Hot-spots during the calcination of MCM-41:a SAXS comparative analysis of a soft mesophase

The phenomenon of microscopic hot-spots, during the calcination of MCM-41, was investigated by quantifying the magnitude of the temperature increase during the calcination of a soft MCM-41 mesophase using a SAXS comparative study. This was performed by thermally treating a soft material that was detemplated via Fenton chemistry followed by equilibrating and drying in a low-surface-tension solvent (n-butanol or N,N-dimethylformamide); these samples have limited structural shrinkage. The resulting samples were thermally treated at increasing temperatures, and the structural shrinkage was compared with that of the directly calcined material. By comparing the structural shrinkage, it was found that the microscopic temperature increase would fall between 190 and 250 C, as deduced from N,N-dimethyl-formamide and n-butanol. The order of magnitude of the temperature increase appears to be consistent with the well-known glow effect. It is, however, substantially higher than the experimentally determined macroscopic temperature increase. Several aspects are discussed to interpret this difference. © 2013 Elsevier B.V.

Thermal detemplation of SBA-15 mesophases. Effect of the activation protocol on the framework contraction

The potential use of the solvothermal extraction (SE) as a preliminary step to calcination for detemplating SBA-15 mesophases is investigated; aiming to reduce the amount of organics to be burnt and thereby the corresponding structural shrinkage. A systematic study was carried out by soxhlet extraction on mesophases hydrothermally aged between 90 and 130 C. The mesophases containing variable amounts of template were then treated by calcination or pyrolysis/calcination. TGA was applied to quantify the template amount after the various treatments. The as obtained materials were characterized by SAXS and Ar ad/desorption for structural and textural information while 1H NMR gave information about the integrity of the as-recycled template. The study shows that solvothermal conditions remove considerably the template, typically from 50 to 10-20 wt.%, mainly extracted from the primary mesopores. Possible reuse of the extracted template is questionable as it is poor in polyethyleneoxide compared to the synthesis block-copolymer, Pluronic P123. For all thermal protocols applied (direct calcination, calcination after solvent-extraction or pyrolysis/calcination after solvent extraction), the thermal shrinkage decreases with the aging temperature; that is consistent with the condensation degree of the silica. For each mesophase, it was found that the thermal shrinkage becomes less pronounced when the material is fully templated; thus the template can serve as structural support or can control the mass transfer of O2 and thereby the oxidation rate of the template burning. © 2013 Elsevier Inc. All rights reserved.

The risk of re-intervention after endovascular aortic aneurysm repair

This thesis studies survival analysis techniques dealing with censoring to produce predictive tools that predict the risk of endovascular aortic aneurysm repair (EVAR) re-intervention. Censoring indicates that some patients do not continue follow up, so their outcome class is unknown. Methods dealing with censoring have drawbacks and cannot handle the high censoring of the two EVAR datasets collected. Therefore, this thesis presents a new solution to high censoring by modifying an approach that was incapable of differentiating between risks groups of aortic complications. Feature selection (FS) becomes complicated with censoring. Most survival FS methods depends on Cox's model, however machine learning classifiers (MLC) are preferred. Few methods adopted MLC to perform survival FS, but they cannot be used with high censoring. This thesis proposes two FS methods which use MLC to evaluate features. The two FS methods use the new solution to deal with censoring. They combine factor analysis with greedy stepwise FS search which allows eliminated features to enter the FS process. The first FS method searches for the best neural networks' configuration and subset of features. The second approach combines support vector machines, neural networks, and K nearest neighbor classifiers using simple and weighted majority voting to construct a multiple classifier system (MCS) for improving the performance of individual classifiers. It presents a new hybrid FS process by using MCS as a wrapper method and merging it with the iterated feature ranking filter method to further reduce the features. The proposed techniques outperformed FS methods based on Cox's model such as; Akaike and Bayesian information criteria, and least absolute shrinkage and selector operator in the log-rank test's p-values, sensitivity, and concordance. This proves that the proposed techniques are more powerful in correctly predicting the risk of re-intervention. Consequently, they enable doctors to set patients’ appropriate future observation plan.

