Use of high energy ball milling on the sintering optimization of alumina ceramics

In this work, the effect of the milling time on the densification of the alumina ceramics with or without 5wt.%Y 2O 3, is evaluated, using high-energy ball milling. The milling was performed with different times of 0, 2, 5 or 10 hours. All powders, milled at different times, were characterized by X-Ray Diffraction presenting a reduction of the crystalline degree and crystallite size as function of the milling time increasing. The powders were compacted by cold uniaxial pressing and sintered at 1550°C-60min. Green density of the compacts presented an increasing as function of the milling time and sintered samples presented evolution on the densification as function of the reduction of the crystallite size of the milled powders. © (2010) Trans Tech Publications.

Biaxial flexural strength of CAD/CAM ceramics.

Aim of the study was to evaluate the biaxial flexural strength of ceramics processed using the Cerec inLab system. The hypothesis was that the flexural strength would be influenced by the type of ceramic. Ten samples (ISO 6872) of each ceramic (N.=50/n.=10) were made using Cerec inLab (software Cerec 3D) (Ø:15 mm, thickness: 1.2 mm). Three silica-based ceramics (Vita Mark II [VM], ProCad [PC] and e-max CAD ECAD]) and two yttria-stabilized tetragonal-zirconia-polycrystalline ceramics (Y-TZP) (e-max ZirCad [ZrCAD] and Vita In-Ceram 2000 YZ Cubes [VYZ]) were tested. The samples were finished with wet silicone carbide papers up to 1200-grit and polished in a polishing machine with diamond paste (3 μm). The samples were then submitted to biaxial flexural strength testing in a universal testing machine (EMIC), 1 mm/min. The data (MPa) were analyzed using the Kruskal-Wallis and Dunn (5%) tests. Scanning electronic microscopy (SEM) was performed on a representative sample from each group. The values (median, mean±sd) obtained for the experimental groups were: VM (101.7, 102.1±13.65 MPa), PC (165.2, 160±34.7 MPa), ECAD (437.2, 416.1±50.1 MPa), ZrCAD (804.2, 800.8±64.47 MPa) and VYZ (792.7, 807±100.7 MPa). The type of ceramic influenced the flexural strength values (P=0.0001). The ceramics ECADa, e-max ZrCADa and VYZa presented similar flexural strength values which were significantly higher than the other groups (PCb and VM IIb), which were similar statistically between them (Dunn's test). The hypothesis was accepted. The polycrystalline ceramics (Y-TZP) should be material chosen for make FPDs because of their higher flexural strength values.

SnO 2 ceramics with low electrical resistivity obtained by microwave sintering

The main aim of this study was to develop dense and conducting SnO 2 ceramics without precipitated phases on the grain boundaries, which was verified using field emission scanning microscopy (FE-SEM) coupled with an energy-dispersive X-ray spectroscopy (FE-SEM/EDS). Two sample groups were investigated, where the first sample group was doped with zinc while the second one was doped with cobalt. The ceramics were prepared using the oxides mixture method and the sintering was carried out in a conventional muffle oven as well as in microwave oven. The results obtained were found to be similar regarding the relative density for the two sintering methods while time and temperature gains were observed for the microwave sintering method. The relative densities obtained were nearly 95%, for the two sintering methods. Concerning the electrical characterization measurements-electric field x current density as well as the environment temperature, the ceramics obtained through the conventional sintering method presented non-ohmic behavior. For the microwave sintered ceramics, we observed an ohmic behavior with electrical resistivity of 1.3 Ωcm for the samples doped with ZnO/Nb 2O 5 and 2.5 Ωcm for that of the samples doped with CoO/Nb 2O 5. The FE-SEM/EDS results for the microwave sintered ceramics indicated a structure with a reduced number of pores and other phases segregated at the grain boundaries, which leads to a better conductive ceramic than the conventional oven sintered samples. The dilatometry analysis determined the muffle sintering temperature and the difference between the densification of cobalt and zinc oxides. The addition of niobium oxide resulted in the decrease in resistivity, which thus led us to conclude that it is possible to obtain dense ceramics with low electrical resistivity based on SnO 2 using commercial oxides by the oxides mixture technique and the microwave oven sintering method. Copyright © 2011 American Scientific Publishers All rights reserved.

