The effect of thermo-mechanical processing by deformation and annealing on the grain boundary configuration of commercially pure Ni-200 is reported in this thesis. Ni-200 is unalloyed, thus avoiding the complex effects associated with alloying elements on the formation and development of different types of grain boundaries. One step strain-recovery with strain levels in the range of 3% to 7.5% (with 1.5% intervals) and annealing temperatures in the range of 800ºC to 1000ºC (with 100ºC intervals) were used in processing. The effects of parameters such as strain level, annealing temperature, annealing time and grain growth on grain boundary configurations were studied. Using Orientation Image Microscopy (OIM) it was found that the Fsp (fraction of special grain boundaries) value of strained samples annealed in the range of 800ºC to 1000ºC began to increase after a critical length of time, after which the Fsp value increased quickly and becoming a maximum in 2~4 minutes. The length of the critical annealing time for the increase of Fsp was shorter in the material with the higher levels of strain at a constant annealing temperature. Also the critical annealing time was shorter when annealed at higher temperatures under a fixed level of strain. The Fsp value increased to 80% from an as received value of about 30% in the samples with varying strain levels. However, the Fsp values only increased from 30% to 45% in the material without strain. Due to grain boundary migration, the Fsp values increased with grain size and became a maximum during the heat treatment of the strained material. In the material without strain however even when grain growth occurred, limited improvement in Fsp values occurred showing that contribution of strain is very important to the formation of special boundaries. By varying the strain levels, annealing temperatures and times, material with high Fsp values in a wide range of grain size can be obtained. Under the present processing conditions used however, multi-cycle was not helpful to the improvement of Fsp. TEM observations indicated dislocation tangles occurred near the grain boundary of the 1x6% strained samples. These dislocation tangles decreased with time at 800˚C and were reduced considerably after 20 minutes. Thermodynamic and kinetic models were used in the calculations of twin density-grain size relationships. The results indicated that the contribution of strain is equivalent to the increase of grain boundary energy, which provided an extra driving force and improved probability of twin embryo formation.

The effect of thermo-mechanical processing by deformation and annealing on the grain boundary configuration of commercially pure Ni-200 is reported in this thesis. Ni-200 is unalloyed, thus avoiding the complex effects associated with alloying elements on the formation and development of different types of grain boundaries. One step strain-recovery with strain levels in the range of 3% to 7.5% (with 1.5% intervals) and annealing temperatures in the range of 800ºC to 1000ºC (with 100ºC intervals) were used in processing. The effects of parameters such as strain level, annealing temperature, annealing time and grain growth on grain boundary configurations were studied. Using Orientation Image Microscopy (OIM) it was found that the Fsp (fraction of special grain boundaries) value of strained samples annealed in the range of 800ºC to 1000ºC began to increase after a critical length of time, after which the Fsp value increased quickly and becoming a maximum in 2~4 minutes. The length of the critical annealing time for the increase of Fsp was shorter in the material with the higher levels of strain at a constant annealing temperature. Also the critical annealing time was shorter when annealed at higher temperatures under a fixed level of strain. The Fsp value increased to 80% from an as received value of about 30% in the samples with varying strain levels. However, the Fsp values only increased from 30% to 45% in the material without strain. Due to grain boundary migration, the Fsp values increased with grain size and became a maximum during the heat treatment of the strained material. In the material without strain however even when grain growth occurred, limited improvement in Fsp values occurred showing that contribution of strain is very important to the formation of special boundaries. By varying the strain levels, annealing temperatures and times, material with high Fsp values in a wide range of grain size can be obtained. Under the present processing conditions used however, multi-cycle was not helpful to the improvement of Fsp. TEM observations indicated dislocation tangles occurred near the grain boundary of the 1x6% strained samples. These dislocation tangles decreased with time at 800˚C and were reduced considerably after 20 minutes. Thermodynamic and kinetic models were used in the calculations of twin density-grain size relationships. The results indicated that the contribution of strain is equivalent to the increase of grain boundary energy, which provided an extra driving force and improved probability of twin embryo formation.

