The influence of internal surface treatments on tensile bond strength for two ceramic systems

Statement of the Problem: the ceramic composition and surface microstructure of all-ceramic restorations are important components of an effective bonding substrate. Hydrofluoric acid and sandblasting are well-known procedures for surface treatment; however, surface treatment for high alumina-containing and lithium disilicate ceramics have not been fully investigated.Purpose: This in vitro study evaluated the tensile bond strength of resin cement to two types of ceramic systems with different surface treatments.Methods and Materials: Thirty specimens of each ceramic system were made according to the manufacturer's instructions and embedded in polyester resin. Specimens of In-Ceram Alumina [1] and IPS Empress 2 [E] were distributed to three groups with differing surface treatments (n=10): sandblasting with 50 jam aluminum oxide (APA); sandblasting with 110 pm aluminum oxide modified with silica particles (ROCATEC System-RS); a combination of sandblasting with APA and 10% hydrofluoric acid etching (HA) for two minutes on In-Ceram and for 20 seconds for IPS Empress 2. After the respective surface treatments, all the specimens were silanated, and Rely-X resin cement was injected onto the ceramic surface and light polymerized. The specimens were stored in distilled water at 37 degrees C for 24 hours and thermally cycled 1,100 times (5 degrees C/55 degrees C). The tensile bond strength test was performed in a universal testing machine at a 0.5 mm/minute crosshead speed.Results: the mean bond strength values (AWa) for IPS Empress 2 were 12.01 +/- 5.93 (EAPA), 10.34 +/- 1.77 (ERS) and 14.49 +/- 3.04 (EHA). The mean bond strength values for In-Ceram Alumina were 9.87 +/- 2.40 JAPA) and 20.40 +/- 6.27 (IRS). All In-Ceram specimens treated with 10% hydrofluoric acid failed during thermal cycling.Conclusion: the Rocatec system was the most effective surface treatment for In-Ceram Alumina ceramics; whereas, the combination of aluminum oxide sandblasting and hydrofluoric acid etching for 20 seconds worked more effectively for Empress 2 ceramics.

Inhibiting effect of citric acid on the pitting corrosion of tin

Potentiostatic and potentiodynamic studies were carried out to establish the inhibiting effects of citric acid on the pitting corrosion of tin. The critical potential (E-crit), which leads to pitting or general corrosion, was determined in sodium perchlorate solution in the pH range 1.0 to 4.0. Pit nucleation and growth, at pH 4.0, can be described by instantaneous nucleation followed by progressive nucleation. The results show that the minimum acid concentration needed to inhibit pitting of tin is 10(-2) M. Pitting occurrence by direct interaction between metal and perchlorate anions was observed.

Dynamical study of ZnO nanocrystal and Zn-HDS layered basic zinc acetate formation from sol-gel route

We have pointed out that zinc based particles obtained from ethanolic solution of a zinc acetate derivative (zinc oxy-acetate, Zn4O(Ac)(6)) are a mixture of nanometer sized ZnO, zinc oxy-acetate, and zinc hydroxide double salt (Zn-HDS). The knowledge of the mechanisms involved in the formation of ZnO and Zn-HDS phases, and the evolution of Zn species in reaction medium was monitored in situ during 14 h by simultaneous measurements of UV-vis absorption and extended X-ray absorption fine structures (EXAFS) spectra. This spectroscopic monitoring was initialized just after the addition of an ethanolic lithium hydroxide solution ([LiOH]/[Zn] = 0. 1) to the reaction medium kept under controlled temperature (40 degrees C). This study points out the first direct evidence of the reaction between ZnO nanoparticles and unreacted zinc oxy-acetate to form a Zn-HDS phase. The dissolution of ZnO and the reprecipitation of Zn-HDS are induced by the gradual release of water mainly produced by ethanol esterification well evidenced by gas chromatography coupled to mass spectroscopy and FT-IR measurements.

SAXS study of the kinetics of formation of ZnO colloidal suspensions

We have investigated, by in situ small-angle X-ray scattering (SAXS), the kinetics of formation of zinc oxide colloidal suspensions obtained after refluxing alcoholic solution of zinc acetate and catalysed by lithium hydroxide. The experimental results demonstrate that the suspensions are composed of colloidal spheroidal particles with a multimodal size distribution. The average radius of the main mode, approximately 2 nm, is invariant but the number of these basic particles continuously increases for increasing hydrolysis reaction time. The other two modes correspond to particles with average radii close to 6 and 10 nm, respectively. The larger particles are formed by coagulation of the smaller ones. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Structure of magnetic poly(oxyethylene)-siloxane nanohybrids doped with Fe-II and Fe-III

