Mechanisms of TL for production of the 230 degrees C peak in natural sodalite

The thermoluminescence (TL) peak in natural sodalite near 230 degrees C which appears only after submitted to thermal treatments and to gamma irradiation has been studied in parallel with electron paramagnetic resonance (EPR) spectrum appearing under the same procedure This study revealed a full correlation between the 230 degrees C TL peak and the eleven hyperfine lines from EPR spectrum In both case the centers disappear at the same temperature and are restored after gamma irradiation A complete model for the 230 C TL peak is presented and discussed In addition to the correlation and TL model specific characteristics of the TL peaks are described (C) 2010 Elsevier B V All rights reserved

Electron paramagnetic resonance and the thermoluminescence emission mechanism of the 280 degrees C peak in natural andalusite crystal

Samples of natural andalusite (Al(2)SiO(5)) crystal have been investigated in terms of thermoluminescence (TL) and electron paramagnetic resonance (EPR) measurements. The TL glow curves of samples previously annealed at 600 degrees C for 30 min and subsequently gamma-irradiated gave rise to four glow peaks at 150, 210, 280 and 350 degrees C. The EPR spectra of natural samples heat-treated at 600 degrees C for 30 min show signals at g = 5.94 and 2.014 that do not change after gamma irradiation and thermal treatments. However, it was observed that the appearance of a paramagnetic center at g=1.882 for the samples annealed at 600 degrees C for 30 min followed gamma irradiation. This line was attributed to Ti(3+) centers. The EPR signals observed at g=5.94 and 2.014 are due to Fe(3+). Correlations between EPR and TL results of these crystals show that the EPR line at g=1.882 and the TL peak at 280 degrees C can be attributed to the same defect center. (C) 2011 Elsevier B.V. All rights reserved.

Correlation between electron paramagnetic resonance and thermoluminescence in natural sodalite

Samples of natural sodalite, Na(8)Al(6)Si(6)O(24)Cl(2), submitted to gamma irradiation and to thermal treatments, have been investigated using the thermoluminescence (TL) and electron paramagnetic resonance (EPR) techniques. Both, natural and heat-treated samples at 500A degrees C in air for 30 min, present an EPR signal around g = 2.01132 attributed to oxygen hole centers. The EPR spectra of irradiated samples show an intense line at g = 2.0008 superimposed by a hyperfine multiplet of 11 lines due to an O(-) ion in an intermediate position with respect to two adjacent Al nuclei. In the TL measurements, the samples were annealed at 500A degrees C for 30 min and then irradiated with gamma doses varying from 0.001 to 20 kGy. All the samples have shown TL peaks at 110, 230, 270, 365, and 445A degrees C. A correlation between the EPR g = 2.01132 line and the 365A degrees C TL peak was observed. A TL model is proposed in which a Na(+) ion acts as a charge compensator when an Al(3+) ion replaces a Si(4+) lattice ion. The gamma ray destruction of the Al-Na complex provides an electron trapped at the Na and a hole trapped at a non-bridging oxygen ion adjacent to the Al(3+) ion.

Thermoluminescence, infrared reflectivity and electron paramagnetic resonance properties of hemimorphite

Silicate mineral hemimorphite has been investigated concerning its TL, IR and EPR properties. A broad TL peak around 180 degrees C and a weaker and narrower peak around 360 degrees C were found in a sample annealed at 600 degrees C for I h and then irradiated. The deconvolution using the CGCD method revealed peaks around 132, 169, 222 and 367 degrees C. The reflectivity measurements showed several bands in the NIR region due to H(2)O, OH and Al-OH complexes. No band was observed in the visible region. The thermal treatments were carried out from similar to 110 to 940 degrees C and dehydration was observed, first causing a diminishing optical absorption in general and the disappearance of water and hydroxyl absorption bands. The EPR spectrum of natural hemimorphite, presented Cu(2+) signals at g = 2.4 and g = 2.1 plus E(1)` signal superposed to Fe(3+) signal around g = 2.0. (C) 2008 Elsevier Ltd. All rights reserved.

Phase change and pyroelectricity in natural hemimorphite

The phase change of a natural hemimorphite sample from Minas Gerais (Brazil) was investigated by two X-ray diffraction (XRD) methods and by near-infrared reflectance spectroscopy. Applying successive thermal treatments, the crystal structure undergoes two orientation conversions. The first one occurs at about 550 degrees C, and it was revealed by the Laue method. Below 500 degrees C, the water molecules were partially expelled without changing the crystal structure. A fact that supports this statement is the sequential disappearance of the water bands at 1400 and 1900 nm by thermal treatment. The second conversion takes place below 939 degrees C. Moreover, at 972 degrees C a phase change to the willemite mineral (alpha-Zn(2)SiO(4)) has been observed. This last conversion was confirmed by the power XRD. In addition, natural hemimorphite displayed a high pyroelectricity, which is related both to the absence of inverse centre and to the presence of molecular water and hydroxyl groups in the crystal structure.

