A força de adesão entre resinas e ligas de metais básicos resulta do embricamento mecânico entre a superfície do metal e a resina e da interação química entre óxidos presentes na superfície dos metais e monômeros adesivos das resinas compostas. A literatura, entretanto, mostra que ainda persistem algumas dúvidas sobre a interação entre os diversos tipos de sistemas adesivos e metais básicos, por isso, essa pesquisa visa: verificar se a presença do Be na composição de ligas a base de Ni-Cr influencia a união metal básico/resina; comparar dois cimentos resinosos adesivos nessa função e verificar a influência da utilização de condicionadores (primers) adesivos metálicos para ligas nobres sobre essa união. Após 2500 termociclos, foram realizados testes de resistência à tração em 160 corpos-de-prova, que consistiam de dois discos de Ni-Cr-Be (Verabond – Aalba Dental Inc., Cordelia, CA-USA) com 6 mm de diâmetro e 2 mm de espessura cimentados entre si, e dois discos de Ni-Cr (Durabond - Odonto Comercial Importadora Ltda, São Paulo, SP), com as mesmas dimensões, cimentados entre si. Foram utilizadas diferentes marcas comerciais de sistemas adesivos: os cimentos resinosos adesivos, Panavia F (Kuraray Co. Ltd.), Bistite II DC (Tokuyama Corp.) e os agente de união (primers adesivos metálicos), Alloy Primer (Kuraray Co. Ltd. ), Metaltite (Tokuyama Corp.) e Cesead Opaque Primer (Kuraray Co. Ltd.). Discos cimentados sem primers serviram como grupo controle. Os resultados mostraram que houve diferença estatisticamente significante entre as duas ligas (Ni-Cr-Be –24,82 ± 7,6 MPa e Ni-Cr - 22,32 ± 7,9 MPa). Já para os cimentos houve superioridade adesiva do cimento Panavia F, que obteve média de resitência adesiva de 27,49 ± 4,8 MPa, sobre o cimento Bistite II, que obteve média de resistência adesiva de 19,63 ± 8,4 MPa. Os primers utilizados não apresentaram influência positiva sobre o Panavia F já que os grupos sem primer para esse cimento obtiveram média de 28,18 ± 5,6 MPa que é equivalente a média dos outros grupos com Panavia. Entretanto, para o cimento Bistite II DC os primers Alloy Primer e Metaltite obtiveram as menores médias, 12,7 ± 7,6 MPa e 15,71 ± 4,8 MPa respectivamente, enquanto sem primer, ou com o Cesead Opaque Primer, as médias foram significantemente superiores, 24.47 ± 6 MPa e 25.70 ± 6,8 Mpa respectivamente. Diante dos resultados conclui-se que os primers adesivos metálicos não potencializaram a adesão de cimentos resinosos adesivos sobre ligas de Ni-Cr. / The bond strength for resin and basic metals comes from the interaction between oxides in the metal surface and adhesive monomers in the composite resins composition. The literature shows that still are some questions about this interaction so this research intends to: verify if the presence of Be at Ni-Cr alloy plays some influence for this union, compare two resin luting cements at this function and study the influence the use of metal primers for noble metals in this mecanism of adhesion. After 2500 thermocycles, tensile bond strength tests were loaded at 160 specimens, which consisted of two metals discs with 6 mm in diameter and 2 mm thick from a Ni-Cr-Be alloy (Verabond – Aalba Dental Inc., Cordelia, CA-USA) bonded togheter and two metal discs from a Ni-Cr alloy (Durabond - Odonto Comercial Importadora Ltda, São Paulo, SP) bonded togheter. Diferent brand adhesive systems were used: the resin cements, Panavia F (Kuraray Co. Ltd.) and Bistite II DC (Tokuyama Corp.) and the metal primers, Alloy Primer (Kuraray Co. Ltd.), Metaltite (Tokuyama Corp.) and Cesead Opaque Primer (Kuraray Co. Ltd.). Nonprimed specimens served as control group. The results indicated that there is statiscal diferences beetwen the two alloys (Ni-Cr-Be –24,82 ± 7,6 MPa e Ni-Cr - 22,32 ± 7,9 MPa). Panavia F had founded greater bond strength (27,49 ± 4,8 MPa) than Bistite DC (19,63 ± 8,4 MPa). The metal primers did not show any positive influence for the Panavia bond strength when we considere that the no primer group had 28,18 ± 5,6 MPa bond strength media which were equivalente to the others Panavia´s groups. However for the Bistite cement, the bond strength for Alloy primer and Metaltite were the lower medias, 12,7 ± 7,6 MPa and 15,71 ± 4,8 MPa respectivally, while the no primer or the Cesead Opaque Primer groups showed superior medias 24,47 ± 6 MPa and 25,70 ± 6,8 MPa respectivally. The outcome of this research shows that the metal primers used did not incresead the bond strength between resin cements and Ni-Cr alloys.