Annotated record of the detailed examination of Mn nodules recovered from the VA04 expedition (R/V Valdivia) in the Pacific Ocean

Twenty-four manganese nodules from the surface of the sea floor and fifteen buried nodules were studied. With three exceptions, the nodules were collected from the area covered by Valdivia Cruise VA 04 some 1200 nautical miles southeast of Hawaii. Age determinations were made using the ionium method. In order to get a true reproduction of the activity distribution in the nodules, they were cut in half and placed for one month on nuclear emulsion plates to determine the alpha-activity of the ionium and its daughter products. Special methods of counting the alpha-tracks resolution to depth intervals of 0.125 mm. For the first time it was possible to resolve zones of rapid growth (impulse growth) with growth rates, s > 50 mm/106 yr and interruptions in growth. With few exceptions the average rate of growth of all nodules was surprisingly uniform at 4-9 mm/10 yr. No growth could be recognized radioactively in the buried nodules. One exceptional nodule has had recent impulse growth and, in the material formed, the ionium is not yet in equilibrium with its daughter products. Individual layers in one nodule from the Indian Ocean could be dated and an average time interval of t = 2600±400 yr was necessary to form one layer. The alternation between iron and manganese-rich parts of the nodules was made visible by colour differences resulting from special treatment of cut surfaces with HCl vapour. The zones of slow growth of one nodule are relatively enriched in iron. Earlier attempts to find paleomagnetic reversals in manganese nodules have been continued. Despite considerable improvement in areal resolution, reversals were not detected in the nodules studied. Comparisons of the surface structure, microstructure in section and the radiometric dating show that there are erosion surfaces and growth surfaces on the outer surfaces of the manganese nodules. The formation of cracks in the nodules was studied in particular. The model of age-dependent nodule shrinkage and cracking surprisingly indicates that the nodules break after exceeding a certain age and/or size. Consequently, the breaking apart of manganese nodules is a continuous process not of catastrophic or discontinuous origin. The microstructure of the nodules exhibits differences in the mechanism of accretion and accretion rate of material, shortly referred to as accretion form. Thus non-directional growth inside the nodules as well as a directional growth may be observed. Those nodules with large accretion forms have grown faster than smaller ones. Consequently, parallel layers indicate slow growth. The upper surfaces of the nodules, protruding into the bottom water appear to be more prone to growth disturbances than the lower surfaces, immersed in the sediment. Features of some nodules show, that as they develop, they neither turned nor rolled. Yet unknown is the mechanism that keeps the nodules at the surface during continuous sedimentation. All in all, the nodules remain the objects of their own distinctive problems. The hope of using them as a kind of history book still seems to be very remote.

Uso da cinza do bagaço da cana-de-açúcar como matéria-prima na substituição dos fundentes para aplicações em porcelanato

The present study aims to evaluate the potential use of bagasse ash from sugar cane (CBC) as a flux, replacing phyllite and/or feldspar in standard industrial mass production of enameled porcelain, verifying the possibility of the CBC contribute to the overall reduction of the coefficient of thermal expansion of the ceramic mass. To this end, as a result of the research, we characterized the raw material components of the standard mass (clay, phyllite, kaolin, feldspar, quartz and talc) and the residue of BCC, by testing by XRF, XRD, AG, DTA and ATG. Specimens (CDP) were manufactured in the dimensions of 100 mm x 50 mm x 8 mm in uniaxial matrix under compaction pressure of 33 MPa, assembled in batches of 3 units subsequently sintered at temperatures of 1150°C to 1210°C by varying the Rating Scale at 10°C, heating and cooling ramp of 50°C/min and 25°C/min, with levels of 1 min, 3 min, 5 min, 8 min, 10 min, 15 min, 30 min and 60 min. analyzing the results of the physical properties of water absorption (WA), linear firing shrinkage (LFS), dilatometric analysis (DTA), flexural strain (SFT) and SEM of the sintered bodies in order to verify the adequacy of CDP to ISO 13006, ISO 10545, NBR 13816 standards; NBR 13817 and NBR 13818. The study showed that the formulations that best suit the requirements of the standards are:. G4 - which was applied in 10% of replacing the CBC phyllite, sintering temperature 1210 ° C for 10 min and porch, and F3 - with application of 7.5% of CBC to replace the feldspar in the sintering temperatures of 1190°C, 1200°C and 1210°C for 10 min and porch. These formulations showed better performance regarding the formation of primary and secondary mullite, with considerable reduction of cracks and pores, meeting the prerequisites of standards for glazed porcelain. The results shows that the use of the CBC as a flux in the preparation of porcelain mass meets standard parameters for the manufacture of the product, and thereby can reduce environmental impact and the cost of production. Therefore, it is recommended to use this residue in the ceramics industry, due to its industrial, commercial and collaborative viability for sustainability.