Influence of chromium concentration on the optical-electronic properties of ruby microstructures

Films of amorphous aluminium nitride (AlN) were prepared by conventional radio frequency sputtering of an Al + Cr target in a plasma of pure nitrogen. The Cr-to-Al relative area determines the Cr content, which remained in the similar to 0-3.5 at% concentration range in this study. Film deposition was followed by thermal annealing of the samples up to 1050 degrees C in an atmosphere of oxygen and by spectroscopic characterization through energy dispersive x-ray spectrometry, photoluminescence and optical transmission measurements. According to the experimental results, the optical-electronic properties of the Cr-containing AlN films are highly influenced by both the Cr concentration and the temperature of the thermal treatments. In fact, thermal annealing at 1050 degrees C induces the development of structures that, because of their typical size and distinctive spectral characteristics, were designated by ruby microstructures (RbMSs). These RbMSs are surrounded by a N-rich environment in which Cr(3+) ions exhibit luminescent features not present in other Cr(3+)-containing systems such as ruby, emerald or alexandrite. The light emissions shown by the RbMSs and surroundings were investigated according to the Cr concentration and temperature of measurement, allowing the identification of several Cr(3+)-related luminescent lines. The main characteristics of these luminescent lines and corresponding excitation-recombination processes are presented and discussed in view of a detailed spectroscopic analysis.

Persistent luminescence of Eu(2+) and Dy(3+) doped barium aluminate (BaAl(2)O(4):Eu(2+),Dy(3+)) materials

Polycrystalline Eu(2+) and Dy(3+) doped barium aluminate materials, BaAl(2)O(4):Eu(2+),Dy(3+), were prepared with solid state reactions at temperatures between 700 and 1500 degrees C. The influence of the thermal treatments on the stability, homogeneity and structure as well as to the UV-excited and persistent luminescence of the materials was investigated by X-ray powder diffraction, SEM imaging and infrared spectroscopies as well as by steady state luminescence spectroscopy and persistent luminescence decay curves, respectively. The IR spectra of the materials prepared at 250, 700, and 1500 degrees C follow the formation of BaAl(2)O(4) composition whereas the X-ray powder diffraction of compounds revealed how the hexagonal structure was obtained. The morphology of the materials at high temperatures indicated important aggregation due to sintering. The luminescence decay of the quite narrow Eu(2+) band at ca. 500 nm shows the presence of persistent luminescence after UV irradiation. The dopant (Eu(2+)) and co-clopant (Dy(3+)) concentrations affect the crystallinity and luminescence properties of the materials. (C) 2009 Elsevier B.V. All rights reserved.

Atom probe tomography investigation of heterogeneous short-range ordering in the 'komplex' phase state (K-state) of Fe-18Al (at.%)

We study an Fe-18Al (at.%) alloy after various thermal treatments at different times (24-336 h) and temperatures (250-1100 °C) to determine the nature of the so-called 'komplex' phase state (or "K-state"), which is common to other alloy systems having compositions at the boundaries of known order-disorder transitions and is characterised by heterogeneous short-range-ordering (SRO). This has been done by direct observation using atom probe tomography (APT), which reveals that nano-sized, ordered regions/particles do not exist. Also, by employing shell-based analysis of the three-dimensional atomic positions, we have determined chemically sensitive, generalised multicomponent short-range order (GM-SRO) parameters, which are compared with published pairwise SRO parameters derived from bulk, volume-averaged measurement techniques (e.g. X-ray and neutron scattering, Mössbauer spectroscopy) and combined ab-initio and Monte Carlo simulations. This analysis procedure has general relevance for other alloy systems where quantitative chemical-structure evaluation of local atomic environments is required to understand ordering and partial ordering phenomena that affect physical and mechanical properties.

