Photoluminescence in ZrO2 doped with Y and La

O objetivo deste trabalho é descrever a síntese e a caracterização óptica de uma solução sólida de óxido de zircônio contendo ítrio e lantânio. Foram misturados citrato de zircônio, nitrato de ítrio e nitrato de lantânio nas proporções 94 mol% ZrO2-6 mol% Y2O3 e 92 mol% ZrO2-6 mol % Y2O3-2 mol % La2O3. A análise de espectroscopia de absorção no infravermelho com tranformada de Fourier mostra material orgânico em decomposição e a análise térmica mostra a transformação de fases da zircônia tetragonal para monoclínica, a perda de água e a desidroxilação do zircônio. A análise por difração de raios X mostra formação de fases homogênea de ZrO2-Y2O3-La2O3 demonstrando que a adição de lantânio não provoca formação de fases, promovendo uma solução sólida baseada em zircônia cúbica. Os espectros de fotoluminescência mostram bandas de absorção em 562 nm e 572 nm (350 ºC) e bandas de absorção específicas em 543 nm, 561 nm, 614 nm e 641 nm (900 ºC). O efeito fotoluminescente a baixas temperaturas é causado por defeitos como (Y Zr,Y O)', (2Y Zr,V O)'' e V O. As emissões em 614 nm e 641 nm são causadas pela transição O-2p -> Zr-4d. Uma emissão em 543 nm pode ser atribuída a centros LaO8 com transição O-2p -> La-5d.

Influência do uso do forno de microondas ou convencional na síntese de ZrO2

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Demulsification of water/sunflower oil emulsions by a tangential filtration process using chemically impregnated ceramic tubes

A tangential filtration process was implemented in this study using porous ceramic tubes made of alpha-alumina produced by the slip-casting technique. These tubes were sintered at 1450 degrees C and characterized by mercury intrusion porosimetry, which revealed a mean pore size of 0.5 mu m. The tubes were chemically impregnated with a zirconium citrate solution, after which they were calcined and heat treated at temperatures of up to 600 and 900 degrees C to eliminate volatile organic compounds and transform the zirconium citrate into zirconium oxide impregnated in the alumina in the form of nanoparticle agglomerates. The microporous pipes were tested on a microfiltration hydraulic system to analyze their performance in the demulsification of sunflower oil and water mixtures. The fluid-dynamic parameters of Reynolds number and transmembrane pressure were varied in the process. The volume of permeate was analyzed by measuring the Total Organic Carbon concentration (TOC), which indicated 99% of oil phase retention. The emulsified mixture was characterized by optical microscopy, while the morphology and composition of the impregnated microporous tubes were analyzed by scanning electron microscopy (SEM). Quantification of the TOC values for the tube impregnated once at 600 degrees C showed the best demulsification performance, with the concentration on permeate smaller than 10 mg/L. The impregnated tube sintered once at 900 degrees C presented low carbon concentration (smaller than 20 mg/L), has the advantage of presenting the greatest trans-membrane flux in relation to the other microporous tube. (c) 2006 Elsevier B.V. All rights reserved.

Mechanochemical synthesis of barium titanate

A powder mixture of BaO and TiO2, was mechanochemically treated in a planetary ball mill in an air atmosphere for up to 4 h, using zirconium oxide vial and zirconium oxide balls as the milling medium. Mechanochemical reaction leads to the gradual formation of BaTiO3 phase. Phase evolution during synthesis and changes in powder size and morphology were monitored by XRD, DSC, IR and TEM analysis and it was shown that the formation of BaTiO3 phase was initiated after 60 min. Extended time of milling directed to formation of higher amount of BaTiO3 perovskite phase. Barium titanate with good crystallinity was formed after 240 min sintering without pre-calcination step was performed at 1330 degrees C for 2 It within heating rate 10 degrees C/min. (c) 2005 Elsevier Ltd. All rights reserved.

Reflux synthesis and hydrothermal processing of ZrO2 nanopowders at low temperature

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Active planar waveguides based on sol-gel Er3+-doped SiO2-ZrO2 for photonic applications: Morphological, structural and optical properties

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

Study of Structure and Properties of Bi4Ti3O12 Prepared by Mechanochemical Syntheses

Bi4Ti3O12 powder was synthesized from bismuth oxide and titanium oxide. Mixture of oxides was milled in zirconium oxide jar in the planetary ball-mill during 1, 3 and 6 h. Extended time of milling directed to formation of higher amount of titanates perovskite phase. Bi4Ti3O12 was formed between 1 and 3 h of milling time. The phase formation of Bi4Ti3O12, crystal structure and powder particle size were followed by XRD, Raman spectroscopy and SEM analysis. After milling for various times the powders were compacted by pressing and isothermal sintering. Sample milled for 3 h and subsequently sintered at 1000C for 24 h exhibit a hysteresis loop, confirming that the synthesized material possesses ferroelectric properties. All results affect that the structure Bi4Ti3O12 is strongly dependent on the milling time.

