Study of the potentiometric response of the doped spinel Li1.05Al0.02Mn1.98O4 for the optimization of a selective lithium ion sensor

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Síntese e caracterização de óxidos de zinco e de magnésio suportados em A1SBA-15 para produção de biodiesel

To overcome the challenge of meeting growing energy demand in a sustainable way, biodiesel has shown very promising as alternative energy can replace fossil fuels, even partially. Industrially, the biodiesel is produced by homogeneous transesterification reaction of vegetable oils in the presence of basic species used as catalysts. However, this process is the need for purification of the esters obtained and the removal of glycerin formed after the reaction. This context, the alternative catalysts have that can improve the process of biodiesel production, aiming to reduce costs and facilitate its production. In this study, the AlSBA-15 support with Si / Al ratio = 50 was synthesized, as like as the heterogeneous catalysts of zinc oxide and magnesium supported on mesoporous AlSBA-15 silica, in the concentrations of 5, 10, 15 and 30 %, relative to the support. The textural properties and structural characterization of catalysts and supports were determined by techniques: X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) coupled to the chemical analyzer, adsorption / desorption of N2, thermal analysis (TG / DTG), absorption spectroscopy in the infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). Characterization results indicated that the support AlSBA-15 retained the hexagonal ordered after the incorporation of zinc oxide and magnesium oxide in the holder. For heterogeneous catalysts, ZnO-AlSBA-15, that was observed the presence of zinc oxide nanoparticles dispersed in the surface and interior channels of the mesoporous and microporous support. The catalytic activity was evaluated by the transesterification reaction of sunflower oil via methylic route, and some reaction parameters were optimized with the most active catalyst in biodiesel production by sunflower oil. For the series of heterogeneous catalysts, the sample with 30 % ZnO supported on AlSBA-15 showed a better conversion of triglyceride to methyl esters, about 95.41 % of reaction conditions: temperature 175 °C, with molar ratio of 42:1, stirring at 200 rpm and under a pressure of 14 bar for 6 h. The catalyst MgO-AlSBA-15 showed no catalytic activity in the studied reactions

Evaluation of the radiopacity of calcium hydroxide- and glass-ionomer-based root canal sealers

Aim To evaluate the radiopacity of calcium hydroxide-based root canal sealers (Acroseal, Sealapex and Sealer 26), a glass-ionomer-based sealer (Activ GP Sealer) and a zinc oxide and eugenol-based sealer (Intrafill).Methodology Five disc-shaped specimens (10 x 1 mm) were fabricated from each material, according to the International Organization for Standardization (ISO) 6876/2001 standard. After setting of the materials, radiographs were taken using occlusal films and a graduated aluminum step-wedge varying from 2 to 16 mm in thickness. The dental X-ray unit (GE1000) was set at 50 Kvp, 10 mA, 18 pulses s(-1) and distance of 33.5 cm. The radiographs were digitized and the radiopacity compared with that of the aluminum step-wedge, using WIXWIN-2000 software (Gendex). Data (mm Al) were submitted to ANOVA and Tukey test.Results Intrafill was the most radiopaque material (7.67 mm Al) followed by Sealer 26 (6.33 mm Al), Sealapex (6.05 mm Al) and Acroseal (4.03 mm Al). Activ GP was the least radiopaque material (1.95 mm Al, P < 0.05).Conclusions The sealers evaluated in this study had different radiopacities. However, except for the glass-ionomer-based sealer, all materials had radiopacity values above the minimum recommended by the ISO standard.

Nanostructure and properties of ZnO films produced by the pyrosol process

Indium doped ZnO films were deposited by the pyrosol process on glass substrates at different temperatures from solutions containing In/Zn molar ratios up to 10%. The nanostructure of the films was investigated using grazing-incidence small angle X-ray scattering (GISAXS). The mass density was determined by X-ray reflectivity and the composition by X-ray photoelectron spectroscopy. The GISAXS measurements revealed an anisotropic pattern for films deposited at 573 and 623 K and a isotropic one for those deposited at higher temperatures. The anisotropic patterns indicate the presence of elongated nanopores with their long axes perpendicular to the film surface. In contrast, the isotropic nature of GISAXS patterns of films grown at high temperatures (673 and 723 K) suggests the presence of spherical voids. The pore size distribution function determined from the isotropic patterns indicates a multimodal size distribution. on the other hand, the measured mass density of the doped films with isotropic nanotexture is higher than that of the anisotropic films while the electric resistivity is significantly lower. This is in agreement with the detected strong reduction of the void density and specific surface area at approximately constant pore size.

