Reflux synthesis and hydrothermal processing of ZrO2 nanopowders at low temperature

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Active planar waveguides based on sol-gel Er3+-doped SiO2-ZrO2 for photonic applications: Morphological, structural and optical properties

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

Organic-inorganic hybrids prepared by carboxylic acid solvolysis: Planar waveguides

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

Zirconia foams prepared by integration of the sol-gel method and dual soft template techniques

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determination of Total Sulfur in Agricultural Samples by High-Resolution Continuum Source Flame Molecular Absorption Spectrometry

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

Study of Structure and Properties of Bi4Ti3O12 Prepared by Mechanochemical Syntheses

Bi4Ti3O12 powder was synthesized from bismuth oxide and titanium oxide. Mixture of oxides was milled in zirconium oxide jar in the planetary ball-mill during 1, 3 and 6 h. Extended time of milling directed to formation of higher amount of titanates perovskite phase. Bi4Ti3O12 was formed between 1 and 3 h of milling time. The phase formation of Bi4Ti3O12, crystal structure and powder particle size were followed by XRD, Raman spectroscopy and SEM analysis. After milling for various times the powders were compacted by pressing and isothermal sintering. Sample milled for 3 h and subsequently sintered at 1000C for 24 h exhibit a hysteresis loop, confirming that the synthesized material possesses ferroelectric properties. All results affect that the structure Bi4Ti3O12 is strongly dependent on the milling time.

Two thermal methods to measure the energy fluence of a brief exposure of diagnostic x rays

This paper describes two simple thermal methods for measuring the energy fluence in J/cm 2 from a diagnostic x-ray exposure. Both detectors absorb essentially 100% of the radiation and give a signal that is directly proportional to the energy fluence of the x-ray beam. One detector measures the thermal effect when a pulse of x rays is totally absorbed in the pyroelectric detector of lead-zirconium-titanate (PZT). The other detector measures the expansion of a gas surrounding a lead disk detector in a photoacoustic chamber. The increased pressure of the gas is transmitted through a 1-mm duct to a sensitive microphone. Both detectors have previously been used to measure the energy fluence rate of continuous x-ray beams in the same energy region using a chopped beam and a lock-in amplifier. Measurement of the energy fluence of a pulse of radiation eliminates the need for the beam chopper and lock-in amplifier and results in a simple, rugged, and inexpensive dosimeter. Either method can be combined with the area of the beam to give an estimate of the imparted energy to the patient from a diagnostic x-ray exposure.

Particle growth during calcination of polycation oxides synthesized by the polymeric precursors method

The particle-growth kinetics of sodium niobate and zirconium titanate powders that were processed by the polymeric precursors method were studied. The growth kinetics that were studied for the particle, in the final stage of crystallization, showed that the growth process occurs in two different stages. For temperatures <800°C, the particle-growth mechanism is associated with surface diffusion, with an activation energy in the range of 40-80 KJ/mol. For temprratures >800°C, particle growth is controlled by densification of the nanometric particle cluster and by a neck-size-controlled particle-growth mechanism. The results suggest that this behavior was typical of the synthesis method, because two different polycation oxides presented the same behavior.

Pressure-induced phase transitions in Zr-rich PbZr1-xTixO3 ceramics

A Raman study of structural changes in the Zr-rich PbZr1-x TixO3 (PZT) system under hydrostatic pressures up to 5.0 GPa is presented. We observe that externally applied pressure induces several phase transitions in PZT ceramics among phases with orthorhombic (Ao), rhombohedral low-temperature (RLT), and rhombohedral high-temperature (RHT) symmetries (all found in PZT at ambient pressure and room temperature). Each of the compositions investigated (0.02 ≤ x ≤ 0.14) exhibits a high-pressure phase with orthorhombic (OI′) symmetry. We further report a detailed study of the pressure dependence of Raman frequencies to elucidate the phase transitions and to provide a set of pressure coefficients for the high-pressure phases.

Raman scattering study of the PbZr1-xTixO3 system: Rhombohedral-monoclinic-tetragonal phase transitions

In this paper we present a Raman-scattering study of the phase transitions in the PbZr1-xTixO3 systems around the morphotropic phase boundary over a wide temperature range. The boundary between rhombohedral and monoclinic phases was found to be a quasivertical line between x = 0.46 and x = 0.47. We also studied the monoclinic-tetragonal phase boundary and our spectroscopic results agree very well with those reported by using x-ray diffraction.