O objetivo deste estudo in vitro foi analisar o comportamento superficial do titânio comercialmente puro (grau 2 ASTM) usinado e obtido pelo processamento de metalurgia do pó sob a ação de diferentes soluções fluoretadas, através da análise do grau de corrosão em microscopia óptica (MO) e da rugosidade superficial. Além disso, o estudo se propôs a comparar essas análises com os resultados obtidos com o titânio fundido da dissertação de mestrado de Barros (2004). Todas as amostras receberam procedimento metalográfico padrão e foram divididas em grupos: Gr.1- saliva artificial com pH 7.0 (controle), Gr.2- gel de flúor fosfato acidulado a 1,23% com pH 3.5, Gr.3- gel de NaF a 2% com pH 6.5, Gr.4- solução de NaF a 0,05% com pH 4.0 e Gr.5- solução de NaF a 0,05% com pH 7.5. As amostras foram expostas a estas soluções por 1, 4, 8 e 16 min, intercaladas com imersão em saliva artificial por 24 h, e depois foram observadas em MO e MEV, a cada intervalo de tempo. As imagens em MO, 100x, foram classificadas através de escores de 0 a 4, conforme o grau de corrosão. A rugosidade foi analisada utilizando o parâmetro Ra. Os resultados da análise de MO foram tratados estatisticamente pelo teste qui-quadrado e da rugosidade pelo teste F de Snedecor e de Bonferroni (p<0,05). Nos três tipos de amostras, o Gr2 apresentou a corrosão mais severa, e os Gr.4 e 5 apresentaram os menores graus de corrosão. Entretanto, nas amostras usinadas o Gr5 apresentou uma corrosão menos acentuada em relação ao Gr4. No Gr3 houve um aumento da corrosão em função do tempo, sendo que as amostras fundidas mostraram este aumento mais rapidamente. Houve um aumento significativo na rugosidade superficial no Gr.2 nos três tipos de amostras. Nos diversos grupos, os valores de rugosidade superficial das amostras fundidas foram significantemente maiores que os das usinadas e as de metalurgia do pó. Os autores concluíram que as soluções fluoretadas de uso odontológico são danosas às superfícies do titânio fundido, usinado e metalurgia do pó, principalmente as soluções com alta concentração de fluoreto. / The purpose of this in vitro study was to analyze the superficial behavior of commercially pure titanium (grade 2, ASTM), obtained by milling or powder metallurgical process, under the action of different fluoride solutions through the analysis of corrosion grade under an optical microscope (OM) and superficial roughness. Furthermore the results obtained from such analyses were compared with the ones of cast titanium from Barross masters degree dissertation (2004). All specimens received the standard metallography procedure for titanium, and were divided into the following groups, according to the attack solution received: Gr.1- synthetic saliva with pH 7.0 (control), Gr.2- 1.23% acidulated phosphate fluoride gel with pH 3.5, Gr.3- 2% NaF gel with pH 6.5, Gr.4- 0.05% NaF solution with pH 4.0, and Gr.5- 0.05% NaF solution with pH 7.5. The specimens were exposed to these solutions for 1, 4, 8, and 16 minutes, and between each of these times they were immersed in synthetic saliva for 24 h. The surfaces of samples were observed under OM and SEM at each interval time. The images of 100x in OM were classified by means of scores which ranged from 0 to 4, according to corrosion grade. The rugosity was analyzed using Ra parameter. The results of OM analysis were statistically treated by means of Chi-square test and of rugosity through Snededor F test and Bonferroni test (p<0,05). In the three different types of samples, the Gr2 presented the most severe corrosion, and the Gr.4 and 5 showed the smallest corrosion grade. However in the milled samples Gr5 showed a less Sharp corrosion than Gr4. The corrosion grade of Gr3 increased according to time, but the cast specimens showed this increase more quickly. There was a significant increase in the superficial rugosity in the Gr.2 in the three types of samples. In the several groups the values of the superficial rugosity of the cast samples were significantly greater than the milled and powder metallurgical ones. The authors concluded that the fluoride solutions used in dentistry are harmful to the surfaces of cast, milled and powder metallurgical titanium, mainly the solutions with high fluoride concentration.