In situ and simultaneous nanostructural and spectroscopic studies of ZnO nanoparticle and Zn-HDS formations from hydrolysis of ethanolic zinc acetate solutions induced by water

The simultaneous formation of nanometer sized zinc oxide (ZnO), and acetate zinc hydroxide double salt (Zn-HDS) is described. These phases, obtained using the sol-gel synthesis route based on zinc acetate salt in alcoholic media, were identified by direct characterization of the reaction products in solution using complementary techniques: nephelometry, in situ Small-Angle X-ray Scattering (SAXS), UV-Vis spectroscopy and Extended X-ray Absorption Fine Structures (EXAFS). In particular, the hydrolytic pathway of ethanolic zinc acetate precursor solutions promoted by addition of water with the molar ratio N = [H2O]/[Zn2+] = 0.05 was investigated in this paper. The aim was to understand the formation mechanism of ZnO colloidal suspension and to reveal the factors responsible for the formation of Zn-HDS in the final precipitates. The growth mechanism of ZnO nanoparticles is based on primary particle (radius approximate to 1.5 nm) rotation inside the primary aggregate (radius < 3.5 nm) giving rise to an epitaxial attachment of particles and then subsequent coalescence. The growth of second ZnO aggregates is not associated with the Otswald ripening, and could be associated with changes in equilibrium between solute species induced by the superficial etching of Zn-HDS particles at the advanced stage of kinetic.

Effect of reaction time on the particle size of ZnO and ZnO : Ce obtained by a sol-gel method

In this work particles of ZnO of size range 33-56 Angstrom were prepared by a sol-gel method. The effect of reaction time on the particle size of ZnO or ZnO:Ce was investigated by transmission electron microscopy measurements, UV-vis absorption and luminescence spectroscopy. A linear increase of the mean particle size is observed as a function of reaction time. The cerium-doped particles are bigger than the pure ZnO ones obtained at the same reaction time. A shift to lower energy at the maximum of the bands is observed in all absorption, emission and excitation spectra as a function of particle growth. From the absorption spectra the optical energy gap values (Eg) for these particles were determined. In the quantum size regime, Eg was found to decrease with particle growth.

Microwave Hydrothermal Synthesis and Photocatalytic Performance of ZnO and M:ZnO Nanostructures (M = V, Fe, Co)

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

Relative bioavailability of zinc in supplemental inorganic and organic sources for Nile tilapia Oreochromis niloticus fingerlings

A 90-day feeding experiment was conducted with sex reversed Nile tilapia (Oreochromis niloticus) fingerlings fed purified or practical diets supplemented with different zinc sources to evaluate fish growth performance and zinc and iron retention in fish bones, fillets, liver, skin and eyes. The relative bioavailability value (RBV) of zinc in the supplemental sources tested was also calculated. Fish were fed with isonitrogenous and isoenergetic purified or practical diets supplemented with 150 mg Zn kg -1, as zinc sulphate monohydrate (ZnSO 4), zinc oxide (ZnO) or zinc amino acid complex (Zn-AA). The feeding trial was conducted in 30, 50 L aquaria where four 0.66 ± 0.01 g (mean ± SD) fingerlings were initially stocked. No significant differences were observed for any growth performance variables (P > 0.05). In practical diets, only ZnSO 4 and ZnO presented bone zinc retention similar to that for the standard zinc source. Zinc concentration in the bone of fish fed practical diet supplemented with Zn-AA (171 ± 3.62 μg g -1) was significantly lower than that verified for the practical diets supplemented with the standard zinc source (200 ± 17.7 μg g -1) or with ZnSO 4 (204 ± 19.9 μg g -1). Assuming the concentration of zinc in bones as the response criterion, the supplemental zinc RBV from ZnSO 4 (105%) was higher than the RBV for Zn-AA (95.1%) or ZnO (94.9%). Iron concentration in the bones of animals fed the non-zinc-supplemented purified diet was significantly higher than that observed for purified diet supplemented with Zn-AA (P < 0,05). The results of the present work allowed us to conclude that ZnSO 4 in relation to ZnO or Zn-AA was the supplemental zinc source with higher zinc bioavailability to Nile tilapia. © 2005 Blackwell Publishing Ltd.