Hybrid organic - inorganic nanocomposites doped with Fe-II and Fe-III ions and exhibiting interesting magnetic properties have been obtained by the sol - gel process. The hybrid matrix of these ormosils ( organically modified silicates), classed as di-ureasils and termed U( 2000), is composed of poly( oxyethylene) chains of variable length grafted to siloxane groups by means of urea crosslinkages. Iron perchlorate and iron nitrate were incorporated in the diureasil matrices, leading to compositions within the range 80 greater than or equal to n greater than or equal to 10, n being the molar ratio of ether-type O atoms per cation. The structure of the doped diureasils was investigated by small-angle X-ray scattering (SAXS). For Fe-II-doped samples, SAXS results suggest the existence of a two-level hierarchical structure. The primary level is composed of spatially correlated siloxane clusters embedded in the polymeric matrix and the secondary, coarser level consists of domains where the siloxane clusters are segregated. The structure of Fe-III-doped hybrids is different, revealing the existence of iron oxide based nanoclusters, identified as ferrihydrite by wide-angle X-ray diffraction, dispersed in the hybrid matrix. The magnetic susceptibility of these materials was determined by zero-field-cooling and field-cooling procedures as functions of both temperature and field. The different magnetic features between Fe-II- and Fe-III-doped samples are consistent with the structural differences revealed by SAXS. While Fe-II-doped composites exhibit a paramagnetic Curie-type behaviour, hybrids containing Fe-III ions show thermal and field irreversibilities.

Quantitative structural analysis of the transition from LT-LixCoO2 to HT-LixCoO2 using the rietveld method: correlation between structure and electrochemical performance

A quantitative phase analysis was made of LiXCoO2 powders obtained by two distinct chemical methodologies at different temperatures (from 400 to 700degreesC). A phase analysis was made using Rietveld refinements based on X-ray diffraction data, considering the LiXCoO2 powders as a multiphase system that simultaneously contained two main phases with distinct, layered and spinel-type structures. The sults showed the coexistence of both structures in LiXCoO2 obtained at low temperature (400 and 500degreesC), although only the layered structure was detected at higher temperatures (600 and 700degreesC, regardless of the chemical powder process employed. The electrochemical performance, evaluated mainly by the cycling reversibility of LiXCoO2 in the form of cathode insertion electrodes, revealed that there is a close correlation between structural features and the electrochemical response, with one of the redox processes (3.3 v/3.9 v) associated only with the presence of the spinel-type structure. (C) 2003 Elsevier B.V. All rights reserved.

Electroluminescence of zinc oxide thin-films prepared via polymeric precursor and via sol-gel methods

Zinc oxide (ZnO) is an electroluminescent (EL) material that can emit light in different regions of electromagnetic spectrum when electrically excited. Since ZnO is chemically stable, inexpensive and environmentally friendly material, its EL property can be useful to construct solid-state lamps for illumination or as UV emitter. We present here two wet chemical methods to prepare ZnO thin-films: the Pechini method and the sol-gel method, with both methods resulting in crystalline and transparent films with transmittance > 85% at 550 nm. These films were used to make thin-film electroluminescent devices (TFELD) using two different insulator layers: lithium fluoride (LiF) or silica (SiO2). All the devices exhibit at least two wide emission bands in the visible range centered at 420 nm and at 380 nm attributed to the electronic defects in the ZnO optical band gap. Besides these two bands, the device using SiO2 and ZnO film obtained via sol-gel exhibits an additional band in the UV range centered at 350 nm which can be attributed to excitonic emission. These emission bands of ZnO can transfer their energy when a proper dopant is present. For the devices produced the voltage-current characteristics were measured in a specific range of applied voltage. (C) 2007 Elsevier B.V. All rights reserved.

Silica-PEG hybrid ormolytes: structure and properties

The effect of lithium salt doping on the structure and ionic conduction properties of silica-polyethyleneglycol composites is reported. These materials, so called ormolytes (organically modified electrolytes), were obtained by the sol-gel process. They have chemical stability due to the covalent bonds between the inorganic (silica) and organic (polymer) phase. The structure of these hybrid materials was investigated by small-angle X-ray scattering (SAXS) as a function of lithium concentration [O]/[Li] (O being the oxygens of the ether type). The spectra have a well-defined peak attributed to the existence of a liquid-like spatial correlation of silica clusters. The ionic conductivity was studied by AC impedance spectroscopy and is maximum for [O]/[Li] = 15. This result is consistent with SAXS and thermo-mechanical analysis measurements and is due to the formation of cross-linking between the polymer chains for the larger lithium concentrations. These materials are solid, transparent, flexible and have an ionic conductivity up to 10(-4) S/cm. (C) 1999 Elsevier B.V. B.V. 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.