A força de adesão entre resinas e ligas de metais básicos resulta do embricamento mecânico entre a superfície do metal e a resina e da interação química entre óxidos presentes na superfície dos metais e monômeros adesivos das resinas compostas. A literatura, entretanto, mostra que ainda persistem algumas dúvidas sobre a interação entre os diversos tipos de sistemas adesivos e metais básicos, por isso, essa pesquisa visa: verificar se a presença do Be na composição de ligas a base de Ni-Cr influencia a união metal básico/resina; comparar dois cimentos resinosos adesivos nessa função e verificar a influência da utilização de condicionadores (primers) adesivos metálicos para ligas nobres sobre essa união. Após 2500 termociclos, foram realizados testes de resistência à tração em 160 corpos-de-prova, que consistiam de dois discos de Ni-Cr-Be (Verabond – Aalba Dental Inc., Cordelia, CA-USA) com 6 mm de diâmetro e 2 mm de espessura cimentados entre si, e dois discos de Ni-Cr (Durabond - Odonto Comercial Importadora Ltda, São Paulo, SP), com as mesmas dimensões, cimentados entre si. Foram utilizadas diferentes marcas comerciais de sistemas adesivos: os cimentos resinosos adesivos, Panavia F (Kuraray Co. Ltd.), Bistite II DC (Tokuyama Corp.) e os agente de união (primers adesivos metálicos), Alloy Primer (Kuraray Co. Ltd. ), Metaltite (Tokuyama Corp.) e Cesead Opaque Primer (Kuraray Co. Ltd.). Discos cimentados sem primers serviram como grupo controle. Os resultados mostraram que houve diferença estatisticamente significante entre as duas ligas (Ni-Cr-Be –24,82 ± 7,6 MPa e Ni-Cr - 22,32 ± 7,9 MPa). Já para os cimentos houve superioridade adesiva do cimento Panavia F, que obteve média de resitência adesiva de 27,49 ± 4,8 MPa, sobre o cimento Bistite II, que obteve média de resistência adesiva de 19,63 ± 8,4 MPa. Os primers utilizados não apresentaram influência positiva sobre o Panavia F já que os grupos sem primer para esse cimento obtiveram média de 28,18 ± 5,6 MPa que é equivalente a média dos outros grupos com Panavia. Entretanto, para o cimento Bistite II DC os primers Alloy Primer e Metaltite obtiveram as menores médias, 12,7 ± 7,6 MPa e 15,71 ± 4,8 MPa respectivamente, enquanto sem primer, ou com o Cesead Opaque Primer, as médias foram significantemente superiores, 24.47 ± 6 MPa e 25.70 ± 6,8 Mpa respectivamente. Diante dos resultados conclui-se que os primers adesivos metálicos não potencializaram a adesão de cimentos resinosos adesivos sobre ligas de Ni-Cr. / The bond strength for resin and basic metals comes from the interaction between oxides in the metal surface and adhesive monomers in the composite resins composition. The literature shows that still are some questions about this interaction so this research intends to: verify if the presence of Be at Ni-Cr alloy plays some influence for this union, compare two resin luting cements at this function and study the influence the use of metal primers for noble metals in this mecanism of adhesion. After 2500 thermocycles, tensile bond strength tests were loaded at 160 specimens, which consisted of two metals discs with 6 mm in diameter and 2 mm thick from a Ni-Cr-Be alloy (Verabond – Aalba Dental Inc., Cordelia, CA-USA) bonded togheter and two metal discs from a Ni-Cr alloy (Durabond - Odonto Comercial Importadora Ltda, São Paulo, SP) bonded togheter. Diferent brand adhesive systems were used: the resin cements, Panavia F (Kuraray Co. Ltd.) and Bistite II DC (Tokuyama Corp.) and the metal primers, Alloy Primer (Kuraray Co. Ltd.), Metaltite (Tokuyama Corp.) and Cesead Opaque Primer (Kuraray Co. Ltd.). Nonprimed specimens served as control group. The results indicated that there is statiscal diferences beetwen the two alloys (Ni-Cr-Be –24,82 ± 7,6 MPa e Ni-Cr - 22,32 ± 7,9 MPa). Panavia F had founded greater bond strength (27,49 ± 4,8 MPa) than Bistite DC (19,63 ± 8,4 MPa). The metal primers did not show any positive influence for the Panavia bond strength when we considere that the no primer group had 28,18 ± 5,6 MPa bond strength media which were equivalente to the others Panavia´s groups. However for the Bistite cement, the bond strength for Alloy primer and Metaltite were the lower medias, 12,7 ± 7,6 MPa and 15,71 ± 4,8 MPa respectivally, while the no primer or the Cesead Opaque Primer groups showed superior medias 24,47 ± 6 MPa and 25,70 ± 6,8 MPa respectivally. The outcome of this research shows that the metal primers used did not incresead the bond strength between resin cements and Ni-Cr alloys.

No description available.