Estudo da adição de resíduos de quartzitos para obtenção de grés porcelanato

In States of Paraíba (PB) and Rio Grande do Norte (RN), northeast of Brazil, the most significant deposits of non-metallic industrial minerals are pegmatites, quartzites and granites, which are located in Seridó region. Extraction of clay, quartz, micas and feldspars occurs mainly in the cities of Várzea (PB), OuroBranco (RN) and Parelhas (RN). Mining companies working in the extraction and processing of quartzite generate large volumes of waste containing about 90% SiO2 in their chemical composition coming from quartz that is one of the basic constituents of ceramic mass for the production of ceramic coating. Therefore, this work evaluates the utilization of these wastes on fabrication of high-quality ceramic products, such as porcelain stoneware, in industrial scale. Characterization of raw materials was based on XRF, XRD, GA, TGA and DSC analysis, on samples composed by 57% of feldspar, 37% of argil and 6% of quartzite residues, with 5 different colors (white, gold, pink, green and black). Samples were synthesized in three temperatures, 1150°C, 1200°C and 1250°C, with one hour isotherm and warming-up tax of 10°C/min. After synthesizing, the specimens were submit to physical characterization tests of water absorption, linear shrinkage, apparently porosity, density, flexural strain at three points. The addition of 6% of quartzite residue to ceramic mass provided a final product with technological properties attending technical norms for the production of porcelain stoneware; best results were observed at a temperature of 1200°C. According to the results there was a high iron oxide on black quartzite, being their use in porcelain stoneware discarded by ethic and structural question, because the material fused at 1250°C. All quartzite formulations had low water absorption when synthesized at 1200°C, getting 0.1% to 0.36% without having gone through the atomization process. Besides, flexural strain tests overcame 27 MPa reaching the acceptance limits of the European Directive EN 100, at 1200°C synthesizing. Thus, the use of quartzite residues in ceramic masses poses as great potential for the production of porcelain stoneware.

Estudo da incorporação de cinza e chamote gerado pela cerâmica vermelha ao próprio processo industrial

The ceramics industry generates waste at various stages of that process, defective products, waste from burning solid fuels, among others. This waste is dumped in landfills, garbage dumps or directly on roads, which has a negative environmental impact. This paper presents a study to incorporate the waste of algaroba wood and chamote (scrap pieces of ceramic already sintered), in to the ceramic material for making sealing blocks. The methodological procedures consist in the characterization of chemical and mineralogical residues, raw materials, and physical-mechanical of the formulations of mixes with clay, silt and waste. By pressing test pieces were produced using a pressure of 200 kgf/cm², varying compositions in the range of 0%, 5%, 10% and 15% by weight of residue. The sintering was performed in a muffle furnace, with the temperature levels of 850 ° C, 900 ° C, 950 ° C, 1000 ° C and 1050 ° C. The evaluated physical and mechanical properties were: Water Absorption, Linear Shrinkage Burning, Apparent Porosity, Apparent Density and Mechanical Resistance to Flexion. Analysis was carried out by Scanning Electron Microscopy on fracture surfaces of the specimens. Evaluation of linear shrinkage property drying and firing , water absorption and mechanical resistance to compression of the sealing blocks 5% wood ash residue, sintered at 900 °C hold temperature in the laboratory the products manufactured on an industrial scale. The main results, it was found on the viability of using the residues of algaroba wood and to confer refractory properties of the ceramic product. The main results, it was concluded feasibility of using the ash residues algaroba wood to impart refractory properties to the ceramic product and the residue of chamote, being derived from the own ceramic product not interfere with the properties, when used in a percentage of up to 5%.Since the residue of chamote being derived from the ceramic product itself had no effect on the properties. Studies in the laboratory have shown that the incorporation of up to 5% of these residues may be adopted as an alternative technology to reduce the environmental impact caused by the industrial sector, without compromising the final properties of the material, since the results on an industrial scale showed absorption values 11.66 and 11.74 of water and waste products respectively, within the parameters of NBR - 15,270, since the mechanical strength was 1.25 MPa and 0.94 MPa respectively for products with and without residue, lower than the minimum required by the technical standard that is 1.5 MPa.

