Microtensile bond strength of a resin cement to feldpathic ceramic after different etching and silanization regimens in dry and aged conditions

Objectives. This study evaluated the durability of bond strength between resin cement and a feldspathic ceramic submitted to different etching regimens with and without silane coupling agent application.Methods. Thirty-two blocks (6.4 mm x 6.4 mm x 4.8 mm) were fabricated using a microparticulate feldspathic ceramic (Vita VM7), ultrasonically cleaned with water for 5 min and randomly divided into four groups, according to the type of etching agent and silanization method: method 1, etching with 10% hydrofluoric (HF) acid gel for I min + silanization; method 2, HF only; method 3, etching with 1.23% acidulated phosphate fluoride (APF) for 5 min + silanization; method 4, APF only. Conditioned blocks were positioned in their individual silicone molds and resin cement (Panavia F) was applied on the treated surfaces. Specimens were stored in distilled water (37 degrees C) for 24 h prior to sectioning. After sectioning the ceramic-cement blocks in x- and Y-axis with a bonded area of approximately 0.6 mm(2), the microsticks of each block were randomly divided into two storage conditions: Dry, immediate testing; TC, thermal cycling (12,000 times) + water storage for 150 d, yielding to eight experimental groups. Microtensile bond strength tests were performed in universal testing machine (cross-head speed: 1 mm/min) and failure types were noted. Data obtained (MPa) were analyzed with three-way ANOVA and Tukey's test (alpha = 0.05).Results. Significant influence of the use of silane (p < 0.0001), storage conditions (p = 0.0013) and surface treatment were observed (p = 0.0014). The highest bond strengths were achieved in both dry and thermocycled conditions when the ceramics were etched with HF acid gel and silanized (17.4 +/- 5.8 and 17.4 +/- 4.8 MPa, respectively). Silanization after HF acid gel and APT treatment increased the results dramatically (14.5 +/- 4.2-17.4 +/- 4.8 MPa) compared to non-silanized groups (2.6 +/- 0.8-8.9 +/- 3.1 MPa) where the failure type was exclusively (100%) adhesive between the cement and the ceramic.Significance. Silanization of the feldspathic ceramic surface after APF or HF acid etching increased the microtensile bond strength results significantly, with the latter providing higher results. Long-term thermocycling and water storage did not decrease the results in silanized groups. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Barium titanate screen-printed thick films

Barium titanate (BT) thick films were prepared from mechanically activated powders based on BaCO(3) and TiO(2). After homogenization and milling in a high-energy vibro mill, the powders were calcined at 700 degreesC for 2 h by slow heating and cooling rates. A thick film paste was prepared by mixing BT fine powders with small amount of low temperature sintering aid and organic binder. The thick films were screen-printed on alumina substrates electroded with Ag-Pd. The BT films were sintered at 850 degreesC for 1 h. The thickness was 25-75 mum depending of number of layers. The microstructure of thick films and the compatibility between BT layers and substrate were investigated by SEM Results of dielectric property measurements are also reported. (C) 2002 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

Photoluminescence in amorphous PLZ

Amorphous and crystalline powder of PLZ was prepared by using the polymeric precursor method. TGA-DSC (Thermal analysis and Differential Scanning Calorimetry) shows the decomposition of polymeric resin, an amorphous phase and the crystallization of powder. Raman scattering of powder shows an amorphous and semicrystalline phase at 450 and 550 degreesC, respectively. XRD (X-ray diffraction pattern) of powder shows high crystallinity at 700 degreesC/3 h. PL (Photoluminescence) analysis of powder at 300 degreesC/3 h shows a broad asymmetric peak at 585 nm and increases of calcining time led to intense peaks of PL at 300 degreesC/6 h. This emission could be attributed to Zr --> O from the oxygen-2p orbitals to the zirconate-3d orbitals. (C) 2003 Elsevier Ltd and Techna S.r.l. All rights reserved.

Effect of oxygen atmosphere on the morphology of LiTaO3 thin films prepared from polymeric precursor method

Lithium tantalate (LiTaO3) thin films with (50:50) stoichiometry were prepared using polymeric organic solution. The 5-layered films were deposited on silicon (100) substrates by spin coating method. The coated substrates were thermally treated at 500degreesC for 3 h under several oxygen atmospheres in order to study the influence of oxygen flow on the crystallinity, microstructure, grain size and roughness of the final film. X-ray diffraction results showed that an oxygen flow of 100 cm(3)/min leads to LiTaO3 thin films with higher crystallinity, without preferential orientation. It was observed by scanning electron microscopy (SEM) that the thickness of thin films decreases when the oxygen flow increases. The atomic force microscopy (AFM) studies showed that the grain size and roughness are strongly influenced by oxygen flow.

