Ferroelectric and structural instability of (Pb,Ca)TiO3 thin films prepared in an oxygen atmosphere and deposited on LSCO thin films which act as a buffer layer

Structural, microstructural and ferroelectric properties of Pb0.90Ca0.10TiO3 (PCT10) thin films deposited using La0.50Sr0.50CoO3 (LSCO) thin films which serve only as a buffer layer were compared with properties of the thin films grown using a platinum-coated silicon substrate. LSCO and PCT10 thin films were grown using the chemical solution deposition method and heat-treated in an oxygen atmosphere at 700 °C and 650 °C in a tube oven, respectively. X-ray diffraction (XRD) and Raman spectroscopy results showed that PCT10 thin films deposited directly on a platinum-coated silicon substrate exhibit a strong tetragonal character while thin films with the LSCO buffer layer displayed a smaller tetragonal character. Surface morphology observations by atomic force microscopy (AFM) revealed that PCT10 thin films with a LSCO buffer layer had a smoother surface and smaller grain size compared with thin films grown on a platinum-coated silicon substrate. Additionally, the capacitance versus voltage curves and hysteresis loop measurement indicated that the degree of polarization decreased for PCT10 thin films on a LSCO buffer layer compared with PCT10 thin films deposited directly on a platinum-coated silicon substrate. This phenomenon can be described as the smaller shift off-center of Ti atoms along the c-direction 〈001〉 inside the TiO6 octahedron unit due to the reduction of lattice parameters. Remnant polarization (P r ) values are about 30 μC/cm2 and 12 μC/cm2 for PCT10/Pt and PCT10/LSCO thin films, respectively. Results showed that the LSCO buffer layer strongly influenced the structural, microstructural and ferroelectric properties of PCT10 thin films. © 2013 Elsevier Ltd and Techna Group S.r.l.

Soft-chemical synthesis, characterization and humidity sensing behavior of WO3/TiO2 nanopowders

Tungsten oxide/titania (WO3/TiO2) nanopowders were synthesized by the polymeric precursor method which varied the WO3 content between 0 and 10 mol%. The powders were thermally treated in a conventional furnace and their structural, microstructural and electric properties were evaluated by X-ray diffraction (XRD), Raman spectrometry, N 2 physisorption, NH3 chemisorption, temperature-programmed reduction (TPR), X-ray absorption near-edge spectroscopy (XANES) in situ XANES and extended X-ray absorption fine structure spectroscopy (EXAFS) and transmission electron microscopy (TEM). XRD and Raman spectrometry confirmed the homogeneous distribution of an amorphous WO3 phase in the TiO 2 matrix which stabilized the anatase phase through the generation of [TiO5·V0] or [TiO5·V 0] complex sites. Conventional TPR-H2 (temperature programmed reduction) along with XANES TPR-H2 and XANES TPR-EtOH showed that WO3/TiO2 sample reduction occurs through the formation of these complex clusters. Moreover, the addition of WO3 promoted an increase in the surface acidity of doped samples as revealed by NH3 chemisorption. The WO3/TiO2 bulk-ceramic samples were further used to estimate their potential application in a humidity sensor in the range of 15-85% relative humidity. Probable reasons that lead to the different humidity sensor responses of samples were given based on the structural and surface characterizations. Correlation between the sensing performance of the sensor and its structural features are also discussed. Although all samples responded as a humidity sensor, the W2T sample (2 mol% added WO3) excelled for sensitivity due to the increase in acid sites, optimum mean pore size and pore size distribution. © 2013 Elsevier B.V.

Chemical and mineralogical characterization of portuguese ceramic tiles in the historic center of São Luís do Maranhão (Brazil): an approximation of the mineralogy and firing temperature of the raw materials

Nesse trabalho, foram caracterizados, pela primeira vez, azulejos históricos portugueses do Centro Histórico de São Luís (CHSL) do Maranhão. A caracterização foi realizada através dos ensaios de microscopia ótica, difração de raios X (DRX) e análise química, visando ao uso dessa informação para a determinação das possíveis matérias-primas utilizadas na sua fabricação, bem como a provável temperatura de queima desses materiais. Os resultados mostraram que a microestrutura desses materiais é constituída por poros de tamanhos variados, apresentando incrustações de calcita e grãos de quartzo de tamanhos inferiores a 500 µm, distribuídos numa matriz de cor rosa-amarelo, onde foram identificadas, por DRX, as fases minerais calcita, gelhenita, wollastonita, quartzo e amorfo. A partir da informação obtida, é possível inferir que as matérias-primas originais estiveram constituídas, provavelmente, por mistura de argilas caoliníticas (Al₂O₃•2SiO,₂•2H₂O), ricas em carbonatos de cálcio e quartzo ou misturas de argilas caoliniticas, quartzo e calcita. Essas matérias-primas originais não atingiram a temperatura de cocção de 950ºC.

Color and shade parameters of ultramarine zeolitic pigments synthesized from kaolin waste

Ultramarine pigments were successful synthesized from zeolite A obtained from kaolin waste. This waste has been used as an excellent source of silicon and aluminum for zeolite synthesis because of its high kaolinite concentrations and low contents of other accessory minerals. The cost is naturally less than the industrialized product. Color additives (Sulfur and Sodium Carbonate) were mixed with different proportions of zeolite A and further calcined for 5 h at 500 °C. They were characterized by XRD and XRF in addition to visual classification by color and shade. These products show colors from blue to green at different shades, both influenced by the amount of additives and cooling rate after calcination. Thus, a different quantity of the same additives in the same zeolitic matrix provides an increase in the color intensity. Cooling rate after calcination induces the color change which is substantially important in the pigments production.

Synthesis and characterization of zeolite NaP using kaolin waste as a source of silicon and aluminum

The synthesis of zeolite NaP using kaolin waste, from the Amazon region, as a predominant source of silicon and aluminum has been studied. The zeolitisation process occurred in hydrothermal conditions using static autoclaving and the effects of time, temperature, and the Si/Al ratio were investigated. The starting material and the phases formed as reaction products were characterized by XRD, SEM and FTIR. The results showed that pure zeolite NaP is hydrothermally synthesized, at 100 °C for 20 hours, using metakaolin waste material in alkaline medium in presence of additional silica. The XRD and SEM analyses indicate that the synthesized zeolite presents good crystallinity.

Vanadium-doped TiO2 anatase nanostructures: the role of V in solid solution formation and its effect on the optical properties

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

Rapid preparation of alpha-FeOOH and alpha-Fe2O3 nanostructures by microwave heating and their application in electrochemical sensors

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Structural and thermal properties of spray-dried methotrexate-loaded biodegradable microparticles

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effects of aging procedures on the topographic surface, structural stability, and mechanical strength of a ZrO2-based dental ceramic

Objective. To determine the effects of different aging methods on the degradation and flexural strength of yttria-stabilized tetragonal zirconia (Y-TZP)Methods. Sixty disc-shaped specimens (0, 12 mm; thickness, 1.6 mm) of zirconia (Vita InCeram 2000 YZ Cubes, VITA Zahnfabrik) were prepared (ISO 6872) and randomly divided into five groups, according to the aging procedures (n=10): (C) control; (M) mechanical cycling (15,000,000 cycles/3.8 Hz/200N); (T) thermal cycling (6,000 cycles/5-55 degrees C/30 s); (TM) thermomechanical cycling (1,200,000 cycles/3.8 Hz/200N with temperature range from 5 C to 55 C for 60s each); (AUT) 12h in autoclave at 134 degrees C/2 bars; and (STO) storage in distilled water (37 degrees C/400 days). After the aging procedures, the monoclinic phase percentages were evaluated by X-ray diffraction (XRD), and topographic surface analysis was performed by 3D profilometry. The specimens were then subjected to biaxial flexure testing (1 mm/min, load 100 kgf, in water). The biaxial flexural strength data (MPa) were analyzed by 1-way ANOVA and Tukey's test (alpha = 0.05). The data for monoclinic phase percentage and profilometry (Ra) were analyzed by Kruskal-Wallis and Dunn's tests.Results. ANOVA revealed that flexural strength was affected by the aging procedures (p = 0.002). The M (781.6 MPa) and TM (771.3 MPa) groups presented lower values of flexural strength than did C (955 MPa), AUT (955.8 MPa), T (960.8 MPa) and STO (910.4 MPa). The monoclinic phase percentage was significantly higher only for STO (12.22%) and AUT (29.97%) when compared with that of the control group (Kruskal-Wallis test, p = 0.004). In addition, the surface roughnesses were similar among the groups (p = 0.165).Signcance. Water storage for 400 days and autoclave aging procedures induced higher phase transformation from tetragonal to monoclinic; however, they did not affect the flexural strength of Y-TZP ceramic, which decreased only after mechanical and thermomechanical cycling. (C) 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Facile synthesis and characterization of ZrO2 nanoparticles prepared by the AOP/hydrothermal route

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

Experimental and theoretical studies of photoluminescence in Zns obtained by microwave-assisted solvothermal method

A shift of the photoluminescence (PL) emission was observed in ZnS prepared by microwave assisted solvothermal method with the increase of the time in microwave. In this work we reported a study of the optical behavior linking with the structural disorder according to XRD and FEG-TEM results. The reduction of intrinsic defects in the lattice is responsible for the decrease of electronic levels in the band gap changing the PL profile. This effect was confirmed by electronic structure calculations.

Effects of the addition of ions barium on the structural and electrical properties of PZT ceramic

Lead zirconate titanate, with Zr/Ti ratio of 53/47 was prepared by the polymeric precursor method. It was investigated the barium (II) modification at 0.0, 0.2, 0.4 and 0.6 mol% in substitution to the lead (II) cation in A site of perovskite structure. The powder samples were characterized by XRD and the diffraction patterns were used to Rietveld refinement. The percentages of tetragonal and rhombohedral phases and a systematic study of the effect of barium (II) on the morphology and the dielectric properties of PZT were carried out. The results showed that the tetragonal phase is favored and the ceramic density is improved with the barium (II) insertion. The Curie temperature (Tc) is increased besides the slight reduction of dielectric constant (Kc).

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.

Pigments based on Cr and Sb doped TiO2 prepared by microemulsion-mediated solvothermal synthesis for inkjet printing on ceramics

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

A relationship between structural and electronic order-disorder effects and optical properties in crystalline TiO2 nanomaterials

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