Estudo da incorporação de cinza e chamote gerado pela cerâmica vermelha ao próprio processo industrial

The ceramics industry generates waste at various stages of that process, defective products, waste from burning solid fuels, among others. This waste is dumped in landfills, garbage dumps or directly on roads, which has a negative environmental impact. This paper presents a study to incorporate the waste of algaroba wood and chamote (scrap pieces of ceramic already sintered), in to the ceramic material for making sealing blocks. The methodological procedures consist in the characterization of chemical and mineralogical residues, raw materials, and physical-mechanical of the formulations of mixes with clay, silt and waste. By pressing test pieces were produced using a pressure of 200 kgf/cm², varying compositions in the range of 0%, 5%, 10% and 15% by weight of residue. The sintering was performed in a muffle furnace, with the temperature levels of 850 ° C, 900 ° C, 950 ° C, 1000 ° C and 1050 ° C. The evaluated physical and mechanical properties were: Water Absorption, Linear Shrinkage Burning, Apparent Porosity, Apparent Density and Mechanical Resistance to Flexion. Analysis was carried out by Scanning Electron Microscopy on fracture surfaces of the specimens. Evaluation of linear shrinkage property drying and firing , water absorption and mechanical resistance to compression of the sealing blocks 5% wood ash residue, sintered at 900 °C hold temperature in the laboratory the products manufactured on an industrial scale. The main results, it was found on the viability of using the residues of algaroba wood and to confer refractory properties of the ceramic product. The main results, it was concluded feasibility of using the ash residues algaroba wood to impart refractory properties to the ceramic product and the residue of chamote, being derived from the own ceramic product not interfere with the properties, when used in a percentage of up to 5%.Since the residue of chamote being derived from the ceramic product itself had no effect on the properties. Studies in the laboratory have shown that the incorporation of up to 5% of these residues may be adopted as an alternative technology to reduce the environmental impact caused by the industrial sector, without compromising the final properties of the material, since the results on an industrial scale showed absorption values 11.66 and 11.74 of water and waste products respectively, within the parameters of NBR - 15,270, since the mechanical strength was 1.25 MPa and 0.94 MPa respectively for products with and without residue, lower than the minimum required by the technical standard that is 1.5 MPa.

Estudo da obtenção de cerâmica composta de alumina e beta alumina sódica utilizando-se resíduo cerâmico de velas de ignição e pó químico de extintores de incêndio

Ceramic materials the alumina base are large industrial applications. They are required for these products, specific characteristics obtained by following strict criteria during the manufacturing process. However, after life, not always these products are reused by a suitable waste management process. In ceramist context, advance research aimed at the reuse of waste aimed at obtaining ceramics and composite materials, with marked reduction of conventional raw materials. Aiming to generate scientific, technological and environmental contribution, this work studied to obtain a composite of alumina ceramic (Al2O3) and sodium beta alumina (NaAl11O17 ), and as starting materials the residue of the ceramic insulator of spark plugs, as a source alumina (Al2O3) powder and unusable sodium bicarbonate (NaHCO3) of fire extinguishers, as a source of sodium oxide (Na2O). The final ceramic product was obtained from a conventional mixture of sodium aluminum oxide in appropriate molar proportions. Sample spark plugs were obtained, discarded by lifetime, specific to a manufacturer, which, after passing through mechanical stress (grinding, magnetic purification, washing, drying and grinding the high energy), which resulted in residue powder with ceramic content of 84.34 % alumina (Al2O3), found by FRX chemical analysis, the phases present and identified by DRX. The dry chemical fire extinguisher, baking soda-based (NaHCO3) with expired, was obtained through direct collection of the waste generated during maintenance. Subjected to heat treatment at 120 °C , the NaHCO3 powder was decomposed in sodium oxide ( Na2O), which, subjected to chemical analysis (FRX) and mineralogical (DRX) revealed a content of 86.62 % sodium oxide (Na2O) . In the following steps the experimental procedure, chemical formulations were made on a molar basis of the starting material (1:9, 1:10 and 1:11 de Na2O/ Al2O3) inclusion of additives, milling parameters, sieve analysis, dilatometry, conformation of specimens, sintering in firing steps at 800 °C , 1000 °C and 1.200 °C with varying stays 30 , 60 and 120 minutes in each of the levels. The characterization of the final product was made by the following physical tests: water absorption, porosity, linear shrinkage, mineralogical analysis by DRX and microstructural analysis by MEV. A higher formation of sodium beta alumina (NaAl11O17), in sintered specimens in levels of 1.200 °C and 120 minutes, despite the prevailing coexistence of alpha phase alumina (Al2O3). From the results obtained opens up prospects for the reuse of waste studied in this work, the potter context and in other technological areas.

