Structural transition on Pb1-xSrxTiO3 produced by chemical method

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Influence of different light sources and photo-activation methods on degree of conversion and polymerization shrinkage of a nanocomposite resin

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Epitaxially grown LiNbO3 thin films by polymeric precursor method

LiNbO3 thin films were grown on (0001) sapphire substrates by a chemical route, using the polymeric precursor method. The overall process consists of preparing a coating solution from the Pechini process, based on metallic citrate polymerization, the precursor films, deposited by dip coating, are then heat treated to eliminate the organic material and to synthesize the phase. In this work, we studied the influence of the heat treatment on the structural and optical properties of single-layered films. Two routes were also investigated to increase the film thickness: increasing the viscosity of the coating solution and/or increasing the number of successively deposited layers. The x-ray diffraction theta -2 theta scans revealed the c-axis orientation of the single- and multilayered films and showed that efficient crystallization can be obtained at temperatures as low as 400 degreesC, the phi-scan diffraction evidenced the epitaxial growth with two in-plane variants, A microstructural study revealed that the films were crack free, homogeneous, and relatively dense. Finally, the investigation of the optical properties (optical transmittance and refractive index) confirmed the good quality of the films. These results indicate that the polymeric precursor method is a promising process to develop lithium niobate waveguides.

New layered double hydroxides intercalated with substituted pyrroles. 1. In situ polymerization of 4-(1H-pyrrol-1-yl)benzoate

The two-dimensional hybrid organic-inorganic materials Zn-2-Cr and Zn-2-Al-LDHs (Layered Double Hydroxides) containing 4-(1H-pyrrol-1yl)benzoate anions as the interlayer anions were synthesized by the co-precipitation method at constant pH followed by subsequent hydrothermal treatment for 72 h. The materials were characterized by PXRD, C-13 CP-MAS NMR, ESR, TGA, and TEM. The basal spacing found by the X-ray diffraction technique is coincident with the formation of bilayers of the intercalated anions. Solid-state C-13 NMR and ESR data strongly suggest the partial in situ polymerization of the 4-(1H-pyrrol-1yl)benzoate anions during coprecipitation. (c) 2006 Elsevier Ltd. All rights reserved.

AN ACTINOMETRIC STUDY OF C2H2 PLASMA POLYMERIZATION AND FILM PROPERTIES

Thin polymer films were grown in radio frequency discharges containing C2H2. Actinometry revealed the trend in the plasma concentration of the CH species as a function of the operating pressure. The C-H bond density in the films, revealed by infrared analysis, was found to increase with the pressure of C2H2 in a similar way to that of the concentration of the CH species in the discharge. From transmission ultraviolet-visible spectroscopy data, optical parameters of the polymers, namely, the refractive index and the optical gap, were calculated. For the range of pressure studied, the refractive index decreased from 1.73 to 1.63 and the optical gap increased from 2.4 to 3.3 eV. Finally, measurements of the residual stress of the polymer films were carried out by the bending beam method, using a He-Ne laser, yielding values from 0.05 to 0.3 GPa. (C) 1995 American Vacuum Society.

Thermal and structural investigation of SnO2/Sb2O3 obtained by the polymeric precursor method

SnO2-based materials are used as sensors, catalysts and in electro-optical devices. This work aims to synthesize and characterize the SnO2/Sb2O3-based inorganic pigments, obtained by the polymeric precursor method, also known as Pechini method (based on the metallic citrate polymerization by means of ethylene glycol). The precursors were characterized by thermogravimetry (TG) and differential thermal analysis (DTA). After characterization, the precursors were heat-treated at different temperatures and characterized by X-ray diffraction. According to the TG/DTA curves basically two-step mass loss process was observed: the first one is related to the dehydration of the system; and the second one is representative to the combustion of the organic matter. Increase of the heat treatment temperature from 500 to 600 degrees C and 700 degrees C resulted higher crystallinity of the formed product.

Preparation and properties of ferroelectric BaTiO3 thin films produced by the polymeric precursor method

Ferroelectric barium titanate thin films were produced by the polymeric precursor method. In this technique, the desired metal cations are chelated in a solution using a hydroxycarboxylic acid as the chelating agent. Barium carbonate and titanium IV isopropoxide were used as precursors for the citrate solution. Ethylene glycol and citric acid were used as polymerization/complexation agents for the process. The crystalline structure of the film annealed at 700 °C had a single perovskite phase with a tetragonal structure. The BaTiO3 film showed good P-E hysteresis loops and C-V characteristics due to the switched ferroelectric domains.

Analysis of polymerization time on abrasive wear of dental resins

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

Fabrication of Zinc Oxide Nanowires/Polymer Composites by Two-Photon Polymerization

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

Indirect doping of microstructures fabricated by two-photon polymerization with gold nanoparticles

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural characterization of Li-MN doped powders prepared by Pechini's method

Pechini's method has been successfully used to prepare Li-doped MgNb2O6(MN) at short time and low temperature. It consists in the preparation of metal citrate solution, which is polymerized at 250°C to form a high viscous resin. This resin was burned in a box type furnace at 400°C/2h and ground in a mortar. Successive steps of calcination up to 900°C were used to form a crystalline precursor. SEM, DTA and XRD were used to characterize the powders. MN precursor powders containing from 0.1 to 5.0 mol% of LiNbO3 additive was prepared aiming better dielectric properties and microstructural characteristics of the PMN prepared from columbite route. SEM analysis showed that particles increased by sintering, forming large agglomerates. The surface area is also substantially reduced with the increase in additive amount above 1.0 mol%. In XRD pattern of the precursor material with 5.0 mol% of additive was observed the LiNbO3 phase of trigonal structure. XRD data were used for Rietveld refinement and a decrease in microstrain and pronounced increase in crystallite size with the increase of LiNbO3 were observed. It is in agreement with the particle morphologies observed by SEM analysis.