FundaÃÃo Cearense de Apoio ao Desenvolvimento Cientifico e TecnolÃgico / O objetivo deste trabalho foi avaliar as caracterÃsticas operacionais (produtividade, eficiÃncia de deposiÃÃo, diluiÃÃo, geometria do cordÃo de solda, custo) e metalÃrgicas (microestrutura, resistÃncia à corrosÃo, propriedades mecÃnicas) de revestimentos de ligas de nÃquel depositados pelo processo plasma pà aplicado internamente em tubos API. Foram utilizadas as ligas de nÃquel Inconel 625 e Hastelloy C-276. Inicialmente foi realizado um estudo preliminar para conhecer os parÃmetros iniciais de soldagem. Em seguida, foi realizado um estudo definitivo com simples deposiÃÃo, aplicando o MÃtodo Taguchi com intuito de selecionar os melhores parÃmetros de cada fator de controle do processo de soldagem plasma pà em um nÃmero reduzido de experimentos. Posteriormente foi realizado um estudo de sobreposiÃÃo de passes e entÃo foi realizada a soldagem definitiva de revestimentos. Nos revestimentos soldados foram realizadas anÃlises das caracterÃsticas geomÃtricas e diluiÃÃo, alÃm de uma caracterizaÃÃo metalÃrgica com uso de microscopia Ãtica, microscopia eletrÃnica de varredura e anÃlise de composiÃÃo quÃmica por EDX. Ainda foram realizadas anÃlises das propriedades mecÃnicas dos revestimentos por meio de ensaios de microdureza, bem como anÃlise de resistÃncia à corrosÃo atravÃs do mÃtodo C da norma ASTM G48-03. Os resultados mostraram que o MÃtodo Taguchi proporcionou uma excelente seleÃÃo de parÃmetros para soldagem de revestimentos. Alguns revestimentos soldados apresentaram baixos nÃveis de diluiÃÃo. A microestrutura dos revestimentos soldados com a liga Inconel 625 foi constituÃda de uma matriz , com precipitaÃÃo de fases secundÃrias tipo Laves, ricas em niÃbio, e carbonitretos de titÃnio e niÃbio. Jà a microestrutura da liga Hastelloy C-276 foi constituÃda de uma matriz  com precipitaÃÃo de fases secundÃrias P e , sendo esta Ãltima fase uma transformaÃÃo parcial da fase P, e ambas as fases ricas em molibdÃnio. Em relaÃÃo Ãs propriedades mecÃnicas, a liga Hastelloy C-276 apresentou maiores nÃveis de dureza comparada com a liga Inconel 625. Jà na resistÃncia a corrosÃo dos revestimentos soldados, a liga Hastelloy C-276 apresentou uma Temperatura CrÃtica de Pite (TCP) em 60 ÂC. Enquanto a liga Inconel 625 apresentou uma TCP de 75 ÂC. / The aim of this study was to evaluate the operational characteristics (productivity, efficiency deposition, dilution of the weld bead geometry and cost) and metallurgical (microstructure, corrosion resistance, mechanical properties) of weld overlay with nickel-based alloys deposited by powder plasma process, applied internally in API pipes. Inconel 625 and Hastelloy C-276 nickel-based alloys were used. A preliminary study was conducted to understand the initial welding parameters and then a definitive study with simple deposition and applying Taguchi method was performed. The Taguchi method was used to select the best parameters of each factor of control in powder plasma welding using a short number of experiments. A study of overlapping passes to subsequent coatings definitive welding was performed. Analysis of geometric characteristics and dilution were performed in welded coatings, and a metallurgical characterization was accomplished using optical microscopy, scanning electron microscopy and EDX. Analysis mechanical properties of the coatings were performed by microhardness tests and it was performed analysis of corrosion resistance using the C method of standard ASTM G48-03. The results showed that the Taguchi method provided excellent selection of welding parameters for coatings. The coatings showed conditions welded to dilution levels low. The microstructure of the coatings welded with Inconel 625 alloy was composed of , with precipitation of secondary phases of the Laves type, rich in niobium, and titanium and niobium carbonitrides. The microstructure of the alloy Hastelloy C-276 was consisted of  with precipitation of secondary phases like  and P, both phases were rich in molybdenum. The mechanical properties the Hastelloy C -276 alloy showed higher levels of hardness compared to Inconel 625 alloy. The Hastelloy C-276 showed a Critical Pitting Temperature (TCP) at 60 ÂC. While Inconel 625 alloy exhibited a TCP, at 75 ÂC.

