Bond strength of a resin cement to high-alumina and zirconia-reinforced ceramics: The effect of surface conditioning

Purpose: The aim of this study was to evaluate the effect of two surface conditioning methods on the microtensile bond strength of a resin cement to three high-strength core ceramics: high alumina-based (In-Ceram Alumina, Procera AllCeram) and zirconia-reinforced alumina-based (In-Ceram Zirconia) ceramics. Materials and Methods: Ten blocks (5 ×6 × 8 mm) of In-Ceram Alumina (AL), In-Ceram Zirconia (ZR), and Procera (PR) ceramics were fabricated according to each manufacturer's instructions and duplicated in composite. The specimens were assigned to one of the two following treatment conditions: (1) airborne particle abrasion with 110-μm Al2O3 particles + silanization, (2) silica coating with 30 μm SiOx particles (CoJet, 3M ESPE) + silanization. Each ceramic block was duplicated in composite resin (W3D-Master, Wilcos, Petrópolis, RJ, Brazil) using a mold made out of silicon impression material. Composite resin layers were incrementally condensed into the mold to fill up the mold and each layer was light polymerized for 40 s. The composite blocks were bonded to the surface-conditioned ceramic blocks using a resin cement system (Panavia F, Kuraray, Okayama, Japan). One composite resin block was fabricated for each ceramic block. The ceramic-composite was stored at 37°C in distilled water for 7 days prior to bond tests. The blocks were cut under water cooling to produce bar specimens (n = 30) with a bonding area of approximately 0.6 mm2. The bond strength tests were performed in a universal testing machine (crosshead speed: 1 mm/min). Bond strength values were statistically analyzed using two-way ANOVA and Tukey's test (≤ 0.05). Results: Silica coating with silanization increased the bond strength significantly for all three high-strength ceramics (18.5 to 31.2 MPa) compared to that of airborne particle abrasion with 110-μm Al2O3 (12.7-17.3 MPa) (ANOVA, p < 0.05). PR exhibited the lowest bond strengths after both Al2O3 and silica coating (12.7 and 18.5 MPa, respectively). Conclusion: Conditioning the high-strength ceramic surfaces with silica coating and silanization provided higher bond strengths of the resin cement than with airborne particle abrasion with 110-μm Al2O3 and silanization.

Low-frequency high-temperature internal friction in Ti-13Nb-13Zr alloy

Recent studies have been done to achieve biomedical alloys containing non-toxic elements and presenting low elastic moduli. It has been reported that Ti-Nb-Zr alloys rich in beta phase, especially Ti-13Nb-13Zr, have potential characteristics for substituting conventional materials such as Ti-6Al-4V, stainless steel and Co alloys. The aim of this work is to study the internal friction (IF) of Ti-13Nb-13Zr (TNZ) alloy due to the importance of the absorption impacts in orthopedic applications. The internal friction of this alloy produced by arc melting was measured using an inverted torsion pendulum with the free decay method. The measurements were performed from 77 to 700 K with heating rate of 1 K/min, in a vacuum better than 10-5 mBar. The results show a relaxation structure at high temperature strongly dependent on microstructure of the material. Qualitative discussions are presented for the experimental results, and the possibility of using the TNZ as a high damping material is briefly mentioned.

Evaluation of Ir-based modifiers in the simultaneous determination of As, Bi, Pb, Sb, and Se in milk by graphite furnace atomic absorption spectrometry