Estudo das propriedades de troca iônica e/ou adsorção da celulose e celuloses modificadas

In this work it was studied the capacity of cellulose and chemically modified celluloses (carboxymethylcellulose, cellulose phosphate and oxicellulose) to adsorb copper(II) cations of aqueous and non aqueous solutions. The influence of the principal physical chemical parameters on the adsorption process was examined using the batch adsorption method and copper(II) perchlorate solutions, the maximum adsorption capacity determined for adsorbents were as follows (mol.g(-1)): cellulose, 0.54 . 10(-5); carboxymethylcellulose, 1.28 . 10(-4); cellulose phosphate, 1.12 . 10(-4); oxicellulose, 0.38 . 10(-4).

Ionic medium effects on equilibrium constants .2. Binary systems comprising some bivalent cations and monocarboxylates in aqueous solution

Simple equations were derived relating stoichiometric protonation constants of several monocarboxylates and formation constants associated with 1:1 complexes involving some bivalent cations and selected monocarboxylates, in aqueous sodium perchlorate media, at 25 degrees C, as a function of ionic strength (I), allowing the interconversion of parameters from one ionic strength to another, up to I = 3.00 M. In addition, thermodynamic formation constants as well as activity coefficients of the species involved in the equilibria were estimated. The results show that the proposed calculation procedure is very consistent with critically selected experimental data.

Thermal properties of fluoride glasses and their gel precursors

Xerogels were prepared from zirconium, barium, aluminum, lanthanum and lithium acetates, corresponding to a Li containing ZBLA composition. The study of their thermal properties (DSC, TG/DTG, FT-IR) showed that they might be used as chemically stable precursors in the preparation of fluoride glasses. Hydrofluoric acid in solution was chosen as a mild fluorinating agent. This newly proposed technique of fluorinating allowed to obtain high quality ZBLALi glass which presents the advantage of higher thermal stability and homogeneity in comparison with the glass obtained using individual commercial fluorides.

An electrode of the second kind for benzoate determination in medicinal syrups

This paper describes the construction of an electrode of the second kind, Pt\Hg\Hg-2(Bzt)(2)\graphite, sensitive to benzoate ion (Bzt). The electrode provides a near-Nernstian response (-58.19 mV/decade at 25 degrees C) to benzoate ion in the concentration range 1.11 x 10(-1) to 5.00 x 10(-4) M at pH 7.0 and ionic strength 0.500-3.00M, adjusted with NaClO4. The electrode is easily constructed, shows a fast response time, is low in cost, has excellent response stability, and has a lifetime greater than 24 months. which is much longer than those earlier reported for other systems. A further salient feature of the electrode is that perchlorate does not interfere in its response, which may be advantageous in the analysis of perchloric acid-treated samples. It was applied to the determination of sodium benzoate in some commercial expectorating medicinal syrups using the standard additions method. The results obtained by the proposed procedure compare very favorably with those obtained through the reference method recommended by the United States Pharmacopeia. (C) 1998 Academic Press.

Effect of thermal treatment temperature on the crystallinity and morphology of LiTaO3 thin films prepared from polymeric precursor method

Lithium tantalate thin films (LiTaO3) with (50:50) stoichiometry were prepared by spin coating method using a polymeric organic solution. The films were deposited on silicon (100) substrates with 4 layers. The substrates were previously cleaned and then the solution of lithium tantalate was deposited by adjusting the speed at 5000 rpm. The thin films deposited were thermally treated from 350 to 600degreesC for 3 hours in order to study the influence of the thermal treatment temperature on the crystallinity, microstructure, grain size and roughness of the final film. X-ray diffraction (XRD) results showed that the films are polycrystalline and secondary phases free. The thickness of films was observed by scanning electron microscopy (SEM). The atomic force microscopy (AFM) studies showed that the grain size and roughness are strongly influenced by thermal treatment.

TG studies of a composite solid rocket propellant based on HTPB-binder

Thermal decomposition kinetics of solid rocket propellants based on hydroxyl-terminated polybutadiene-HTPB binder was studied by applying the Arrhenius and Flynn-Wall-Ozawa's methods. The thermal decomposition data of the propellant samples were analyzed by thermogravimetric analysis (TG/DTG) at different heating rates in the temperature range of 300-1200 K. TG curves showed that the thermal degradation occurred in three main stages regardless of the plasticizer (DOA) raw material, the partial HTPB/IPDI binder and the total ammonium perchlorate decompositions. The kinetic parameters E-a (activation energy) and A (pre-exponential factor) and the compensation parameter (S-p) were determined. The apparent activation energies obtained from different methods showed a very good agreement.