Beneficiamentos da cinza de casca de arroz residual com vistas à produção de cimento composto e/ou pozolânico

A cinza de casca de arroz é um resíduo agro-industrial decorrente do processo de queima da casca de arroz, sendo largamente encontrada no Rio Grande do Sul, pois, historicamente, este Estado é o maior produtor de arroz no Brasil, com cerca de 45% da produção nacional. Empregada como fonte de energia, a casca de arroz é queimada em diversas empresas; algumas, devido à sua natureza, incorporam a cinza ao produto, mas a maioria não encontra outro destino que não o descarte em forma de aterro, criando, assim, um problema ambiental de poluição do solo, do ar e de rios e córregos. No entanto, devido à presença de elevado percentual de sílica (SiO2) na sua constituição, a cinza de casca de arroz pode ter vários empregos. Na construção civil, pode ser empregada como pozolana, conforme vários estudos já vêm demonstrando. Porém, encontra restrições por motivos como sua cor escura, que confere aos cimentos, argamassas e concretos aos quais é adicionada, uma coloração também escura, e a falta de uniformidade apresentada em termos de características químicas e, principalmente, mineralógicas. A cor escura não é um problema de ordem técnica, mas estética e de aceitação no mercado. Já a composição mineralógica está associada à atividade pozolânica e a falta de uniformidade do material disponível implica na incerteza do grau de reatividade. Este trabalho teve o objetivo de verificar a viabilidade técnica do emprego de cinzas de casca de arroz residuais na confecção de cimentos Portland composto e/ou pozolânico, a partir de beneficiamentos das mesmas, que associam tratamentos físicos, químicos e/ou térmicos, os quais têm como finalidade reverter e/ou minimizar os aspectos negativos citados. Para tanto, foram empregadas três cinzas de casca de arroz, oriundas de diferentes processos de produção e com composições mineralógicas distintas. Após definidos os tratamentos a serem aplicados, através de seleção pelos critérios de cor e composição mineralógica, as cinzas tratadas foram avaliadas quanto à sua pozolanicidade, pelo Índice de Atividade Pozolânica (IAP) da NBR 5752 e também por um IAP alterado, proposto neste trabalho. A produção de cimentos com CCA beneficiada se deu a partir de um cimento base com substituição por CCA, em massa e em diferentes percentuais. Tais cimentos foram avaliados quanto à resistência à compressão, aos tempos de pega, à pozolanicidade e à expansibilidade a quente. A análise dos dados obtidos indica que os tratamentos propostos e/ou a associação deles resultam em beneficio no desempenho das cinzas, em pelo menos um dos vários aspectos considerados. A presente pesquisa permite concluir que as CCA residuais têm potencial para serem empregadas na produção de cimentos, tanto aquelas menos cristalinas, quanto as mais cristalinas. Para tanto, devem ser beneficiadas, sendo pelo menos submetidas a tratamento físico para redução de sua granulometria. Se outros objetivos forem pretendidos, como coloração clara, os tratamentos térmico ou químico podem ser empregados.

Estudo da sinterização do aço inox 316L reforçado com 3% Carbeto de Tântalo - TaC

The present work shows a contribution to the studies of development and solid sinterization of a metallic matrix composite MMC that has as starter materials 316L stainless steel atomized with water, and two different Tantalum Carbide TaC powders, with averages crystallite sizes of 13.78 nm and 40.66 nm. Aiming the metallic matrix s density and hardness increase was added different nanometric sizes of TaC by dispersion. The 316L stainless steel is an alloy largely used because it s high resistance to corrosion property. Although, its application is limited by the low wear resistance, consequence of its low hardness. Besides this, it shows low sinterability and it cannot be hardened by thermal treatments traditional methods because of the austenitic structure, face centered cubic, stabilized mainly in nickel presence. Steel samples added with TaC 3% wt (each sample with different type of carbide), following a mechanical milling route using conventional mill for 24 hours. Each one of the resulted samples, as well as the pure steel sample, were compacted at 700 MPa, room temperature, without any addictive, uniaxial tension, using a 5 mm diameter cylindrical mold, and quantity calculated to obtain compacted final average height of 5 mm. Subsequently, were sintered in vacuum atmosphere, temperature of 1290ºC, heating rate of 20ºC/min, using different soaking times of 30 and 60 min and cooled at room temperature. The sintered samples were submitted to density and micro-hardness analysis. The TaC reforced samples showed higher density values and an expressive hardness increase. The complementary analysis in optical microscope, scanning electronic microscope and X ray diffractometer, showed that the TaC, processed form, contributed with the hardness increase, by densification, itself hardness and grains growth control at the metallic matrix, segregating itself to the grain boarders