Anfis applied to the prediction of surface roughness in grinding of advanced ceramics

This paper introduces a methodology for predicting the surface roughness of advanced ceramics using Adaptive Neuro-Fuzzy Inference System (ANFIS). To this end, a grinding machine was used, equipped with an acoustic emission sensor and a power transducer connected to the electric motor rotating the diamond grinding wheel. The alumina workpieces used in this work were pressed and sintered into rectangular bars. Acoustic emission and cutting power signals were collected during the tests and digitally processed to calculate the mean, standard deviation, and two other statistical data. These statistics, as well the root mean square of the acoustic emission and cutting power signals were used as input data for ANFIS. The output values of surface roughness (measured during the tests) were implemented for training and validation of the model. The results indicated that an ANFIS network is an excellent tool when applied to predict the surface roughness of ceramic workpieces in the grinding process.

Influência de protocolos de jateamento na rugosidade da superfície de uma cerâmica de zircônia tetragonal parcialmente estabilizada por ítria

Objective: To evaluate the influence of different air abrasion protocols on the surface roughness of an yttria-stabilized polycrystalline tetragonal zirconia) (Y-TZP) ceramic, as well as the surface topography of the ceramic after the treatment. Method: Fifty-four specimens (7.5×4×7.5mm) obtained from two ceramic blocks (LAVA, 3M ESPE) were flattened with fine-grit sandpaper and subjected to sintering in the ceramic system's specific firing oven. Next, the specimens were embedded in acrylic resin and the surfaces to be treated were polished in a polishing machine using sandpapers of decreasing abrasion (600- to 1,200-grit) followed by felt discs with 10μm and 3μm polishing pastes and colloidal silica. The specimens were then randomly assigned to 9 groups, according to factors particle and pressure(n=6): Gr1- control; Gr2- Al 2O 3(50μm)/2.5 bar; Gr3- Al 2O 3(110μm)/2.5 bar; Gr4- SiO 2(30μm)/2.5 bar; Gr5- SiO 2(30μm)/2.5 bar; Gr6- Al 2O 3(50μm)/3.5 bar; Gr7- Al2O3(110μm)/3.5 bar; Gr8- SiO 2(30μm)/3.5 bar; Gr9- SiO 2(30μm)/3.5 bar. After treatments, surface roughness was analyzed by a digital optical profilometer and the morphology was examined by scanning electron microscopy (SEM). Data (μm) were subjected to statistical analysis by Dunnett's test (5%), two-way ANOVA and Tukey's test (5%). Results: The type of particle (p=0.0001) and the pressure (p=0.0001) used in the air abrasion protocols influenced the surface roughness values among the experimental groups (ANOVA). The mean surface roughness values (μm) obtained for the experimental groups (Gr2 to Gr9) were, respectively: 0.37 D; 0.56 BC; 0.46 BC; 0.48 CD; 0.59 BC; 0.82 A; 0.53B CD; 0.67 AB. The SEM analysis revealed that Al 2O 3, regardless of the particle size and pressure used, caused damage to the surface of the specimens, as it produced superficial damages on the ceramic, in the form of grooves and cracks. Conclusion: Al2O3 (110 μm/3.5 bar) air abrasion promoted the highest surface roughness on the ceramics, but it does not mean that this protocol promotes better ceramic-cement union compared to the other air abrasion protocols.

Effect of brushing with conventional versus whitening dentifrices on surface roughness and biofilm formation of dental ceramics

The aim of this study was to evaluate the effect of conventional and whitening dentifrices on the weight loss, surface roughness, and early in situ biofilm formation on the surface of dental ceramics. Standardized feldspar ceramic specimens (Vita VM7 and Vita VM13) were submitted to the following experimental conditions: no brushing; brushing without a dentifrice; brushing with a conventional dentifrice; and brushing with a whitening dentifrice. A brushing machine was used to simulate brushing. The mass and surface roughness of all specimens from the test groups were evaluated prior to and after brushing. Ten participants used an oral device for eight hours to evaluate the biofilm formed in situ on the specimens. Scanning electron microscopy was used for qualitative and quantitative analysis of the biofilm. ANOVA and Tukey tests were used to analyze the results of weight loss, surface roughness, and presence of bacteria. A one-way Kruskal-Wallis test was used for bacterial colonization results. For both ceramics, brushing with a whitening dentifrice resulted in weight loss that was significantly greater when compared to brushing without a dentifrice or with a conventional dentifrice. Increased surface roughness was noticed on VM13 ceramic samples with both dentifrices, whereas only conventional dentifrice had a significant effect on the surface roughness of VM7 samples. For both VM7 and VM13, no difference was found between the experimental conditions with regard to the presence or number of bacteria. Cocci and short rods were the predominant microbial morphotypes. Granular or fibrillar acellular material partially covered the specimens. Brushing with a whitening dentifrice resulted in significant weight loss of ceramic restorations, while brushing with both conventional and whitening dentifrices can roughen ceramic surfaces. The increase in roughness was not clinically significant to contribute to increased biofilm formation.

