47 resultados para Hybrid material


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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Here we describe the preparation of iron(II) porphyrinosilica in a simple one-pot reaction, where the -SO2Cl groups present in the phenyl rings of FeTDCSPP+ react with 3-aminopropyltriethoxysilane and tetraethoxysilane in the presence of a nitrogenous base, leading to iron(III) porphyrinosilica. In this same procedure, molecular cavities containing regularly spaced functional groups are created through the molecular imprinting technique, in which the nitrogenous base coordinated to the iron(III) porphyrin serves as a template. The removal of such template in a Soxhlet extractor leads to a cavity with the same shape and size as the nitrogenous base, enabling the construction of shape-selective catalysts mimicking cytochrome P-450. Five different imprinting molecules have been used: imidazole, 1-methylimidazole, 2-methylbenzimidazole, 4-phenylimidazole and miconazole and ultra-violet/visible absorption spectroscopy, thermogravimetric analysis and electron paramagnetic resonance carried out. (C) 1999 Elsevier B.V. B.V. All rights reserved.

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In recent years studies concerning the applications of lignocellulosic/ inorganic couples have resulted in the development of an interesting class of functional materials. In this work a cellulose/NbOPO 4.nH 2O hybrid using cellulose from surgacane bagasse was prepared and characterized in order to test for adsorption applications. The preparation process was conducted by carrying out metallic niobium dilution in hydrofluoric acid in the presence of nitric acid, then adding boric acid to form the complex and, finally, the cellulose sugar cane bagasse was added. Concentrated phosphoric acid was also inserted to precipitate hydrous niobium phosphate particles in the cellulose fiber. This material was characterized by X-ray diffractometry (XRD), thermogravimetry (TG/DTG), and scanning electronic microscopy (SEM) connected to an energy dispersive spectrophotometer (EDS). Results by SEM/EDS show that NbOPO 4.nH 2O was present in structure of the cellulose. During the preparation of the material, using boric acid it was observed that the formation of precipitate occurred in a shorter time than the material prepared without boric acid.

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The aim of this study was to evaluate the internal fit, marginal adaptation, and bond strengths of inlays made of computer-aided design/computer-aided manufacturing feldspathic ceramic and polymer-infiltrated ceramic. Twenty molars were randomly selected and prepared to receive inlays that were milled from both materials. Before cementation, internal fit was achieved using the replica technique by molding the internal surface with addition silicone and measuring the cement thicknesses of the pulpal and axial walls. Marginal adaptation was measured on the occlusal and proximal margins of the replica. The inlays were then cemented using resin cement (Panavia F2.0) and subjected to two million thermomechanical cycles in water (200 N load and 3.8-Hz frequency). The restored teeth were then cut into beams, using a lathe, for microtensile testing. The contact angles, marginal integrity, and surface patterns after etching were also observed. Statistical analysis was performed using two-way repeated measures analysis of variance (p<0.05), the Tukey test for internal fit and marginal adaptation, and the Student t-test for bond strength. The failure types (adhesive or cohesive) were classified on each fractured beam. The results showed that the misfit of the pulpal walls (p=0.0002) and the marginal adaptation (p=0.0001) of the feldspathic ceramic were significantly higher when compared to those of the polymer-infiltrated ceramic, while the bond strength values of the former were higher when compared to those of the latter. The contact angle of the polymer-infiltrated ceramic was also higher. In the present study, the hybrid ceramic presented improved internal and marginal adaptation, but the bond strengths were higher for the feldspathic ceramic.