Evaluation of marginal microleakage in Class II cavities: Effect of microhybrid, flowable, and compactable resins

Objective: The goal of the present study was to evaluate the microleakage on the cementum/dentin and enamel surfaces in Class II restorations, using different kinds of resin composite (microhybrid, flowable, and compactable). Method and materials: Forty human caries-free molars were extracted and selected. Eighty Class II standardized cavities were made in the cervical wall at the cementoenamel junction (CEJ) and at the mesial and distal surfaces. The teeth were divided into four groups: G1 - adhesive system + microhybrid resin composite Z100; G2 - adhesive system + compactable resin composite Prodigy Condensable; G3 - adhesive system + flowable resin composite Revolution + Z100 resin composite; G4 - adhesive system + Revolution fluid resin + compactable resin composite Prodigy Condensable. The adhesive system used in this study was Scotchbond Multi-Purpose Plus. The specimens were thermocycled in baths of 5°C and 55°C for 1,000 cycles and immersed in 50% silver nitrate solution. The specimens then were sectioned and evaluated on degree of dye penetration. Results: The results were evaluated using the nonparametric Kruskall-Wallis test, which showed a statistically significant difference between groups G1 and G4, G2 and G4, and G3 and G4. Conclusions: None of the materials was able to eliminate the marginal microleakage at the cervical wall; the application of a low-viscosity resin composite combined with a compactable resin composite significantly decreased the microleakage.

Optimization of neutral hydrolysis reaction of post-consumer PET for chemical recycling

The neutral hydrolysis reaction of post-consumer poly(ethylene terephthalate) in solid state was studied through the reaction of the polymer with water at the molar ratio 1:91 with autogenous pressure. Two sizes of post-consumer PET flakes and temperatures of 135 °C, 170°C and 205°C with pressures of 4.0 atm, 7.5 atm and 13.5 atm, respectively, were considered. With reaction time equal to 6h, the method reached 99% depolymerization at 205°C, 8.2% at 170 °C and 1.7% at 135°C. The reaction extension was measured by separating the terephthalic acid formed in the process and calculating by gravimetry how much material could still be reacted. Through the viscosimetry of diluted, solutions and the counting of carboxylic end groups in the remaining material from the gravimetric assay, it was possible to suggest that the reaction occurs randomly and in the whole volume of the polymeric particle and not solely on the surface. The terephthalic acid obtained and then purified was characterized by elemental analysis, magnetic nuclear resonance, size and panicle size distribution and spectrophotometry in the visible spectrum, and it was similar to the petrochemical equivalent, with purity recorded in carbon base equal to 99.9%.

U-Pb geochronology of the southern Brasília belt (SE-Brazil): Sedimentary provenance, Neoproterozoic orogeny and assembly of West Gondwana

