Microscopic and dielectric analyses of vanadium and tungsten modified barium zirconium titanate ceramics

Dielectric spectroscopy was used in this study to examine polycrystalline vanadium and tungstendoped BaZr 0.1Ti 0.90O 3 (BZT10:2V and BZT10:2W) ceramics obtained by the mixed oxide method. According to X-ray diffraction analyses, addition of vanadium and tungsten lead to ceramics free of secondary phases. SEM analyses reveal that both dopants result in slower oxygen ion motion and consequently lower grain growth rate. Temperature dependence dielectric study showed normal ferroelectric to paraelectric transition well above the room temperature for the BZT10 and BZT10:2V ceramics. However, BZT10:2W ceramic showed a relaxor-like behavior near phase transition characterized by the empirical parameter γ. Piezoelectric force microscopy images reveals that the piezoelectric coefficient is strongly influenced by type of donor dopant suggesting promising applications for dynamic random access memories and data-storage media. Copyright © 2010 American Scientific Publishers All rights reserved.

Mechanical Property Assessment of Bone Healing around a Titanium-Zirconium Alloy Dental Implant

Background: It has been reported that titanium-zirconium alloy with 13-17% zirconium (TiZr1317) implants show higher biomechanical stability and bone area percentage relative to commercially pure titanium (cpTi) grade 4 fixtures. Purpose: This study aimed to determine whether the higher stability for TiZr1317 implants is associated with higher mechanical properties of remodeling bone in the areas around the implants. Materials and Methods: This study utilized 36 implants (n=18: TiZr1317, n=18: cpTi), which were placed in the healed ridges of the mandibular premolar and first molar of 12 mini pigs (n=3 implants/animal). After 4 weeks in vivo, the samples were retrieved, and resin-embedded histologic sections of approximately 100μm in thickness were prepared. In order to determine the nanomechanical properties, nanoindentation (n=30 tests/specimen) was performed on the bone tissue of the sections under wet conditions with maximum load of 300μN (loading rate: 60μN/s). Results: The mean (±standard deviation) elastic modulus (E) and hardness (H) for the TiZr1317 group were 2.73±0.50GPa and 0.116±0.017GPa, respectively. For the cpTi group, values were 2.68±0.51GPa and 0.110±0.017GPa for E and H, respectively. Although slightly higher mechanical properties values were observed for the TiZr1317 implants relative to the cpTi for both elastic modulus and hardness, these differences were not significant (E=p>0.75; H=p>0.59). Conclusions: The titanium-zirconium alloy used in this study presented similar degrees of nanomechanical properties to that of the cpTi implants. © 2013 Wiley Periodicals, Inc.

Structural and dielectric properties of polyvinyl alcohol/barium zirconium titanate polymer-ceramic composite

The polyvinyl alcohol (PVA)/barium zirconium titanate Ba[Zr0.1Ti0.9]O3 (BZT) polymer-ceramic composites with different volume percentage are obtained from solution mixing and hot-pressing method. Their structural and electrical properties are characterized by X-ray diffraction (XRD), Rietveld refinement, cluster modeling, scanning electron microscope and dielectric study. XRD patterns of PVA/BZT polymer-ceramics composite (with 50% volume fractions) indicate no obvious differences than the XRD patterns of pure BZT which shows that the crystal structure is still stable in the composite. The scanning electron micrograph indicates that the BZT ceramic is dispersed homogeneously in the polymer matrix without agglomeration. The dielectric permittivity (ε r) and the dielectric loss (tan δ) of the composites increase with the increase of the volume fraction of BZT ceramic. Theoretical models are employed to rationalize the dielectric behavior of the polymer composites. The dielectric properties of the composites display good stability within a wide range of temperature and frequency. The excellent dielectric properties of these polymer-ceramic composites indicate that the BZT/PVA composites can be a candidate for embedded capacitors. © 2013 Elsevier B.V.

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.

Physicochemical and mechanical properties of zirconium oxide and niobium oxide modified Portland cement-based experimental endodontic sealers

Aim: To evaluate the physicochemical and mechanical properties of Portland cement-based experimental sealers (ES) with different radiopacifying agents (zirconium oxide and niobium oxide micro- and nanoparticles) in comparison with the following conventional sealers: AH Plus, MTA Fillapex and Sealapex. Methodology: The materials were tested for setting time, compressive strength, flow, film thickness, radiopacity, solubility, dimensional stability and formaldehyde release. Data were subjected to anova and Tukey tests (P < 0.05). Results: MTA Fillapex had the shortest setting time and lowest compressive strength values (P < 0.05) compared with the other materials. The ES had flow values similar to the conventional materials, but higher film thickness (P < 0.05) and lower radiopacity (P < 0.05). Similarly to AH Plus, the ES were associated with dimensional expansion (P > 0.05) and lower solubility when compared with MTA Fillapex and Sealapex (P < 0.05). None of the endodontic sealers evaluated released formaldehyde after mixing. Conclusion: With the exception of radiopacity, the Portland cement-based experimental endodontic sealers presented physicochemical properties according to the specifications no 57 ANSI/ADA (ADA Professional Product Review, 2008) and ISO 6876 (Dentistry - Root Canal Sealing Materials, 2012, British Standards Institution, London, UK). The sealers had setting times and flow ability that was adequate for clinical use, satisfactory compressive strength and low solubility. Additional studies should be carried out with the purpose of decreasing the film thickness and to determine the ideal ratio of radiopacifying agents in Portland cement-based root canal sealers. © 2013 International Endodontic Journal.

