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.

Morphological and luminescent studies on nanosized Er, Yb-Yttrium oxide up-converter prepared from different precursors

In this paper, we report luminescent and morphological studies with yttrium oxide samples doped with ytterbium and erbium. The samples were prepared by the combustion method and also from different precursors: oxalate, basic carbonate and polymeric resin. All powders were identified Lis being an yttrium oxide with a C-form structure, independent of the employed precursor. From mean crystallite size measurements, it was verified that oxides prepared through the polymeric precursor and combustion methods lead to the smallest crystallite size. Particle shape and size were investigated by SEM and TEM, and showed that both the oxalate precursor and the combustion methods do not provide oxide materials of suitable shape or size, on the other hand. The basic carbonate and polymeric precursors resulted in spherically shaped particles with an average diameter of 90 and 15 run. respectively, Upon 980 run diode laser excitation, green and red emission lines were detected for all samples and were assigned to the H-2(11/2) S-4(3/2) -> I-4(15/2) and (4)Fg(9/2) -> 4I(15/12) transitions, respectively. Such transitions are characteristic for Er3+ and result from energy transfer from Yb3+ energy levels, F-2(7/2) -> F-2(5/2). A relationship between the decrease in the mean crystallite size and the enhancement in red emission was also established as well as the influence of the presence of a high percentage of Yb-3 Both factors promote ET from Yb3+ (F-2(5/2)) to Er3+ (I-4(11/2)). (c) 2004 Elsevier B.V. All rights reserved.

Study of the morphological alterations to enamel and dentin in human and bovine teeth after irradiation with Er : YAG laser

Objective: the purpose of this study is to make use of scanning electron microscopy in order to comparatively analyze the morphological alterations to human and bovine enamel and dentin. Earlier data: Many a morphological study involving Er:YAG laser can be found in the literature. Still, not a single study comparing the effects of this infrared laser in human and bovine teeth has been reported. Materials and Methods: Thirty-two slices of human and bovine enamel and dentin were evenly divided into four groups. With the exception of the control group, the samples were irradiated with Er:YAG laser, focused at a distance of 12 mm and a 10-Hz frequency, with 150, 250, and 350 mJ of output energy per pulse for 10 seconds. After irradiation all specimens were observed under a scanning electron microscope. Results: There was practically no morphological difference for those samples that underwent 150 mJ/pulse irradiation. The dentin exposed to 250 mJ had a few open dentinal tubules. These were seen in enamel after a 350 mJ irradiation, in which the energy was able to reach the dentin. Conclusions: the breadth of this study allows us to state that the pattern between the species grew more heterogenous as the energy density was increased and that irradiation with 150 mJ/pulse resulted in greater likeness in human and bovine enamel and dentin.

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.

Ferroelectric state analysis in grain boundary of Na0.85Li0.15NbO3 ceramic

The electric and dielectric properties of the grain boundary of Na0.85Li0.15NbO3 lead-free ferroelectric-semiconductor perovskite were investigated. The impedance spectroscopy was carried out as a function of a thermal cycle. The sodium lithium niobate was synthesized by a chemical route based on the evaporation method. Dense ceramic, relative density of 97%, was prepared at 1423 K for 2 h in air atmosphere. ac measurements were carried out in the frequency range of 5 Hz-13 MHz and from 673 to 1023 K. Theoretical adjust of the impedance data was performed to deriving the electric parameters of the grain boundary. The electric conductivity follows the Arrhenius law, with activation energy values equal to 1.55 and 1.54 eV for heating and cooling cycle, respectively. The nonferroelectric state of the grain boundary and its correlation with symmetry are discussed in the temperature domain. (C) 2003 American Institute of Physics.