Effect of ultrasonic treatment on surface crystallization of calcium bismuth borate glasses

Transparent glasses in CaO-Bi2O3-B2O3 system were fabricated via the conventional melt-quenching technique. X-ray powder diffraction (XRD) and differential thermal analysis (DTA) carried out on the as-quenched samples confirmed their amorphous and glassy nature respectively. The surface crystallization behaviour of these glasses with and without ultrasonic surface treatment (UST) was monitored using XRD, optical microscopy and scanning electron microscopy (SEM). The volume fraction, depth of crystallization and the (001) orientation factor for the heat treated samples with and without UST were compared. The ultrasonically-treated samples on subsequent heat treatment were found to crystallize at lower temperatures associated with the highest degree of orientation factor (0.95) in contrast with those of non-UST samples. These surface crystallized glasses were found to exhibit nonlinear optical behaviour emitting green light (532 nm) when they were exposed to the infrared radiation (1064 nm) using Nd:YAG laser.

Host dependent frequency upconversion of Er3+-doped oxyfluoride germanate glass

Er3+-doped oxyfluoride germanate glasses have been synthesized by the conventional melting and quenching method. The Judd-Ofelt intensity parameters were calculated based on the Judd-Ofelt theory and absorption spectra measurements. With the substitution of PbF2 for PbO, the Omega(2) parameter decreases, while the Omega(6) parameter increases. These change trends indicate that fluoride anions come to coordinate erbium cations and the covalency of the Er-O bond decreases. Structural and thermal stability properties were obtained by Raman spectra and differential thermal analysis, indicating that PbF2 plays an important role in the formation of glass network and has an important influence on the maximum phonon energy and thermal stability of host glasses. Intense green and red emissions centered at 525, 546, and 657 nm, corresponding to the transitions H-2(11/2) -> I-4(15/2), S-4(3/2) -> I-4(15/2), and F-4(9/2) -> I-4(15/2), respectively, were simultaneously observed at room temperature. With increasing PbF2 content, the intensity of red (657nm) emissions increases significantly, while that of the green (525 and 546nm) emission increases slightly. The results indicate that PbF, has more influence on the red (657nm) emission than the green (525 and 546nm) emissions in oxyfluoride germanate glasses. The possible upconversion luminescence mechanisms have also been estimated and discussed. (c) 2005 Elsevier B.V. All rights reserved.

Composition dependent frequency upconversion luminescence in Er3+-doped oxychloride germanate glasses

Er3+ -doped oxychloride germanate glasses have been synthesized by conventional melting and quenching method. Structural and thermal stability properties were obtained based on the Raman spectra and differential thermal analysis, indicating that PbCl2 plays an important role in the formation of glass network and has an important influence on the maximum phonon energy and thermal stability of host glasses. Intense green and red emissions centered at 525, 546, and 657 nm, corresponding to the transitions H-2(11/2) -> I-4(15/2), S-4(3/2) -> I-4(15/2), and F-4(9/2) -> I-4(15/2), respectively, were observed at room temperature. With increasing PbCl2 content, the intensity of green (525 and 546 nm) emissions increases significantly, while the red (657 nm) emission increases slowly. The results indicate that PbCl2 has more influence on the green emissions than the red emission in oxychloride germanate glasses. The possible upconversion luminescence mechanisms has also been estimated and discussed. (c) 2005 Elsevier Ltd. All rights reserved.

