com as cargas negativas dos corantes utilizados na indústria têxtil: amarelo reativo GR, vermelho reativo RB e azul reativo RN. O estudo de adsorção mostrou que o filossilicato contendo cloreto de octadecildimetil(3-trimetoxissilil-propil)amônio, Fil-COTA, foi o material que apresentou a maior capacidade de adsorção, 1343 mg gpara o corante amarelo GR, 1286 mg g para o azul reativo RN e 344 mg gpara o vermelho reativo RB. Também foram realizados testes em amostras reais de efluente têxtil. Os resultados mostraram que não é necessário ajustar o pH inicial, a saturação do material ocorre após 3 h, sendo necessária uma massa mínima de 2,5 g dm de Fil-COTA. Portanto, este material é promissor no tratamento de efluentes têxteis reais. / Abstract: Magnesium phyllosilicates and mesoporous silicas, with organic groups anchored onto an inorganic polymeric backbones were studied for dye removal. In the synthesis of the organofunctionalized nanostructured materials, the silylanting agents, (H3CO)3Si-R1, where R1 represents carbonic chain containing functional groups: 3-aminopropyltrimethoxysilane, octadecyl (3-trimethoxysylilpropyl)ammonium chloride, 3 ¿ mercaptopropyltri-methoxysilane, 3-ethylenediaminetrymethoxysilane and 3-diethy-lenetriaminetrymethoxysilane were employed. The sol-gel process was used and phyllosilicates with inorganic lamellar structures similar to those of natural silicate and mesoporous silicas were obtained using the surfactant CTAB as template to direct inorganic structure in the latter case. The pendent molecules in pores of the new material with positive charge interact with the negative charge of the dyes used in the textile industry: reactive yellow GR, reactive red RB and reactive blue RN. The adsorption study showed that the phyllosilicate containing octadecyldimethyl(3-trimethoxysilylpropyl)ammonium chloride, Fil-COTA, presented the highest adsorption capacity, 1343 mg g for reactive yellow GR, 1286 mg g for reactive blue RN and 344 mg g for reactive red RB. Real samples of textile effluents were also tested. The results showed that it is not necessary to ajust the inicial pH, surface saturation occurs after 3 h and the minimum mass necessary is 2,5 g dm of Fil-COTA. Thus, this is a promising material for textile effluent treatement. / Doutorado / Quimica Inorganica / Doutor em Ciências

Philosophiae Doctor - PhD / The results of this study show that novel mesoporous carbons were obtained as inverse replica of SBA-15, HMS and MCM-41 silica templates, with a large pore diameter (2-4 nm), a BET surface area of 1867, 874 and 910 m2g–1 respectively for CA_SBA-15_LPG_105, CA_HMS_LPG_80 and CA_MCM- 41_LPG_80 with bimodal pore size distribution (PSD) in the mesopores range. The results obtained show that mesoporous carbon with graphitic structures can be synthesized via the LPG route. / South Africa

The objective of this work was to synthesize functionalized mesoporous silsesquioxanes with high concentrations of amine groups. During typical sol-gel syntheses, these materials are obtained by co-condensation of organic precursors with suitable linkers, such as tetraethoxysilane, necessary to prevent the mesoporous structure from collapsing. Thus, concentrations of amine groups in organosilicas usually do not exceed 2.7-3.4 mmol g -1. The use of bridged bis-trimethoxysilanes, however, allowed formation of mesoporous materials with no linker. Polycondensation of bis-trimethoxysilanes containing amine groups was conducted in acidic, neutral and basic media, resulting in high yields of solid bridged silsesquioxanes. Gelation occurred quickly if no acid or base was added to the reaction mixture. The hybrid organic/ inorganic nature of obtained materials was confirmed by FT-IR and MAS CP NMR spectroscopy. Elemental analysis showed that amino group concentration in the products was 3.3-4.1 mmol g -1. Measurement of particle size distribution confirmed that choice of reaction media significantly affects particle sizes and agglomeration degrees, with the largest agglomerates (up to 50 μm) formed in basic media. A morphology study, using smallangle X-Ray scattering, displayed two-level fractal structures composed of aggregated 6.5-10.5 nm particles. Reactions in the presence of a surfactant resulted in formation of mesoporous structures. Furthermore, the obtained bridged silsesquioxanes were thermally stable down to 260 °C, but could reversibly absorb water and CO 2 at temperatures below 120 °C. Thus, condensation of the bridged precursor without a linker resulted in formation of a highly functionalized mesoporous material.