Different modifiers (IrCl3, W+IrCl3, Zr+IrCl 3) and coatings (Ir, W-Ir, Zr-Ir) were evaluated for the simultaneous determination of arsenic, bismuth, lead, antimony, and selenium in milk by graphite furnace atomic absorption spectrometry using the 'end-capped' transversely heated graphite atomizer (THGA). Integrated platform, pretreated with Zr-Ir as permanent modifier, was elected as the optimum surface modification resulting in up to 250 firings. Two additional recoatings were possible without significant changes in the analytical performance (750 firings). For 20 μL of matrix-matched standard solutions using diluted (1:10) milk samples, typical correlation coefficients between integrated absorbance and analyte concentration (5.00-20.0 μg/L) was always better than 0.999. The levels of the analytes found in commercial milk samples were lower than the limit of detection: 2.9 μg/L As, 2.9 μg/L Bi, 1.8 μg/L Pb, 1.9 μg/L Sb, and 2.5 μg/L Se. Recoveries were found within the following intervals: 88-114% for As, 89-118% for Bi, 89-113% for Pb, 91-115% for Sb, and 92-115% for Se. The relative standard deviations (n = 12) were ≤2% (As), ≤ 5% (Bi), ≤ 1.4% (Pb), ≤ 3% (Sb), and 5% (Se), and the respective calculated characteristic masses were 54 pg As, 55 pg Bi, 40 pg Pb, 56 pg Sb, and 51 pg Se.

Geoquímica de gnaisses do arco magmático de goiás na região sul do estado de goiás

Granitic to trondhjemitic gneisses from the Pontalina region in the southern part of Goiás State, Central Brazil, have calcic to calc-alkaline, metaluminous to peraluminous compositions. They have low concentrations of alkaline elements, and are enriched in Ba, Sr, K, Rb in relation to Nb, Y, Zr and REE, and have negative anomalies of Nb and Ti, features which are similar to those of magmas generated in magmatic arc environments. Those rocks were previously interpreted as part of the basement of the Brasília Belt, attributed to the Archean to Paleoproterozoic, but new Sm - Nd isotopic data indicate a neoproterozoic age (TDM = 0,9 a 1,2 Ga), and the preliminary geochemical data reveal compositions similar to the gneisses of the other regions belonging to the Goiás Magmatic Arc.

Observation of piezoelectric response on tungsten doped barium zirconium titanate ceramics

This study describes observation of piezoelectric response of Ba(Zr 0.10Ti 0.90.O3 ceramics modified with tungsten (BZT:2W) by the mixed oxide method. According to X ray diffraction analysis, the ceramics are free of secondary phases. Transmission electron microscopy (TEM) analyses reveals the absence of segregates in the grain boundaries indicates the high solubility of WO3 in the BZT matrix. The dielectric permittivity measured at a frequency of 10 KHz was equal to 6500 with dieletric loss of 0.15. A typical hysteresis loop was observed at room temperature. Electron Paramagnetic Resonance (EPR) analyses reveals that substitution of W6+ by Ti4+ causes distortion in the crystal structure changing lattice parameter. Polarization reversal was investigated by applying dc voltage through a conductive tip during the area scanning. Piezoelectric force microscopy images reveals that in-plane response may not change its sign upon polarization switching, while the out-of-plane response does. Copyright © 2010 American Scientific Publishers.

Microstructure, crystalline phase, and dielectric property analyses of TiO2 composition with ZrO2 addition

For microwave applications, including mobile and satellite communications, ceramic resonators should have a high dielectric constant, low dielectric losses, and high frequency stability. In this sense, TiO2-ZrO 2 ceramics have been investigated as a function of sintering behavior, phase composition, and microstructure. The ceramics were densified reaching a value of about 86% of theoretical density at 1400°C sintering temperature. The ceramics are prepared by mixing raw materials with the following TiO2-ZrO2 weight % ratio: 100 to 0, 90 to 10, and 80 to 20, respectively. The measured dielectric constants are between 79 and 88 values, while the quality factor due to dielectric losses are between 2820 and 5170. These results point out the influence of Ti/Zr ratio on controlling the dielectric properties. © (2010) Trans Tech Publications.