The Brasília belt borders the western margin of the São Francisco Craton and records the history of ocean opening and closing related to the formation of West Gondwana. This study reports new U-Pb data from the southern sector of the belt in order to provide temporal limits for the deposition and ages of provenance of sediments accumulated in passive margin successions around the south and southwestern margins of the São Francisco Craton, and date the orogenic events leading to the amalgamation of West Gondwana. Ages of detrital zircons (by ID-TIMS and LA-MC-ICPMS) were obtained from metasedimentary units of the passive margin of the São Francisco Craton from the main tectonic domains of the belt: the internal allochthons (Araxá Group in the Áraxá and Passos Nappes), the external allochthons (Canastra Group, Serra da Boa Esperança Metasedimentary Sequence and Andrelândia Group) and the autochthonous or Cratonic Domain (Andrelândia Group). The patterns of provenance ages for these units are uniform and are characterised as follows: Archean- Paleoproterozoic ages (3.4-3.3, 3.1-2.7, and 2.5-2.4Ga); Paleoproterozoic ages attributed to the Transamazonian event (2.3-1.9Ga, with a peak at ca. 2.15Ga) and to the ca. 1.75Ga Espinhaço rifting of the São Francisco Craton; ages between 1.6 and 1.2Ga, with a peak at 1.3Ga, revealing an unexpected variety of Mesoproterozoic sources, still undetected in the São Francisco Craton; and ages between 0.9 and 1.0Ga related to the rifting event that led to the individualisation of the São Francisco paleo-continent and formation of its passive margins. An amphibolite intercalation in the Araxá Group yields a rutile age of ca. 0.9Ga and documents the occurrence of mafic magmatism coeval with sedimentation in the marginal basin. Detrital zircons from the autochthonous and parautochthonous Andrelândia Group, deposited on the southern margin of the São Francisco Craton, yielded a provenance pattern similar to that of the allochthonous units. This result implies that 1.6-1.2Ga source rocks must be present in the São Francisco Craton. They could be located either in the cratonic area, which is mostly covered by the Neoproterozoic epicontinental deposits of the Bambuí Group, or in the outer paleo-continental margin, buried under the allochthonous units of the Brasília belt. Crustal melting and generation of syntectonic crustal granites and migmatisation at ca. 630Ma mark the orogenic event that started with westward subduction of the São Francisco plate and ended with continental collision against the Paraná block (and Goiás terrane). Continuing collision led to the exhumation and cooling of the Araxá and Passos metamorphic nappes, as indicated by monazite ages of ca. 605Ma and mark the final stages of tectonometamorphic activity in the southern Brasília belt. Whilst continent-continent collision was proceeding on the western margin of the São Francisco Craton along the southern Brasília belt, eastward subduction in the East was generating the 634-599Ma Rio Negro magmatic arc which collided with the eastern São Francisco margin at 595-560Ma, much later than in the Brasília belt. Thus, the tectonic effects of the Ribeira belt reached the southernmost sector of the Brasília belt creating a zone of superposition. The thermal front of this event affected the proximal Andrelândia Group at ca. 588Ma, as indicated by monazite age. The participation of the Amazonian craton in the assembly of western Gondwana occurred at 545-500Ma in the Paraguay belt and ca. 500Ma in the Araguaia belt. This, together with the results presented in this work lead to the conclusion that the collision between the Paraná block and Goiás terrane with the São Francisco Craton along the Brasília belt preceded the accretion of the Amazonian craton by 50-100 million years. © 2003 Elsevier B.V. All rights reserved.

Effect of cyclic compressive loading on the bond strength of an adhesive system to dentin after collagen removal

Purpose: The objective of this study was to verify the effect of cyclic compressive loading on the shear bond strength of an adhesive system following collagen removal. Materials and Methods: Sixty bovine teeth were divided into 4 groups based on the adhesive procedure used: groups 1 and 2 - etching with 35% phosphoric acid and application of the Single Bond adhesive system; groups 3 and 4 - after etching, a 10% sodium hypochlorite solution was applied for 1 min before the application of the adhesive. In all the specimens, a Z100 resin cylinder was built up over the bond area. Groups 2 and 4 were submitted to 500,000 cycles with a load of 100 N. Results: The mean values for the shear bond test (MPa) were: group 1: 7.37 ± 1.15; group 2: 5.72 ± 1.66; group 3: 5.95 ± 1.21; group 4: 3.66 ± 1.12. There was no difference between groups 1 and 2 (p > 0.01). Between groups 1 and 3, 2 and 4, and 3 and 4 there was a significant difference (p < 0.01). The majority of the specimens demonstrated an adhesive failure. Conclusion: The application of sodium hypochlorite on dentin decreased the values of shear bond strength, as did the load cycling in the group treated with sodium hypochlorite.

Photoluminescence-structure relationships in ormosils for integrated optical devices

Planar waveguides with low losses in the infrared (from 0.6-1.1 dB/cm) were prepared with sol-gel derived poly(oxyethylene)/siloxane hybrid doped with zirconium(IV) n-propoxide (ZPO) and methacryloxypropyltrimethoxysilane (MAPTMS). The doped nanohybrids were characterized by small angle X-ray scattering, 29Si nuclear magnetic resonance and photoluminescence spectroscopy and compared with the undoped hybrid material. The results indicate an effective interaction between the zirconium particles and the siliceous nanodomains. © 2005 Materials Research Socicty.