Avaliação de complexos de inclusão na inibição do aço carbono em meio ácido

A indústria de petróleo e gás apresenta sérios problemas relacionados à corrosão. Nas petroquímicas e nas instalações de refino de petróleo, as falhas em materiais estão relacionadas com a corrosão, além disso, os processos de corrosão de metais são problemas no mundo, causando ônus em processos industriais e gerando situações de risco como a corrosão de pilares metálicos em pontes ou em fuselagens de aviões. Dentre os meios corrosivos, um muito comum é o meio ácido, que será o meio estudado neste trabalho. Com todos os problemas citados, se faz necessário o estudo de inibidores de corrosão com alta eficiência, estabilidade e que, preferencialmente, não agridam o meio ambiente. Alguns inibidores de corrosão apresentam solubilidade limitada em água, sendo necessária a utilização de alguns solventes não tão amigáveis ao meio ambiente. Então, propôs-se formar um complexo de inclusão para tornar possível a solubilização de inibidores convencionais em solução aquosa, como algumas tioureias, que apresentam solubilidade limitada em água. Essa completa solubilização do inibidor de corrosão orgânico em meio aquoso é possível com a utilização de um aditivo (hospedeiro) capaz de encapsular tais moléculas (convidados) via interações não covalentes, de modo a alcançar o máximo desempenho de inibição. Para a formação do complexo de inclusão foi usado como molécula hospedeira, a α e a β hidroxipropilciclodextrina e como molécula convidada a dibenziltioureia. A intenção foi testar a melhora da ação inibidora da corrosão do aço carbono em meio de HCl 1mol.L-1 com ensaios de perda de massa, de impedância, polarização e microscopia eletrônica de varredura (MEV), além de evidenciar a formação destes complexos de inclusão através da espectroscopia de absorção vibracional no infravermelho, espectroscopia de RMN de 1H, espectroscopia de absorção no Ultra-violeta e análise térmica diferencial (DTA)

Studies on the magnetism of cobalt ferrite nanocrystals synthesized by hydrothermal method

Fe-Co/CoFe2O4 nanocomposite and CoFe2O4 nanopowders were prepared by the hydrothermal method. The structure of magnetic powders were characterized by X-ray diffraction diffractometer (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), thermal gravity analysis (TGA) and differential thermal analysis (DTA) analysis, X-ray photoelectron spectrometry (XPS), and Fourier transform infrared spectra (FTIR) techniques, while magnetic properties were determined by using a vibrating sample magnetometer (VSM) at room temperature.

Tunable Luminescence in Monodisperse Zirconia Spheres

In this article, monodisperse spherical zirconia (ZrO2) particles with a narrow size distribution were prepared by the controlled hydrolysis of zirconium butoxide in ethanol, followed by heat treatment in air at low temperature from 300 to 500 degrees C. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric and differential thermal analysis (TG/DTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), photoluminescence (PL) spectra, kinetic decay, and electron paramagnetic resonance were used to characterize the samples. The experimental results indicate that the annealed ZrO2 samples exhibit broad, intense visible photoluminescence. The annealing temperature is indispensable for the luminescence of the obtained ZrO2 particles. The emission colors of the ZrO2 samples can be tuned from blue to nearly white to dark orange by varying the annealing temperature.

A study of NiZnCu-ferrite/SiO2 nanocomposites with different ferrite contents synthesized by sol-gel method

Ni0.65Zn0.35Cu0.1Fe1.9O4/SiO2 nanocomposites with different weight percentages of NiZnCu-ferrite dispersed in silica matrix were successfully fabricated by the sol-gel method using tetraethylorthosilicate (TEOS) as a precursor of silica, and metal nitrates as precursors of NiZnCu ferrite. The thermal decomposition process of the dried gel was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The obtained Ni0.65Zn0.35Cu0.1Fe1.9O4/SiO2 nanocomposites were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM), Mossbauer spectroscopy and vibrating sample magnetometry (VSM). The formation of stoichiometric NiZnCu-ferrite dispersed in silica matrix is confirmed when the weight percentage of ferrite is not more than 30%. Samples with higher ferrite content have small amount of alpha-Fe2O3. The transition from the paramagnetic to the ferromagnetic state is observed as the ferrite content increases from 20 to 90wt%.

