Os componentes automotivos em geral devem atender a especificações rigorosas de propriedades mecânicas, requisitos de limpeza inclusionária, entre outros. Enxofre e alumínio são elementos adicionados ao banho líquido de aço que desempenham um papel importante na obtenção destas propriedades. Porém, eles que dificultam o processo de produção por lingotamento contínuo por favorecerem a formação de partículas sólidas de alto ponto de fusão, que podem causar a obstrução das válvulas de lingotamento e dificultar o processo de desenvolvimento de aços com alta limpeza inclusionária. O objetivo do presente trabalho foi estudar a composição química do aço DIN 38MnSiVS6, focando nos elementos químicos que afetam a formação e remoção de inclusões, assim como a composição química da escória e outros parâmetros da aciaria como a temperatura e a lingotabilidade do processo de produção em escala industrial. Neste estudo, foi avaliada a hipótese de melhoria da lingotabilidade e da limpeza do aço através da alteração da etapa de adição de enxofre e também da quantidade de adição de cálcio Amostras de aço retiradas ao longo do processo foram analisadas através de microscopia ótica e eletrônica de varredura e também por ultrassom por imersão. Os dados de composição química foram sobrepostos a janelas de lingotabilidade e as características das escórias foram avaliadas por simulação termodinâmica. Foram avaliadas as correlações entre os resultados das diferentes técnicas de análise e com as referências de literatura. A hipótese de redução da quantidade de cálcio se mostrou satisfatória tanto para a melhoria da lingotabilidade quanto para a limpeza do aço. Porém, a alteração da etapa de adição de enxofre necessita de mais testes para comprovar sua eficiência. Dentre as técnicas empregadas, o uso do microscópio eletrônico de varredura acoplado a um sistema automatizado de análise de inclusões (ASPEX) se mostrou como uma ferramenta vantajosa por fornecer uma ampla gama de informações que podem auxiliar no entendimento da lingotabilidade e da limpeza inclusionária do aço. / Automotive components in general must meet stringent specifications of mechanical properties, inclusionary cleanliness requirements, among others. Sulfur and aluminum are elements added to the liquid steel bath which play an important role in obtaining these properties, but which hinder the production process by continuous casting by favoring the formation of solid particles of high melting point, that can cause the nozzle clogging and hamper the development process of steels with high inclusionary cleanliness. The aim of the present work is to study the chemical composition of the DIN 38MnSiVS6 steel, focusing on the chemical elements that affect the formation and removal of inclusions, as well as the chemical composition of the slag and other parameters such as temperature and castability in an industrial scale production process. In this study, the hypothesis steel cleanliness improvement was evaluated by changing the stage of sulfur addition as well as the amount of calcium addition. Steel samples collected throughout the process were analyzed by optical and scanning electron microscopy, and by immersion ultrasound. The chemical composition data were superimposed on liquid windows and the slag characteristics were evaluated by thermodynamic simulation. The correlations between the results of the different analysis techniques and the literature references were evaluated. The hypothesis of reduction in the amount of calcium was satisfactory both for the improvement of the castability and for the cleanliness of the steel, but the change of the sulfur addition stage requires more tests to prove its efficiency. The scanning electron microscope coupled with an automated inclusion analysis system (ASPEX) has proved to be an advantageous tool to provide a wide range of information that can help in the understanding of the castability and cleanliness of steel.

A limpeza dos aços está diretamente associada ao conteúdo de óxidos dos mesmos, sendo que os diferentes tipos de inclusões não-metálicas presentes podem prejudicar desde os processos de fabricação e conformação até as características necessárias para a aplicação do produto final. As inclusões se formam e se modificam ao longo dos processos de fabricação, e estão relacionadas principalmente às práticas de refino secundário e de lingotamento. Essas inclusões estão sempre presentes nos aços, de modo que é impossível se produzir um aço completamente livre das mesmas. Atualmente, existe uma série de pesquisas buscando o desenvolvimento de práticas e de processos para incrementar a limpeza dos aços. Entre essas está o desenvolvimento de novos materiais refratários adequados às diversas etapas de uma Aciaria. Com especial importância na limpeza dos aços estão as práticas e tecnologias aplicadas no lingotamento contínuo. Neste trabalho foi avaliada a influência do uso de nitrogênio injetado através de poros no colo das válvulas submersas sobre a lingotabilidade e limpeza dos produtos laminados a partir de tarugos. Para este estudo foram testadas diferentes vazões de gás e depois mensurado seu efeito. As técnicas utilizadas para a avaliação foram: verificação da abertura dos tampões; índice de sucateamento nas linhas de inspeção; severidade em ultrassom pelo método de imersão; análise dos teores de oxigênio total e nitrogênio e análise pelo método de distribuição de valores extremos da maior inclusão estimada. Os resultados práticos foram então comparados entre os lotes escolhidos para o teste. Verificou-se através dos dados coletados boa compatibilidade entre as diferentes variáveis e coerência