Optical properties of Mg doped LiNbO3 thin films grown by polymeric precursor method.

Polymeric precursor solution was used to deposit by spin-coating pure and Mg doped LiNbO3 thin films on sapphire substrates. The effects of magnesium addition on crystallinity, morphology and optical properties of the annealed films were investigated. X-ray diffraction patterns indicate the oriented growth of the films. AFM studies show that the films are very homogeneous, dense and present smooth surfaces. The refractive index and optical losses obtained by the prism coupling method were influenced by the magnesium addition.

Separation of dielectric and space charge polarizations in CaCu3Ti4O12/CaTiO3 composite polycrystalline systems

The complex analysis of dielectric/capacitance is a very useful approach to separate different polarization contributions existing in polycrystalline ceramics. In this letter, the authors use this type of spectroscopic analysis to separate the bulk's dielectric dipolar relaxation contributions from the polarization contribution due to space charge in the grain boundaries of a CaCu3Ti4O12/CaTiO3 polycrystalline composite system. The bulk dielectric dipolar relaxation was attributed to the self-intertwined domain structures from the CaCu3Ti4O12 phase coupled to the dipole relaxation from the CaTiO3 phase, while the space charge relaxation was attributed to the Schottky-type potential barrier responsible for the highly non-Ohmic properties observed in this composite polycrystalline system.

Hot-pressed 9.5/65/35 PLZT prepared by the polymeric precursor method

A 9.5/65/35 PLZT ceramic with a Pb-0.905 La-0.095 (Zr-0.65 Ti-0.35)(0.976) O-3 + 35 w% PbO formula was prepared using the Pechini method for powder preparation and two-step sintering in an oxygen atmosphere. Thr first step consisted of sintering at 1200 degrees C for 4 h with slow heating and cooling rates. The second step consisted of hot pressing at 1200 degrees C for 3 h, with slow heating and cooling rates and pressing pressures of 20 MPa (initial pressure) and 40 MPa (at sintering temperature). Investigations were made of the powder phase formation and powder morphology, i.e. The structure of sintered and hot-pressed PLZT ceramics. SEM microstructural analyses were carried out on the sintering and hot-pressing processes. (C) 2000 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

Evolution of CaCu3Ti4O12 varistor properties during heat treatment in vacuum

Calcium copper titanate (CaCu3Ti4O12) ceramic varistors were prepared by solid-state method. The samples were several times heat treated in vacuum and the evolution of electrical characteristics were monitored by current density versus electric field measurements and impedance spectroscopy. Repeated heat treatments in vacuum (900 degrees C for 1 h, 0.01 Torr) lead to a desorption of oxygen adsorbed at the grain boundaries and consequently to a degradation of the varistor properties. During further successive heat treatments some oxygen from the grain interior moves to the grain boundary thereby partially restoring the varistor properties. (c) 2006 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Nonlinear behavior of TiO2 center dot Ta2O5 center dot MnO2 material doped with BaO and Bi2O3

A study was made on the effect of the addition of BaO (0.025-0.05 mol%) and Bi2O3 (0.025-0.05 mol%) to the TiO2.Ta2O5.MnO2 material. The samples were characterized by X-ray diffraction, and current-voltage measurements were accomplished for determination of the nonlinear coefficient. An analysis was made to evaluate the microstructural characteristics of the materials. The most appropriate sintering conditions for the materials were analyzed with the purpose of obtaining the best nonlinear coefficient associated with the smallest breakdown electric field. After sintering at 1400 degreesC for 2 h, a low-voltage (30 V cm(-1)) varistor was obtained, which, however, presented a low nonlinear coefficient (6). It was found that the sintering conditions must be controlled in order to improve the electrical properties of these materials. (C) 2004 Elsevier B.V. All rights reserved.

