Effect of ceria content on the sintering of ZrO2 based ceramics synthesized from a polymeric precursor

Zirconia-ceria powders with ceria concentration varying from 0 to 12 mol% were synthesized using a polymeric precursor route based on the Pechini process. Powder characteristics were evaluated with regard to the crystallite size, BET surface area, phase distribution, nitrogen adsorption/desorption behavior, and agglomeration state. Sintering was studied considering the shrinkage rate, densification, grain size, and phase evolution. It was demonstrated that the synthesis method is effective to prepare nanosized powders of tetragonal zirconia single-phase. Sinterability mainly depended on the agglomeration state of powders and the monoclinic phase content, fully tetragonal zirconia ceramic, with grain size of 2.4 mu m, was obtained after addition of at least 9 mol% ceria and sintering at 1500 degrees C for 4 h. (C) 2000 Elsevier B.V. Ltd. All rights reserved.

Dielectric spectroscopy on Bi3Zn2Sb3O14 ceramic: an approach based on the complex impedance

The dielectric properties and loss of Bi1.5ZnSb1.5O7 a poor-semiconducting ceramic were investigated by impedance spectroscopy, in the frequency range from 5 Hz to 13 MHz. Electric measurements were performed from 100 to 700 degreesC. Pyrochlore type phase was synthesized by the polymeric precursor method. Dense ceramic with 97% of the theoretical density was prepared by sintering via constant heating rate. The dielectric permittivity dependence as a function of frequency and temperature showed a strong dispersion at frequency lower than 10 kHz. The losses (tan delta) exhibit slight dependence with the frequency at low temperatures presenting a strong increase at temperatures higher than 400 degreesC. A decrease of the loss magnitude occurs with increasing frequency. Relaxation times were extracted using the dielectric functions Z(omega) and M(omega). The plots of the relaxation times tau(Z'), and tau(M) as a function of temperature follow the Arrhenius law, where a single slope is observed with activation energy values equal to 1.38 and 1.37 eV, respectively. (C) 2003 Elsevier Ltd. All rights reserved.

Structural effects of Li and K additives on the columbite precursor and 0.9PMN-0.1PT powders

Single-phase perovskite 0.9Pb(Mg1/3Nb2/3)O-3-0.1PbTiO(3) (PMN-PT) powders were prepared by using a Ti-modified columbite precursor (MNT) obtained by the polymeric precursor method. The innovation consists in the preparation of Ti-modified columbite in order to react directly with a stoichiometric amount of PbO to obtain pyrochlore-free PMN-PT powders. It has been shown that titanium oxide forms a solid solution with columbite (MN) and does not affect the obtaining of a single-phase columbite precursor. Thus, a high amount of perovskite phase can be obtained by reaction with PbO at 800 degreesC for 2 h. Effects of K and Li additives on the structure of MNT and PMN-PT were studied. X-ray diffraction studies were carried out to verify the phase formation at each processing step and these data were used for structural refinement by the Rietveld method. Both K and Li additives increase the crystallinity of MNT powders, being this effect more intense for the Li-doped samples. For PMN-PT samples the additives cause an insignificant decrease in the amount of perovskite phase. The morphology of the PMN-PT powder depends on the type of the additive. (C) 2003 Elsevier B.V All rights reserved.

Vertical marginal discrepancy of ceramic copings with different ceramic materials finish lines and luting agents: An in vitro evaluation

Statement of problem. Prosthetic restorations that fit poorly may affect periodontal health and occlusion. Studies that have evaluated the accuracy of fit of ceramic restorations before and after cementation assessed primarily intracoronal restorations.Purpose. This in vitro study evaluated the effect of different finish lines, ceramic manufacturing techniques, and luting agents on the vertical discrepancy of ceramic copings.Material and methods. Two stainless steel molars were prepared for complete crowns with 2 different finish lines (heavy chamfer and rounded shoulder); each molar was duplicated to fabricate 90 copings. A total of 180 copings generated 18 groups (n=10 for each finish line-coping material-luting agent combination). Luting agents tested included zinc phosphate, resin-modified glass ionomer (Fuji Plus), and resin composite cements (Panavia F). A metal frame was developed on which to screw the stainless steel model and a ceramic coping; the distance (mum) between 2 predetermined points was measured before and after cementation by a profile projector under a torquing force. A 4-way ANOVA with repeated measurements was performed to assess the influence of each factor in the vertical marginal discrepancy: 3 between-coping factors (finish line-coping material-luting agent) and 1 within-coping factor (before and after cementation) (alpha=.05).Results. Procera copings presented the lowest mean values (P<.05) of vertical marginal discrepancy before and after cementation (25/44 mum) when compared to Empress 2 (68/110 mum) and InCeram Alumina copings (57/117 mum), regardless of any combinations among all finish lines and luting agents tested.Conclusion. Considering each factor separately, the ceramic manufacturing technique appeared to be the most important factor tested for the definitive vertical discrepancy of all-ceramic copings, with lower mean values for Procera copings.

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.