dos resultados com os relatos da literatura. O uso de gás nitrogênio se mostrou ser potencialmente benéfico para a melhoria da limpeza e lingotabilidade do aço, apesar de mais testes serem necessários para a validação das hipóteses levantadas. / The steel cleanliness is directly associated to its inclusion content. The different kind of non-metallic inclusion can harm from the manufacturing and forming processes up to the demanding characteristics for the final products. The inclusions are formed and modified along the steel manufacturing process, and they are related mainly to the secondary refining and casting of steel. These inclusions are always present in the steel, so it is hardly possible to produce steels completely free of them. Nowadays, there are several fields of research concerning with the development of practices and processes to improve steel cleanliness. The development of new lining materials which are suitable for each melting shop step is one of these fields. With special importance over the steel cleanliness issue, the practices and technologies applied to the continuous casting process can be cited. In this work, the influence of nitrogen injection though the pores of the submerged entry nozzle over the castability and cleanliness of rolled products was evaluated. For this study, different gas flows were tested and then measured its effects. The techniques used for the evaluation were: stopper rod opening; rejection index during the inspection lines; severity in immersion ultra-sonic inspection; total oxygen and nitrogen content analysis and largest inclusion diameter estimated by extreme values distribution. The practical results for each lot of steel were then compared. It was verified from, the collected data, good compatibility between these different variables and coherency of the results with the experiences reported in the literature. The use of nitrogen gas showed itself to be potentially good for the improvement of cleanliness and castability of steel, though more trials are necessary for the validation of the considered hypothesis.

Há uma demanda por competitividade entre as indústrias de aços, a fim de alcançar a excelência definida pelo termo clean steel. O processo de desgaseificação a vácuo (VD) ocorre durante o Refino Secundário de aços especiais. Sua principal função é remover gases indesejáveis, especialmente o hidrogênio. Entretanto, durante este processo, o fenômeno de flotação e a absorção de inclusões são reportados. O objetivo do presente trabalho foi estudar a viscosidade de escórias e a capacidade da estação de desgaseificação a vácuo do tipo tanque na limpeza de aços sob uma perspectiva industrial. Para realizar este objetivo, foram coletadas amostras de escória e aço antes e após a etapa de vácuo. Os resultados em limpeza de aço foram relacionados à energia de agitação durante o tratamento a vácuo (associada a um parâmetro cinético - βs) e ao efeito da viscosidade de escórias. É possível observar um decréscimo expressivo na população de inclusões entre as condições antes e após tratamento de desgaseificação a vácuo. A remoção de inclusões durante o vácuo atinge 64, 75 e 78% para as faixas de diâmetro de 2,5-5, 5-15 e ≥ 15 μm, respectivamente. Após o processo de desgaseificação, a composição das inclusões não-metálicas aproxima-se da composição química da escória. O processo de agitação na estação de desgaseificação a vácuo promove uma diminuição significativa na densidade de inclusões na faixa de diâmetro de 2,5-15 μm. Além disso, ao aumentar a intensidade do parâmetro cinético, a composição química de inclusões não-metálicas foi afetada e o teor de enxofre presente no aço líquido foi reduzido. Quanto às viscosidades efetiva das escórias, conclui-se que, para valores mais baixos (0,20 Pa.s) aumenta-se a capacidade da escória na remoção de inclusões, enquanto que valores mais altos (> 0,40 Pa.s) aparentaram ser prejudiciais à limpeza do aço. / There is a demand in competitiveness within the steel industry towards achieving excellence defined by clean steel term. The process of vacuum degassing (VD) occurs during the secondary refining of special steels. Its main function is to remove undesirable gases, primarily hydrogen. However, during this process, flotation phenomenon and inclusions absorption are reported. The aim of the present work was to study the slag viscosity and vacuum degassing (tank type) capacity in steel cleanliness from an industry perspective. To achieve this objective, slag and steel samples were taken before and after vacuum stage. The results in steel cleanliness were related to the stirring energy of the vacuum station (associated to a kinetic parameter – βs) and to the effect of slag viscosity. It is possible to observe an expressive decrease in the population of inclusions between the conditions before and after vacuum degassing treatment. The removal of inclusions during the vacuum stage reaches 64, 75 and 78% in the diameter ranges of 2,5-5, 5-15 and ≥ 15 μm, respectively. After the degassing process, the composition of non-metallic inclusions seemed to approach the slags’ chemical compositions. The stirring process in the vacuum degassing station promotes a significant decrease in the inclusion density with 2,5-15 μm diameter range. Also, by increasing the kinetic parameter intensity, the composition of non-metallic inclusions was affected. The sulfur content present in liquid steel was reduced. Regarding the effective viscosities of slags, it was concluded that lower values (0,20 Pa.s) increased slag capacity in inclusion removal, whereas higher values (> 0,40 Pa.s) was detrimental to steel cleanliness.