Investigation of electrical properties of tantalum doped SnO2 varistor system

Ta2O5 doped SnO2 varistor systems containing 0.5 mol% ZnO and 0.5 mol% Coo were prepared by mixed oxide method. Considering that ZnO and Coo oxides are densification additives only the SnO(2)center dot ZnO center dot CoO ceramics cannot exhibit electrical nonlinearity. A small amount of Ta2O5 improves the nonlinear properties of the samples greatly. The height and width of the defect barriers were calculated. It was found that samples doped with 0.05 mol% Ta2O5 exhibit the highest density (98.5%), the lowest electric breakdown field (E-b = 1100 V/cm) and the highest coefficient of nonlinearity (alpha = 11.5). The effect of Ta2O5 dopant could be explained by the substitution of Ta5+ by Sn4+. A grain-boundary defect barrier model for the SnO(2)center dot ZnO center dot CoO center dot Ta2O5 varistor system was also introduced. (c) 2004 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Impedance spectroscopy of SnO2: CoO during sintering

SnO2:m mol% CoO (0.5 less than or equal to m less than or equal to 6.0) ceramic specimens were studied by impedance spectroscopy in the 5 Hz-13 MHz frequency range during heating cold-pressed specimens from room temperature to 1250 degrees C. The electrical resistivity during sintering decreases from 4 to 6 orders of magnitude in the 400-1500 K temperature range depending on the amount of CoO. An increase in electrical resistivity in the 570-670 K range is related to the release of adsorbed water. The results for the 970-1500 K show that the higher the amount of the CoO addition, the lower is the temperature at which SnO2:CoO reaches a minimum electrical resistivity. This suggests that oxygen point defects created by dissolution of cobalt ions in the SnO2 lattice are controlling the densification rate of these ceramics.

Preparation of SrBi2Ta2O9 ferroelectric thick films by electrophoretic deposition using aqueous suspensions

SrBi2Ta2O9 ferroelectric thick films were prepared by electrophoretic deposition (EPD). For that, ceramic powders were prepared by chemical method in order to obtain compounds with chemical homogeneity. The polymeric precursor method was used for the synthesis of the SrBi2Ta2O9 powder. The crystallographic structure of the powder was examined by X-ray diffraction, and the surface area was determined by single point BET adsorption. The 0.03 vol% suspension was formed by dispersing the powder in water using two different polymers as dispersants: an ester polyphosphate (C213) and an ammonium polyacrilate (Darvan 821-A). The influence of the different dispersants on the powder surface properties were investigated by zeta potential measurements. The films were deposited on platinum-coated alumina and Pt/Ti/SiO2/Si substrates by electrophoretic deposition using a 4 mA constant current, for 10 min, with two parallel electrodes placed at a separation distance of 3 min in the suspension. Several cycles of deposition-drying of the deposit was carried out until the desired thickness was obtained. After thermal treatment at temperatures ranging from 700 to 1000degreesC, the films were characterized by X-ray diffraction and scanning electron microscopy.

Recent research developments in SnO2-based varistors

This paper discusses some advances in research conducted on SnO2-based electroceramics. The addition of different dopants, as well as several thermal treatments in oxidizing and inert atmospheres, were found to influence the microstructure and electrical properties of SnO2-based varistor ceramics. Measurements taken by impedance spectroscopy revealed variations in the height and width of the potential barrier resulting from the atmosphere in which thermal treatments were performed. High nonlinear coefficient values, which are characteristic of high-voltage and commercial ZnO varistors, were obtained for these SnO2-based systems. All the systems developed here have potentially promising varistor applications. (C) 2004 Elsevier B.V. All rights reserved.

Seeding of PMN powders made by the Pechini method

The partial oxalate method, with the columbite route, associated with the Pechini method, was used to obtain a very fine ceramic powder at low temperature. Using this route it was possible to obtain a very reactive powder and to synthesize a lead magnesium niobate (PMN) powder with up to 100% of perovskite phase at a lower temperatures than the PbO melting point. The influence of the BaTiO3 and PbTiO3 seeds in the phase formation, along with time and temperature during the PMN calcination, was also investigated. The amount of 2% of BaTiO3 seeds promoted PMN powder formation with 100% of perovskite phase and a very narrow particle size distribution. (C) 2001 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

Non-Linear Dielectric Properties of PLMN-PT Relaxor Ferroelectrics

Recent investigations on the non-linear (NL) dielectric properties of relaxor ferroelectrics systems, not only as ceramic bodies, but also, in thin films, have showed a significant technological and scientific interest. The most common practical applications of relaxors include multilayer capacitors and actuators. In this work, non-linear dielectric properties of hot-pressed (1-x)[Pb1 -(3/2) yLayMg1/3Nb2/3O3]-xPbTiO3 (PLMN-PT) ferroelectric ceramics were investigated. The NL properties were obtained by using the measurements of the dielectric permittivity of the material as a function of the AC electric field with variable amplitude in the frequency and temperature range of 100 Hz-1 MHz and 50-450 K, respectively. An anomalous behavior of the non-linear dielectric response was observed when submitted to high electric fields levels. The obtained results were analyzed concerning one of the models for the dielectric response of relaxors ferroelectrics materials currently discussed in the literature.