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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
21

InfluÃncia da remoÃÃo do colÃgeno e do uso de oxalato de potÃssio na resistÃncia de uniÃo de adesivos simplificados à dentina / Influence of collagen removal and the use of potassium oxalate in the bond strength of simplified adhesives to dentine

Francisco ClÃudio Fernandes Alves e Silva 25 September 2008 (has links)
FundaÃÃo de Amparo à Pesquisa do Estado do Cearà / O objetivo deste estudo in vitro foi avaliar a resistÃncia de uniÃo atravÃs de teste de microtraÃÃo (RUÂT) e a observaÃÃo do padrÃo de fratura atravÃs de anÃlise com microscÃpio Ãtico (MO) de dois sistemas adesivos: XP Bond (Dentsply) e Prime & Bond NT (Dentsply), aplicados sobre dentina de dentes humanos com aplicaÃÃo prÃvia de hipoclorito de sÃdio (NaOCl) a 10% e oxalato monopotÃssio mono-hidrogenado 3% (BisBlock - Bisco). Trinta e dois terceiros molares humanos hÃgidos recÃm extraÃdos tiveram suas coroas seccionadas no terÃo oclusal, prÃximo à junÃÃo amelo-dentinÃria, onde a dentina foi exposta e planificada usando lixas de SiC de granulaÃÃo 600 atravÃs de uma politriz giratÃria refrigerada a Ãgua. Posteriormente os dentes foram separados aleatoriamente em 8 grupos a saber: G1 (XP) - XP Bond; G2 (XPH) â NaOCl 10% + XP Bond; G3 (XPO) - oxalato de potÃssio + XP Bond; G4 (XPHO) â NaOCl 10% + oxalato de potÃssio + XP Bond; G5 (PB) Prime & Bond NT; G6 (PBH) â NaOCl 10% + Prime & Bond NT; G7 (PBO) - oxalato de potÃssio + Prime & Bond NT, e G8 (PBHO) â NaOCl 10% + oxalato de potÃssio + Prime & Bond NT. ApÃs a aplicaÃÃo dos tratamentos, foram confeccionadas coroas com compÃsitos Esthet X (Dentsply), cor A-2. Essas coroas foram confeccionadas atravÃs de incrementos de 2 mm de espessura, com fotoativaÃÃo de 20 s por incremento, atà atingirem 6 mm de altura. Os dentes foram submetidos a ensaio de microtraÃÃo e anÃlise do padrÃo de fratura foi realizada atravÃs de MO. As fraturas foram classificadas como: adesiva, coesiva e mista. Os resultados obtidos, MÃdia(DP) no ensaio de microtraÃÃo (RUÂT) foram: XP â 35,225(15,470)Aa, XPH â 23,405(12,425)Ba, XPO â 15,492(9,168)Cb, XPHO â 16,389(11,108)Cb, PB â 27,589(11,265)Ab, PBH â 25,457(12,044)Aa, PBO â 31,631(14,391)Aa e PBHO â 26,263(8,912)Aa. ApÃs anÃlise estatÃstica (Kruskal-Wallis, Dunn e Mann-Whitney, α=0,05), verificou-se que o adesivo XP Bond apresentou maior resistÃncia de uniÃo (RU) que o Prime & Bond NT; O uso de NaOCl 10% e oxalato de potÃssio interferem negativamente no XP Bond e nÃo causaram alteraÃÃes na RU do Prime & Bond NT quando aplicados tanto conjuntamente como isolados. A anÃlise microscÃpica do padrÃo de fratura mostrou que a maioria dos espÃcimes fraturou na interface adesiva. / The aim of this in vitro study was to evaluate two adhesive systems: XP Bond (Dentsply) and Prime & Bond NT (Dentsply), applied on human tooth dentine with previous application of sodium hypochlorite (NaOCl) 10% and potassium oxalate (BisBlock - Bisco), by means of test of microtensile bond strength (ÂTBS), and standard of fracture analysis through optical microscope (OM). Thirty two non-carious human third molars were selected and had its oclusal enamel removed to produce flat dentin surface which was prepared using sandpapers (SiC) of granulation 600 through a politriz with the intention of standardize the smear layer. After that the teeth were divided in 8 groups: G1 (XP) - XP Bond; G2 (XPH) â 10% sodium hypochlorite + XP Bond; G3 (XPO) - potassium oxalate + XP Bond; G4 (XPHO) â 10% sodium hypochlorite + potassium oxalate + XP Bond; G5 (PB) - Prime & Bond NT; G6 (PBH) â 10% sodium hypochlorite + Prime & Bond NT; G7 (PBO) â potassium oxalate + Prime & Bond NT, e G8 (PBHO) â 10% sodium hypochlorite + potassium oxalate + Prime & Bond NT. After the treatments had been performed, crowns with resin composite Esthet X (Dentsply), color A-2 were built. These crowns were done through increments of 2 mm of thickness, with photo polymerization of 20 s for increment, until reaching 6 mm of height. The samples then had been parted for the attainment of beams with transversal section of 0.8 mm, to be performed under ÂTBS. The mechanical assay was carried through a machine of universal assay. The beams used in the microtensile test had been used later for the analysis of the standard of breaking through an OM. The results gotten in ÂTBS, Means(SD), were: XP â 35.225(15.470)Aa, XPH â 23.405(12.425)Ba, XPO â 15.492(9.168)Cb, XPHO â 16.389(11.108)Cb, PB â 27.589(11.265)Ab, PBH â 25.457(12.044)Aa, PBO â 31.631(14.391)Aa and PBHO â 26.263(8.912)Aa. After the values had been submitted to the statistical analysis (Kruskal-Wallis, Dunn e Mann-Whitney, α=0.05), was verified that XP Bond had better bond strength than Prime & Bond NT (control groups), and the 10% NaOCl treatment and potassium oxalate usage had decreased the bond strength of XP Bond and did not cause any statistical interference on Prime & Bond NT, even its usage was either together or isolated. The microscopic analysis of the breaking standard showed that almost all os specimens had adhesive fractures.
22

