Repair bond strength of a resin composite to alumina-reinforced feldspathic ceramic

This study compared the microtensile bond strength of a repair resin to an alumina-reinforced feldspathic ceramic (Vitadur-alpha, Vita) after 3 surface conditioning methods: Group 1, etching with 9.6% hydrofluoric acid for 1 minute plus rinsing and drying, followed by application of silane for 5 minutes; group 2, airborne particle abrasion with 110-mm aluminum oxide using a chairside air-abrasion device followed by silane application for 5 minutes; group 3, chairside tribochemical silica coating with 30-mu m SiOx followed by silane application for 5 minutes (N = 30). Group 1 presented the highest mean bond strength (19.7 +/- 3.8 MPa), which was significantly higher than those of groups 2 (10 +/- 2.6 MPa) and 3 (10.4 +/- 4 MPa) (P <.01). Scanning electron microscope analysis of the failure modes demonstrated predominantly mixed types of failures, with adhesive and/or cohesive failures in all experimental groups.

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.

Electrical measurements in doped zirconia-ceria ceramics

Zirconia-ceria powders with 12 mol % of CeO2 doped with 0.3 mol% of iron, copper, manganese and nickel oxides were synthesized by the conventional mixed oxide method. These systems were investigated with regard to the sinterability and electrical properties. Sintering was studied considering the shrinkage rate, densification, grain size, and phase evolution. Small amount of dopant such as iron reduces sintering temperature by over 150degreesC and more than 98% of tetragonal phase was retained at room temperature in samples sintered at 1450degreesC against 1600degreesC to stabilize the tetragonal phase on pure ZrO2-CeO2 system. The electrical conductivity was measured using impedance spectroscopy and the results were reported. The activation energy values calculated from the Arrhenius's plots in the temperature range of 350-700degreesC for intragrain conductivities are 1.04 eV.

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.

Screen printed PLZT thick films prepared from nanopowders

The gap between the bulk materials and thin films can be filled with thick films suitably designed and appropriate processed. Thick films of complex system like lead-lanthanum-zirconium titanate (PLZT) is difficult to produce by simple solid-state reaction keeping compositional homogeneity and optimal grain size distribution. In the present work, PLZT thick films were fabricated by screen-printing technique from nanosized powders obtained through soft chemistry by polymeric precursor method. Thick film paste was obtained by mixing PLZT fine powders and organic vehicle. The upper and bottom electrodes based on Ag-Pd and functional component based on PLZT were screen-printed on alumina substrate and after that annealed in air atmosphere. The powder morphology, microstructure, dielectric and ferroelectric properties of 9.5/65/35 PLZT thick films were analysed. (c) 2007 Elsevier Ltd. All rights reserved.

PZT ceramics obtained from mechanochemically synthesized powders

PZT ceramics were obtained from the mechanochemically synthesized powders. Milling and sintering conditions were optimized based on results of density measurements, as well as on microstructural and electrical characterization. As a result, highly dense and homogeneous ceramics were obtained. Excellent microstructural properties resulted in good electrical properties. Samples showed values of dielectric constants reaching 12800 at the Curie temperature, as well as low dielectric loss under the optimal processing conditions. High values of remanent polarization, reaching 60 muC cm(-2), indicate high internal polarizability. (C) 2003 Kluwer Academic Publishers.

Properties and in vivo investigation of nanocrystalline hydroxyapatite obtained by mechanical alloying