Luminescent properties of rare-earth-doped CaWO4 phosphor films prepared by the Pechini sol-gel process

CaWO4 phosphor films doped with rare-earth ions (Eu3+, Dy-,(3+) Sm3+, Er3+) were prepared by the Pechini sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, thermogravimetric and differential thermal analysis, atomic force microscopy, and photoluminescence spectra, as well as lifetimes, were used to characterize the resulting powders and films. The results of the XRD analysis indicated that the films began to crystallize at 400degreesC and that the crystallinity increased with elevation of the annealing temperature. The doped rare-earth ions showed their characteristic emissions in crystalline CaWO4 phosphor films due to energy transfer from WO42- groups to them. Both the lifetimes and PL intensities of the doped rare-earth ions increased with increasing annealing temperature, from 500 to 900degreesC, and the optimum concentrations for Eu3+, Dy3+, Sm3+, Er3+ were determined as 30, 1.5, 1.5, 0.5 at.% of Ca2+ in CaWO4 films annealed at 900degreesC, respectively.

TG-DTA properties of new nonlinear optical materials: K(2)Ln(NO3)(5)center dot 2H(2)O (Ln = La, Ce, Pr, Nd, Sm)

Single crystals of K(2)Ln(NO3)(5). 2H(2)O (KLnN) (Ln = La, Ce, Pr, Nd, Sm) were grown from aqueous solution. The thermogravimetric analysis and differential thermal analysis curves of KLnN demonstrate that the processes of dehydration, melting, irreversible phase transformation and decomposition of NO3- take place in sequence in the heating processes (except KCN). There are three stages in the decomposition of NO3- in KLnN (Ln = La, Nd, Sm) while two in KLnN (Ln = Ce, Pr). K(2)Ln(NO3)(5) is formed at about 225 degrees C by the reaction of KNO3 and Ln(NO3)(3). nH(2)O (Ln = La, Ce, Pr, Nd). (C) 2000 Elsevier Science Ltd. All rights reserved.

Síntese de pigmentos cerâmicos inorgânicos nanométricos e encapsulados com estrutura core-shell pela rota dos precursores poliméricos

The present work has as objective the development of ceramic pigments based in iron oxides and cobalt through the polymeric precursor method, as well as study their characteristics and properties using methods of physical, chemical, morphological and optical characterizations.In this work was used iron nitrate, and cobalt citrate as precursor and nanometer silica as a matrix. The synthesis was based on dissolving the citric acid as complexing agent, addition of metal oxides, such as chromophores ions and polymerization with ethylene glycol. The powder obtained has undergone pre-ignition, breakdown and thermal treatments at different calcination temperatures (700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C). Thermogravimetric analyzes were performed (BT) and Differential Thermal Analysis (DTA), in order to evaluate the term decomposition of samples, beyond characterization by techniques such as BET, which classified as microporous materials samples calcined at 700 ° C, 800 º C and 900 º C and non-porous when annealed at 1000 ° C and 1100 º C, X-ray diffraction (XRD), which identified the formation of two crystalline phases, the Cobalt Ferrite (CoFe2O4) and Cristobalite (SiO2), Scanning Electron Microscopy (SEM) revealed the formation of agglomerates of particles slightly rounded;and Analysis of Colorimetry, temperature of 700 °C, 800 °C and 900 °C showed a brown color and 1000 °C and 1100 °C violet

Estudo de massa cerâmica triaxial visando à otimização do ciclo de queima da indústria de cerâmica estrutural