Biomimetic Growth and Morphology Control of Calcium Oxalates / Biomimetisches Wachstum und Morphologie Kontrolle von Calcium Oxalaten

Thomas, Annu 25 November 2009 (has links) (PDF)
With respect to the principles of biomineralization, it is of interest to study the crystallization of calcium oxalates under various experimental conditions. Calcium oxalates play decisive roles as biominerals in plants and as pathological “urinary/kidney stones” in vertebrates. Calcium oxalate exists in three different hydration states; calcium oxalate monohydrate (COM, monoclinic, a = 6.290(1)Å, b = 14.583(1)Å, c = 10.116(1)Å, β = 109.46°, P21/c), calcium oxalate dihydrate (COD, tetragonal, a = b = 12.371(3)Å, c = 7.357(2)Å, α = β = γ = 90°, I4/m) and calcium oxalate trihydrate (COT, triclinic, a = 6.11(1)Å, b = 7.167(2)Å, c = 8.457(2)Å, α = 76.5(2)°, β = 70.35(2)°, γ = 70.62(2)°, P ). Monoclinic COM and tetragonal COD are the most common phyto-crystals and the main constituents of kidney and urinary stones. The occurrence of calcium oxalates in plants represents a useful biogenesis (protection against herbivores) unlike the devastating occurrence in renal tubules. Therefore, biomineralization can be physiological or pathological. A systematic investigation of the morphological evolution of calcium oxalates in the presence of organic components is essential for understanding the mechanism of “pathological biomineralization”. In order to understand the pathological biomineralization of uroliths, it is necessary grow calcium oxalates comparable in morphology under similar growth conditions. The formation of calcium oxalate stones within a gelatinous state of proteins, polysaccharides, lipids and other biomacromolecules under a flow of supersaturated urine supports the fact that an “organic” gel model can simulate the process of urinary stone formation under in vitro conditions. Furthermore, synthetic polymers with precisely known functions and solution behaviours are better choices to understand the interaction of acidic proteins with calcium oxalates. Therefore, as a first step to unravel the complex pathology of uro/nephro lithiasis, we started to examine the structure and morphology of calcium oxalates crystallized in the presence of organic additives such as the sodium salt of polyacrylic acid (PAA) as well as agar gel. The influence of initial calcium oxalate concentration, pH and concentration of the additives on the formation of hydration states of calcium oxalates have been investigated along with the stated general methods. Apart from the three hydrated forms, calcium oxalate exists also in the anhydrous form (COA). Although three modifications of COA (α, β and γ) are reported in the literatures, the crystal structures and phase transformations were controversially discussed. We have been able to reveal the crystal structure of the β-modification of the anhydrous calcium oxalate by a combination of atomistic simulations and Rietveld refinements on the basis of powder X-ray diffraction pattern. β-COA belongs to the monoclinic system with unit cell parameters, a = 6.1644(3)Å, b = 7.3623(2)Å, c = 9.5371(5)Å, β = 90.24(2)°, P2/m (No. 10). The dehydration of COM was mimicked in silico to receive an initial model of the crystal structure of anhydrous calcium oxalate. This general approach may also be accessible for other decomposition processes ending up with crystalline powders of unknown crystal structure. No evidence for transformations from or to the α- or γ- modifications was found during our investigations. The growth pattern of COD crystals precipitated from aqueous solutions in the presence of PAA is clearly dependent on the concentration of PAA. By increasing the concentration of PAA, the shape of COD