Sintering temperature influence on microwave dielectric properties of TiO2-ZrO2 ceramics

Dielectric ceramics have been widely investigated and used for microwave applications such as resonators and filters. The present study deals with the influence of sintering temperature on microwave dielectric properties of TiO2 ceramics with 10, 20, and 30 wt% ZrO2. Three compositions have been developed through mixing procedures and then tested for each sintering temperature: 1500 and 1400°C. X-ray diffraction and scanning electron microscopy are carried out aiming to explain the ceramic behavior of each sample. The dielectric constants of different ceramics for both temperatures varied from 85.4 to 62.6, while their quality factor due to dielectric losses varied from 3110 to 1630. The Q decrease is attributed to the non uniform grain growth and to the obtained crystalline phases. The best microwave parameters were obtained for the ceramics sintered at 1400°C, which can be applied in microwave circuits as dielectric resonators. © (2010) Trans Tech Publications.

Thickness dependence of structure and piezoelectric properties at nanoscale of polycrystalline PZT thin films

Lead zirconate titanate Pb(Zr 0.50Ti 0.50)O 3 (PZT) thin films were deposited by a polymeric chemical method on Pt(111)/Ti/SiO2/Si substrates to understand the mechanisms of phase transformations and the effect of film thickness on the structure, dielectric and piezoelectric properties in these films. PZT films pyrolyzed at temperatures higher than 350 °C present a coexistence of pyrochlore and perovskite phases, while only perovskite phase grows in films pyrolyzed at temperatures lower than 300 °C. For pyrochlore-free PZT thin films, a small (100) orientation tendency near the film-substrate interface was observed. Finally, we demonstrate the existence of a self-polarization effect in the studied PZT thin films. Results suggest that Schottky barriers and/or mechanical coupling near the filmsubstrate interface are not primarily responsible for the observed self-polarization effect in our films. © 2012 IEEE.

Analysis of the bioactive surface of Ti-35Nb-7Zr alloy after alkaline treatment and solution body fluid

The purpose of this work was to evaluate the Ti-35Nb-7Zr experimental alloy after surface treatment and soaking in solution body fluid (SBF) to form bonelike apatite. The Ti-35Nb-7Zr alloy was produced from commercially pure materials (Ti, Nb and Zr) by an arc melting furnace. All ingots were submitted to sequences of heat treatment (1100 °C/2 h and water quenching), cold working by swaging procedures and heat treatment (1100 °C/2 h and water quenching). Discs with 13 mm diameter and 3 mm in thickness were cut. The samples were immersed in NaOH aqueous solution with 5 M at 60 °C for 72 h, washed with distilled water and dried at 40 °C for 24 h. After the alkaline treatment, samples were heat treated in both conditions: at 450 and 600 °C for 1 h in an electrical furnace in air. Then, they were soaking in SBF for 24 h to form an apatite layer on the surface. The surfaces were investigated by using scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), infrared spectroscopy (FTIR) and contact angle measurements. The results indicate that calcium phosphate could form on surface of Ti-35Nb-7Zr experimental alloy. © Springer-Verlag Berlin Heidelberg 2013.

Local electronic structure, optical bandgap and photoluminescence (PL) properties of Ba(Zr0.75Ti0.25)O3 powders

Ba(Zr0.75Ti0.25)O3 (BZT-75/25) powders were synthesized by the polymeric precursor method. Samples were structurally characterized by X-ray diffraction (XRD), Rietveld refinement, X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) techniques. Their electronic structures were evaluated by first-principle quantum mechanical calculations based on density functional theory at the B3LYP level. Their optical properties were investigated by ultraviolet-visible (UV-Vis) spectroscopy and photoluminescence (PL) measurements at room temperature. XRD patterns and Rietveld refinement data indicate that the samples have a cubic structure. XANES spectra confirm the presence of pyramidal [TiO5] clusters and octahedral [TiO6] clusters in the disordered BZT-75/25 powders. EXAFS spectra indicate distortion of Ti-O and Ti-O-Ti bonds the first and second coordination shells, respectively. UV-Vis absorption spectra confirm the presence of different optical bandgap values and the band structure indicates an indirect bandgap for this material. The density of states demonstrates that intermediate energy levels occur between the valence band (VB) and the conduction band (CB). These electronic levels are due to the predominance of 4d orbitals of Zr atoms in relation to 3d orbitals of Ti atoms in the CB, while the VB is dominated by 2p orbitals related to O atoms. There was good correlation between the experimental and theoretical optical bandgap values. When excited at 482 nm at room temperature, BZT-75/25 powder treated at 500 C for 2 h exhibited broad and intense PL emission with a maximum at 578 nm in the yellow region. © 2013 Elsevier Ltd. All rights reserved.