Abstract: Silica gels containing embedded heteropolyacids were synthesized in acidic media by co-condensation of tetraethoxysilane with phosphotungstic or phosphomolybdic acids using the sol-gel technique. Surfactants dodecylamine, sodium dodecylsulfate, trimethylstearylammonium chloride, and Pluronic P123 were used as templates. The effect of the synthesis conditions on their structure and morphology was studied. All materials were mesoporous but contained micropores in their structures. Presence of bands of Keggin structures in fourier transform infrared spectroscopy spectra along with absence of X-ray diffraction patterns of crystalline heteropolyacids confirmed their fine incorporation into silica network. Particle sizes of modified materials were 500–1100 nm except for the W-containing sample obtained with trimethylstearylammonium chloride, which was significantly lower. This unusual effect was attributed to stabilization of primary silica nanoparticles by interactions between the surfactant and heteropolyacid. High ratio heteropolyacid/tetraethoxysilane resulted in partial loss of porosity. Obtained results might be used for optimization of synthesis of effective catalysts and adsorbents containing heteropolyacids in mesoporous structure. Graphical Abstract: [InlineMediaObject not available: see fulltext.]

[ES] Se ha desarrollado un método de síntesis "verde" de compuestos metal orgánicos en medio acuoso, a temperatura y presión ambientes, fácilmente escalable y con tiempos de cristalización muy cortos (10 min). El método se ha aplicado con éxito a la síntesis de trimesatos de metales divalentes isoreticulares y con fórmula general M3(BTC)2·12 H2O (M = Ni2+, Co2+, Cu2+ y Zn2+; BTC = trimesato). La estructura de estos materiales presenta dos tipos de centros metálicos ("puente" y "ter-minales") en proporción 2 a 1, ambos con coordinación octaédrica y unidos a 4 moléculas de H2O y a dos oxígenos carboxilato del ligando. Usando este método de síntesis, se han preparado también series de compuestos bimetálicos isoreticulares de Co-Ni y Co-Zn en todo el rango de concentraciones, así como compues-tos de Mn-Ni con una concentración máxima de Mn2+ del 50%. Mediante la combinación de difracción de rayos X (en polvo y de monocristal) y microscopía EDX/SEM se ha demostrado que los compuestos bimetálicos forman verdaderas disoluciones sólidas (no meras mezclas de fases) y que los iones metálicos se dis-tribuyen homogéneamente en todo el cristal. Además, el análisis detallado de la variación de los parámetros de celda con la composición en compuestos Co-Ni y Co-Zn aporta fuertes evidencias de que los iones Co2+ ocupan preferentemente las posiciones "terminales". Se ha evaluado la actividad de los compuestos preparados como catalizadores para la oxidación aeróbica de cumeno (CM) a cumeno hidroperóxido (CHP). El com-puesto monometálico de Co2+, Co-BTC, presentó una elevada actividad, aunque la selectividad a CHP obtenida fue relativamente baja (69%), ya que los iones Co2+ catalizan también la descomposición del CHP formado. Una buena estrategia para optimizar esta selectividad consistió en aislar los iones Co2+ en una matriz de Ni-BTC (que es inerte tanto para la oxidación de CM como para la descomposición de CHP). Así, al disminuir la concentración de iones Co2+ en compuestos bimetálicos Co-Ni se observó un aumento de la selectividad a CHP de hasta el 91% para el material con un 5% de Co. Se ha calculado que estadísticamente el 73% de los iones Co2+ en este material se encuentran aislados, por lo que la des-composición/sobreoxidación del CHP se ve muy limitada. Usando una variación del método de síntesis, se han obtenido también compuestos isoreticulares de Co2+ en los que los ligandos trimesato se han reemplazado parcialmente por ligandos isoftálico o 5-aminoisoftálico. Al utilizar estos com-puestos como catalizadores para la oxidación aeróbica de CM, se ha observado que la introducción de este segundo ligando (y en particular del 5-aminoisoftálico) en la red metal-orgánica facilita la descomposición del CHP formado y aumenta la selectividad final a 2-fenil-2-propanol (PP). Esto se ha atribuido a la creación de defectos puntuales en la red del material, que presentan una mayor actividad para la descomposición de CHP. Siguiendo con la oxidación de CM como reacción modelo, se ha evaluado la actividad