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A composite of cellulose extracted from bagasse with Nb2O5 center dot nH(2)O in three different proportions (16.67, 37.5 and 50.0 wt%) was prepared using the co-precipitation method. The materials were characterized by X-ray diffractometry (XRD), Fourier transform infra-red spectroscopy (FTIR), thermogravimetric analysis (TG/DTG), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). TG data obtained show that the presence of inorganic material influenced slightly the stability of the hybrid material. The precipitation of 16.67 wt.% of oxide was sufficient to inhibit the combustion peaks present in the DSC curve of cellulose. This work will help find new applications for these materials. Published by Elsevier Ltd.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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In this work, a new organic-inorganic hybrid material has been synthesized by the incorporation of croconate ion into a calcium polyphosphate coacervate. The hybrid so obtained was characterized by means of electronic and vibrational spectroscopies. The material is a homogeneous mixture described by a structural model, which includes helical chains of polyphosphate ions, where the calcium ion occupies the internal vacancies of the structure. The croconate ion appears to be occupying the regions outside the polymeric structure, surrounded by several water molecules. The electronic spectrum of the incorporated material shows a broad band peaking at the same wavelength region (363 nm) observed for the aqueous solution of croconate ion, and manifesting the Jahn-Teller effect as evidenced by the doublet structure of the band. The infrared spectrum is widely dominated by the absorption bands of the polyphosphate ion and the appearance of the carbonyl stretching band at ca. 1550 cm(-1) indicates the presence of croconate ion incorporated in the structure. The Raman spectrum of the material shows several vibrational bands related to the oxocarbon moiety; most of them are shifted in comparison with the free ion. These shifts can be understood in terms of strong hydrogen bonding interactions between water molecules and the oxocarbon moiety. The low temperature methodology proposed here can be well used in the preparation of new phosphate glasses containing organic moieties opening the route to an entirely new class of hybrid glasses. (c) 2004 Elsevier B.V All rights reserved.

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Hybrid siloxane-polymethylmethacrylate (PMMA) nanocomposites with covalent bonds between the inorganic (siloxane) and organic (polymer) phases were prepared by the sot gel process through hydrolysis and polycondensation of 3-(trimethoxysilyl)propylmethacrylate (TMSM) and polymerization of methylmethacrylate (MMA) using benzoyl peroxide (BPO) as initiator. The effect of MMA, BPO and water contents on the viscoelastic behaviour of these materials was analysed during gelation by dynamic rheological measurements. The changes in storage (G') and loss moduli (G), complex viscosity (eta*) and phase angle (6) were measured as a function of the reaction time showing the viscous character of the sot in the initial step of gelation and its progressive transformation to an elastic gel. This study was complemented by Si-29 and C-13 solid-state nuclear magnetic resonance (NMR/MAS) measurements of dried gel. The analysis of the experimental results shows that linear chains are formed in the initial step of the gelation followed by a growth of branched structures and formation of a three-dimensional network. Near the gel point this hybrid material demonstrates the typical scaling behaviour expected from percolation theory.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Rare earth complexes (RE) can be incorporated in silica matrixes, originating organic/inorganic hybrid materials with good thermal stability and high rare earth emission lines. In this work, the hybrid material was obtained by the polymeric precursor method and ultrasonic dispersed with spherical silica particles prepared by the Stöber Method. The Raman spectra indicated that the Eu3+ ions are involved in a polymeric structure formed as consequence of the chelation and polyesterification reactions of this ion with citric acid and ethylene glycol. After the ultrasonic stirring, 2-hydroxynicotinic ligand will also compose this polymeric rigid structure. The TGA/DTA analysis showed that this polymeric material was thermal decomposed at 300 °C. Moreover, this process allows the chelating process of the 2-hydroxynicotinic acid ligand to the Eu3+ ions. The 29Si NMR showed that the ultrasonic dispersion of the reactants was not able to promote the functionalization of the silica particles with the 2-hydroxynicotinic acid ligand. Moreover, heat treatment promotes the [Eu(HnicO2)3] complex particles incorporation into silica pores. At this temperature, the TGA curve showed that only the thermal degradation of ethylene glycol and citric acid used during the experimental procedure occurs. The silica and hybrid materials are composed by spherical and aggregated particles with particle size of approximately 450 nm, which can be influenced by the heat treatment. These materials also present an absorption band located at 337 nm. The photoluminescent study showed that when the hybrid samples were excited at 337 nm wavelength, the ligand absorbs the excitation light. Part of this energy is transferred to the Eu3+ ion, which main emission, 5D0→ 7F2, is observed in the emission spectrum at 612 nm. As the heating temperature increases to 300 C, the energy transfer is more favorable. The lifetime values showed that the Eu3+ emission is enhanced due to the energy transfer process in the powders. © 2013 Elsevier B.V. All rights reserved.