Apparent absorption of zinc from supplemental inorganic and organic sources to Nile tilapia Oreochromis niloticus juveniles

Nile tilapia Oreochromis niloticus fingerlings were fed with purified or practical diets, supplemented with 150 Ing Zn/kg, from different sources. Dry matter (DM), crude protein (CP), ether extract (EE), and gross energy (GE) apparent digestibility coefficients (ADC), as well as zinc, copper, calcium, and phosphorus apparent absorption coefficients (AAC) were determined by the addition of 0.1% chromic oxide to the diets. The supplemental zinc sources utilized were commercial grade zinc sulfate monohydrate (ZnSO 4), zinc oxide (ZnO) and a zinc amino acid complex (Zn-AA). Analytical grade zinc sulfate heptahydrate was also utilized as a standard reference zinc source. There was a significant difference between purified (74.9%) and practical (41.3%) zinc AAC for the ZnO supplemented diets (P < 0.05). The supplemental zinc sources presented similar AAC when purified diets were utilized. However, ZnSO 4 was the best supplemental zinc source when practical type diets were used. There were no significant differences between supplemental zinc AAC from ZnS0 4 (68.9%), and supplemental zinc AAC from Zn-AA (61.3%) in practical diets, but Zn-AA diet showed a statistically lower zinc AAC when compared with the standard zinc source diet (75.6%). The practical diet supplemented with ZnO had the worst supplemental zinc AAC (41.3%). Dietary copper (74.21%), calcium (70.9%), and phosphorus (71.9%) AAC of the practical diets supplemented with ZnO were statistically lower (P < 0.05) than the respective AAC of the practical ZnSO 4 supplemented diets (83.6%, 84.1%, 87.1%).The ADC of the practical ZnO supplemented diet for DM (76.3%), CP (88.6%), EE (82.4%), and GE (81.6%) were statiscally lower than the respective ADC of the ZnSO 4 practical diet (86.0, 92.7, 93.6, 89.6%, respectively) and those ADC of the Zn-AA practical diet (84.7, 92.7, 93.7, 88.2%, respectively) (P < 0.05). Hence, these results indicate that ZnSO 4 and Zn-AA have equivalent intestinal absorption as supplemental zinc sources for Nile tilapia juveniles and both are superior to ZnO. © Copyright by the World Aquaculture Society 2005.

SnO 2 ceramics with low electrical resistivity obtained by microwave sintering

The main aim of this study was to develop dense and conducting SnO 2 ceramics without precipitated phases on the grain boundaries, which was verified using field emission scanning microscopy (FE-SEM) coupled with an energy-dispersive X-ray spectroscopy (FE-SEM/EDS). Two sample groups were investigated, where the first sample group was doped with zinc while the second one was doped with cobalt. The ceramics were prepared using the oxides mixture method and the sintering was carried out in a conventional muffle oven as well as in microwave oven. The results obtained were found to be similar regarding the relative density for the two sintering methods while time and temperature gains were observed for the microwave sintering method. The relative densities obtained were nearly 95%, for the two sintering methods. Concerning the electrical characterization measurements-electric field x current density as well as the environment temperature, the ceramics obtained through the conventional sintering method presented non-ohmic behavior. For the microwave sintered ceramics, we observed an ohmic behavior with electrical resistivity of 1.3 Ωcm for the samples doped with ZnO/Nb 2O 5 and 2.5 Ωcm for that of the samples doped with CoO/Nb 2O 5. The FE-SEM/EDS results for the microwave sintered ceramics indicated a structure with a reduced number of pores and other phases segregated at the grain boundaries, which leads to a better conductive ceramic than the conventional oven sintered samples. The dilatometry analysis determined the muffle sintering temperature and the difference between the densification of cobalt and zinc oxides. The addition of niobium oxide resulted in the decrease in resistivity, which thus led us to conclude that it is possible to obtain dense ceramics with low electrical resistivity based on SnO 2 using commercial oxides by the oxides mixture technique and the microwave oven sintering method. Copyright © 2011 American Scientific Publishers All rights reserved.