has been found to change from tetragonal bi-pyramids with dominant (101) pyramidal faces to tetragonal prisms with dominant (100) prism faces and finally to dumbbells. At still higher PAA concentrations, the morphology is reverted back to rod-like tetragonal prisms. Apart from these experiments, the interaction of PAA with (100) and (101) crystal faces of COD was explored with the aid of atomistic simulations. The simulation confirmed that during the development of the aggregates, strong interactions of PAA with the (100) faces take over control of morphologies. Our investigations show that the inner architecture of all the morphological varieties of COD was found to be dominated by an inner “core” consisting of thin elongated crystallites together with incorporated PAA and an outer “shell” formed as a consequence of secondary nucleation processes. We propose that for all types of COD aggregates, relative proportion of calcium oxalate and PAA dictates the shape and formation of nanometer sized crystallites which then aggregate and align to form the core. Such cores enriched with PAA may act as the sites for secondary nucleation events of calcium oxalate crystallites which then cover the core like a shell. In vitro experimental models for the growth of calcium oxalates can give valuable information on the growth and aggregation of urinary stones. Therefore, the “double diffusion technique” in agar gel matrix has been used for the biomimetic growth of calcium oxalate (COM) stones. A great variety of morphological forms of COM are produced in agar gel matrices (2 wt.-% agar gel of pH 8.5) ranging from platy crystallites to dumbbells and spherulites. The COM dumbbells and spherulites are assumed to be formed by the aggregation of smaller crystallites as a consequence of increased supersaturation inside the gel. Moreover, an increase of the pH value of the agar gel has been found to suppress the growth of COM and favours the growth of COD. The morphology of COD crystals grown in 2 wt.-% agar gel of pH 11.5 includes tetragonal prisms and dumbbells. The system calcium oxalate/ PAA/ H2O is a suitable model system for the investigation of principles of biomineral growth (shape development) in general. Our results demonstrate that the double diffusion technique in agar gel is a convenient route to grow calcium oxalate aggregates showing close resemblance to biogenic calculi and to study their ontogeny.
23

A quantitative assessment of the anti-nutritional properties of Canadian pulses

Shi, Lan 22 December 2015 (has links)
This study has assessed the effects of pulse type and processing (soaking and cooking) on antinutritional factors (α-amylase inhibitor, trypsin inhibitor, chymotrypsin inhibitor, lectins, phytic acid and oxalates) in a wide range of Canadian pulses, using soybean as a control. The contents of these antinutrients in Canadian pulses varied widely, but the levels were generally lower than those found in soybean. Analysis of variance indicated that both pulse type and processing had significant effects (P < 0.0001) on the investigated seeds. Soaking markedly decreased the contents of α-amylase inhibitor, trypsin inhibitor, chymotrypsin inhibitor, lectins and oxalates, but had no impact on phytic acid. Cooking of presoaked seeds appeared to be more effective; all proteinaceous antinutrients (α-amylase inhibitor, trypsin inhibitor, chymotrypsin inhibitor and lectins) were decreased by 80 – 100%, and significant reductions in phytic acid content (11 – 39%) were observed for all pulses, except common beans and soybean. / February 2016
24

Thermal, spectroscopic and x-ray diffraction studies of copper(II) 1,2,4,5-Benzenetetracarboxylates and copper(II) oxalate a study of metal-organic frameworks

