961 resultados para SOLVOTHERMAL ROUTE
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Herein we demonstrate a facile template-free sonochemical strategy to synthesize mesoporous g-C3N4 with a high surface area and enhanced photocatalytic activity. The TEM and nitrogen adsorption–desorption studies confirm mesoporous structure in g-C3N4 body. The photocatalytic activity of mesoporous g-C3N4 is almost 5.5 times higher than that of bulk g-C3N4 under visible-light irradiation. The high photocatalytic performance of the mesoporous g-C3N4 was attributed to the much higher specific surface area, efficient adsorption ability and the unique interfacial mesoporous structure which can favour the absorption of light and separation of photoinduced electron–hole pairs more effectively. A possible photocatalytic mechanism was discussed by the radicals and holes trapping experiments. Interestingly, the synthesized mesoporous g-C3N4 possesses high reusability. Hence the mesoporous g-C3N4 can be a promising photocatalytic material for practical applications in water splitting as well as environmental remediation.
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Hierarchical ZnO “rod like” architecture was successfully synthesized via reverse micellar route and characterized by various techniques. The FESEM studies show controlled decomposition of zinc oxalate into ZnO “rod like” architecture at 500 °C with slow heat rate at 1°/min. Interestingly, improved photocatalytic activity was observed for the degradation of Rhodamine B, due to the self assembly of hexagonal nanoparticles of zinc oxide forming hierarchical ZnO “rod like” architecture which can greatly enhance the light utilization rate due to its special architecture and enlarge the specific surface area, providing more reaction sites and promoting mass transfer. More importantly, the reusability studies of this architecture were most economical.
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High surface area nanosized α-alumina has been obtained by thermally treating a sol-gel-derived mesophase at 1200 C; the mesophase was synthesized by a sol-gel route involving evaporation induced self-assembly (EISA) of a hydrolyzed gel from Al-tri-sec-butoxide in s-BuOH in the presence of a nonionic surfactant (EO20PO70EO20), HCl as catalyst, and water (H2O/Al = 6). The activated material renders moderate surface areas of about 8.4-10 m2 g-1, associated with significant crystallite coarsening. The key aspect to produce smaller crystallites is making the mesophase more resistant to coarsening. This was achieved by enhancing the condensation step by treating the hydrolyzed gel with tetrabutyl ammonium hydroxide (TBAOH) before evaporation. The characteristics of the mesophase indicate condensation of the primary particles with less AlO5 unsaturated sites, at the expense of a lower solid yield due to small crystallites dissolution. The activated TBAOH condensed EISA material is composed of α-alumina aggregated crystallites of about 60-100 nm, and the material possesses surface areas ranging from 16 to 24 m2 g -1 due to the improved resistance to coarsening. At least two aspects are suggested to play a role in this. The worm-hole morphology of the mesophase aggregates yields high particle coordination, which favors densification rather than coarsening. Furthermore, the decrease of the AlO5 defect sites by the TBAOH condensation makes the mesophase less reactive and consequently more resistant to coarsening. © 2013 American Chemical Society.
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Binary skutterudite CoSb3 nanoparticles were synthesized by solvothermal method. The nanostructuring of CoSb3 material was achieved by the inclusion of various kinds of additives. X-ray diffraction examination indicated the formation of the cubic phase of CoSb3. Structural analysis by transmission electron microscopy analysis further confirmed the formation of crystalline CoSb3 nanoparticles with high purity. With the assistance of additives, CoSb3nanoparticles with size as small as 10 nm were obtained. The effect of the nanostructure of CoSb3on the UV–visible absorption and luminescence was studied. The nanosized CoSb3 skutterudite may find application in developing thermoelectric devices with better efficiency. K
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Magnesium borate hydroxide (MBH) nanowhiskers were synthesized using a one step hydrothermal process with different surfactants. The effect surfactants have on the structure and morphology of the MBH nanowhiskers has been investigated. The X-ray diffraction profile confirms that the as-synthesized material is of single phase, monoclinic MgBO2(OH). The variations in the size and shape of the different MBH nanowhiskers have been discussed based on the surface morphology analysis. The annealing of MBH nanowhiskers at 500 °C for 4 h has significant effect on the crystal structure and surface morphology. The UV–vis absorption spectra of the MBH nanowhiskers synthesized with and without surfactants show enhanced absorption in the low-wavelength region, and their optical band gaps were estimated from the optical band edge plots. The photoluminescence spectra of the MBH nanowhiskers produced with and without surfactants show broad emission band with the peak maximum at around 400 nm, which confirms the dominant contribution from the surface defect states.
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This thesis is part of research on new materials for catalysis and gas sensors more active, sensitive, selective. The aim of this thesis was to develop and characterize cobalt ferrite in different morphologies, in order to study their influence on the electrical response and the catalytic activity, and to hierarchize these grains for greater diffusivity of gas in the material. The powders were produced via hydrothermal and solvothermal, and were characterized by thermogravimetric analysis, X-ray diffraction, scanning electron microscopy, transmission electron microscopy (electron diffraction, highresolution simulations), and energy dispersive spectroscopy. The catalytic and electrical properties were tested in the presence of CO and NO2 gases, the latter in different concentrations (1-100 ppm) and at different temperatures (room temperature to 350 ° C). Nanooctahedra with an average size of 20 nm were obtained by hydrothermal route. It has been determined that the shape of the grains is mainly linked to the nature of the precipitating agent and the presence of OH ions in the reaction medium. By solvothermal method CoFe2O4 spherical powders were prepared with grain size of 8 and 20 nm. CoFe2O4 powders exhibit a strong response to small amounts of NO2 (10 ppm to 200 ° C). The nanooctahedra have greater sensitivity than the spherical grains of the same size, and have smaller response time and shorter recovery times. These results were confirmed by modeling the kinetics of response and recovery of the sensor. Initial tests of catalytic activity in the oxidation of CO between temperatures of 100 °C and 350 °C show that the size effect is predominant in relation the effect of the form with respect to the conversion of the reaction. The morphology of the grains influence the rate of reaction. A higher reaction rate is obtained in the presence of nanooctahedra. In order to improve the detection and catalytic properties of the material, we have developed a methodology for hierarchizing grains which involves the use of carbonbased templates.
