Grain size effect on the structural and dielectric properties of Pb0.85La0.15TiO3 ferroelectric ceramic compound

This paper presents a study of the influence of particle size on the structural and dielectric properties of Pb0.85La0.15TiO3 (PLT15) ferroelectric ceramic samples. The samples were prepared with average grain size of 1.69 +/- 0.08 mu m and 146 +/- 8 nm using, respectively, conventional and spark plasma sintering techniques. A decrease in the tetragonality degree as the crystallite size decreased was explained by an internal stress caused by the existence of a large amount of grain boundaries. The local structure exhibited no significant modification and the dielectric measurements showed a diffuse phase transition and a reduction in the permittivity magnitude at T-m as the average grain size decreased. The nanostructured ceramic sample prepared at a relatively lower temperature and sintering time presented a dielectric constant value of approximately 2000 at room temperature. (c) 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Effect of different surfactants on the shape, growth and photoluminescence behavior of MnWO4 crystals synthesized by the microwave-hydrothermal method

In this communication, we report the effect of different surfactants [cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulfate (SDS) and sodium bis(2-ethylhexyl)sulfosuccinate (AOT)] on the shape, growth and photoluminescence (PL) behavior of manganese tungstate (MnWO4) crystals synthesized by the microwave-hydrothermal (MH) method at 413 K for 45 min. These crystals were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), ultraviolet-visible (UV-vis) absorption spectroscopy and PL measurements. XRD patterns proved that these crystals have a monoclinic structure. FE-SEM images showed that MnWO4 crystals exhibit different shapes and growth mechanisms depending on the surfactant employed. The CTAB cationic surfactant promotes the hindrance of small nuclei that leads to the formation of flake-like nanocrystals, while SDS and AOT anionic surfactants promote a growth of crystals to plate-like and leaf-like crystals due to considerable size effect of counter-ions (RSO4- and RSO2O-) and an increase in Na+ ion remnants. UV-vis absorption spectroscopy revealed different optical band gap values due to modifications in the shape, surface and crystal size. Finally, the effect of surfactants on the crystal shapes and average crystal size distribution causing changes in the PL behavior of MnWO4 crystals was explained. (C) 2011 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.

Evaluation of the micro-hardness and fracture toughness of amorphous and partially crystallized 3CaO center dot P2O5-SiO2-MgO bioglasses

In this work, the effect of the indentation load on the results of hardness and fracture toughness, determined by Vickers micro-hardness measurements, of some glasses and glass-ceramics has been investigated. Furthermore, in order to verify the effect of crystallinity on the results, glasses of composition 52.75 wt.% 3CaO center dot P2O5, 30 wt.% SiO2 and 17.25 wt.% MgO were fused at 1600 degrees C for 4 h and annealed at 700 degrees C for 2h, and further heat-treated at 700, 775, 800 and 900 degrees C for 4h. The obtained materials were analyzed by high resolution X-ray diffraction, HRXRD, to determine the crystallization degree in function of the heat-treatment temperature. The hardness of the different specimens was determined by Vickers' micro-hardness measurements under various loads. It has been observed that with increasing crystallization of the materials their hardness increased. Furthermore, it has been possible to verify the so-called indentation size effect (ISE), i.e. hardness decreases as the indentation depth, under higher loads, increases. This effect has been more pronounced in the glass-ceramic samples. Fracture toughness has been determined by the crack length induced by the Vickers indentations and relating them to the applied loads. Glass materials presented a fracture pattern with characteristics of cleavage, forming cracks of the half-penny shaped type, while the glass-ceramic materials exhibited crack bridging effects and Palmqvist type cracks. (C) 2011 Elsevier B.V. All rights reserved.

beta-ZnMoO4 microcrystals synthesized by the surfactant-assisted hydrothermal method: Growth process and photoluminescence properties

In this communication, we investigate the effect of different surfactants: cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulfate (SDS) and polyvinylpyrrolidone (PVP-K40) on the growth process of zinc molybdate (beta-ZnMoO4) microcrystals synthesized under hydrothermal conditions at 140 degrees C for 8 h. These microcrystals were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and photoluminescence (PL) measurements. XRD patterns proved that these crystals are monophasic and present a wolframite-type monoclinic structure. FE-SEM images revealed that the surfactants modified the crystal shapes, suggesting the occurrence of distinct crystal growth processes. The CTAB cationic surfactant promotes the hindrance of small nuclei that leads to the formation of rectangle-like crystals, SDS anionic surfactant induces a growth of irregular hexagons with several porous due to considerable size effect of counter-ions on the crystal facets, PVP-K40 non-ionic surfactant allows a reduction in size and thickness of plate-like crystals, while without surfactants have the formation of irregular plate-like crystals. Finally, the PL properties of beta-ZnMoO4 microcrystals were explained by means of different shape/size, surface defects and order-disorder into lattice. (C) 2011 Elsevier B.V. All rights reserved.

Effect of pre-flaring and file size on the accuracy of two electronic apex locators

Objective: This ex vivo study evaluated the effect of pre-flaring and file size on the accuracy of the Root ZX and Novapex electronic apex locators (EALs). Material and methods: The actual working length (WL) was set 1 mm short of the apical foramen in the palatal root canals of 24 extracted maxillary molars. The teeth were embedded in an alginate mold, and two examiners performed the electronic measurements using #10, #15, and #20 K-files. The files were inserted into the root canals until the "0.0" or "APEX" signals were observed on the LED or display screens for the Novapex and Root ZX, respectively, retracting to the 1.0 mark. The measurements were repeated after the pre-flaring using the S1 and SX Pro-Taper instruments. Two measurements were performed for each condition and the means were used. Intra-class correlation coefficients (ICCs) were calculated to verify the intra-and inter-examiner agreement. The mean differences between the WL and electronic length values were analyzed by the three-way ANOVA test (p<0.05). Results: ICCs were high (>0.8) and the results demonstrated a similar accuracy for both EALs (p>0.05). Statistically significant accurate measurements were verified in the pre-flared canals, except for the Novapex using a #20 K-file. Conclusions: The tested EALs showed acceptable accuracy, whereas the pre-flaring procedure revealed a more significant effect than the used file size.

Effect of the relationship between particle size, inter-particle distance, and metal loading of carbon supported fuel cell catalysts on their catalytic activity

The effect of the relationship between particle size (d), inter-particle distance (x(i)), and metal loading (y) of carbon supported fuel cell Pt or PtRu catalysts on their catalytic activity, based on the optimum d (2.5-3 nm) and x(i)/d (>5) values, was evaluated. It was found that for y < 30 wt%, the optimum values of both d and x(i)/d can be always obtained. For y >= 30 wt%, instead, the positive effect of a thinner catalyst layer of the fuel cell electrode than that using catalysts with y < 30 wt% is concomitant to a decrease of the effective catalyst surface area due to an increase of d and/or a decrease of x(i)/d compared to their optimum values, with in turns gives rise to a decrease in the catalytic activity. The effect of the x(i)/d ratio has been successfully verified by experimental results on ethanol oxidation on PtRu/C catalysts with same particle size and same degree of alloying but different metal loading. Tests in direct ethanol fuel cells showed that, compared to 20 wt% PtRu/C, the negative effect of the lower x(i)/d on the catalytic activity of 30 and 40 wt% PtRu/C catalysts was superior to the positive effect of the thinner catalyst layer.