Obtenção e caracterização de nanopartículas de argilominerais

Natural nanoclays are of great interest particularly for the production of polymer-based nanocomposites. In this work, kaolinite clays from two natural deposits in the State of the Rio Grande do Norte and Paraiba were purified with thermal treatment and chemical treatments, and characterized. Front to the gotten data, had been proposals methodologies for elimination or reduction of coarse particle texts, oxide of iron and organic substance. These methodologies had consisted of the combination of operations with thermal treatments, carried through in electric oven, and acid chemical attacks with and hydrogen peroxide. The Analyzers Thermogravimetric was used to examine the thermal stability of the nanoclays. The analysis indicated weight losses at temperatures under 110 ºC and over the temperature range of 350 to 550 ºC. Based on the thermal analysis data, the samples were submitted to a thermal treatment at 500 °C, for 8 h, to remove organic components. The X-ray diffraction patterns indicated that thermal treatment under 500 °C affect the basic structure of kaolinite. The BET surface area measurements ranged from 32 to 38 m2/g for clay samples with thermal treatment and from 36 to 53 m2/g for chemically treated samples. Thus, although the thermal treatment increased the surface area, through the removal of organic components, the effect was not significant and chemical treatment is more efficient, not affect the basic structure of kaolinite, to improve particle dispersion. SEM analysis confirms that the clay is agglomerated forming micron-size particles

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

Composição química e digestibilidade da vagem de algarobeira (prosopis juliflora, (sw) dc) submetida a diferentes tratamentos térmicos

The ground pods of mesquite (GPM) was submitted to different thermal treatments for two hours after wanted temperature stabilization, for making of the treatments: A = ground pods of mesquite without heat treatment (approximately 30 degrees C); B = The ground pods of mesquite treated at 60 degrees C; C = The ground pods of mesquite treated at 80 degrees C; D = The ground pods of mesquite treated at 100 degrees C and E = The ground pods of mesquite treated at 120 degrees C. Soon after, samples were collected for accomplishment for chemical analyses and in vitro digestibility. A completely randomized design with three replications was utilized. The DM, CP, NFE, CF, ADF, celluloses, lignin, ash and CE values, did not were affected (P>0.05) by temperature. It was observed a quadratic effect (P<0.01) on the contents of EE, decreasing linear effect (P<0.01) on the CC and increasing linear effect on the NDF (P<0.01) and Hemicellulose (P<0.05) contents. The in vitro dry matter digestibility and the in vitro organic matter digestibility were not affected (P>0.05) by temperature. on the other hand the in vitro protein digestibility level, showed a quadratic effect (P<0.05), decreasing after 54 degrees C.

Síntese de pigmentos cerâmicos inorgânicos nanométricos pela rota dos precursores poliméricos

Considering the constant evolution of technology in growth and the need for production techniques in the ceramics area to move forward together, we sought in this study, the research and development of polymeric precursor method to obtain inorganic ceramic pigments. Method that provides quality to obtain the precursor powders of oxides and pigments at the same time, offers time and cost advantages, such as reproducibility, purity and low temperature heat treatment, control of stoichiometry. This work used chromium nitrate and iron nitrate as precursors. The synthesis is based on the dissolution of citric acid as a complexing agent, addition of metal oxides, such as ion chromophores; polymerization with ethylene glycol and doping with titanium oxide. Passing through precalcination, breakdown, thermal treatments at different temperatures of calcination (700 to 1100 oC), resulting in pigments: green for chromium oxide deposited on TiO2 (CrTiO3) and orange for iron oxide deposited on TiO2 ( FeTiO3). Noticing an increase of opacity with increasing temperature. Were performed thermal analysis (TG and ATD) in order to evaluate its thermodecomposition. The powders were also characterized by techniques such as XRD, revealing the formation of crystalline phases such as iron titanate (FeTiO3) and chrome titanate (CrTiO3), SEM, demonstrating formation of rounded particles for both oxides and Spectroscopy in the UV-Visible Region, verifying the potential variation and chromaticity os pigments. Thus, the synthesized oxides were within the requirements to be applied as pigments and shown to be possible to propose its use in ceramic materials

Superação da dormência de sementes de capim colonião

O objetivo da pesquisa foi o de identificar tratamentos capazes de superar a dormência e elevar a taxa de germinação das sementes de Panicum maximum Jacq., passíveis de utilização visando semeadura a campo. Para tanto, sementes foram submetidas a tratamentos de imersão em H2SO4 (98%, 36N) por 5 minutos, de umedecimento do substrato de germinação com KNO3 (0,2%) e a tratamentos térmicos de 40, 55, 70 e 85OC por períodos de exposição de 5, 10 e 15h, em estufa com circulação forçada de ar. As sementes tratadas foram avaliadas por meio do teste de germinação, finalizado pelo teste de tetrazólio nas sementes não germinadas, bimestralmente, ao longo de 6 meses de armazenamento. Foi constatado que os tratamentos químicos (KNO3 e H2SO4) e térmicos (40, 55, 70 e 85 oC por 5, 10 e 15 h) são eficientes na superação da dormência que, não necessariamente, é revertida em elevação da taxa de germinação. A utilização da temperatura de 40oC reduz a taxa de dormência promovendo elevação na taxa de germinação das sementes.