Influence of ceramic surface conditioning and resin cements on microtensile bond strength to a glass ceramic

Statement of problem. It is not clear how different glass ceramic surface pretreatments influence the bonding capacity of various luting agents to these surfaces.Purpose. The purpose of this study was to evaluate the microtensile bond strength (mu TBS) of 3 resin cements to a lithia disilicate-based ceramic submitted to 2 surface conditioning treatments.Material and methods. Eighteen 5 X 6 X 8-mm ceramic (IPS Empress 2) blocks were fabricated according to manufacturer's instructions and duplicated in composite resin (Tetric Ceram). Ceramic blocks were polished and divided into 2 groups (n=9/treatment): no conditioning (no-conditioning/control), or 5% hydrofluoric acid etching for 20 seconds and silanization for 1 minute (HF + SIL). Ceramic blocks were cemented to the composite resin blocks with I self-adhesive universal resin cement (RelyX Unicem) or 1 of 2 resin-based luting agents (Multilink or Panavia F), according to the manufacturer's instructions. The composite resin-ceramic blocks were stored in humidity at 37 degrees C for 7 days and serially sectioned to produce 25 beam specimens per group with a 1.0-mm(2) cross-sectional area. Specimens were thermal cycled (5000 cycles, 5 degrees C-55 degrees C) and tested in tension at 1 mm/min. Microtensile bond strength data (MPa) were analyzed by 2-way analysis of variance and Tukey multiple comparisons tests (alpha=.05). Fractured specimens were examined with a stereomicroscope (X40) and classified as adhesive, mixed, or cohesive.Results. The surface conditioning factor was significant (HF+SIL > no-conditioning) (P<.0001). Considering the unconditioned groups, the mu TBS of RelyX Unicem was significantly higher (9.6 +/- 1.9) than that of Multilink (6.2 +/- 1.2) and Panavia F (7.4 +/- 1.9). Previous etching and silanization yielded statistically higher mu TBS values for RelyX Unicem (18.8 +/- 3.5) and Multilink (17.4 +/- 3.0) when compared to Panavia F (15.7 +/- 3.8). Spontaneous debonding after thermal cycling was detected when luting agents were applied to untreated ceramic surfaces.Conclusion. Etching and silanization treatments appear to be crucial for resin bonding to a lithia disilicate-based ceramic, regardless of the resin cement used.

Nanocoating of Al2O3 additive on ZrO2 powder and its effect on the sintering behaviour in ZrO2 ceramic

ZrO2 powder was coated with Al2O3 precursor generated by a polymeric precursor method in aqueous solution. The system of nanocoated particles formed a core shell-like structure in which the particle is the core and the nanocoating (additive) is the shell. A new approach is reported in order to control the superficial mass transport and the exaggerated grain growth during the sintering of zirconia powder. Transmission electron microscopy (TEM) observations clearly showed the formation of an alumina layer on the surface of the zirconia particles. This layer modifies the sintering process and retards the maximum shrinkage temperature of the pure zirconia.

Textured PbZr0.3Ti0.7O3 thin films produced by polymeric precursor method using microwave oven

PbZr0.3Ti0.7O3 (PZT) films were produced by polymeric precursor route and deposited by spin-coater technique on Pt(111)/Ti/SiO2/Si(100) substrates. The films were heat-treated using different furnaces: (a) a conventional furnace, at 700 degrees C; and (b) a domestic microwave oven, at 600 degrees C. The X-ray patterns revealed that both films are single phase and reflections were identified as belongs to the PZT phase. The intensity of these reflections showed a (111), (001) and (100) preferred orientation. Morphological and electrical characterizations showed that all samples present a rather different microstructure and both with high spontaneous polarization.

The effect of ceramic surface treatment on bonding to densely sintered alumina ceramic