Arbetet som utförts är en material studie som inriktar sig på nickel-krom-molybdenbaserade legeringar som används i dagens våt skrubber. Eftersom kraven på mängden utsläpp av svaveldioxid är en viktig miljöfråga, skapar detta ett behov för användandet av en våt skrubber. Den här produkten befinner sig i anläggningar där förbränningsmotorer finns och förekommer i princip i alla större fartyg. Rökgasen som motorerna släpper ifrån sig är skadlig för miljön och därför absorberas flödet in till en våt skrubber där en förbränning sker. Rökgasen separeras med hjälp av ett antal sprinklers som är placerade ovanpå gas ingången i en skrubber. Med hjälp av havsvatten som samlas upp och sluts till skrubbern injiceras detta genom sprinklers sen vidare nedåt på rökgasen som separerar föroreningar ifrån den gasen som är tänkt ska kondensera genom och ut i atmosfären. Havsvatten tillsammans med föroreningarna samlas på botten av skrubbern och samlas i tankar. Denna miljö är väldigt skadlig för materialet som produkten består av, framför allt på botten där materialet riskerar att korrodera som mest. Arbetet beskriver ett antal typer av korrosion och förklarar innebörden av de olika typerna så att det enklare går att förstå sammanhanget med miljön och omständigheternas påverkan på legeringarna. Syftet i arbetet är att studera de olika legeringarna och beskriva de med hjälp av den litteraturstudie som gjorts. Med hjälp av insamlad data av tester som tidigare utförts enligt standard, har detta tolkats och bidragit till evalueringen av de olika legeringarna. De grundläggande tester som används vid evaluering av legeringarnas karaktär är tester där en bit av materialet doppas ned i en specifik lösning med olika omständigheter och villkor. Detta räcker inte för att säkerställa en hållbar livscykel för en våt skrubber och därför evalueras legeringarna även med hjälp av olika fälttester. Teoretiska studier på tester i aggressiva miljöer används för att resultera rangordningen av de olika materialen och även ett nytt material undersöks vid namnet alloy 2120. / This thesis work is a study of materials which focus on nickel-chromium-molybdenum-based alloys used in today’s wet scrubbers. Since the requirements for emissions of sulfur dioxide is a major environmental issue, this creates a need for the use of a wet scrubber. This product is in installations where combustion engines are available and are basically in all larger vessels. The flue gas that engines emit are harmful to the environment and for that reason, the flow is absorbed into a wet scrubber where combustion takes place. The flue gas is separated by a number of sprinklers placed above of the gas in a scrubber. Collected seawater is used to separate the gas through the sprinklers that injects the water on top of the flue gas where impurities is separated from the gas that will condense out to the atmosphere. The water fluid together with the contaminants is collected on the bottom of the scrubber and into the tanks. This environment is very harmful to the material that the product is made of, in particular on the bottom where the material is more susceptible for corrosion. The work describes several types of corrosion and the meaning of the different types so that the reader easily can understand the impact of the environment on the alloys. The type of corrosion that occurs primarily in scrubbers is pitting corrosion and is considerate to be a highly local type of corrosion, and the most dangerous type. Pitting occurs when the protective oxide layer does not have time to repassivate and can also lead to other types of corrosion. Due to the dangerous work environment, the risk for corrosion to occur is high and therefore, focus is put on this specific material group. The purpose of this work was to study the alloys and describe them with the help of a literature study. Using data collected from tests previously performed in accordance with standards, the collected data has been interpreted and contributing to the evaluation of the various alloys. The basic tests used in the evaluation of the nature of the alloy are tests in which a piece of material immersed in a specific solution with different circumstances and conditions. This is not enough to ensure a sustainable life cycle for a wet scrubber and therefore, alloys is evaluated using various field tests as well. Theoretical studies on tests in aggressive environments is used to result the ranking of the various materials and also a new material is examined by the name alloy 2120.

O presente trabalho visou desenvolver ligas à base de Níquel-Cromo para prótese dentária, que confiram as melhores características metalúrgicas e químicas para posterior produção e aplicação. Para isto foram adquiridas amostras de ligas comerciais de 8 fabricantes. Os materiais foram caracterizados em termos de composição química, propriedades mecânicas, caracterização microestrutural, temperatura de fusão, coeficiente de expansão térmica, corrosão e biocompatibilidade. Para isto, utilizou-se as fluorescência de raios X (XRF-WDS), ICP-OES, ensaios de tração, ensaios de dureza, ensaios de corrosão, avaliação de citotoxicidade, microscopia eletrônica de varredura (MEV), microanálise eletrônica (EDS), difratometria de Raios X (DRX), análise térmica diferencial (DTA), dilatometria e avaliação de fluidez. A maioria dos resultados composicionais não condiz com as composições fornecidas pelos fabricantes. Os resultados mostraram claramente a presença de um eutético típico formado pelas fases Niss e NiBe nas ligas contendo Be, que pode ser considerado uma \"impressão digital\" da presença deste elemento nestas ligas. É possível verificar a formação de intermetálicos na região interdendritica para as ligas isentas de Be, sendo identificado um siliceto (Nb6Ni16Si7) em uma das ligas, que possui temperatura de inicio de fusão inferior ao eutético Niss e NiBe das ligas com Be. De uma forma geral, os resultados dos ensaios de dureza mostraram valores superiores de dureza para as ligas com Be. Foi escolhida uma das ligas comerciais para a reprodução em escala laboratorial (LAB) e industrial (IND). Estas ligas produzidas apresentaram as mesmas características microestruturais, químicas e físicas da liga comercial. Nos ensaios de fluidez, a liga LAB apresentou o mesmo comportamento da liga comercial. A liga IND apresentou limite de escoamento e módulo de elasticidade de ?e0,02%= 810MPa e E= 200 GPa, respectivamente. Os ensaios de corrosão mostraram comportamento passivo tanto para a liga comercial quanto para a liga IND em saliva artificial e enxaguante bucal. O ensaio de citotoxicidade da liga IND indicou comportamento não citotóxico em controle negativo (Chapa de Ti). Os resultados obtidos com a liga IND indicam a possibilidade de fabricação desta liga Ni-Cr para próteses dentárias