Lamprecht, Emmanuel January 2008 (has links)
Novel and known metal organic frameworks with copper(II), sodium and 1,2,4,5-benzenetetracarboxylate were prepared by ambient precipitation, solvothermal and gel-synthesis methods, and characterized by single-crystal X-ray diffraction, X-ray powder diffraction, infrared spectroscopy, differential scanning calorimetry, and thermogravimetry with FTIR evolved-gas analysis. Some of these complexes were investigated for guest inclusion properties with water (the original guest species), methanol, ethanol and pyridine. The gel-synthesis products were the most interesting. The novel threedimensional metal-organic framework complex Cu₂ Na(OH)L·7H₂O (where L=1,2,4,5-benzenetetracarboxylate) -formed by gel-synthesis- is a covalent three-dimensional metal organic framework polymer with open channels containing both guest water molecules and water molecules coordinated to sodium. The structure collapsed on dehydration, but was essentially restored to the original structure on rehydration in moist air. On exposure of the dehydrated material to methanol and ethanol vapour, significant uptake of these solvents was observed, and the resolvated structures closely resembled that of the parent material. On heating in dry nitrogen, small amounts of methanol and ethanol remained until about 280 °C, when loss of the remaining guest triggered decomposition of the framework. The related complex, Cu₂¼(OH)½ L·7½H₂O (or possibly Cu₂⅓ (OH)⅔L·8H₂O) -formed by gel-synthesis- had a different physical appearance to Cu₂Na(OH)L·7H₂O above, but had nearly identical X-ray diffraction pattern, mid-infrared spectrum and thermal behaviour. The novel complex Cu₄Na₄L₃·14H₂O -formed by gel-synthesis- is a covalent three-dimensional metal-organic framework with small channels containing both guest water molecules and water coordinated to sodium and copper. Upon dehydration the structure collapsed, but on rehydration in moist air the original structure was partly restored. The dehydrated material did not absorb methanol. Known two-dimensional polymeric complexes [Cu₂L·6H₂O]·4H₂O and [Cu₂L·4H₂O]·2H₂O were also obtained by gel-synthesis, and were characterized and investigated for guest inclusion properties. The structures of these complexes collapsed on dehydration, and were only partly restored on rehydration in saturated water vapour. The dehydrated materials did not absorb methanol. The two-dimensional polymeric mixed-ligand complex Cu₂(pyridine)₄·6H₂O -formed very slowly by gel-synthesis- was characterized by TG-FTIR, and was shown to undergo a complicated decomposition involving the loss of water and pyridine, carbon dioxide and carbon monoxide in various stages. Solvothermal synthesis did not yield materials suitable for single-crystal X-ray diffraction studies or inclusion studies, producing only an anhydrous or hemihydrate complex with the formula Cu₂L·0.65H2O. Ambient precipitation syntheses did not yield materials suitable for singlecrystal diffraction studies, forming products approximately equivalent to the complexes [Cu₂L·6H₂O]·4H₂O and Cu₂¼(OH)½L·7 ½H₂O above. During the course of the above study it was discovered that, on changing the DSC purge from nitrogen to argon, the normally exothermic carboxylate decompositions appeared to become endothermic. The effects of the supposedly inert atmospheres of argon and nitrogen on the decomposition-mechanism of copper(II) oxalate -a well-studied copper carboxylate- were therefore studied by DSC, TG, TG-FTIR and XRPD. DSC experiments were performed in nitrogen and argon at different flow-rates, in various mixtures of nitrogen and argon, and at various heating rates. Regardless of the proportions of nitrogen and argon, the DSC residues consisted mainly of copper metal, a small amount of copper(I) oxide (cuprite) and, in some circumstances, traces of copper(II) oxide (tenorite). Also, regardless of whether TG-FTIR experiments were performed under argon or nitrogen, the gaseous decomposition products consisted mainly of carbon dioxide, with traces of carbon monoxide being detected over part of the decomposition period. Various explanations for the thermal behaviour are discussed, and it is possible that small amounts of O2 or monatomic oxygen were given off during the decomposition under argon. The design and implementation of a low-cost prototype X-ray proportional counter detector system, consisting of a hybrid analog-digital computer built using commonly available electronic components, is presented. This system was designed to replace ageing discrete-transistor designs still in use in earlier X-ray diffractometers. The prototype performs the functions of pulse-shaping, pulseheight discrimination, counting and scaling, and provides both digital and scaled analog outputs.
25