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O objetivo deste estudo in vitro foi analisar o comportamento superficial do titânio comercialmente puro (grau 2 ASTM) usinado e obtido pelo processamento de metalurgia do pó sob a ação de diferentes soluções fluoretadas, através da análise do grau de corrosão em microscopia óptica (MO) e da rugosidade superficial. Além disso, o estudo se propôs a comparar essas análises com os resultados obtidos com o titânio fundido da dissertação de mestrado de Barros (2004). Todas as amostras receberam procedimento metalográfico padrão e foram divididas em grupos: Gr.1- saliva artificial com pH 7.0 (controle), Gr.2- gel de flúor fosfato acidulado a 1,23% com pH 3.5, Gr.3- gel de NaF a 2% com pH 6.5, Gr.4- solução de NaF a 0,05% com pH 4.0 e Gr.5- solução de NaF a 0,05% com pH 7.5. As amostras foram expostas a estas soluções por 1, 4, 8 e 16 min, intercaladas com imersão em saliva artificial por 24 h, e depois foram observadas em MO e MEV, a cada intervalo de tempo. As imagens em MO, 100x, foram classificadas através de escores de 0 a 4, conforme o grau de corrosão. A rugosidade foi analisada utilizando o parâmetro Ra. Os resultados da análise de MO foram tratados estatisticamente pelo teste qui-quadrado e da rugosidade pelo teste F de Snedecor e de Bonferroni (p<0,05). Nos três tipos de amostras, o Gr2 apresentou a corrosão mais severa, e os Gr.4 e 5 apresentaram os menores graus de corrosão. Entretanto, nas amostras usinadas o Gr5 apresentou uma corrosão menos acentuada em relação ao Gr4. No Gr3 houve um aumento da corrosão em função do tempo, sendo que as amostras fundidas mostraram este aumento mais rapidamente. Houve um aumento significativo na rugosidade superficial no Gr.2 nos três tipos de amostras. Nos diversos grupos, os valores de rugosidade superficial das amostras fundidas foram significantemente maiores que os das usinadas e as de metalurgia do pó. Os autores concluíram que as soluções fluoretadas de uso odontológico são danosas às superfícies do titânio fundido, usinado e metalurgia do pó, principalmente as soluções com alta concentração de fluoreto. / The purpose of this in vitro study was to analyze the superficial behavior of commercially pure titanium (grade 2, ASTM), obtained by milling or powder metallurgical process, under the action of different fluoride solutions through the analysis of corrosion grade under an optical microscope (OM) and superficial roughness. Furthermore the results obtained from such analyses were compared with the ones of cast titanium from Barross masters degree dissertation (2004). All specimens received the standard metallography procedure for titanium, and were divided into the following groups, according to the attack solution received: Gr.1- synthetic saliva with pH 7.0 (control), Gr.2- 1.23% acidulated phosphate fluoride gel with pH 3.5, Gr.3- 2% NaF gel with pH 6.5, Gr.4- 0.05% NaF solution with pH 4.0, and Gr.5- 0.05% NaF solution with pH 7.5. The specimens were exposed to these solutions for 1, 4, 8, and 16 minutes, and between each of these times they were immersed in synthetic saliva for 24 h. The surfaces of samples were observed under OM and SEM at each interval time. The images of 100x in OM were classified by means of scores which ranged from 0 to 4, according to corrosion grade. The rugosity was analyzed using Ra parameter. The results of OM analysis were statistically treated by means of Chi-square test and of rugosity through Snededor F test and Bonferroni test (p<0,05). In the three different types of samples, the Gr2 presented the most severe corrosion, and the Gr.4 and 5 showed the smallest corrosion grade. However in the milled samples Gr5 showed a less Sharp corrosion than Gr4. The corrosion grade of Gr3 increased according to time, but the cast specimens showed this increase more quickly. There was a significant increase in the superficial rugosity in the Gr.2 in the three types of samples. In the several groups the values of the superficial rugosity of the cast samples were significantly greater than the milled and powder metallurgical ones. The authors concluded that the fluoride solutions used in dentistry are harmful to the surfaces of cast, milled and powder metallurgical titanium, mainly the solutions with high fluoride concentration.

Conselho Nacional de Desenvolvimento CientÃfico e TecnolÃgico / A indÃstria de petrÃleo requer materiais com caracterÃsticas especÃficas como a alta resistÃncia mecÃnica e à corrosÃo, por isso tem investido em pesquisas de novos materiais. Destas pesquisas surgem possibilidades da utilizaÃÃo dos aÃos inoxidÃveis superduplex para atender tais expectativas, no entanto, o efeito dos ciclos tÃrmicos de soldagem pode ser prejudicial Ãs propriedades destas ligas, por meio da alteraÃÃo microestrutural ferrita/austenita e da precipitaÃÃo de fases intermetÃlicas. Desta forma, este trabalho tem como objetivo avaliar a influÃncia da energia de soldagem sobre a resistÃncia à corrosÃo e as transformaÃÃes microestruturais na soldagem multipasse, pelo processo MIG/MAG, do aÃo inoxidÃvel superduplex UNS S32760. Foram produzidas e utilizadas juntas soldadas modificando-se a energia de soldagem nos nÃveis 0,5, 1,0 e 2,0 kJ/mm. Duas regiÃes da junta soldada foram obtidas para estudo: a Zona Fundida (ZF) e a Zona Afetada pelo Calor (ZAC). Uma amostra sem sofrer soldagem foi utilizada como referÃncia. A resistÃncia à corrosÃo foi avaliada por meio das tÃcnicas eletroquÃmicas: monitoramento