Estudo da obtenção de cerâmica composta de alumina e beta alumina sódica utilizando-se resíduo cerâmico de velas de ignição e pó químico de extintores de incêndio

Ceramic materials the alumina base are large industrial applications. They are required for these products, specific characteristics obtained by following strict criteria during the manufacturing process. However, after life, not always these products are reused by a suitable waste management process. In ceramist context, advance research aimed at the reuse of waste aimed at obtaining ceramics and composite materials, with marked reduction of conventional raw materials. Aiming to generate scientific, technological and environmental contribution, this work studied to obtain a composite of alumina ceramic (Al2O3) and sodium beta alumina (NaAl11O17 ), and as starting materials the residue of the ceramic insulator of spark plugs, as a source alumina (Al2O3) powder and unusable sodium bicarbonate (NaHCO3) of fire extinguishers, as a source of sodium oxide (Na2O). The final ceramic product was obtained from a conventional mixture of sodium aluminum oxide in appropriate molar proportions. Sample spark plugs were obtained, discarded by lifetime, specific to a manufacturer, which, after passing through mechanical stress (grinding, magnetic purification, washing, drying and grinding the high energy), which resulted in residue powder with ceramic content of 84.34 % alumina (Al2O3), found by FRX chemical analysis, the phases present and identified by DRX. The dry chemical fire extinguisher, baking soda-based (NaHCO3) with expired, was obtained through direct collection of the waste generated during maintenance. Subjected to heat treatment at 120 °C , the NaHCO3 powder was decomposed in sodium oxide ( Na2O), which, subjected to chemical analysis (FRX) and mineralogical (DRX) revealed a content of 86.62 % sodium oxide (Na2O) . In the following steps the experimental procedure, chemical formulations were made on a molar basis of the starting material (1:9, 1:10 and 1:11 de Na2O/ Al2O3) inclusion of additives, milling parameters, sieve analysis, dilatometry, conformation of specimens, sintering in firing steps at 800 °C , 1000 °C and 1.200 °C with varying stays 30 , 60 and 120 minutes in each of the levels. The characterization of the final product was made by the following physical tests: water absorption, porosity, linear shrinkage, mineralogical analysis by DRX and microstructural analysis by MEV. A higher formation of sodium beta alumina (NaAl11O17), in sintered specimens in levels of 1.200 °C and 120 minutes, despite the prevailing coexistence of alpha phase alumina (Al2O3). From the results obtained opens up prospects for the reuse of waste studied in this work, the potter context and in other technological areas.

Anodic oxidation of InP in KOH electrolytes

The anodic behavior of InP in 1 mol dm-3 KOH was investigated and compared with its behavior at higher concentrations of KOH. At concentrations of 2 mol dm-3 KOH or greater, selective etching of InP occurs leading to thick porous InP layers near the surface of the sustrate. In contrast, in 1 mol dm-3 KOH, no such porous layers are formed but a thin surface film is formed at potentials in the range 0.6 V to 1.3 V. The thickness of this film was determined by spectroscopic ellipsometry as a function of the upper potential and the measured film thickness corresponds to the charge passed up to a potential of 1.0 V. Anodization to potentials above 1.5 V in 1 mol dm- 3 KOH results in the growth of thick, porous oxide films (~ 1.2 µm). These films are observed to crack, ex-situ, due to shrinkage after drying in ambient air. Comparisons between the charge density and film thickness measurements indicate a porosity of approximately 77% for such films.