Mechanical alloying has been used successfully to produce nanocrystalline powders of hydroxyapatite (HA) using three different procedures. The milled HA was studied by X-ray diffraction, Infrared, Raman scattering spectroscopy and Scanning Electron Microscopy (SEM). We obtained HA with different degrees of crystallinity and time of milling. The grain size analysis through SEM and XRD shows particles with dimensions of 36.9, 14.3 and 35.5 nm (for (R1), (R2) and (R3), respectively) forming bigger units with dimensions given by 117.2, 110.8 and 154.4 nm (for (R1), (R2) and (R3), respectively). The Energy-Dispersive Spectroscopy (EDS) analysis showed that an atomic ratio of Ca/P= 1.67, 1.83 and 1.50 for reactions (R1), (R2) and (R3), respectively. These results suggest that the R1 nanocrystalline ceramic is closer to the expected value for the ratio Ca/P for hydroxyapatite, which is 513 congruent to 1.67. The bioactivity analysis shows that all the samples implanted into the rabbits can be considered biocompatible, since they had been considered not toxic, bad not caused inflammation and reject on the part of the organisms of the animals, during the period of implantation. The samples implanted in rabbits had presented new osseous tissue formation with the presence of osteoblasts cells. (C) 2004 Elsevier B.V. All rights reserved.

The effect of heating rate on the sintering of agglomerated NaNbO3 powders

The effect of heating rate on the sintering of agglomerated NaNbO3 powders, processed by the polymeric precursors method, was studied. The results showed that the presence of agglomerated powder leads to a heterogeneous microstructure, with bimodal grain size distribution, after sintering. Using a high heating rate, the sintering of agglomerated particles was inhibits, leading to a homogeneous microstructure, with single grain size distribution. (C) 1998 Kluwer Academic Publishers.

Study of Ti-modified columbite route and the effect of lithium doping in 0.9PMN-0.1PT ceramics

The influence of lithium on the structural characteristics of PMN-PT ceramic was studied. The synthesis of PMN-PT powders using this precursor leads to the formation of high amount of perovskite phase. The insertion of Li(+) ions in B-site affects the microstructure because the rise in mass transport changes the mechanical characteristics of sintered ceramic. Higher values of K(m) and T(m) were gotten when lithium is inserted into perovskite phase. Secondary phase was found when lithium content increase beyond 1 mol%, besides the occurrence of transgranular fractures in sintered ceramic. Also, the additive acts increasing the relaxor behavior.

Wet-chemical synthesis of magnesium niobate nanoparticles powders

Nanosized and highly reactive magnesium mobate (MgNb2O6) powders were successfully synthesized by a new wet-chemical method by means of the dissolution of Nb2O5 center dot 5H(2)O and in a solution of oxalic acid followed by the addition of stoichiometric amounts of magnesium carbonate. The Nb-Mg-oxalic acid solution was evaporated resulting in a dry and amorphous powder that was calcined in the temperature range from 200 to 900 degrees C for 2 h. The crystallization process from the amorphous state to the crystalline MgNb2O6 was followed by thermal analysis. The calcined powders characterized by FT-Raman spectroscopy, X-ray diffraction (XRD) and their morphology examined by high resolution scanning electron microscopy (HR-SEM). Pure MgNb2O6, free from the second phases and obtained at 800 degrees C was confirmed by a combined analysis using XRD and FT-Raman. The average diameter of the particles was calculated from the HR-SEM image as 70 urn approximately. This technique allows a better mixing of the constituent elements and thus a better reactivity of the mixture to obtain pre-reaction products with high purity at lower temperatures and reducing cost. It can offer a great advantage in the PMN-PT formation with respect to the solid-state synthesis. (c) 2006 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Dielectric properties of Na1-xLixNbO3 ceramics from powders obtained by chemical synthesis

Ultra-fine powders of Na1-xLixNbO3 (x=0; 0.06; 0.09; 0.12) were synthesized by the Polymeric Precursors Method. Such powders had their orthorhombic structures determined by X-ray diffraction and their surface area determined by BET isotherms (less than 10 m(2) g(-1)). Densification was followed by dilatometric study. The powders, calcined at 700 degrees C for 5 h, were sintered at 1290 degrees C during 2 h under ambient atmosphere with no application of extra pressure. The samples with relative densities higher than 95% were analyzed by impedance spectroscopy at room temperature, under a signal amplitude of 1 V-rms. Dielectric constants of about 180 and dielectric loss factor of about 0.03 were measured showing small dependence with frequency. The electrical properties were similar to those obtained for samples sintered by hot pressing. (C) 1999 Elsevier B.V. Limited and Techna S.r.l. All rights reserved.

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.