catalítica de compuestos isoreticulares de cobalto con ligandos bispirazolato funcionalizados con distintos grupos (CoBPZ, CoBPZ-NO2 y CoBPZ-NH2). En este caso se ha observado una clara influencia del ligando utilizado sobre la acti-vidad catalítica y la selectividad a CHP o PP del material. Mientras que el Co-BPZ presenta una baja conversión de CM y una elevada selectividad a CHP, Co-BPZ-NH2 presenta las características opuestas: una elevada velocidad de reacción pero una baja selectividad a CHP. En este último caso, el producto mayoritario forma-do es el PP. Por último, el estudio de MOFs de cationes divalentes como catalizadores de oxidación se ha completado con una reacción de síntesis de quinazolina mediante acoplamiento oxidativo de bencilamina y 2-aminoacetofenona usando TBHP co-mo oxidante. Como catalizadores para esta reacción se ha utilizado el trimesato de / [CAT] S'ha desenvolupat un mètode de síntesi "verda" de compostos metall orgànics en medi aquós, a temperatura i pressió ambients, fàcilment escalable i amb temps de cristal·lització molt curts (10 min). El mètode s'ha aplicat amb èxit a la síntesi de trimesats de metalls divalents isoreticular i amb fórmula general M3(BTC)2·12 H2O (M = Ni2+, Co2+, Cu2+ y Zn2+; BTC = trimesat). L'estructura d'aquests materials presenta dos tipus de centres metàl·lics ("pon" i "terminals") en una proporció de 2 a 1, ambdós amb coordinació octaèdrica i units a 4 molècules d'aigua i a 2 oxígens carboxilat del lligand. Emprant aquest mètode de síntesi, s'han preparat també sèries de compostos bimetàl·lics isoreticular de Co-Ni i Co-Zn en tot el rang de concentracions, així com compostos de Mn-Ni amb una concentració màxima de Mn2+ del 50%. Mitjançant l'ús combinat de difracció de raigs X (en pols i de monocristall) i microscòpia EDX/SEM s'ha demostrat que els compostos bimetàl·lics formen vertaderes dissolucions sòlides (no simples mescles de fase) i que els ions metàl·lics es distribueixen homogèniament en tot el cristall. A més, l'anàlisi detallat de la variació dels paràmetres de cel·la amb la composició de compostos Co-Ni i Co-Zn aporta fortes evidències de que els ions Co2+ ocupen preferentment les posicions "terminals". S'ha avaluat l'activitat dels compostos preparats com a catalitzador per a l'oxidació aeròbica de cumè (CM) a cumè hidroperòxid (CHP). El compost monometàl·lic de Co2+, Co-BTC, presenta una elevada activitat, encara que la selectivitat a CHP obtinguda és relativament baixa (69%), ja que els ions Co2+ catalitzen també la descomposició del CHP format. Una bona estratègia per optimitzar aquesta selectivitat consisteix en aïllar els ions Co2+ en una matriu de Ni-BTC (que és inert tant per a l'oxidació de CM com per a la descomposició de CHP). Així, a mesura que disminueix la concentració d'ions Co2+ en compostos bimetàl·lics Co-Ni s'observa un augment de la selectivitat a CHP de fins el 91% per al material amb un 5% de cobalt. S'ha calculat que estadísticament el 73% dels ions Co2+ d'aquest material es troben aïllats, de manera que la descomposició/sobreoxidació del CHP es veu molt limitada. Emprant una variació del mètode de síntesi, s'han obtingut també compostosisoreticulars de Co2+ en els que els lligands trimesat s'han reemplaçat parcialment per lligands isoftàlic o 5-aminoisoftàlic. Quan aquest compostos s'usen com a catalitzadors per a l'oxidació aeròbica de CM, sobserva que la introducció d'aquest segon lligand (i en particular del 5-aminoisoftàlic) en la xarxa metallorgànica es facilita la descomposició del CHP format i augmenta la selectivitat final a 2-fenil-2-propanol (PP). Això s'ha atribuït a la creació de defectes puntuals en la xarxa del material, que presenten una major activitat per a la descomposició del CHP. Seguint amb l'oxidació de CM com a reacció model, s'ha avaluat l'activitat catalítica de compostosisoreticulars de cobalt amb lligands bispirazolat funcionalitzats amb distints grups (CoBPZ, CoBPZ-NO2 i CoBPZ-NH2). En aquest cas s'ha observat una clara influència del lligand utilitzat sobre l'activitat catalítica i la selectivitat a CHP o PP del material. Mentre que el CoBPZ presenta una baixa conversió de CM i una elevada selectivitat a CHP, CoBPZ-NH2 presenta les característiques oposades: una elevada velocitat de reacció però una baixa selectivitat a CHP. En aquest últim cas, el producte majoritari format és el PP. Per últim, l'estudi de MOFs amb cations divalent como a catalitzadors d'oxidació s'ha completat amb una reacció de síntesi de quinazolina mitjançant acoblament oxidatiu de benzilamina i 2-aminoacetofenona emprant TBHP como a oxidant. Com a catalitzadors per aquesta reacció s'ha utilitzat el trimesat de coure, HKUST-1, així com materials isoreticular amb lligands mixtes obtinguts reemplaçant pa / [EN] A "green" synthesis method has been developed for the preparation of metal organic frameworks in aqueous media, which is easily scalable, at room tempera-ture, ambient pressure and very short crystallization times (10 min). This method has been successfully applied to the synthesis of isoreticular divalent metal trimesates of general formula M3(BTC)2·12 H2O (M = Ni2+, Co2+, Cu2+ y Zn2+; BTC = trimesate). The structure of these compounds features two types of metal centers ("bridging" and "terminal") in a 2 to 1 ratio, both with octahedral coordina-tion and linked to 4 water molecules and 2 carboxylate oxygens of the ligand. Using this method, two series of bimetallic isoreticular compounds of Co-Ni and Co-Zn have also been prepared in all range of compositions, as well as bimetallic Mn-Ni compounds up to a maximum concentration of 50% of Mn2+. A combined X-ray diffraction (powder and single crystal) and EDX/SEM has shown that these bimetallic compounds form true solid solutions (not simple mixture of phases) and that both ions distribute homogeneously throughout the crystal. A detailed analysis of the variation of cell parameters with the composition strongly sug-gests that Co2+ ions occupy preferentially the "terminal" positions of the frame-work. The materials obtained with the above method have been evaluated as catalysts for the aerobic oxidation of cumene (CM) to cumene hydroperoxide (CHO). The monometallic Co2+ compound, Co-BTC, showed a high catalytic activity, but a relatively low selectivity to CHP 69%), since the Co2+ ions can also catalyze the decomposition of the formed CHP. A good strategy to optimize the CHP selectivity consisted in isolating the Co2+ ions into a Ni-BTC (which is inert for both CM oxidation and CHP decomposition). In this way, as the concentration of Co2+ ions in the bimetallic Co-Ni compound decreases, a parallel increase of the CHP selec-tivity was observed, up to 91% for the material with 5% of Co. In this compound, 73% of the total Co2+ ions are statistically isolated, so that decomposi-tion/overoxidation of CHP is unlikely to occur. By using a variation of the above synthesis method, additional isoreticular Co2+ compounds have been prepared in which the trimesate ligands have been partially replaced by either isophthalic or 5-aminoisophthalic. When these compounds were used as catalysts for the aerobic oxidation of cumene, we observed that the introduction of this second ligand (in particular in the case of 5-aminoisophthalic) into the framework facilitates decomposition of CHP and in-creases the final selectivity to 2-phenyl-2-propanol (PP). This has been attributed to the progressive creation of point defects in the framework, having a higher activity for CHP decomposition. Following with the aerobic oxidation of CM as model reaction, we evaluated the catalytic activity of isoreticular cobalt compounds having bispyrazolate ligands bearing differnent functional groups (CoBPZ, CoBPZ-NO2 and CoBPZ-NH2). In this case, there is a clear influence of the ligand used on the catalytic activity of the material and the obtained selectivity to CHP or PP. While CoBPZ showed a low CM conversion and high CHP selectivity, the opposite properties are obtained for the Co-BPZ-NH2: i.e., a high reaction rate but a low CHP selectivity. In this latter case, the major product of the reaction was PP. Finally, the evaluation of divalent MOFs as oxidation catalysts has been complet-ed by addressing the synthesis of quinazoline through the oxidative coupling reaction of benzylamine and 2-aminoacetophenone using TBHP as oxidant. As catalysts for this reaction we have used a copper trimesate, HKUST-1, as well as isoreticular mixed-ligand compounds obtained by partially replacing trimesate ligands by 5-hydroxyisophthalic (OH-isophthalic). / Nowacka, AE. (2019). Divalent Metal Organic Frameworks as Heterogeneous Oxidation Catalysts [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/129872 / TESIS

Les nanosciences représentent, actuellement, un domaine de recherche en pleine expansion grâce aux nombreuses applications auxquelles elles peuvent être associées, et en particulier à la course à la miniaturisation des systèmes. De plus, il a rapidement été montré que les propriétés physico-chimiques des matériaux à l’échelle nanométrique sont modifiées parfois de manière drastique, à cause par exemple des effets quantiques apparaissant à des tailles aussi petites, mais aussi en raison des effets de confinement. Le confinement de molécules ou de particules à l’échelle nanoscopique nécessite donc la fabrication de matériaux hôtes possédant ce qu’il convient d’appeler des sites de confinement, c’est-à-dire des sites possédant une taille voisine de celle du système à insérer. Ce type de matériau est désormais relativement connu, et deux familles monopolisent l’intérêt, à savoir la silice mésoporeuse, aussi et récemment utilisé, les verres bioactifs à base de silice ayant des caractéristiques contrôlées qui constituent des matériaux hôtes de confinement qui peuvent être immergés dans des fluides complexes tel que le plasma sanguin synthétique. Pour réaliser ces travaux on a besoins d’appliquer plusieurs techniques de caractérisations telles que la diffusion des Rayons X et des Neutrons, la Microscopie Electronique à Balayage et à Transmission, la spectroscopie Infrarouge à Transformé de Fourier etc...De plus, ces dernières années, des systèmes microfluidiques ont été utilisés pour élaborer des émulsions doubles, des microcapsules ou des microparticules, avec la particularité d’obtenir des populations très monodisperses par rapport à celles obtenues avec des techniques plus traditionnelles et de morphologie contrôlée. Dans le domaine pharmaceutique, ces capacités sont particulièrement intéressantes pour la synthèse de médicaments à libération contrôlée. Elles permettent d’obtenir des particules monodisperses de polymère encapsulantes pour lesquelles l’effet de relargage brutal est diminué et qui possèdent des vitesses de relargage plus lentes que celles observées avec des procédés de fabrication conventionnels. / Nanoscience currently represent a growing area of research through the many applications for which they may be associated, particularly in the race for miniaturization of systems. In addition, it was quickly demonstrated that the physico-chemical properties of nanoscale materials are sometimes changed drastically, for example because of quantum effects occurring at sizes as small, but also because of confinement effects .Confinement of molecules or particles at the nanoscale therefore requires the manufacture of host materials with what to call containment sites, that is to say, sites with a size close to that of the system insert. This type of material is now relatively well known, and two families monopolize the interest, ie the mesoporous silica, and also recently used bioactive glasses based on silica having controlled characteristics that are host materials containment can be immersed in complex fluids such as synthetic blood plasma.To do this work several characterization techniques we need to apply, including the spread of X-rays and neutrons, the Scanning Electron Microscopy and Transmission, Infrared spectroscopy Transformed Fourier etc ...Moreover, in recent years, microfluidic systems were used to prepare double emulsions, microcapsules or microparticles, with the particularity to obtain highly monodisperse populations compared to those obtained with more traditional and controlled morphology techniques. In the pharmaceutical field, these capabilities are particularly interesting for the synthesis of controlled release to drugs. They enable polymer monodisperse particles encapsulating why the sudden release effect is decreased and have slower release rates than those observed with conventional manufacturing processes

京都大学 / 0048 / 新制・課程博士 / 博士(農学) / 甲第20426号 / 農博第2211号 / 新制||農||1048(附属図書館) / 学位論文||H29||N5047(農学部図書室) / 京都大学大学院農学研究科応用生命科学専攻 / (主査)教授 加納 健司, 教授 植田 充美, 教授 三上 文三 / 学位規則第4条第1項該当 / Doctor of Agricultural Science / Kyoto University / DFAM

京都大学 / 0048 / 新制・課程博士 / 博士(農学) / 甲第20715号 / 農博第2244号 / 新制||農||1053(附属図書館) / 学位論文||H29||N5081(農学部図書室) / 京都大学大学院農学研究科応用生命科学専攻 / (主査)教授 加納 健司, 教授 宮川 恒, 教授 三芳 秀人 / 学位規則第4条第1項該当 / Doctor of Agricultural Science / Kyoto University / DFAM