Microtensile bond strength of a resin cement to glass infiltrated zirconia-reinforced ceramic: The effect of surface conditioning

This study evaluated the effect of three surface conditioning methods on the microtensile bond strength of resin cement to a glass-infiltrated zirconia-reinforced alumina-based core ceramic. Thirty blocks (5×5×4 mm) of In-Ceram Zirconia ceramics (In-Ceram Zirconia-INC-ZR, VITA) were fabricated according to the manufacturer's instructions and duplicated in resin composite. The specimens were polished and assigned to one of the following three treatment conditions (n=10): (1) Airborne particle abrasion with 110 μm Al2O3 particles + silanization, (2) Silica coating with 110 μm SiOx particles (Rocatec Pre and Plus, 3M ESPE) + silanization, (3) Silica coating with 30 μm SiOx particles (CoJet, 3M ESPE) + silanization. The ceramic-composite blocks were cemented with the resin cement (Panavia F) and stored at 37 °C in distilled water for 7 days prior to bond tests. The blocks were cut under coolant water to produce bar specimens with a bonding area of approximately 0.6 mm2. The bond strength tests were performed in a universal testing machine (cross-head speed: 1 mm/min). The mean bond strengths of the specimens of each block were statistically analyzed using ANOVA and Tukey's test (α≤0.05). Silica coating with silanization either using 110 μm SiOx or 30 μm SiOx particles increased the bond strength of the resin cement (24.6±2.7 MPa and 26.7±2.4 MPa, respectively) to the zirconia-based ceramic significantly compared to that of airborne particle abrasion with 110-μm Al2O3 (20.5±3.8 MPa) (ANOVA, P<0.05). Conditioning the INC-ZR ceramic surfaces with silica coating and silanization using either chairside or laboratory devices provided higher bond strengths of the resin cement than with airborne particle abrasion using 110 μm Al2O3. © 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

Adhesive cementation of zirconia posts to root dentin: Evaluation of the mechanical cycling effect

This study evaluated the effect of mechanical cycling on the bond strength of zirconia posts to root dentin. Thirty single-rooted human teeth were transversally sectioned to a length of 16 mm. The canal preparation was performed with zirconia post system drills (CosmoPost, Ivoclar) to a depth of 12 mm. For post cementation, the canals were treated with total-etch, 3-steps All-Bond 2 (Bisco), and the posts were cemented with Duolink dual resin cement (Bisco). Three groups were formed (n = 10): G1 - control, no mechanical cycling; G2 - 20,000 mechanical cycles; G3 - 2,000,000 mechanical cycles. A 1.6-mm-thick punch induced loads of 50 N, at a 45° angle to the long axis of the specimens and at a frequency of 8 Hz directly on the posts. To evaluate the bond strengths, the specimens were sectioned perpendicular to the long axis of the teeth, generating 2-mm-thick slices, approximately (5 sections per teeth), which were subjected to the push-out test in a universal testing machine at a 1 mm/min crosshead speed. The push-out bond strength was affected by the mechanical cycling (1-way ANOVA, p = .0001). The results of the control group (7.7 ± 1.3 MPa) were statistically higher than those of G2 (3.9 ± 2.2 MPa) and G3 (3.3 ± 2.3 MPa). It was concluded that the mechanical cycling damaged the bond strength of zirconia posts to root dentin.

Effect of different radiopacifying agents on the physicochemical properties of white portland cement and white mineral trioxide aggregate

Introduction: The aim of this study was to evaluate the pH, calcium ion release, setting time, and solubility of white mineral trioxide aggregate (WMTA) and white Portland cement (WPC) combined with the following radiopacifying agents: bismuth oxide (BO), calcium tungstate (CT), and zirconium oxide (ZO). Methods: Fifty acrylic teeth with root-end filling material were immersed in ultrapure water for measurement of pH and calcium release (atomic absorption spectrophotometry) at 3, 24, 72, and 168 hours. For evaluation of setting time, each material was analyzed according to the American Society for Testing and Materials guidelines 266/08. The solubility test was performed according to American National Standards Institute/American Dental Association specification no. 57/2000. Solubility, setting time, and pH values were compared by using analysis of variance and Tukey test, and the values of calcium release were compared by the Kruskal-Wallis and Miller tests. The significance level was set at 5%. Results: The pH and calcium release were higher at 3 and 24 hours. WPC was the material with the higher values for both properties. WMTA had the greatest solubility among all materials (P <.05). All radiopacifiers increased the setting time of WPC, and WMTA had the shortest setting time among all materials (P < .05). Conclusions: All materials released calcium ions. Except for WPC/CT at 168 hours, all materials promoted an alkaline pH. On the basis of the obtained results, ZO and CT can be considered as potential radiopacifying agents to be used in combination with Portland cement. Copyright © 2012 American Association of Endodontists.