Microstructure of ceramics TiO2 obtained by protein consolidation

Porous ceramics can be produced by adding starch (corn, potato) and protein (animal or vegetable) to raw material as pore forming element. In this study, titanium dioxide ceramics were formed by vegetable protein consolidation. Soybean was chosen as the binding agent and pore forming. The samples, which were produced in cylindrical shape, had the following processing: material mixture, gelling, drying, pre-sintering and sintering. Heated platinum microscopy were performed by using suspensions with different compositions in order to verify protein gelling capacity and better know the temperature in which this process occurs. The samples were characterized by apparent porosity and roughness measurement. Besides, imaging by light microscopy was also performed in order to determine the sample morphology and porosity. © (2012) Trans Tech Publications, Switzerland.

Caracterização química e mineralógica de azulejos portugueses do centro histórico de São Luís-MA (Brasil): Uma aproximação à mineralogia e à temperatura de queima das matérias-primas

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influence of polishing procedures on the surface roughness of dental ceramics made by different techniques

The aim of this study was to evaluate the influence of 2 different surface polishing procedures - glazing (GZ) and manual polishing (MP) - on the roughness of ceramics processed by computer-aided design/computer-aided manufacturing (CAD/CAM) and conventional systems (stratification technique). Eighty ceramic discs (diameter: 8 mm, thickness: 1 mm) were prepared and divided among 8 groups (n = 10) according to the type of ceramic disc and polishing method: 4 GZ and 4 MP. Specimens were glazed according to each manufacturer's recommendations. Two silicone polishing points were used on the ceramic surface for manual polishing. Roughness was measured using a surface roughness tester. The roughness measurements were made along a distance of 2 mm on the sample surface and the speed of reading was 0.1 mm/s. Three measurements were taken for each sample. The data (μm) were statistically analyzed using analysis of variance (ANOVA) and Tukey's test (α = 0.05). Qualitative analysis was performed using scanning electron microscopy (SEM). The mean (± SD) roughness values obtained for GZ were: 1.1 ± 0.40 μm; 1.0 ± 0.31 μm; 1.6 ± 0.31 μm; and 2.2 ± 0.73 μm. For MP, the mean values were: 0.66 ± 0.13 μm; 0.43 ± 0.14 μm; 1.6 ± 0.55 μm; and 2.0 ± 0.63 μm. The mean roughness values were significantly affected by the ceramic type (P = 0.0001) and polishing technique (P = 0.0047). The SEM images confirmed the roughness data. The manually polished glass CAD/CAM ceramics promoted lower surface roughness than did the glazed feldspathic dental ceramics.

Infrared to visible up-conversion emission in Er3+/Yb 3+ codoped fluoro-phosphate glass-ceramics

Erbium Er3+ and ytterbium Yb3+ codoped fluoro-phosphate glasses belonging to the system NaPO3-YF 3-BaF2-CaF2 have been prepared by the classical melt-quenching technique. Glasses containing up to 10 wt% of erbium and ytterbium fluorides have been obtained and characterized using differential scanning calorimetry (DSC) and UV-visible and near-infrared spectroscopy. Transparent and homogeneous glass-ceramics have been then reproducibly synthetized by appropriate heat treatment above glass transition temperature of a selected parent glass. Structural investigations of the crystallization performed through X-ray diffractometry (XRD) and scanning electron microscopy (SEM) have evidenced the formation of fluorite-type cubic crystals based during the devitrification process. Finally, infrared to visible up-conversion emission upon excitation at 975 nm has been studied on the Er3+ and Yb 3+ codoped glass-ceramics as a function of thermal treatment time. A large enhancement of intensity of the up-conversion emissions-about 150 times- has been observed in the glass-ceramics if compared to the parent glass one, suggesting an incorporation of the rare-earth ions (REI) into the crystalline phase. © 2012 The American Ceramic Society.