Quantum mechanical modeling of excited electronic states and their relationship to cathodoluminescence of BaZrO3

First-principles calculations set the comprehension over performance of novel cathodoluminescence (CL) properties of BaZrO3 prepared through microwave-assisted hydrothermal. Ground (singlet, s*) and excited (singlet s** and triplet t**) electronic states were built from zirconium displacement of 0.2 Å in {001} direction. Each ground and excited states were characterized by the correlation of their corresponding geometry with electronic structures and Raman vibrational frequencies which were also identified experimentally. A kind of optical polarization switching was identified by the redistribution of 4dz2 and 4dxz (Zr) orbitals and 2pz O orbital. As a consequence, asymmetric bending and stretching modes theoretically obtained reveal a direct dependence with their polyhedral intracluster and/or extracluster ZrO6 distortions with electronic structure. Then, CL of the as-synthesized BaZrO3 can be interpreted as a result of stable triplet excited states, which are able to trap electrons, delaying the emission process due to spin multiplicity changes. © 2013 AIP Publishing LLC.

Synthesis and characterization of lead zirconate titanate (PZT) obtained by two chemical methods

Lead zirconate titanate (PZT) was synthesized at the ratio of Zr/Ti=52/48 using two synthesis methods: the polymeric precursor method (PPM) and the microwave-assisted hydrothermal method (MAHM). The synthesized materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), particle size distribution by sedimentation, hysteresis measurements and photoluminescence (PL). The results showed that PZT powders are composed of tetragonal and rhombohedral phases. Different particle sizes and morphologies were obtained depending upon the synthesis method. From the hysteresis loop verified that PZT powders synthesized by the PPM have a typical loop of ferroelectric material and are more influenced by spatial charges while particles synthesized by the MAHM have a hysteresis loop similar to paraelectric material and are less influenced by spatial charges. Both samples showed PL behavior in the green region (525 nm) whereas the sample synthesized by the PPM showed higher intensity in spectra. © 2013 Elsevier Ltd and Techna Group S.r.l.

Local order of Pb1-xLaxZr0.40Ti 0.60O3 ferroelectric ceramic materials probed by X-ray absorption and Raman spectroscopies

This paper reports on the structural characterization of Pb 1-xLaxZr0.40Ti0.60O3 (PLZT) ferroelectric ceramic compositions prepared by the conventional solid state reaction method. X-ray absorption spectroscopy (XAS) and Raman spectroscopy were used to probe the local structure of PLZT samples that exhibits a normal and relaxor ferroelectric behavior. From the Zr K-edge and Pb LIII-edge EXAFS spectra, a considerable dissymmetry of Zr and Pb sites was observed in all samples, including those showing a long-range order cubic symmetry and a relaxor behavior. The Raman spectroscopy results confirmed the existence of a local disorder in all PLZT samples through the observation of Raman active vibrational modes. The variation in the intensity of the E(TO 3) mode in the PLZT relaxor samples indicates that the process of correlation between nanodomains stabilizes at temperatures lower than T m. © 2013 Elsevier B.V. All rights reserved.

Influência da dopagem com oxigênio nas propriedades anelásticas e biocompatibilidade de ligas Ti-5%pNb e Ti-10%pNb

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

Geoestatística aplicada à acumulação da precipitação pluviométrica com radar meteorológico

Pós-graduação em Agronomia (Energia na Agricultura) - FCA