Effect of air-particle abrasion protocols on the biaxial flexural strength, surface characteristics and phase transformation of zirconia after cyclic loading

This study evaluated the effect of air-particle abrasion protocols on the biaxial flexural strength, surface characteristics and phase transformation of zirconia after cyclic loading. Disc-shaped zirconia specimens (Ø: 15mm, thickness: 1.2mm) (N=32) were submitted to one of the air-particle abrasion protocols (n=8 per group): (a) 50μm Al2O3 particles, (b) 110μm Al2O3 particles coated with silica (Rocatec Plus), (c) 30μm Al2O3 particles coated with silica (CoJet Sand) for 20s at 2.8bar pressure. Control group received no air-abrasion. All specimens were initially cyclic loaded (×20,000, 50N, 1Hz) in water at 37°C and then subjected to biaxial flexural strength testing where the conditioned surface was under tension. Zirconia surfaces were characterized and roughness was measured with 3D surface profilometer. Phase transformation from tetragonal to monoclinic was determined by Raman spectroscopy. The relative amount of transformed monoclinic zirconia (FM) and transformed zone depth (TZD) were measured using XRD. The data (MPa) were analyzed using ANOVA, Tukey's tests and Weibull modulus (m) were calculated for each group (95% CI). The biaxial flexural strength (MPa) of CoJet treated group (1266.3±158A) was not significantly different than that of Rocatec Plus group (1179±216.4A,B) but was significantly higher than the other groups (Control: 942.3±74.6C; 50μm Al2O3: 915.2±185.7B,C). Weibull modulus was higher for control (m=13.79) than those of other groups (m=4.95, m=5.64, m=9.13 for group a, b and c, respectively). Surface roughness (Ra) was the highest with 50μm Al2O3 (0.261μm) than those of other groups (0.15-0.195μm). After all air-abrasion protocols, FM increased (15.02%-19.25%) compared to control group (11.12%). TZD also showed increase after air-abrasion protocols (0.83-1.07μm) compared to control group (0.59μm). Air-abrasion protocols increased the roughness and monoclinic phase but in turn abrasion with 30μm Al2O3 particles coated with silica has increased the biaxial flexural strength of the tested zirconia. © 2013 Elsevier Ltd.

Air-particle abrasion on zirconia ceramic using different protocols: Effects on biaxial flexural strength after cyclic loading, phase transformation and surface topography

This study evaluated the effect of different air-particle abrasion protocols on the biaxial flexural strength and structural stability of zirconia ceramics. Zirconia ceramic specimens (ISO 6872) (Lava, 3M ESPE) were obtained (N=336). The specimens (N=118, n=20 per group) were randomly assigned to one of the air-abrasion protocols: Gr1: Control (as-sintered); Gr2: 50 μm Al2O3 (2.5 bar); Gr3: 50 μm Al2O3 (3.5 bar); Gr4: 110 μm Al2O3(2.5 bar); Gr5: 110 μm Al2O3 (3.5 bar); Gr6: 30 μm SiO2 (2.5 bar) (CoJet); Gr7: 30 μm SiO2(3.5 bar); Gr8: 110 μm SiO2 (2.5 bar) (Rocatec Plus); and Gr9: 110 μm SiO2 (3.5 bar) (duration: 20 s, distance: 10 mm). While half of the specimens were tested immediately, the other half was subjected to cyclic loading in water (100,000 cycles; 50 N, 4 Hz, 37 °°C) prior to biaxial flexural strength test (ISO 6872). Phase transformation (t→m), relative amount of transformed monoclinic zirconia (FM), transformed zone depth (TZD) and surface roughness were measured. Particle type (p=0.2746), pressure (p=0.5084) and cyclic loading (p=0.1610) did not influence the flexural strength. Except for the air-abraded group with 110 μm Al2O3 at 3.5 bar, all air-abrasion protocols increased the biaxial flexural strength (MPa) (Controlnon-aged: 1030±153, Controlaged: 1138±138; Experimentalnon-aged: 1307±184-1554±124; Experimentalaged: 1308±118-1451±135) in both non-aged and aged conditions, respectively. Surface roughness (Ra) was the highest with 110 μm Al2O3(0.84 μm. FM values ranged from 0% to 27.21%, higher value for the Rocatec Plus (110 μm SiO2) and 110 μm Al2O3 groups at 3.5 bar pressure. TZD ranged between 0 and 1.43 μm, with the highest values for Rocatec Plus and 110 μm Al2O3 groups at 3.5 bar pressure. © 2013 Elsevier Ltd.

Citotoxicidade e ação antimicrobiana do cimento Portland associado a diferentes agentes radiopacificadores

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estudo da formação de espumas cerâmicas à base de zircônio a partir do processo sol-gel

Pós-graduação em Química - IQ