Influence of barium and strontium addition on the ratio c/a of PZT obtained by the polymeric precursor method

Lead zirconate titanate powder, with Zr/Ti ratio of 50/50 was prepared by Pechini method after adding up to 10,0 mol% of Ba +2 and Sr +2 ions. Tetragonal phase is favored by the increase of barium and strontium concentration in the LiNbO 3 crystal lattice. The ratio c/a for tetragonal phase increases with the content of Ba +2 and Sr +2.

Evaluation of interface characterization and adhesion of glass ceramics to commercially pure titanium and gold alloy after thermal- and mechanical-loading

Objectives. This study evaluated the effect of thermal- and mechanical-cycling on the shear bond strength of three low-fusing glassy matrix dental ceramics to commercial pure titanium (cpTi) when compared to conventional feldspathic ceramic fused to gold alloy.Methods. Metallic frameworks (diameter: 5 min, thickness: 4 mm) (N = 96, n = 12 per group) were cast in cpTi and gold alloy, airborne particle abraded with 150 mu m aluminum oxide. Low-fusing glassy matrix ceramics and a conventional feldspathic ceramic were fired onto the alloys (thickness: 4mm). Four experimental groups were formed; Gr1 (control group): Vita Omega 900-Au-Pd alloy; Gr2: Ticeram-cpTi; Gr3: Super Porcelain Ti-22-cpTi and G4: Vita Titankeramik-cpTi. While half of the specimens from each ceramic-metal combination were randomly tested without aging (water storage at 37 C for 24h only), the other half were first thermocycled (6000 cycles, between 5 and 55 C, dwell time: 13 s) and then mechanically loaded (20,000 cycles under SON load, immersion in distilled water at 37 C). The ceramic-alloy interfaces were loaded under shear in a universal test machine (cross-head speed: 0.5 mm/min) until failure occur-red. Failure types were noted and the interfaces of the representative fractured specimens from each group were examined with stereo microscope and scanning electron microscope (SEM). in an additional study (N = 16, n = 2 per group), energy dispersive X-ray spectroscopy (EDS) analysis was performed from ceramic-alloy interfaces. Data were analyzed using ANOVA and Tukey's test.Results. Both ceramic-metal combinations (p < 0.001) and aging conditions (p < 0,001) significantly affected the mean bond strength values. Thermal- and mechanical-cycling decreased the bond strength (MPa) results significantly for Gr3 (33.4 +/- 4.2) and Gr4 (32.1 +/- 4.8) when compared to the non-aged groups (42.9 +/- 8.9, 42.4 +/- 5.2, respectively). Gr1 was not affected significantly from aging conditions (61.3 +/- 8.4 for control, 60.7 +/- 13.7 after aging) (p > 0.05). Stereomicroscope images showed exclusively adhesive failure types at the opaque ceramic-cpTi interfacial zone with no presence of ceramic on the substrate surface but with a visible dark titanium oxide layer in Groups 2-4 except Gr1 where remnants of bonder ceramic was visible. EDS analysis from the interfacial zone for cpTi-ceramic groups showed predominantly 34.5-85.1% O(2) followed by 1.1-36.7% Aland 0-36.3% Si except for Super Porcelain Ti-22 where a small quantity of Ba (1.4-8.3%), S (0.7%) and Sn (35.3%) was found. In the Au-Pd alloy-ceramic interface, 56.4-69.9% O(2) followed by 15.6-26.2% Si, 3.9-10.9% K, 2.8-6% Na, 4.4-9.6% Al and 0-0.04% Mg was observed.Significance. After thermal-cycling for 6000 times and mechanical-cycling for 20,000 times, Triceram-cpTi combination presented the least decrease among other ceramic-alloy combinations when compared to the mean bond strength results with Au-Pd alloy-Vita Omega 900 combination. (c) 2008 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Radiative association of Ti and O atoms

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Analysis of Ca-PZT powder obtained by the Pechini and partial oxalate methods

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Sintering and characterization of PLZT (9/65/35)

PLZT(9/65/35) obtained by association between the Pechini method (ZT) and partial oxalate (PLZT) was prepared. The stoichiometric phase and monophasic (cubic) PLZT obtained by calcination did not occur after sintering. The sintering process, by using two stages, caused a liquid phase formation due to a PbO excess (5 and 10 wt%). Samples with high density (similar to 8 g/cm(3)) and optical transparency(similar to 12%) were obtained. However, an equilibrium between the excess of PbO of sample/atmosphere PbO leads to a segregated PbO phase on the boundaries of the microstructure. A diffusion of Zr, Ti and La ions from PLZT to PbO phase promoted a stoichiometric deviation of the matrix and modified the optical and dielectric characteristics. (C) 2000 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

The effect of isostructural seeding on the microstructure and piezoelectric properties of PZT ceramics

Pechini's method was used to prepare lead titanate zirconate with Zr/Ti ratio equal to 53/47. X-ray diffraction data revealed the presence of a rhombohedral phase, rich in zirconium, due to difference in carbonate stabilities, in PZT ceramics calcined at 600 degrees C. Infrared spectroscopy presented COO- bonds in the 1400 cm(-1) region, which disappeared after calcining at 700 degrees C. Seeds with rhombohedral (PZT 57/43) or tetragonal structure (PZT 45/55) were added to the precursor. The microstructure was differentially influenced by the nature of seed particles. Rhombohedral nuclei promoted preferential crystallization of lead zirconate. This heterogeneity directly reflected on values of k(p) and d(33). (C) 1999 Elsevier B.V. Limited and Techna S.r.l. All rights reserved.

Titanium and zirconium complexes containing sterically hindered hydrotris(pyrazolyl)borate ligands: synthesis, structural characterization, and ethylene polymerization studies

The synthesis, characterization and ethylene polymerization behavior of a set of Tp'MCl3 complexes (4, M = Ti, Tp' HB(3-neopentyl-pyrazolyl)(3)(-) (Tp(NP)); 5, M = Ti, Tp'= HB(3-tert-butyl-pyrazolyl)(3)(-) (Tp(tBu)); 6, M = Ti, Tp' = HB(3-phenyl-pyrazolyl)(3)(-) (Tp(Ph)); 7, M = Zr, Tp' = HB(3-phenyl-pyrazolyl)(3)(-) (Tp(ph)); 8, M = Zr, Tp' = HB(3-tert-butyl-pyrazolyl)(3)(-) (Tp(tBu))) is described. Treatment of these tris(pyrazolyl)borate Group IV compounds with methylalumoxane (MAO) generates active catalysts for ethylene polymerization. For the polymerization reactions performed in toluene at 60 degreesC and 3 atm of ethylene pressure, the activities varied between 1.3 and 5.1 X 10(3) g of PE/mol[M](.)h. The highest activity is reached using more sterically open catalyst precursor 4. The viscosity-average molecular weights ((M-v) over bar) of the PE's produced with these catalyst precursors varying from 3.57 to 20.23 x 10(5) gmol(-1) with melting temperatures in the range of 127-134 degreesC. Further polymerization studies employing 7 varying Al/Zr molar ratio and temperature of polymerization showed that the activity as well as the polymer properties are dependent on these parameters. In that case, higher activity was attained at 60 degreesC. The viscosity-average molecular weights of the polyethylene's decreases with increasing AI/Zr molar ratio. (C) 2003 Elsevier B.V. All rights reserved.

Electronic structure of Pb1-xLaxTiO3 ferroelectric materials from Ti 2p and O 1s soft x-ray absorption spectroscopy

The electronic structure of Pb1-xLaxTiO3 (PLT) compounds for x ranging from 0 to 30 at. % of La is investigated by means of soft x-ray absorption near edge structure (XANES) at the Ti L-3,L-2 and O K edges. The greatest modification in the structure of the Ti 2p XANES spectra of the PLT compounds is observed in the region of the high energy peak of the L-3 edge (e(g) states), which exhibits a splitting in the undoped sample. As the amount of lanthanum increases, this splitting becomes less pronounced. This modification is interpreted as a decrease in the degree of disorder of titanium atoms, which is correlated to the substitution of Pb by La atoms. The structural changes observed at the low energy peaks of the O K-edge XANES spectra of the PLT compounds may be interpreted in terms of hybridization between O 2p, Ti 3d, and Pb 6p orbitals. A decrease in the degree of hybridization observed as Pb atoms are replaced by La atoms may be related to the differences in the ferroelectric properties observed between x=0.0 and x=0.30 compounds. (c) 2006 American Institute of Physics.

Otimização das propriedades fotoluminescentes de nanoestruturas preparadas via síntese hidrotérmica assistida por micro-ondas

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Local structure and hybridization states in Ba0.9Ca0.1Ti1-xZrxO3 ceramic compounds: Correlation with a normal or relaxor ferroelectric character

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

Modeling the dielectric response of lanthanum modified lead zirconate titanate ferroelectric ceramics-an approach to the phase transitions in relaxor ferroelectrics

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

Dielectric and ferroelectric characteristics of barium zirconate titanate ceramics prepared from mixed oxide method

Barium zirconium titanate (BZT) ceramics were prepared by mixed oxide method. X-ray diffraction showed the presence of a single phase while Raman scattering confirmed structural transitions as a function of different Zr/Ti ratio. The addition of Zr strongly influenced the crystal structure and electrical properties of the ceramics. A typical hysteresis loops were observed for all investigated compositions. BZT ceramics with 15 mol% Zr have shown a ferroelectric to paraelectric transition at around 77 degrees C. (C) 2007 Published by Elsevier B.V.

Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid

Anatase nanoparticles were obtained through a modified sol-gel route from titanium isopropoxide modified with acetic acid in order to control hydrolysis and condensation reactions. The modification of Ti(O(i)Pr)(4) with acetic acid reduces the availability of groups that hydrolyze and condense easily through the formation of a stable complex whose structure was determined to be Ti(OCOCH(3))(O(i)Pr)(2) by means of FTIR and (13)C NMR. The presence of this complex was confirmed with FTIR in the early stages of the process. A doublet in 1542 and 1440 cm(-1) stands for the asymmetric and symmetric stretching vibrations of the carboxylic group coordinated to Ti as a bidentate ligand. The gap of 102 cm(-1) between these signals suggests that acetate acts preferentially as a bidentate rather than as a bridging ligand between two titanium atoms. The use of acetic acid as modifier allows the control of both the degree of condensation and oligomerization of the precursor and leads to the preferential crystallization of TiO(2) in the anatase phase. A possible reaction pathway toward the formation of anatase is proposed on the basis of the intermediate species present in a 1:1 Ti(O(i)Pr)(4):CH(3)COOH molar system in which esterification reactions that introduce H(2)O into the reaction mixture were seen to be negligible. The Rietveld refinement and TEM analysis revealed that the powder is composed of isotropic anatase nanocrystallites.

Hyperfine interaction measurements on ceramics: PZT revisited

The solid solution of PbZr1-xTixO3, known as lead-zirconate titanate (PZT), was probably one of the most studied ferroelectric materials, especially due to its excellent dielectric, ferroelectric and piezoelectric properties. The highest piezoelectric coefficients of the PZT are found near the morphotropic phase boundary (MPB) (0.46 <= x <= 0.49), between the tetragonal and rhombohedral regions of the composition-temperature phase diagram. Recently, a new monoclinic phase near the MPB was observed, which can be considered as a bridge between PZT's tetragonal and rhombohedral phases. This work is concerned with the study of the structural properties of the ferroelectric PZT (Zr/Ti = 52/48, 53/47) by hypertine interaction (HI) measurements obtained from experiments performed by using the nuclear spectroscopy time differential perturbed angular correlation (TDPAC) in a wide temperature range. (c) 2006 Elsevier B.V. All rights reserved.

Electrical characterization of lead zirconate titanate prepared by organic solution route

Two series of lead zirconate titanate (PZT) ceramics with composition Zr/Ti approximate to 53/47 have been prepared by the organic solution route. The effects on the electrical properties of calcination temperature in one series and of sintering time period in the other were examined. Dielectric constant, electrical conductivity and impedance spectroscopy results differed from one series to the other, probably due to differences in structure of the precursor powders, as seen by X-ray diffraction. Tetragonal and rhombohedral phases predominate in the powders used, respectively, in the calcined and sintered series. Physical and electrical behavior of ceramics prepared from predominantly rhombohedral powder suggests the evaporation of PbO. The presence of two semi-circles in impedance plots leads to the association of the low frequency semi-circle to the presence of PbO, which, apparently, was not eliminated from ceramics prepared from predominantly tetragonal powder. (C) 2001 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.