Over recent years the structural ceramics industry in Brazil has found a very favorable market for growth. However, difficulties related to productivity and product quality are partially inhibiting this possible growth. An alternative for trying to solve these problems and, thus, provide the pottery industry the feasibility of full development, is the substitution of firewood used in the burning process by natural gas. In order to contribute to this process of technological innovation, this paper studies the effect of co-use of ceramic phyllite and kaolin waste on the properties of a clay matrix, verifying the possible benefits that these raw materials can give to the final product, as well as the possibility of such materials to reduce the heat load necessary to obtain products with equal or superior quality. The study was divided into two steps: characterization of materials and study of formulations. Two clays, a phyllite and a residue of kaolin were characterized by the following techniques: laser granulometry, plasticity index by Atterberg limits, X-ray fluorescence, X-ray diffraction, mineralogical composition by Rietveld, thermogravimetric and differential thermal analysis. To study the formulations, specifically for evaluation of technological properties of the parts, was performed an experimental model that combined planning involving a mixture of three components (standard mass x phyllite x kaolin waste) and a 23 factorial design with central point associated with thermal processing parameters. The experiment was performed with restricted strip-plot randomization. In total, 13 compositional points were investigated within the following constraints: phyllite ≤ 20% by weight, kaolin waste ≤ 40% by weight, and standard mass ≥ 60% by weight. The thermal parameters were used at the following levels: 750 and 950 °C to the firing temperature, 5 and 15 °C/min at the heating rate, 15 and 45min to the baseline. The results showed that the introduction of phyllite and/or kaolin waste in ceramic body produced a number of benefits in properties of the final product, such as: decreased absorption of water, apparent porosity and linear retraction at burn; besides the increase in apparent specific mass and mechanical properties of parts. The best results were obtained in the compositional points where the sum of the levels of kaolin waste and phyllite was maximal (40% by weight), as well as conditions which were used in firing temperatures of 950 °C. Regarding the prospect of savings in heat energy required to form the desired microstructure, the phyllite and the residue of kaolin, for having small particle sizes and constitutions mineralogical phases with the presence of fluxes, contributed to the optimization of the firing cycle.

Síntese e caracterização de CuNb2O6 e CuNbC através de reação sólido- sólido e gás- sólido a baixa temperatura

The refractory metal carbides have proven important in the development of engineering materials due to their properties such as high hardness, high melting point, high thermal conductivity and high chemical stability. The niobium carbide presents these characteristics. The compounds of niobium impregnated with copper also have excellent dielectric and magnetic properties, and furthermore, the Cu doping increases the catalytic activity in the oxidation processes of hydrogen. This study aimed to the synthesis of nanostructured materials CuNbC and niobium and copper oxide from precursor tris(oxalate) oxiniobate ammonium hydrate through gas-solid and solid-solid reaction, respectively. Both reactions were carried out at low temperature (1000°C) and short reaction time (2 hours). The niobium carbide was produced with 5 % and 11% of copper, and the niobium oxide with 5% of copper. The materials were characterized by X-Ray Diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), X-Ray Fluorescence Spectroscopy (XRF), infrared spectroscopy (IR), thermogravimetric (TG) and differential thermal analysis (DTA , BET and particle size Laser. From the XRD analysis and Rietveld refinement of CuNbC with S = 1.23, we observed the formation of niobium carbide and metallic copper with cubic structure. For the synthesis of mixed oxide made of niobium and copper, the formation of two distinct phases was observed: CuNb2O6 and Nb2O5, although the latter was present in small amounts

Caracterização de matérias-primas regionais e desenvolvimento de formulações de massas cerâmicas para porcelanato

Initially concentrated in some poles at the South and Southeast regions of Brazil, the ceramic tiles industry became wide during the 80 s decade, with a disconcentration industrial and regional pulverization. The competitiveness in the ceramic tiles internal and external consumers markets, it has debtor the industries to invest in sophisticated products each time more, either in design or the technology, but, mainly, in its final properties. Amongst the diverse types of ceramic coating, the porcelanato if has detached had to its process of technological production and excellent characteristics techniques. The Porcelanato is currently the material for coatings that presents the best technical and aesthetic features when compared with others ceramics found on the market. The chemical composition and the others raw materials characteristics have an importance that must to be ally to the inherent characteristics of fabrication process, essentially those related to the cycle of burning. This work had as purpose to develop formularizations of ceramic mass for production of porcelanato without glass coating, pertaining to the group BIa (text of absorption of water ≤ 0.5%) and with resistance superior mechanics 35MPa from raw materials characterized. The ceramic raw materials selected to the development of this study (A1 and A2 clays, feldspate, talc and quartz) were submitted to the following tests: X-ray fluorescence - chemical analysis determination; X-ray diffraction - Analysis of the stages mineralogics; Laser granulometry - size distribution of particles; and Differential thermal analysis - thermal behavior. Were performed tests of absorption of water, lineal retraction of it burns, apparent specific mass and rupture tension the flexing. The results had evidenced that the formularizations that had the A1 clay and talc on its composition were efficient for the porcelanato production remaining their technological characteristics inside of the intervals of variation desired by the Norms of the ABNT