A study of irradiation effects in solids

Brown, Michael Ewart January 1966 (has links)
One of the primary objects of this research was to determine, if possible, the nature of the radiation damage prior to thermal decomposition. The X-ray study has not wholly achieved this although more information has been derived from it than from similar work on AgMnO₄ However, the diffuse reflections obtained do indicate, quite strongly, the creation of point defects during irradiation. This is of value since such assumptions have been made in the explanation of the kinetics of decomposition of a number of irradiated solids (BaN₆,CaN₆). In addition the X-ray work has suggested future research which should produce useful information; namely, a precise study of the diffuse reflections. Another object of the research was to attempt to determine what characteristics, if any, of the kinetics of the decomposition of an unirradiated solid would predetermine a marked irradiation effect. It is obvious that the type of nuclear growth which occurs e.g. branching chain, or power law, does not characterise a substance with regard to a possible irradiation effect . The photosensitivity, or otherwise, also does not determine whether there will be an irradiation effect. However, the one property that the substances which have been studied, have in common, is a polyatomic anion, but here again ammonium dichromate does not show an acceleration of the decomposition after irradiation. Consequently it is considered that it is not possible to say, a priori, whether a solid will undergo an accelerated decomposition after irradiation. Each new solid, unless it belongs to a particular class e.g. the alkaline earth azides , must be considered afresh. Nevertheless it does appear that the irradiation effect can take two forms: - (i) the production of an unstable compound e.g. nickel oxalate, the decomposition of which affects the normal pyrolysis; and (ii) the production of point defects which determine the nature of the subsequent thermal decomposition e.g . CaN₆ . It is possible that the effect requires an interaction of the created point defects with the existing line defects.
26

Métodos de processamento e sinterização alternativos para obtenção de pastilhas de (Bi, Pb) - Sr - Ca - Cu - O / Alternative processing and sintering methods to obtain (Bi,Pb) Sr - Ca - Cu O pellets

Rubo, Elisabete Aparecida Andrello 20 December 1994 (has links)
Este trabalho trata da obtenção e caracterização de cerâmicas do sistema supercondutor Bi:Pb:Sr:Ca:Cu:O. O pó cerâmico foi feito por dois processos, mistura de óxidos/carbonatos e co-precipitação de oxalatos, com o objetivo de se estabelecer o procedimento mais favorável ao aparecimento da fase de temperatura critica de 110K. A caracterização do pó precursor foi feita através das técnicas de Plasma Indutivamente Acoplado (ICP), Picnometria, Sedigrafia, Difração de Raios X e Microscopia Eletrônica de Varredura. Na etapa de sinterização do pó estudamos, paralelamente a sinterização convencional, uma técnica alternativa de aplicação de corrente elétrica simultaneamente à ação da temperatura com o objetivo de acelerar a reação de formação e promover, possivelmente, uma maior fração da fase de mais alta temperatura critica. Ao final do processamento as amostras foram caracterizadas estruturalmente, por difração de raios X, e quanto às propriedades elétrica (resistividade elétrica) e magnética (susceptibilidade magnética). Na análise comparativa das características elétricas e estruturais das pastilhas obtidas convencional e quimicamente não observamos diferenças significativas entre elas. No entanto as medidas de susceptibilidade magnética mostraram uma grande diversificação de fases com temperaturas criticas abaixo de 110K, para a pastilha obtida por co-precipitação de oxalatos. Também verificamos que a fase 2223 encontra-se, nessa amostra, em maior proporção do que na pastilha proveniente de pó convencional. O processo alternativo de sinterização promoveu algumas alterações no comportamento da resistividade elétrica do material / This work is about the obtaining and characterizing pellets of the Bi:Pb:Sr:Ca:Cu:O system. The powder was prepared by two processes: oxide/carbonate mixture and oxalate co-precipitation. These two processes were used in order to establish the most favorable process to the 110 K phase formation. The characterization techniques were Inductively Coupled Plasma, Picnometry, Sedigraphy, X Ray Diffraction and SEM. The sinterization was made by conventional and an alternative techniques. The alternative one consists in applying electrical current simultaneously to the temperature action. The expectation was that this technique would accelerate the reactions and consequently, to promote higher volume fraction of the 110K phase. The pellets were structural, electrical and magnetically characterized by X Ray Diffraction, SEM, electrical resistivity and magnetic susceptibility. In the analysis of the electrical and structural characterization of the pellets made by both processing methods, we could not find any difference between them. But, the magnetization measurements indicated that there are numerous phases with critical temperature below 110 K, in addition a higher fraction of 2223 phase, in the pellet made by co-precipitation of oxalates. The alternative sintering process promoted a few alterations in the behavior of the electrical resistivity as a function of the applied temperature
27