do potencial de circuito aberto, polarizaÃÃo potenciodinÃmica, espectroscopia de impedÃncia eletroquÃmica e da temperatura crÃtica de pite (CPT). Os ensaios eletroquÃmicos mostraram que a ZAC da energia 1,0 kJ/mm se mostrou mais susceptÃvel a corrosÃo. O ensaio CPT nÃo mostrou diferenÃa significativa nos resultados. A nucleaÃÃo dos pites ocorreu na fase ferrÃtica tanto na regiÃo da ZAC e ZF e nÃo apresentou uma relaÃÃo com as regiÃes onde havia a precipitaÃÃo de fases intermetÃlicas.Os resultados indicaram que a energia de soldagem foi o fator que exerceu maior influÃncia sobre o teor mÃdio de ferrita na regiÃo da raiz das juntas. Houve precipitaÃÃes de nitretos de cromo em todas as energias e de fase sigma na energia de 1,0 kJ/mm e 2,0 kJ/mm. Foi observado que as composiÃÃes quÃmicas entre as fases ferrita e austenita sÃo bastante semelhantes, porÃm a fase ferrÃtica apresentou um PREN inferior ao da austenita. / The oil industry requires materials with special properties such as high mechanical and corrosion resistance, so it has invested in research of new materials.These researches permit the use of super duplex stainless steels to meet such expectations.However, the effect of welding thermal cycles can be harmful to the properties of these alloys by modifying ferrite/austenite microstructure and intermetallic phases precipitation. The aim of this work is therefore to evaluate the influence of heat input on corrosion resistance and microstructural transformations of super duplex stainless steel UNS S32760 in multipass welding process MIG/MAG. The samples were produced and welded joints were prepared by modifying the heat input at levels of 0.5, 1.0 and 2.0 kJ/mm.Two regions of the welded joint were obtained for study: moltenzone (ZF) and the heat affected zone (ZAC). A sample unwelding was used as reference. The corrosion resistance was evaluated by means of electrochemical techniques: open circuit potentialmonitoring,potentiodynamic polarization, electrochemical impedance spectroscopy and determination of critical pitting temperature (CPT).The electrochemical tests showed that ZAC energy 1.0 kJ/mm was more susceptible to corrosion. The CPT test showed no significant difference in the results., The nucleation of pits occurred in the ferritic phase in both the regions ZAC and ZF and did not show a relationship with the regions where precipitation occurred intermetallic phases. The results indicated that the heat input was the factor that had the greatest influence on the average content of ferrite in the root zone of the joints. There was precipitation of chromium nitrides in all samples and sigmaphase in the samples of 1.0 kJ/mm and 2.0 kJ/mm. It was observed that the chemical compositions between the ferrite and austenite phases are fairly similar, but the ferrite phase has presented a pitting resistance equivalente (PREN) lower than the austenite.

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Made available in DSpace on 2014-10-09T12:33:21Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:06:31Z (GMT). No. of bitstreams: 0 / Neste trabalho foi investigado o efeito de vários tratamentos para modificação da superfície na resistência à corrosão do alumínio AA1050 com o objetivo de identificar um potencial substituto ao tratamento de cromatização. Os tratamentos adotados consistiram inicialmente de polimento da superfície até acabamento 1 m, seguido por uma etapa comercial. Este tratamento foi utilizado como preparação preliminar da superfície, anterior aos demais tratamentos testados. Amostras com o tratamento preliminar foram submetidas a diferentes tratamentos de modificação da superfície, especificamente, imersão em solução com moléculas auto-organizáveis (SAM) à base de difosfonato, imersão em água fervente para acelerar o crescimento de óxido-hidróxido de alumínio; uma combinação destes dois últimos tratamentos e cromatização em solução à base de cromo hexavalente. O comportamento de corrosão do alumínio AA1050 submetido aos diferentes tipos de tratamentos foi investigado por ensaios eletroquímicos como: medidas de potencial a circuito aberto em função do tempo de imersão, espectroscopia de impedância eletroquímica e ensaios de polarização potenciodinâmica. Utilizou-se solução de 0,5 M de Na2SO4 como meio corrosivo, tamponada a pH = 4,0. Microscopia eletrônica de varredura e análises semi-quantitativas de espectroscopia de energia dispersiva também foram utilizadas como medidas complementares nessa investigação. Observou-se que o tratamento com moléculas auto-organizáveis não se mostrou eficiente para proteção à corrosão para longos períodos de tempo em comparação aos demais tratamentos. A proteção fornecida pelos tratamentos, SAM e em solução a base de cromo hexavalente foi inferior à esperada. A etapa de boemitização ou crescimento acelerado de óxido-hidróxido de alumínio em água fervente se mostrou uma etapa essencial para aumento do desempenho frente à corrosão do alumínio AA1050. Os resultados obtidos para amostras submetidas ao tratamento de aceleração do crescimento de óxi-hidróxido seguido por imersão em solução com moléculas auto-organizáveis proporcionou uma melhora significativa na resistência à corrosão da superfície comparada aos demais tratamentos. / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第18277号 / 工博第3869号 / 新制||工||1593(附属図書館) / 31135 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 松原 英一郎, 教授 杉村 博之, 教授 邑瀬 邦明 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM