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Polyvinyl alcohol/Poly-aniline/Vanadium Oxide nanocomposite-based macroscopic fibers have been generated by using a redox reaction addressed while performing an extrusion shaping process. The resulting composites have been thoroughly characterized via a large set of techniques such as SEM, SAXS, XRD and FTIR, in order to determine aniline effects over final materials' structures and properties. Thus, the perturbation of the preferential orientation of the V2O5 nano-ribbons toward the fiber main axis, induced by aniline Red-ox intercalation, has been observed. Also, the partial reduction of V5+ species to V4+ ones, due to the strongly oxidizing character of the first ones toward aniline, has been revealed by Electron Spin Resonance (ESR). Moreover, these fibers are able to detect 5 ppm of ethanol within 3-5 seconds at 42 °C, and possess a toughness of 12 J.g-1.
A complete solid state NMR characterization of the vanadium oxides Cs[V3O8] and Cs2[V6O16].0.7H2O is proposed. We used 51V and 133Cs MAS NMR to investigate the local environment of cesium and vanadium nuclei and 2D 1H- 133Cs CP MAS HETCOR experiments to explore the connectivities between cesium ions and water molecules in the interlamellar space.
Vanadium oxide-collagen hybrid nanocomposites were prepared by adding a V2O5 sol to a dilute collagen solution. 51V MAS NMR spectroscopy shows that the inorganic phase is composed of the decavanadate [H2V10O28]4− polyanion and V2O5 ribbon-like particles. The broadening of the 51V signals and the absence of Bragg peaks in the XRD pattern suggest a strong disorder concerning the organization of the V2O5 particles and of the decavanadate species in the composites. Analogous hybrid nanocomposites were obtained with a solution that contains only the decavanadate species, showing that the cohesion in the hydrid material results mainly from electrostatic interactions between decavanadate [H2V10O28]4− polyanions and positively-charged collagen helices.
Upon extrusion process, first vanadium oxide macroscopic fibers have been obtained. They are associated to longitudinal Young modulus from 15 to 25 GPa and depict strong high scale textural anisotropy as observed through cross-polarized microscopy. TEM observations and SAXS experiments reveal that those macroscopic fibers are made of nanoscopic ribbons associated to preferential orientation parallel to the macroscopic fiber main axis, while XRD and NMR investigations reveal a microstructure close to the V2O5.1.8H2O xerogels. These fibers can detect down to 0.1 ppm of ethanol within 16 seconds at 40°C.
The synthesis of vanadium oxide nanotubes containing phosphorus (VPOx-NT) is described. A mixture of V2O5.nH2O gels, phosphoric acid and hexadecylamine was heated under hydrothermal conditions at 180°C for 7 days. The VPOx nanotubes were characterized by X-ray diffraction, scanning and transmission electron microscopy, 51V and 31P solid state NMR. In-situ experiments were performed in order to get a better understanding of the mechanism of these nanotubes formation.
Various cations (Li+, Na+, K+, NH4+, Cs+, Mg2+, Ca2+, Ba2+) were introduced during the formation of a V2O5. nH2O gel. Cation intercalated Xy V2O5. nH2O (y = 0.3 for X = Li+, Na+, K+, NH4+ or y = 0.15 for Mg2+, Ca2+, Ba2+) were first obtained at room temperature but some of them evolve upon ageing into a new phase: XV3O8. nH2O for X = Na+, K+, NH4+ and Cs+ or XV6O16. nH2O for X = Mg2+, Ca2+, Ba2+. All the vanadium oxide phases were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and infrared spectroscopy (IR); the supernatant solutions were analysed by 51V NMR spectroscopy. These vanadium oxide phases exhibit a layered structure with cations and water molecules intercalated within the interlayer space. The formation of the different phases depends mainly on the pH of the supernatant solution and on the nature of the cation.
Mesoporous silica materials have been studied for the time-dependent delivery of bioactive agents. It has already been shown that ibuprofen molecules can be encapsulated with loading as high as 30 wt% in MCM-41 silica, functionalized or not by amino groups. Interactions between the guest molecules and the host matrix have been investigated by 1H, 29Si and 13C solid state NMR spectroscopy. These experiments demonstrate an extremely high mobility of the ibuprofen molecules when the matrix is not functionalized, despite of the presence of a carboxylic function on the ibuprofen molecules. On the contrary, when the silica matrix is functionalized by amino groups, the 13C NMR response shows a strong restriction in mobility suggesting the existence of interactions between the amino groups and the carboxylic groups.
Tetramethylammonium (TMA) polyoxovanadates have been precipitated from aqueous solutions aroundpH 7. Decavanadate clusters (TMA)4[H2V10O28]•4H2O are formed at room temperature whereas a layered (TMA)[V4O10] mixed valence compound is formed under hydrothermal conditions. 51V NMR spectra recorded on the solution at different temperatures show that upon heating decavanadate clusters are progressively transformed into cyclic [V4O12]4− metavanadates. This suggests that the mixed valence polyoxovanadates are formed via the ring opening polymerization of metavanadate precursors.
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