Effect of Leaving Ligands of Platinum(II) Diamine Complexes on DNA and Protein Residues

Kolli, Ramya 01 May 2013 (has links)
Platinum compounds are widely used drugs in cancer treatments. Although DNA is the biological target, reaction of platinum compounds with proteins is also potentially significant. Our objective is to study the effects of leaving ligands on the relative reactivity between 5'-GMP (guanosine 5' phosphate), a key DNA target, and N-Acetyl - L-Methionine (N-AcMet), a key protein target. We have used NMR spectroscopy to monitor reactions with N-AcMet and 5'-GMP added to a platinum complex to see which products are formed preferentially. Previous research showed that both a non-bulky complex such as [Pt(en)(D2O)2]2+ [en=ethylenediamine], and a bulky complex such as [Pt(Me4en)(D2O)2]2+ [Me4en= N, N, N', N'-tetramethylethylenediamine] react more quickly with 5'-GMP than with N-AcMet. To improve the activity of platinum compounds in our current research, oxalates as leaving ligands are used. The results suggest that [Pt(en)(Ox)] [Ox= oxalate] reacts faster with N-AcMet than with 5'-GMP. Also, [Pt(Me4en)(Ox)] reacts slowly with 5'-GMP without N-AcMet and the reaction favors N-AcMet when both ligands are added simultaneously. Interestingly, the formation of the sulfur-oxygen chelate is slow enough to be observable in the oxalate reaction; but the mono product is not independently observed in the dinitrate complex.
28

Obtencao de ceramicas de ceria - samaria - gadolinia para aplicacao como eletrolito em celulas a combustivel de oxido solido (SOFC) / Obtaining of ceria - samaria - gadolinia ceramics for application as solid oxide fuel cell (SOFC) electrolyte

ARAKAKI, ALEXANDER R. 09 October 2014 (has links)
Made available in DSpace on 2014-10-09T12:27:27Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:06:53Z (GMT). No. of bitstreams: 0 / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP
29

Métodos de processamento e sinterização alternativos para obtenção de pastilhas de (Bi, Pb) - Sr - Ca - Cu - O / Alternative processing and sintering methods to obtain (Bi,Pb) Sr - Ca - Cu O pellets

Elisabete Aparecida Andrello Rubo 20 December 1994 (has links)
Este trabalho trata da obtenção e caracterização de cerâmicas do sistema supercondutor Bi:Pb:Sr:Ca:Cu:O. O pó cerâmico foi feito por dois processos, mistura de óxidos/carbonatos e co-precipitação de oxalatos, com o objetivo de se estabelecer o procedimento mais favorável ao aparecimento da fase de temperatura critica de 110K. A caracterização do pó precursor foi feita através das técnicas de Plasma Indutivamente Acoplado (ICP), Picnometria, Sedigrafia, Difração de Raios X e Microscopia Eletrônica de Varredura. Na etapa de sinterização do pó estudamos, paralelamente a sinterização convencional, uma técnica alternativa de aplicação de corrente elétrica simultaneamente à ação da temperatura com o objetivo de acelerar a reação de formação e promover, possivelmente, uma maior fração da fase de mais alta temperatura critica. Ao final do processamento as amostras foram caracterizadas estruturalmente, por difração de raios X, e quanto às propriedades elétrica (resistividade elétrica) e magnética (susceptibilidade magnética). Na análise comparativa das características elétricas e estruturais das pastilhas obtidas convencional e quimicamente não observamos diferenças significativas entre elas. No entanto as medidas de susceptibilidade magnética mostraram uma grande diversificação de fases com temperaturas criticas abaixo de 110K, para a pastilha obtida por co-precipitação de oxalatos. Também verificamos que a fase 2223 encontra-se, nessa amostra, em maior proporção do que na pastilha proveniente de pó convencional. O processo alternativo de sinterização promoveu algumas alterações no comportamento da resistividade elétrica do material / This work is about the obtaining and characterizing pellets of the Bi:Pb:Sr:Ca:Cu:O system. The powder was prepared by two processes: oxide/carbonate mixture and oxalate co-precipitation. These two processes were used in order to establish the most favorable process to the 110 K phase formation. The characterization techniques were Inductively Coupled Plasma, Picnometry, Sedigraphy, X Ray Diffraction and SEM. The sinterization was made by conventional and an alternative techniques. The alternative one consists in applying electrical current simultaneously to the temperature action. The expectation was that this technique would accelerate the reactions and consequently, to promote higher volume fraction of the 110K phase. The pellets were structural, electrical and magnetically characterized by X Ray Diffraction, SEM, electrical resistivity and magnetic susceptibility. In the analysis of the electrical and structural characterization of the pellets made by both processing methods, we could not find any difference between them. But, the magnetization measurements indicated that there are numerous phases with critical temperature below 110 K, in addition a higher fraction of 2223 phase, in the pellet made by co-precipitation of oxalates. The alternative sintering process promoted a few alterations in the behavior of the electrical resistivity as a function of the applied temperature
30