Chemical Modification of Palm Fibres Surface with Zirconium Oxychloride

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Microparticulated and nanoparticulated zirconium oxide added to calcium silicate cement: Evaluation of physicochemical and biological properties

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Radiopacity, pH and antimicrobial activity of Portland cement associated with micro- and nanoparticles of zirconium oxide and niobium oxide

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

Structural and functional characterization of barium zirconium titanate/epoxy composites

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

Effect of zirconium oxide and zinc oxide nanoparticles on physicochemical properties and antibiofilm activity of a calcium silicate-based material

The aim of the present study was to evaluate the antibiofilm activity against Enterococcus faecalis, compressive strength. and radiopacity of Portland cement (PC) added to zirconium oxide (ZrO2), as radiopacifier, with or without nanoparticulated zinc oxide (ZnO).The following experimental materials were evaluated: PC, PC + ZrO2, PC + ZrO2 + ZnO (5%), and PC + ZrO2 + ZnO (10%). Antibiofilm activity was analyzed by using direct contact test (DCT) on Enterococcus faecalis biofilm, for 5 h or 15 h. The analysis was conducted by using the number of colony-forming units (CFU/mL). The compressive strength was performed in a mechanical testing machine. For the radiopacity tests, the specimens were radiographed together with an aluminium stepwedge. The results were submitted to ANOVA and Tukey tests, with level of significance at 5%. The results showed that all materials presented similar antibiofilm activity (

Influence of addition of calcium oxide on physicochemical properties of Portland cement with zirconium or niobium oxide

Context: Calcium oxide (CaO) may be added to mineral trioxide aggregate (MTA) or Portland cement (PC) to improve physicochemical and biological properties. Aims: To evaluate the physicochemical properties of PC associated with radiopacifiers and CaO. Materials and Methods: MTA Angelus, PC + 30% zirconium oxide (Zr), or 30% niobium oxide (Nb) associated with 10 or 20% of CaO were evaluated. Gilmore needles were used to evaluate initial and final setting time. Compressive strength was evaluated after the periods of 24 hours and 21 days. pH was analyzed after 3, 12, 24 hours, 7, 14, 21 days. Solubility and flow tests were performed based on the ISO 6876. The data obtained were submitted to analysis of variance and Tukey tests (P ≤ 0.05). Results: The associations with 10% CaO showed greater strength that the associations with 20% CaO. The shortest initial setting time was observed for the association PC + Zr + 20% CaO and MTA. All the cements presented alkaline pH. The flow of all cements was similar. The highest solubility was found in the associations with 20% CaO. Conclusion: The addition of CaO to PC favored the alkaline property and the PC + Zr + 20% CaO presented setting time similar to MTA.

Chemical characterization and bioactivity of epoxy resin and Portland cement-based sealers with niobium and zirconium oxide radiopacifiers

The purpose of this study was to characterize and to evaluate the bioactivity potential of experimental root canal sealers (ES) based on Portland cement, epoxy resin with nano- and micro-particles of niobium or zirconium oxide used as radiopacifiers in comparison to AH Plus and MTA Fillapex. Methods Specimens of the sealers (10 mm in diameter × 1 mm thick) were prepared and the radiopacity was evaluated according to ISO 6876 (2012) specifications. Characterization of the sealers was performed under the scanning electron microscope (SEM) immediately after setting and after immersion for 28 days in Hank's balanced salt solution (HBSS). In addition X-ray energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy were also performed. The pH and calcium ion release were measured after 1, 7, 14, 21 and 28 days after completion of seating using a digital pH meter and an atomic absorption spectrophotometer, respectively. Results The experimental sealers exhibited an average radiopacity of 2.5 mm thickness of aluminum, which was similar to MTA Fillapex (P > 0.05) and inferior to AH Plus (P < 0.05). AH Plus did not show bioactivity. Although the experimental sealers did not exhibit the formation of hydration product, they encouraged the deposition of crystalline spherical structures of calcium deficient phosphate. The highest pH and calcium release values were observed with the experimental sealers (P < 0.01). ES-Nb-micro was the only sealer to present hexagonal shaped crystal deposition. Significance Novel root canal sealers based on a mixture of Portland cement, epoxy resin and radiopacifier exhibited a degree of bioactivity although no evidence of cement hydration was demonstrated on material characterization. The radiopacifier particle size had limited effect on the sealer microstructure and chemical properties.

Zirconium-methacrylate oxoclusters as new hybrid materials for the modification of epoxy systems

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Dynamical Elastic Moduli of the Ti-13Nb-13Zr biomaterial alloy by mechanical spectroscopy

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

Effect of heavy interstitials on anelastic properties of Nb-1.0 wt% Zr alloys

The mechanical properties of metals with bcc structure, such as niobium and its alloys, have changed significantly with the introduction of heavy interstitial elements. These interstitial elements (nitrogen, for example), present in the alloy, occupy octahedral sites and constitute an elastic dipole of tetragonal symmetry and might produce anelastic relaxation. This article presents the effect of nitrogen on the anelastic properties of Nb-1.0 wt% Zr alloys, measured by means of mechanical spectroscopy using a torsion pendulum. The results showed complex anelastic relaxation structures, which were resolved into their constituent peaks, representing each relaxation process. These processes are due to stress-induced ordering of the interstitial elements around the niobium and zirconium of the alloy.