em escala industrial. / This study aimed to develop nickel-chromium base alloys for dental prostheses with the best characteristics for subsequent production and application. Samples were acquired from eight manufacturers of commercial alloys. The materials were characterized in terms of chemical composition, mechanical properties, microstructure, melting temperature, coefficient of thermal expansion, corrosion and biocompatibility. For this, we have used X-ray fluorescence (XRF-WDS), ICP-OES, tensile tests, hardness testing, corrosion testing, evaluation of cytotoxicity, scanning electron microscopy (SEM), electron probe microanalysis (EDS) , X-ray diffraction (XRD), differential thermal analysis (DTA), dilatometry and evaluation of fluidity. Most of the chemical compositional determined in this study were not consistent with the compositions provided by the manufacturers. The results clearly showed the presence of a typical eutectic microstructure formed by Niss and NiBe in alloys containing Be, which can be considered a \"fingerprint\" of the presence of this element in these alloys. It was possible to verify the formation of intermetallics in the interdendritic region of the Be-free alloys. In one of the alloys this intermetallic was identified as (Nb6Ni16Si7), this alloy presenting a initial melting temperature below the eutectic melting of the Niss+NiB eutectic. Overall, the results of hardness tests showed superior hardness for alloys with Be. One of the commercial alloys was chosen for reproduction in laboratory (LAB) and industrial (IND) scales. The alloys produced showed the same microstructural characteristics, chemical and physical characteristics of the commercial alloy. In the fluidity tests, the LAB alloy showed the same behavior of the commercial alloy. The IND alloy presented yield strength and modulus of elasticity ?e0, 02% = 810MPa, E = 200 MPa, respectively. The corrosion tests showed passive behavior for both commercial and IND alloy in artificial saliva and mouthwash solutions. The cytotoxicity assay indicated that the IND alloy is not cytotoxic in the negative control (Ti plate). The results obtained with the IND alloy indicate the possibility of fabrication this alloy for dental prosthesis on an industrial scale.

O presente trabalho visou desenvolver ligas à base de Níquel-Cromo para prótese dentária, que confiram as melhores características metalúrgicas e químicas para posterior produção e aplicação. Para isto foram adquiridas amostras de ligas comerciais de 8 fabricantes. Os materiais foram caracterizados em termos de composição química, propriedades mecânicas, caracterização microestrutural, temperatura de fusão, coeficiente de expansão térmica, corrosão e biocompatibilidade. Para isto, utilizou-se as fluorescência de raios X (XRF-WDS), ICP-OES, ensaios de tração, ensaios de dureza, ensaios de corrosão, avaliação de citotoxicidade, microscopia eletrônica de varredura (MEV), microanálise eletrônica (EDS), difratometria de Raios X (DRX), análise térmica diferencial (DTA), dilatometria e avaliação de fluidez. A maioria dos resultados composicionais não condiz com as composições fornecidas pelos fabricantes. Os resultados mostraram claramente a presença de um eutético típico formado pelas fases Niss e NiBe nas ligas contendo Be, que pode ser considerado uma \"impressão digital\" da presença deste elemento nestas ligas. É possível verificar a formação de intermetálicos na região interdendritica para as ligas isentas de Be, sendo identificado um siliceto (Nb6Ni16Si7) em uma das ligas, que possui temperatura de inicio de fusão inferior ao eutético Niss e NiBe das ligas com Be. De uma forma geral, os resultados dos ensaios de dureza mostraram valores superiores de dureza para as ligas com Be. Foi escolhida uma das ligas comerciais para a reprodução em escala laboratorial (LAB) e industrial (IND). Estas ligas produzidas apresentaram as mesmas características microestruturais, químicas e físicas da liga comercial. Nos ensaios de fluidez, a liga LAB apresentou o mesmo comportamento da liga comercial. A liga IND apresentou limite de escoamento e módulo de elasticidade de ?e0,02%= 810MPa e E= 200 GPa, respectivamente. Os ensaios de corrosão mostraram comportamento passivo tanto para a liga comercial quanto para a liga IND em saliva artificial e enxaguante bucal. O ensaio de citotoxicidade da liga IND indicou comportamento não citotóxico em controle negativo (Chapa de Ti). Os resultados obtidos com a liga IND indicam a possibilidade de fabricação desta liga Ni-Cr para próteses dentárias em escala industrial. / This study aimed to develop nickel-chromium base alloys for dental prostheses with the best characteristics for subsequent production and application. Samples were acquired from eight manufacturers of commercial alloys. The materials were characterized in terms of chemical composition, mechanical properties, microstructure, melting temperature, coefficient of thermal expansion, corrosion and biocompatibility. For this, we have used X-ray fluorescence (XRF-WDS), ICP-OES, tensile tests, hardness testing, corrosion testing, evaluation of cytotoxicity, scanning electron microscopy (SEM), electron probe microanalysis (EDS) , X-ray diffraction (XRD), differential thermal analysis (DTA), dilatometry and evaluation of fluidity. Most of the chemical compositional determined in this study were not consistent with the compositions provided by the manufacturers. The results clearly showed the presence of a typical eutectic microstructure formed by Niss and NiBe in alloys containing Be, which can be considered a \"fingerprint\" of the presence of this element in these alloys. It was possible to verify the formation of intermetallics in the interdendritic region of the Be-free alloys. In one of the alloys this intermetallic was identified as (Nb6Ni16Si7), this alloy presenting a initial melting temperature below the eutectic melting of the Niss+NiB eutectic. Overall, the results of hardness tests showed superior hardness for alloys with Be. One of the commercial alloys was chosen for reproduction in laboratory (LAB) and industrial (IND) scales. The alloys produced showed the same microstructural characteristics, chemical and physical characteristics of the commercial alloy. In the fluidity tests, the LAB alloy showed the same behavior of the commercial alloy. The IND alloy presented yield strength and modulus of elasticity ?e0, 02% = 810MPa, E = 200 MPa, respectively. The corrosion tests showed passive behavior for both commercial and IND alloy in artificial saliva and mouthwash solutions. The cytotoxicity assay indicated that the IND alloy is not cytotoxic in the negative control (Ti plate). The results obtained with the IND alloy indicate the possibility of fabrication this alloy for dental prosthesis on an industrial scale.