Multi-View Weighted Network

Extensive investigation has been conducted on network data, especially weighted network in the form of symmetric matrices with discrete count entries. Motivated by statistical inference on multi-view weighted network structure, this paper proposes a Poisson-Gamma latent factor model, not only separating view-shared and view-specific spaces but also achieving reduced dimensionality. A multiplicative gamma process shrinkage prior is implemented to avoid over parameterization and efficient full conditional conjugate posterior for Gibbs sampling is accomplished. By the accommodating of view-shared and view-specific parameters, flexible adaptability is provided according to the extents of similarity across view-specific space. Accuracy and efficiency are tested by simulated experiment. An application on real soccer network data is also proposed to illustrate the model.

Fabrication and evaluation of NiO/Y2O3-stabilized-ZrO2 hollow fibers for anode-supported micro-tubular solid oxide fuel cells

In this work NiO/3mol% Y₂O₃-ZrO₂ (3YSZ) and NiO/8mol% Y₂O₃-ZrO₂ (8YSZ) hollow fibers were prepared by phase-inversion. The effect of different kinds of YSZ (3YSZ and 8YSZ) on the porosity, electrical conductivity, shrinkage and flexural strength of the hollow fibers were systematically evaluated. When compared with Ni-8YSZ the porosity and shrinkage of Ni-3YSZ hollow fibers increases while the electrical conductivity decreases, while at the same time also exhibiting enhanced flexural strength. Single cells with Ni-3YSZ and Ni-8YSZ hollow fibers as the supported anode were successfully fabricated showing maximum power densities of 0.53 and 0.67Wcm^-2 at 800°C, respectively. Furthermore, in order to improve the cell performance, a Ni-8YSZ anode functional layer was added between the electrolyte and Ni-YSZ hollow fiber. Here enhanced peak power densities of 0.79 and 0.73Wcm^-2 were achieved at 800°C for single cells with Ni-3YSZ and Ni-8YSZ hollow fibers, respectively.

Engineering properties of alkali-activated natural pozzolan concrete

The development of alkali-activated binders with superior engineering properties and longer durability has emerged as an alternative to ordinary portland cement (OPC). It is possible to use alkali-activated natural pozzolans to prepare environmentally friendly geopolymer cement leading to the concept of sustainable development. This paper presents a summary of an experimental work that was conducted to determine mechanical strength, modulus of elasticity, ultrasonic pulse velocity, and shrinkage of different concrete mixtures prepared with alkali-activated Iranian natural pozzolans—namely Taftan andesite and Shahindej dacite, both with and without calcining. Test data were used for Taftan pozzolan to identify the effects of water-binder ratios (w/b) and curing conditions on the properties of the geopolymer concrete, whereas the influence of material composition was studied by activating Shahindej pozzolan both in the natural and calcined states. The results show that alkali-activated natural pozzolan (AANP) concretes develop moderate-to-high mechanical strength with a high modulus of elasticity and a shrinkage much lower than with OPC.

Internal cooling in rotational molding-A review

Rotational molding suffers from a relatively long cycle time, which hampers more widespread growth of the process. During each cycle, both the polymer and mold must be heated from room temperature to above polymer melting temperature and subsequently cooled to room temperature. The cooling time in this process is relatively long due to the poor thermal conductivity of plastics. Although rapid external cooling is possible, internal cooling rates are the major limitation. This causes the process to be uneconomical for large production runs of small parts. Various researchers have strived to minimize cycle times by applying various internal cooling procedures. This article presents a review of these methods, including computer simulations and practical investigations published to date. The effects of cooling rate on the morphology, shrinkage, warpage, and impact properties of rotationally molded polyolefins are also highlighted. In general, rapid and symmetrical cooling across the mold results in smaller spherulite size, increased mechanical properties and less potential warpage or distortion in moldings. POLYM. ENG. SCI., 2011. ©2011 Society of Plastics Engineers.