Statement of problem. Ceramic surface treatment is crucial for bonding to resin. High crystalline ceramics are poorly conditioned using traditional procedures.Purpose. The purpose of this study was to evaluate the effect of silica coating on a densely sintered alumina ceramic relative to its bond strength to composite, using a resin luting agent.Material and methods. Blocks (6 X 6 X 5 mm) of ceramic and composite were made. The ceramic (Procera AllCeram) surfaces were polished, and the blocks were divided into 3 groups (n = 5): SB, airborne-particle abrasion with 110-mu m Al(2)O(3); RS, silica coating using Rocatec System; and CS, silica coating using CoJet System. The treated ceramic blocks were luted to the composite (W3D Master) blocks using a resin luting agent (Panavia F). Specimens were stored in distilled water at 37 degrees C for 7 days and then Cut in 2 axes, x and y, to obtain specimens with a bonding area of approximately 0.6 mm(2) (n = 30). The specimens were loaded to failure in tension in a universal testing machine, and data were statistically analyzed using a randomized complete block design analysis of variance and Tukey's test (alpha=.05). Fractured surfaces were examined using light microscopy and scanning electron microscopy to determine the type of failure. Energy-dispersive spectroscopy was used for surface compositional analysis.Results. Mean bond strength values (MPa) of Groups RS (17.1 +/- 3.9) (P = .00015) and CS (18.5 +/- 4.7) (P=.00012) were significantly higher than the values of Group SB (12.7 +/- 2.6). There was no statistical difference between Groups RS and CS. All failures occurred at the adhesive zone.Conclusion. Tribochemical silica coating systems increased the tensile bond strength values between Panavia F and Procera AllCeram ceramic.

Influence of seed particle frequency on the phase formation and on the microstructure of 0.88 PZN-0.07 BT-0.05 PT ceramic

The Pechini method as well as the simultaneous addition of seeds particles and dopant solutions of BaTiO3 (BT) and PbTiO3 (PT) were used to prepare the perovskite phase 0.88 PZN-0.07 BT-0.05 PT. To study the influence of seed particle frequency on the synthesis of the PZN ceramic, two ranges of seed particle size were used: the range from 30 to 100 nm, termed small seed particles (frequency of 10(15) particles/cm(3)); and the range from 100 to 900 nm, termed large seed particles (frequency of 10(13) particles/cm(3)). The crystalline nuclei size influenced the calcining process, the sintering process and the microstructure. Samples prepared with lower seed frequency displayed more amount of pyroclore phase, need higher temperatures for sintering and showed a more heterogeneous microstructure with poor dielectric properties. (C) 2000 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

Preparation of ceramic membranes from surface modified tin oxide nanoparticles

The preparation of crack-free SnO2 supported membranes requires the development of new strategies of synthesis capable to allow controlled changes of surface chemistry and to improve the processability of supported layers. In this way, the controlled modification of the SnO2 nanoparticle surface by adding capping molecules like Tiron(R) ((OH)(2)C6H2(SO3Na)(2)) during the sol-gel process was studied, aiming to obtain high performance membranes. Colloidal suspensions were prepared by hydrolyzing SnCl4.5H(2)O aqueous solution with NH4OH in presence of Tiron(R). The effect of the amount of Tiro(R) (from I to 20 wt.%) on the structural features of nanoparticles, powder redispersability and particle-solution interface properties was investigated by X-ray powder diffraction (XRPD), extended X-ray absorption fine structure (EXAFS), quasi-elastic light scattering and electrophoretic mobility measurements. XRPD and EXAFS results showed that the addition of Tiron(R) up to 20 wt.% to colloidal suspensions does not affect the crystallite size of SnO2 primary particles, determined around 2-3 nm. This value is comparable to the hydrodynamic size measured after redispersion of powder prepared with amount of Tiro(R) higher than 7.5 wt.%, indicating the absence of condensation reactions between primary particles after the initial precipitation step. As a consequence the powder with amount of Tiron(R) > 7.5 wt.%, can be fully redispersed in aqueous solution at pH greater than or equal to I I until a nanoparticle concentration of 6 vol.%. The electrophoresis measurements showed a decrease of the isoelectric point by increasing the amount of grafted Tiron(R) at the SnO2 nanoparticle surface, resulting in negatively charged particle-solution interface in all the studied pH range (2-11). These features govern the gelation process favoring the preparation of crack-free SnO2 supported membranes. The control exercised by Tiron(R) modifying agent in the aggregation process allows the fine-tuning of the porosity, from 0.124 to 0.065 cm(3) g(-1), and mean pore size, from 6.4 to 1.9 nm, as the amount of grafted molecules increases from 0 to 10 wt.%. In consequence, the membrane cut-off determined by filtration of polyethylene glycol standard solutions can be screened from 1500 to 3500 g mol(-1). (C) 2002 Elsevier B.V. B.V. All rights reserved.