L’eau supercritique peut être utilisée comme caloporteur à haute pression pour améliorer le rendement des centrales électriques. Pour un concept de réacteur nucléaire, la durée de vie des matériaux est un paramètre important en termes de sécurité. Par conséquent, les critères de sélection des matériaux pour un concept de réacteur à l’eau supercritique concernent les propriétés mécaniques à haute température pour une bonne tenue au fluage et à l’irradiation mais également une résistance à la corrosion généralisée et à la corrosion sous contrainte. Ce travail à pour objectif d’améliorer la compréhension des mécanismes de corrosion en eau supercritique à 600°C et 25 MPa pour des alliages c.f.c contenant du fer, du nickel et du chrome. Des essais de corrosion ont été réalisés sur des autoclaves échantillons d’alliages 316L et 690 en prenant en compte l’état de surface. Les couches d’oxydes formées ont été décrites en termes de morphologie, de composition et de structure, après caractérisations par microscopie électronique à balayage, par spectroscopie à décharge luminescente et par diffraction des rayons X. Si un comportement de type gazeux de l’eau supercritique est attendu dans les conditions d’essai, les résultats montrent une dissolution significative de certains éléments de l’alliage. Par conséquent, la corrosion en eau supercritique peut être considérée comme similaire à la corrosion aqueuse avec un effet de la température qui peut influencer la diffusion en phase solide par exemple. Pour l’alliage 690, la couche d’oxyde protectrice formée sur une surface polie est composée de chromine et surmontée d’un chromite ou d’un spinelle mixte de nickel et de fer. La double couche d’oxyde formée sur une surface de même finition pour l’alliage 316L semble moins protectrice. La couche externe de magnétite est poreuse et la couche interne riche en chrome est non homogène. Pour chaque alliage, l’étude des mécanismes de diffusion, grâce à des expériences utilisant des marqueurs ou des traceurs, révèle une croissance de la couche d’oxyde contrôlée par un processus anionique. Cependant, l’état de surface influence fortement les mécanismes de formation des couches d’oxyde. La comparaison des résultats sur l’acier suggère qu’il y a une concurrence entre l’oxydation du fer et celle du chrome. Une quantité suffisante de chrome est nécessaire pour former une fine couche d’oxyde protectrice. Les surfaces très déformées ou à microstructure à grains très fins conduisent à des fines couches d’oxyde de chrome, grâce à une forte densité de site de germination ou grâce aux courts-circuits de diffusion du chrome. L’état de surface est donc déterminant pour l’acier mais le même paramètre engendre des effets différents pour l’alliage à base de nickel. Les surfaces usinées deviennent sensibles à une oxydation interne du chrome, même si une fine couche d’oxyde continue et riche en chrome et manganèse se forme. Ce phénomène suggère une diffusion accélérée concurrentielle entre l’oxygène et le chrome. Pour conclure, ce travail propose un mécanisme de croissance de la couche d’oxyde dans chaque cas et discute des conditions favorables à la formation d’une couche d’oxyde protectrice riche en chrome dans l’optique d’une application au réacteur à eau supercritique. / Supercritical water can be use as a high pressure coolant in order to improve the thermodynamic efficiency of power plants. For nuclear concept, lifetime is an important safety parameter for materials. Thus materials selection criteria concern high temperature yield stress, creep resistance, resistance to irradiation embrittlement and also to both uniform corrosion and stress corrosion cracking.This study aims for supplying a new insight on uniform corrosion mechanism of Fe-Ni-Cr f.c.c. alloys in deaerated supercritical water at 600°C and 25MPa. Corrosion tests were performed on 316L and 690 alloys as sample autoclaves taking into account the effect of surface finishes. Morphologies, compositions and crystallographic structure of the oxides were determined using FEG scanning electron microscopy, glow discharge spectroscopy and X-ray diffraction. If supercritical water is expected to have a gas-like behaviour in the test conditions, the results show a significant dissolution of the alloy species. Thus the corrosion in supercritical water can be considered similar to corrosion in under-critical water assuming the higher temperature and its effect on the solid state diffusion. For alloy 690, the protective oxide layer formed on polished surface consists of a chromia film topped with an iron and nickel mixed chromite or spinel. The double oxide layer formed on 316L steel seems less protective with an outer porous layer of magnetite and an inhomogeneous Cr-rich inner layer. For each alloy, the study of the inner protective scale growth mechanisms by marker or tracer experiments reveals that diffusion in the oxide scale is governed by an anionic process. However, surface finishes impact deeply the growth mechanisms. Comparisons between the results for the steel suggest that there is a competition between the oxidation of iron and chromium in supercritical water. Sufficient available chromium is required in order to form a thin oxide layer. Highly deformed or ultra fine microstructure surfaces lead to thin chromium rich oxide layers thanks to either diffusion short circuiting or increasing Cr oxide nucleation site. The nature of the surface is a determining factor in the steel instance. The same parameter breeds different effects for the Ni-based alloy. Machined surfaces lead to internal oxidation on alloy 690 even if a thin Cr and Mn rich oxide scale is formed. Competitive diffusion of oxygen and Cr species through the diffusion short circuit paths of the alloy is suggested. This work proposes oxide growth mechanisms for each case. Finally the conditions leading to the formation of chromium-rich protective oxide films in supercritical water are discussed.