Estudo das propriedades termofísicas com variação da expansibilidade de compósito desenvolvido com matriz PUR-NOP e carga funcional de argilomineral

In this study were conducted experimental procedures for determination of variation of the expandability of rigid polyurethane foam (PUR) from a natural oil polyol (NOP), specifically the Castor oil plant, Ricinus communis, pure and additions of the vermiculite in phase dispersed in different percentage within a range from 0% to 20%, mass replacement. From the information acquired, were defined the parameters for production of bodies of test, plates obtained through controlled expansion, with the final volume fixed. Initially, the plates were subjected to thermal performance tests and evaluated the temperature profiles, to later be extracted samples duly prepared in accordance with the conditions required for each test. Was proceeded then the measurement of the coefficient of thermal conductivity, volumetric capacity heat and thermal diffusivity. The findings values were compared with the results obtained in the tests of thermal performance, contributing to validation of the same. Ultimately, it was investigated the influence that changes in physical-chemical structure of the material had exerted on the variation of thermophysical quantities through gas pycnometry, scanning electron microscopy (SEM) combined with energy dispersive X-ray fluorescence spectroscopy (EDXRF), infrared spectroscopy using Fourier transform (FTIR), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). Based on the results obtained was possible to demonstrate that all load percentage analyzed promoted an increase in the potential expansion (PE) of the resin. In production of the plates, the composites with density near at the free expansion presented high contraction during the cure, being the of higher density adopted as definitive standard. In the thermal performance tests, the heating and cooling curves of the different composites had presented symmetry and values very close for lines of the temperature. The results obtained for the thermophysical properties of composites, showed little difference in respect of pure foam. The percentage of open pores and irregularities in the morphology of the composites were proportionate to the increment of vermiculite. In the interaction between the matrix and dispersed phase, there were no chemical transformations in the region of interface and new compounds were not generated. The composites of PUR-NOP and vermiculite presented thermal insulating properties near the foam pure and percentage significantly less plastic in its composition, to the formulation with 10% of load

Incorporação de cinzas da casca de café na produção de placas cerâmicas para revestimento

Brazil is the world s leading coffee producer. In 2008, 45.99 million of 60 kg bags of benefited coffee were produced. In the process of improvement 50% is grain and 50% is husk, thus, 1.38 million tons of coffee husk are produced annually. The husk is used as combustible in the drying and improvement ovens in the coffee farms, generating ash as residue. These ashes contain a high concentration of alkaline metals and earth metals, mainly K2O and CaO. This work studies the use of this residue in the ceramic tiles industry, as fluxing agents in substitution to the feldspar. Ten mixtures with equal ratios of clay and kaolin, proceeding from Bahia and the residue (varying from 30 to 5%) were defined and produced in uniaxial tool die of 60x20mm with approximately 5 mm of thickness and 45MPa compacting pressure. The samples were fired in four different temperatures: 1100 °C, 1150 °C, 1185 °C and 1200 °C during 60 minutes and characterized by means of X-ray fluorescence, X-ray diffraction, gravimetric thermal analysis and differential thermal analysis. The results of water absorption, apparent porosity, linear shrinkage, XRD, dilatometry, flexural strength and SEM were also analysed. The test specimen with addition of 10% of ash fired in 1200 °C resulted in 0.18% water absorption and 40.77 MPa flexural strength, being classified as porcelain stoneware tiles according to ABNT, UNI and ISO norms