Influence of the LiNbO3 and KNbO3 seeds on the sintering and electrical properties of PMN ceramic

The effect of LiNbO3 and KNbO3 seeds on the microstructure and dielectric characteristics of PMN ceramic prepared by columbite route have been investigated with the addition of 0, 1, and 2-wt% of seeds. X-ray diffraction, Scanning Electron Microscopy and an impedance analyzer were used to characterize the influence of seeds on physical characteristics and dielectric properties of PMN. LiNbO3 -seeded PMN samples present a significant increase in the amount of perovskite phase. The addition of LiNbO3 seeds in sintered PMN ceramics at 1100degreesC during 4 h causes a decrease in the porosity and the amount of pyrochlore phase. Weight losses during sintering of PMN ceramics are suppressed more significantly for LiNbO3 -seeded PMN. T-m of PMN ceramics changes with seeds concentration. KNbO3 seeds displace T-m to lower temperature whereas LiNbO3 causes its elevation. Dielectric constants of approximately 13,000 at 1 kHz was measured at -5degreesC in PMN ceramics with 1-wt% of LiNbO3 seeds.

Negative temperature coefficient thermistor based on Bi3Zn2Sb3O14 ceramic: An oxide semiconductor at high temperature

Bi1.5ZnSb1.5O7 dielectric ceramic with pyrochlore structure was investigated by impedance spectroscopy from 400 to 750 degreesC. Pyrochlore was synthesized by the polymeric precursor method, a chemical synthesis route derived from Pechini's method. The grain or bulk resistance exhibits a sensor temperature characteristic, being a thermistor with a negative temperature coefficient (NTC). Only a single region was identified on the resistance curve investigated. The NTC thermistor characteristic parameter (beta) is equal to 7140 degreesC, in the temperature range investigated. The temperature coefficient of the resistance (alpha) was derived, being equal to -4.46x10(-2) degreesC(-1) at 400 degreesC. The conduction mechanism and relaxation are discussed. (C) 2003 American Institute of Physics.

Improvement of the ferroelectric properties of ABO(3) (A= Pb, Ca, Ba; B=Ti, Zr) films

High-quality ABO(3)/LaNiO3 (A = Ph, Ca, Ba; B = Ti, Zr) hetero structures have been grown on LaAlO3 (1 0 0) substrate by the chemical solution deposition method and crystallized by a microwave oven technique. The structural, morphological and electric properties were characterized by means of X-ray diffraction (XRD), atomic force microscope (AFM), and dielectric and ferroelectric measurements. XRD patterns revealed single-phase polycrystalline and oriented thin films whose feature depends on the composition of the films. The AFM surface morphologies showed a smooth and crack-free surface with the average grain size ranging from 116 to 300 nm for both LaNiO3 electrode and the ferroelectric films. Dielectric measurements on these samples revealed dielectric constants as high as 1800 at frequency of 100 KHz. Such results showed that the combination of the chemical solution method with the microwave process provides a promising technique to grow high-quality thin films with good dielectric and ferroelectric properties. (c) 2005 Elsevier Ltd. All rights reserved.

Barium strontium titanate nanocrystalline thin films prepared by soft chemical method

Barium strontium titanate (Ba0.65Sr0.35TiO3) nanocrystalline thin films, which were produced by the soft chemical method, were crystallized at low temperature using a domestic microwave oven. A SiC susceptor were used to absorb the microwave energy and rapidly transfer the heat to the film. Low microwave power and short time have been used. The films obtained are crack-free, well-adhered, and fully crystallized. The microstructure displayed a polycrystalline nature with nanograin size. The metal-BST-metal structure of the thin films treated at 700 degrees C show food electric properties. The ferroelectric nature of the BST35 thin film was indicated by buttertly- shaped C-V curves. The capacitance-frequency curves reveal that the dielectric constant may reach a value up to 800 at 100kHz. The dissipation factor was 0.01 at 100kHz. The charge storage density as function of applied voltage graph showed that the charge storage densities are suitable for use in trench type 64 Mb ( 1-5 mu C/cm(2) and 265 Mb (2-11 mu C/cm(2)) DRAMs. (C) 2007 Elsevier Ltd. All rights reserved.

Rietveld refinements of SnO(2) ceramic powders doped with ZnO, WO(3), CoO, Nb(2)O(5) and MoO(3)

Polycrystalline materials of SnO(2) doped with ZnO, WO(3), CoO, Nb(2)O(5), and MoO(3). were synthesized by solid state reaction. X-ray powder diffraction data were collected with Cu K(alpha) radiation from a Rigaku-Rint 2000 rotating anode source. The structural and profile parameters were refined by the Rietveld method using GSAS [2]. The obtained residual parameters are R(wp) = 11,93% and R(Bragg) = 4,19%. The refined profile parameters indicate no anisotropic crystallite microstrain. The refinement results and Fourier differences calculations indicate that the dopants do not occupy interstitial sites in the crystal structure of SnO(2).

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.