The influence of "C-factor" and light activation technique on polymerization contraction forces of resin composite

Objectives: This study evaluated the influence of the cavity configuration factor ("C-Factor") and light activation technique on polymerization contraction forces of a Bis-GMA-based composite resin (Charisma, Heraeus Kulzer). Material and Methods: Three different pairs of steel moving bases were connected to a universal testing machine (Emic DL 500): groups A and B - 2x2 mm (CF=0.33), groups C and D - 3x2 mm (CF=0.66), groups E and F - 6x2 mm (CF=1.5). After adjustment of the height between the pair of bases so that the resin had a volume of 12 mm(3) in all groups, the material was inserted and polymerized by two different methods: pulse delay (100 mW/cm(2) for 5 s, 40 s interval, 600 mW/cm(2) for 20 s) and continuous pulse (600 mW/cm(2) for 20 s). Each configuration was light cured with both techniques. Tensions generated during polymerization were recorded by 120 s. The values were expressed in curves (Force(N) x Time(s)) and averages compared by statistical analysis (ANOVA and Tukey's test, p<0.05). Results: For the 2x2 and 3x2 bases, with a reduced C-Factor, significant differences were found between the light curing methods. For 6x2 base, with high C-Factor, the light curing method did not influence the contraction forces of the composite resin. Conclusions: Pulse delay technique can determine less stress on tooth/restoration interface of adhesive restorations only when a reduced C-Factor is present.

A method to investigate the shrinkage stress developed by resin-composites bonded to a single flat surface

Objectives. To purpose a method for predicting the shrinkage stress development in the adhesive layer of resin-composite cylinders that shrink bonded to a single flat surface, by measuring the deflection of a glass coverslip caused by the shrinkage of the bonded cylinders. The correlation between the volume of the bonded resin-composite and the stress-peak was also investigated. Methods. A glass coverslip deflection caused by the shrinkage of a bonded resin-composite cylinder (diameter: d = 8 mm, 4 mm, or 2 mm, height: h = 4 mm, 2 mm, 1 mm, or 0.5 mm) was measured, and the same set-up was simulated by finite element analysis (3D-FEA). Stresses generated in the adhesive layer were plotted versus two geometric variables of the resin-composite cylinder (C-Factor and volume) to verify the existence of correlations between them and stresses. Results. The FEA models were validated. A significant correlation (p < 0.01, Pearson's test) between the stress-peak and the coverslip deflection when the resin-composites were grouped by diameter was found for diameters of 2 and 4 mm. The stress-peak of the whole set of data showed a logarithmic correlation with the bonded resin-composite volume (p < 0.001, Pearson's test), but did not correlate with the C-Factor. Significance. The described method should be considered for standardizing the stress generated by the shrinkage of resin-composite blocks bonded to a single flat surface. (C) 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Indirect doping of microstructures fabricated by two-photon polymerization with gold nanoparticles

Nanoplasmonics and metamaterials sciences are rapidly growing due to their contributions to photonic devices fabrication with applications ranging from biomedicine to photovoltaic cells. Noble metal nanoparticles incorporated into polymer matrix have great potential for such applications due to their distinctive optical properties. However, methods to indirectly incorporate metal nanoparticles into polymeric microstructures are still on demand. Here we report on the fabrication of two-photon polymerized microstructures doped with gold nanoparticles through an indirect doping process, so they do not interfere in the two-photon polymerization (2PP) process. Such microstructures present a strong emission, arising from gold nanoparticles fluorescence. The microstructures produced are potential candidates for nanoplasmonics and metamaterials devices applications and the nanoparticles production method can be applied in many samples, heated simultaneously, opening the possibility for large scale processes. (C) 2012 Optical Society of America

5-substituted triazolinyls as novel counter radicals in controlled radical polymerization

The work is devoted to synthesis of new triazolinyl stable radical derivatives with different substituents at the 5-position of the triazolinyl ring. Obtained results showed great influence of these substituents on the stability of the radical. Electron-rich aromatic substituents at this position stabilize the radical while electron-poor aromatics decrease the stability of the triazolinyl. The triazolinyl radicals synthesized were used as additives for kinetic investigations of controlled radical polymerization of styrene and methylmethacrylate (MMA). The studies performed showed that the more stable radicals provide better control for the polymerization of styrene. In the same time certain instability of the radical is required for realization of controlled polymerization of methylmethacrylate. Based on the kinetic investigations controlled radical polymerization of a variety of monomers including 4-vinylpyridine (4-VP), ethylmethacrylate (EMA), 2,2,2-trifluoroethylmethacrylate (FEMA) and n-butylmethacrylate (BMA)was successfully carried out. Polystyrene and polymethylmethacrylate macroinitiators prepared by triazolinyl mediated controlled radical polymerization were efficiently reinitiated in the presence of a variety of monomers leading to the formation of block copolymers. Using this method PS-b-P-4-VP, PMMA-b-PS, PMMA-b-PBMA, PMMA-b-PFEMA, and PMMA-b-Poly-tert-butylacrylate were successfully synthesized. The results obtained during this work showed the efficiency and flexibility of the method allowing preparation of a range of advanced macromolecular structures.