Fe K-edge X-ray absorption spectroscopy study of Pb(Fe2/3W 1/3)O3-PbTiO3 multiferroic ceramics

The present paper is a comprehensive study concerning Fe K-edge X-ray absorption spectroscopy (XAS) measurements, which were performed to characterize the local structure of (1 - x)Pb(Fe2/3W1/3)O 3-xPbTiO3 samples as a function of temperature and PbTiO3 content. Results obtained by the fits of extended X-ray absorption fine structure consist with rhombohedral symmetry for Pb(Fe 2/3W1/3)O3 composition at temperatures lower than room temperature. This result is in apparent disagreement with X-ray and neutron diffraction characterization which have been reported. This apparent disagreement is related to the fact that XAS probes the short-range order, whereas X-ray diffraction provides structural information about the average structure. Moreover, as the PbTiO3 content increases, a disorder has been detected at local structure of the FeO6 octahedron. Analysis of X-ray absorption near edge structure spectra did not show modifications in intensity nor energy of transitions. © 2013 American Institute of Physics.

Morphotropic phase boundary and electrical properties of 1-x[Bi 0.5Na0.5]TiO3 -xBa[Zr0.25Ti 0.75]O3 lead-free piezoelectric ceramics

Lead-free solid solutions (1-x)Bi0.5Na0.5TiO 3 (BNT)-xBaZr0.25Ti0.75O3 (BZT) (x=0, 0.01, 0.03, 0.05, and 0.07) were prepared by the solid state reaction method. X-ray diffraction (XRD) and Rietveld refinement analyses of 1-x(BNT)-x(BZT) solid solution ceramic were employed to study the structure of these systems. A morphotropic phase boundary (MPB) between rhombohedral and cubic structures occured at the composition x=0.05. Raman spectroscopy exhibited a splitting of the (TO3) mode at x=0.05 and confirmed the presence of MPB region. Scanning electron microcopy (SEM) images showed a change in the grain shape with the increase of BZT into the BNT matrix lattice. The temperature dependent dielectric study showed a gradual increase in dielectric constant up to x=0.05 and then decrease with further increase in BZT content. Maximum coercive field, remanent polarization and high piezoelectric constant were observed at x=0.05. Both the structural and electrical properties show that the solid solution has an MPB around x=0.05. © 2012 Elsevier Ltd and Techna Group S.r.l.

Dielectric and structural characterization of Pb1-xAxZr0.40Ti0.60O3 (A = Sr, Ca) ferroelectric ceramics

This paper reports the influence of Sr- and Ca-substitution on the structural and ferroelectric properties of Pb1-xSrxZr0.40Ti0.60O3 (PSZT) and Pb1-xCaxZr0.40Ti0.60O3 (PCZT) ceramic systems. The dielectric measurements show that these substitutions cause a diffuse behavior in the dielectric permittivity curves for all samples. According to the X-ray absorption near-edge structure (XANES) spectra collected at Ti K- and LIII-edge, when Pb was replaced by Sr or Ca, a decrease in the local distortion around Ti atoms in the TiO6 octahedron could be observed. The O K-edge XANES spectra also revealed that the hybridization between O 2p and Pb 6sp states decreased as the amount of Sr or Ca atoms increased. Based on these results, it was possible to ascertain that the ferroelectric behavior in PSZT and PCZT samples bears a close correlation to the hybridization weakening between O 2p and Pb 6 sp states. © 2013 by American Scientific Publishers.

Surface agents' influence on the flexural strength of bilaminated ceramics

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Effect of yttrium doping in barium zirconium titanate ceramics: A structural, impedance, modulus spectroscopy study

In the current article, we studied the effect of yttrium [Y3+] ions' substitution on the structure and electric behavior of barium zirconate titanate (BZT) ceramics with a general formula [Ba1-x Y 2x/3](Zr0.25Ti0.75)O3 (BYZT) with [x = 0, 0.025, 0.05] which were prepared by the solid-state reaction method. X-ray diffraction patterns indicate that these ceramics have a single phase with a perovskite-type cubic structure. Rietveld refinement data confirmed [BaO 12], [ZrO6], [TiO6], [YO6] clusters in the cubic lattice. The Y3+ ions' effects on the electric conductivity behavior of BZT ceramics as a function of temperature and frequency are described, which are based on impedance spectroscopy analyses. The complex impedance plots display a double semicircle which highlights the influences of grain and grain boundary on the ceramics. Impedance analyses showed that the resistance decreased with the increasing temperature and resulted in a negative temperature coefficient of the resistance property in all compositions. Modulus plots represent a non-Debye-type dielectric relaxation which is related to the grain and grain boundary as well as temperature-dependent electric relaxation phenomenon and an enhancement in the mobility barrier by Y3+ ions. Moreover, the electric conductivity increases with the replacement of Ba 2+ by Y3+ ions may be due to the rise in oxygen vacancies. © 2013 The Minerals, Metals & Materials Society and ASM International.