Made available in DSpace on 2014-12-17T14:57:48Z (GMT). No. of bitstreams: 1 TatianaOS.pdf: 1077719 bytes, checksum: 1af290e905d0475a70cb7e3bdfc3f743 (MD5) Previous issue date: 2008-07-19 / Metal ceramic restorations matches aesthetic and strength, and in your making occurs an interface oxide layer, wetting resulting and atomic and ionic interactions resulting between metal, oxide and porcelain. However, frequent clinical fails occurs in this restoration type, because lost homogeneous deposition oxide layer and lost interface bond. Thus, in this study, thought depositate homogeneous oxide films above Ni-Cr samples surfaces polite previously, at plasma oxide environment. Six samples was oxided at 300 and 400?C at one hour, and two samples was oxided in a comum chamber at 900?C, and then were characterized: optical microscopic, electronic microscopic, micro hardness, and X ray difratometry. Colors stripes were observed at six samples plasma oxided and a grey surface those comum oxided, thus like: hardness increase, and several oxides from basic metals (Ni-Cr) / As restaura??es odontol?gicas metalocer?micas combinam est?tica e resist?ncia, havendo na sua confec??o a forma??o de uma camada ?xida na interface metal-porcelana, que ? resultante das intera??es at?micas e i?nicas que ocorrem entre o metal, o ?xido e a porcelana, resultando na ades?o qu?mica entre o metal e a porcelana. Entretanto, s?o comuns as falhas cl?nicas observadas neste tipo de restaura??o, devido ? falta de uniformidade na deposi??o da camada ?xida e da conseq?ente perda de adesividade na interface. O objetivo do presente trabalho foi realizar a deposi??o de filmes ?xidos uniformes sobre a superf?cie de amostras compostas por liga met?lica odontol?gica de Ni-Cr previamente polidas, a partir de processamento em atmosfera oxidante a plasma. As amostras foram oxidadas a plasma a 300? e 400?C durante uma hora, enquanto outras foram oxidadas em forno resistivo, a temperatura de 900 ?C, tamb?m durante uma hora. Foram realizadas caracteriza??es do ?xido formado utilizando: microscopia ?ptica e eletr?nica de varredura, microdureza, e difratometria de Raios-X. Observou-se a forma??o de faixas e zonas de diversas cores nas amostras oxidadas a plasma e a forma??o de uma superf?cie de cor acinzentada nas amostras oxidadas em forno comum. Ocorreu a ades?o da porcelana ao metal nas amostras oxidadas a plasma, assim como nas oxidadas convencionalmente. Entretanto, no tratamento a plasma ocorreu a forma??o de ?xidos adesivos a temperatura de 300? e 400?C, o que representa um ganho energ?tico, quando se compara ? temperatura preconizada para os tratamentos convencionais, que margeia os 900?C. Al?m disso, o tratamento a plasma permitiu uma varia??o na t?cnica de tratamento convencional, a da n?o realiza??o do jateamento do metal com ?xido de alum?nio, para a promo??o do embricamento mec?nico

Il est important pour l’industrie nucléaire de mener des études amont pour mieux appréhender les phénomènes en lien avec la corrosion des alliages chromino-formeurs. Cette étude a pour objectif de mieux comprendre les paramètres influant sur les mécanismes et la cinétique de croissance des couches de chromine formées par oxydation à haute température. Ce travail s’articule en deux parties complémentaires : une partie de modélisation qui est focalisée sur les aspects cinétiques, et une partie expérimentale axée sur la compréhension des mécanismes de croissance de la chromine. La partie modélisation a pour objectif de prendre en compte l’effet des courts-circuits de diffusion dans la description des cinétiques de croissance de la chromine. Le but est d’évaluer quantitativement comment une diffusion mixte par le volume et les joints de grains peut influencer la cinétique de croissance d’une couche d’oxyde dont la microstructure évolue avec le temps. Ce travail a été réalisé à l’aide de modèles analytiques et grâce à de nouveaux développements d’un modèle numérique existant (EKINOX). Plusieurs lois de croissance de grains ont été étudiées (croissance parabolique, croissance cubique et prise en compte de l’existence d’un gradient de taille de grains dans la couche d’oxyde). Une étude paramétrique a été réalisée pour étudier l’influence de la vitesse de croissance des grains sur la cinétique de croissance de la couche de chromine. Ces simulations ont permis d’évaluer la déviation de lacinétique d’oxydation par rapport à la loi parabolique simple suivant la vitesse de croissance des grains d’oxyde, choisie comme donnée d’entrée du modèle. Ces calculs permettent également d’évaluer les ordres de grandeurs de la durée du régime transitoire durant lequel l’évolution de la taille de grains de l’oxyde influence la cinétique d’oxydation de façon significative. Les cinétiques d’oxydation calculées pour les différents cas étudiés ont été extrapolées à l’aide des méthodes classiquement utilisées dans le domaine