Obtencao de ceramicas de ceria - samaria - gadolinia para aplicacao como eletrolito em celulas a combustivel de oxido solido (SOFC) / Obtaining of ceria - samaria - gadolinia ceramics for application as solid oxide fuel cell (SOFC) electrolyte

ARAKAKI, ALEXANDER R. 09 October 2014 (has links)
Made available in DSpace on 2014-10-09T12:27:27Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:06:53Z (GMT). No. of bitstreams: 0 / O óxido de cério (CeO2), quando dopado com óxidos de terras raras, tem sua condutividade iônica aumentada, possibilitando seu uso como eletrólito de Células a Combustível de Óxido Sólido de Temperatura Intermediária (IT-SOFC), que são operadas entre 500 e 700°C. Os aditivos ou dopantes mais eficientes para o aumento da condutividade iônica são a samária (óxido de samário Sm2O3) e a gadolínia (óxido de gadolínio Gd2O3), com concentrações molares entre 10 e 20%. Neste contexto foram sintetizados, neste trabalho, pós de composição Ce0,8(SmGd)0,2O1,9 pelas rotas de síntese por coprecipitação de hidróxidos, carbonatos e oxalatos. O efeito do tratamento hidrotérmico foi avaliado para pós precipitados com hidróxido de amônio. Utilizou-se, como matériasprimas, concentrados de terras raras contendo 90% em massa de CeO2 e outro contendo 51% de Sm2O3 e 30% de Gd2O3, ambos provenientes do processamento da monazita. Estes concentrados foram utilizados devido ao menor custo em relação às matérias-primas puras adquiridas comercialmente e a semelhança química dos demais elementos de terras raras contidos. Inicialmente, foram definidas as condições das etapas de coprecipitação e a influência da temperatura de calcinação nas características dos pós e produtos sinterizados. Os resultados obtidos mostraram que os pós calcinados na faixa de temperatura entre 450 e 800ºC apresentam elevada área de superfície específica (90-150 m2.g-1) e estrutura cristalina cúbica tipo fluorita da céria, indicando a formação da solução sólida. Observou-se, por microscopia eletrônica de varredura, que a forma das partículas e dos aglomerados é função do tipo de agente precipitante. As análises dilatométricas indicaram maior taxa de retração em temperatura próxima a 1300-1350ºC. Entretanto, valores elevados de densificação (>95% DT) são obtidos em temperaturas superiores a 1400ºC. A síntese por coprecipitação de hidróxidos seguida pelo tratamento hidrotérmico demonstrou ser uma rota promissora para cristalização, em baixas temperaturas (200oC), de nanopós à base de céria, mantendo-se elevados os valores de área de superfície específica (cerca de 100 m2.g-1). Cerâmicas com densificação superior a 95%DT foram obtidas em menores temperaturas de sinterização (1400oC), quando comparadas às provenientes de pós cristalizados por calcinação. / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

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