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Metal Organic Frameworks (MOFs) are hybrids materials, often crystalline, consisting of metal or metal clusters, connected by polytopic organic ligands repetitively, leading to structures, usually porous. In this work, MOFs based on lanthanide ions (La3+ and Gd3+) and dicarboxylate type of ligands (isophthalic and terephthalic acids), were synthesized by hydrothermal, solvothermal and hydro(solvo)thermal methods. The effects of the synthetic route as well as the type of heating, conventional or by microwave, on the structure and properties of MOFs were studied. The powder samples obtained were characterized by X-ray diffraction, infrared spectroscopy, thermal analysis and scanning electron microscopy. The results suggest that the addition of an organic or inorganic base is needed to promote the deprotonation of the ligand, since in the samples prepared by the hydrothermal method, without the use of a base, no formation of the metalorganic framework was observed. On the other hand, the presence of DMF as solvent or cosolvent, afforded the deprotonation of the ligand with the consequent formation of MOFs. At least two different crystalline structures were identified for the samples prepared with terephthalic acid. These samples are isostructural with those reported for phases Eu(1,3-BDC)DMF, Eu2(1,4-BDC)3 (DMF)2 and Tb(1,4-BDC)H2O. The presence of water in the reaction medium in the hydro(solvo)thermal method, provoked the growth of the structure different from that observed in the absence of water. This can be explained by the difference in the coordination mode of water and DMF to lanthanide ions. Although not identified by XRD, the samples prepared with isophthalic acid, also present metalorganic structures, which was confirmed by the presence of the characteristic displacement of the carbonyl group band in their infrared spectra, compared to the spectrum of the pure ligand. This shift was also observed in the samples prepared with terephthalic acid. Thermal analisys shows that the metal organic frameworks do not collapse occurs at a temperature below 430°C.The analysis of scanning electron microscopy suggests that the morphology of powders is highly dependent on the type of heating used, conventional or by microwave.
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Date of Acceptance: 05/06/2015
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Date of Acceptance: 05/06/2015
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Date of Acceptance: 05/06/2015
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General note: Title and date provided by Bettye Lane.
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General note: Title and date provided by Bettye Lane.
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Mémoire numérisé par la Direction des bibliothèques de l'Université de Montréal.
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A prerequisite for vaccine-mediated induction of CD8+ T-cell responses is the targeting of dendritic cell (DC) subsets specifically capable of cross-presenting antigen epitopes to CD8+ T cells. Administration of a number of cationic adjuvants via the intraperitoneal (i.p.) route has been shown to result in strong CD8+ T-cell responses, whereas immunization via e.g. the intramuscular (i.m.) or subcutaneous (s.c.) routes often stimulate weak CD8+ T-cell responses. The hypothesis for this is that self-drainage of the adjuvant/antigen to the lymphoid organs, which takes place upon i.p. immunization, is required for the subsequent activation of cross-presenting lymphoid organ-resident CD8α+ DCs. In contrast, s.c. or i.m. immunization usually results in the formation of a depot at the site of injection (SOI), which hinders the self-drainage and targeting of the vaccine to cross-presenting CD8α+ DCs. We investigated this hypothesis by correlating the biodistribution pattern and the adjuvanticity of the strong CD8+ T-cell inducing liposomal cationic adjuvant formulation 09 (CAF09), which is composed of dimethyldioctadecylammonium bromide/monomycoloyl glycerol liposomes with polyinosinic:polycytidylic acid electrostatically adsorbed to the surface. Biodistribution studies with radiolabeled CAF09 and a surface-adsorbed model antigen [ovalbumin (OVA)] showed that a significantly larger fraction of the vaccine dose localized in the draining lymph nodes (dLNs) and the spleen 6 h after i.p. immunization, as compared to after i.m. immunization. Studies with fluorescently labelled OVA + CAF09 demonstrated a preferential association of OVA + CAF09 to DCs/monocytes, as compared to macrophages and B cells, following i.p. immunization. Administration of OVA + CAF09 via the i.p. route did also result in DC activation, whereas no DC activation could be measured within the same period with unadjuvanted OVA and OVA + CAF09 administered via the s.c. or i.m. routes. In the dLNs, the highest level of activated, cross-presenting CD8α+ DCs was detected at 24 h post immunization, whereas an influx of activated, migrating and cross-presenting CD103+ DCs to the dLNs could be measured after 48 h. This suggests that the CD8α+ DCs are activated by self-draining OVA + CAF09 in the lymphoid organs, whereas the CD103+ DCs are stimulated by the OVA + CAF09 at the SOI. These results support the hypothesis that the self-drainage of OVA + CAF09 to the draining LNs is required for the activation of CD8α+ DCs, while the migratory CD103+ DCs may play a role in sustaining the subsequent induction of strong CD8+ T-cell responses.