Supplementation of diets for Santa Ines sheep with organic and inorganic zinc sources

This research was conducted with objective to evaluate the effect of different zinc (Zn) sources and doses in the diet for Santa Ines sheep. Forty lambs at weaning, with 18.4 kg of body weight were supplemented with three different sources of zinc (zinc oxide (ZnO), zinc amino acid and zinc proteinate) and three doses of zinc (200, 400 and 600 mg/kg DM) added to the basal diet. At every 28 days, animals were weighted and blood samples were collected for analyses of zinc (Zn), alkaline phosphatase and immunoglobulin G (IgG) and M (IgM). At the end of experiment, liver samples were collected for determination of the hepatic zinc levels. Zinc was analyzed with atomic absorption spectrophotometer, while phosphatase alkaline and immunoglobulins G and M were analyzed using Laborlab and Bioclin kits, respectively. There was no effect of diets on phosphatase alkaline levels and hepatic zinc, but there was difference in the plasmatic zinc levels and IgG and IgM levels. Based on the accumulation of hepatic zinc, the estimate of the zinc bioavailability, through the regression equation, showed that supplementation with organic and inorganic sources of zinc did not differ in the diet of Santa Ines sheep. © 2012 Sociedade Brasileira de Zootecnia.

XAS/WAXS time-resolved phase speciation of chlorine LDH thermal transformation: Emerging roles of isovalent metal substitution

The XAS/WAXS time-resolved method was applied for unraveling the complex mechanisms arising from the evolution of several metastable intermediates during the degradation of chlorine layered double hydroxide (LDH) upon heating to 450 °C, i.e., Zn2Al(OH)6·nH2O, ZnCuAl(OH)6·nH2O, Zn2Al 0.75Fe0.25(OH)6·nH2O, and ZnCuAl0.5Fe0.5(OH)6·nH2O. After a contraction of the interlamellar distance, attributed to the loss of intracrystalline water molecules, this distance experiences an expansion (T > 175-225 °C) before the breakdown of the lamellar framework around 275-295 °C. Amorphous prenucleus clusters with crystallo-chemical local order of zinc-based oxide and zinc-based spinel phases, and if any of copper-based oxide, are formed at T > 175-225 °C well before the loss of stacking of LDH layers. This distance expansion has been ascribed to the migration of Zn II from octahedral layers to tetrahedral sites in the interlayer space, nucleating the nano-ZnO or nano-ZnM2O4 (M = Al or Fe) amorphous prenuclei. The transformation of these nano-ZnO clusters toward ZnO crystallites proceeds through an agglomeration process occurring before the complete loss of layer stacking for Zn2Al(OH)6· nH2O and Zn2Al0.75Fe0.25(OH) 6·nH2O. For ZnCuAl(OH)6·nH 2O and ZnCuAl0.5Fe0.5(OH)6· nH2O, a cooperative effect between the formation of nano-CuO and nano-ZnAl2O4 amorphous clusters facilitates the topochemical transformation of LDH to spinel due to the contribution of octahedral CuII vacancy to ZnII diffusion. © 2013 American Chemical Society.

Photo-Induced Conductivity of Heterojunction GaAs/Rare-Earth Doped SnO2

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

SeP hole injection layer for devices based on organic materials

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

An investigation into the influence of zinc precursor on the microstructural, photoluminescence, and gas-sensing properties of ZnO nanoparticles

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)