de l’oxydation à haute température : la méthode « log-log» et la méthode dite du « kp local ». La comparaison des extrapolations et des solutions exactes permet de proposer des « bonnes pratiques » à adopter pour interpréter les cinétiques d’oxydation expérimentales. Dans la partie expérimentale de ce travail, des essais d’oxydation d’un alliage modèle Ni-30Cr à 700°C sous atmosphère d’argon technique (10-5 atm de O2) ont été réalisés en thermobalance pour des durées allant de 30 minutes à 50 heures. La couche de chromine formée à l’issue de ces essais a été finement caractérisée afin de déterminer le mécanisme d’oxydation ainsi que l’étape cinétiquement limitante. Dans les conditions de l’étude, la couche d’oxyde formée a été identifiée comme étant de la chromine de structure corindon dont les grains adoptent une orientation préférentielle de croissance <0001>. La cinétique d’oxydation suit une loi parabolique au terme d’un régime transitoire de 3 h environ. La valeur de la constante cinétique parabolique kp a été évaluée pendant le régime stationnaire et est égale à 10-15 cm2 s-1. Des expériences d’oxydation séquencée et de marqueurs ont également été réalisées. Elles ont permis de mettre en évidence une croissance anionique de la couche de chromine. La croissance de l’oxyde apparait, selon les essais de marquage isotopique dans 18O2, contrôlée par la diffusion de l’oxygène par les joints de grains et le volume de l’oxyde. Les analyses complémentaires des couches d’oxyde, par photoélectrochimie, suggèrent que le défaut majoritaire permettant cette diffusion est la lacune d’oxygène. Enfin, la morphologie de la couche d’oxyde indique une croissance plus rapide de la couche au niveau des joints de grains de métal / This thesis aims to better understand the kinetics and mechanisms of growth of chromia scales. This work is articulated in two complementary parts, on the one hand a modeling part which studies the kinetic aspects, and on the other hand an experimental part centered on the characterization of chromia growth understanding of the mechanisms. The purpose of the modeling part is to take into account the effect of diffusion short circuits in chromia the growth kinetics. The aim is to understand how a dual diffusion by both volume and grain boundaries can impact oxidation kinetics. This approach helps to define "good practices" for experimental oxidation kinetics interpretation. This modeling work was done using analytical models EKINOX numerical model. Several grain growth laws have been studied (parabolic growth, cubic growth, and grain size gradient). In addition, a parametric study was carried out to study the influence of grain growth rate on the growth kinetics of chromia. Calculations of oxidation kinetics for the various cases treated made it possible to conclude that the taking into account diffusion short circuits and their proportion evolution in time generates a deviation of the oxidation kinetics from a simple parabolic law. The rate of oxidation kinetics calculated varies with the growth rate of the oxide grains chosen as input data of the modelling. When kinetics are treated using a kinetic law involving a growth rate that changes over time, it is possible to determine the time range for which the evolution of oxide grain size significantly influences the oxidation kinetics. The oxidation kinetics modeled for the different cases were extrapolated using the methods conventionally used in high temperature oxidation, the log-log method and the local kp method. To extrapolate experimental kinetics, it is recommended to use the local kp method beforehand in order to know if the steady state has been reached. For the second experimental part, oxidation tests of the model alloy Ni-30Cr at 700°C in technical argon atmosphere were carried out. The chromia layer formed at the end of these tests was finely characterized in order to determine the oxidation mechanism as well as the kinetically limiting step. Under the conditions of the study, the nature of the oxide layer was identified as chromia. The oxidation kinetics follows a parabolic law after a transient stage that lasts about 3 hours. The stationary kp value has been determined. The mechanism of chromia growth has been identified as the diffusion of oxygen by the grain boundaries and the volume of the oxide. The morphology of the oxide layer indicates a faster oxidation over the grain boundaries of the metal. Finally, the chromine grains adopt a preferential orientation in the <0001> direction of the corundum structure. Chromium depletion profiles have been determined in the metal substrate and indicate a more pronounced chromium depletion at the grain boundaries of the metal. The type of semiconduction was determined in chromine and reveals an n-type semiconduction for an oxidation time of 7 h and an n-type and insulating semiconduction for an oxidation time of 50 h.