Os componentes automotivos em geral devem atender a especificações rigorosas de propriedades mecânicas, requisitos de limpeza inclusionária, entre outros. Enxofre e alumínio são elementos adicionados ao banho líquido de aço que desempenham um papel importante na obtenção destas propriedades. Porém, eles que dificultam o processo de produção por lingotamento contínuo por favorecerem a formação de partículas sólidas de alto ponto de fusão, que podem causar a obstrução das válvulas de lingotamento e dificultar o processo de desenvolvimento de aços com alta limpeza inclusionária. O objetivo do presente trabalho foi estudar a composição química do aço DIN 38MnSiVS6, focando nos elementos químicos que afetam a formação e remoção de inclusões, assim como a composição química da escória e outros parâmetros da aciaria como a temperatura e a lingotabilidade do processo de produção em escala industrial. Neste estudo, foi avaliada a hipótese de melhoria da lingotabilidade e da limpeza do aço através da alteração da etapa de adição de enxofre e também da quantidade de adição de cálcio Amostras de aço retiradas ao longo do processo foram analisadas através de microscopia ótica e eletrônica de varredura e também por ultrassom por imersão. Os dados de composição química foram sobrepostos a janelas de lingotabilidade e as características das escórias foram avaliadas por simulação termodinâmica. Foram avaliadas as correlações entre os resultados das diferentes técnicas de análise e com as referências de literatura. A hipótese de redução da quantidade de cálcio se mostrou satisfatória tanto para a melhoria da lingotabilidade quanto para a limpeza do aço. Porém, a alteração da etapa de adição de enxofre necessita de mais testes para comprovar sua eficiência. Dentre as técnicas empregadas, o uso do microscópio eletrônico de varredura acoplado a um sistema automatizado de análise de inclusões (ASPEX) se mostrou como uma ferramenta vantajosa por fornecer uma ampla gama de informações que podem auxiliar no entendimento da lingotabilidade e da limpeza inclusionária do aço. / Automotive components in general must meet stringent specifications of mechanical properties, inclusionary cleanliness requirements, among others. Sulfur and aluminum are elements added to the liquid steel bath which play an important role in obtaining these properties, but which hinder the production process by continuous casting by favoring the formation of solid particles of high melting point, that can cause the nozzle clogging and hamper the development process of steels with high inclusionary cleanliness. The aim of the present work is to study the chemical composition of the DIN 38MnSiVS6 steel, focusing on the chemical elements that affect the formation and removal of inclusions, as well as the chemical composition of the slag and other parameters such as temperature and castability in an industrial scale production process. In this study, the hypothesis steel cleanliness improvement was evaluated by changing the stage of sulfur addition as well as the amount of calcium addition. Steel samples collected throughout the process were analyzed by optical and scanning electron microscopy, and by immersion ultrasound. The chemical composition data were superimposed on liquid windows and the slag characteristics were evaluated by thermodynamic simulation. The correlations between the results of the different analysis techniques and the literature references were evaluated. The hypothesis of reduction in the amount of calcium was satisfactory both for the improvement of the castability and for the cleanliness of the steel, but the change of the sulfur addition stage requires more tests to prove its efficiency. The scanning electron microscope coupled with an automated inclusion analysis system (ASPEX) has proved to be an advantageous tool to provide a wide range of information that can help in the understanding of the castability and cleanliness of steel.

A limpeza dos aços está diretamente associada ao conteúdo de óxidos dos mesmos, sendo que os diferentes tipos de inclusões não-metálicas presentes podem prejudicar desde os processos de fabricação e conformação até as características necessárias para a aplicação do produto final. As inclusões se formam e se modificam ao longo dos processos de fabricação, e estão relacionadas principalmente às práticas de refino secundário e de lingotamento. Essas inclusões estão sempre presentes nos aços, de modo que é impossível se produzir um aço completamente livre das mesmas. Atualmente, existe uma série de pesquisas buscando o desenvolvimento de práticas e de processos para incrementar a limpeza dos aços. Entre essas está o desenvolvimento de novos materiais refratários adequados às diversas etapas de uma Aciaria. Com especial importância na limpeza dos aços estão as práticas e tecnologias aplicadas no lingotamento contínuo. Neste trabalho foi avaliada a influência do uso de nitrogênio injetado através de poros no colo das válvulas submersas sobre a lingotabilidade e limpeza dos produtos laminados a partir de tarugos. Para este estudo foram testadas diferentes vazões de gás e depois mensurado seu efeito. As técnicas utilizadas para a avaliação foram: verificação da abertura dos tampões; índice de sucateamento nas linhas de inspeção; severidade em ultrassom pelo método de imersão; análise dos teores de oxigênio total e nitrogênio e análise pelo método de distribuição de valores extremos da maior inclusão estimada. Os resultados práticos foram então comparados entre os lotes escolhidos para o teste. Verificou-se através dos dados coletados boa compatibilidade entre as diferentes variáveis e coerência dos resultados com os relatos da literatura. O uso de gás nitrogênio se mostrou ser potencialmente benéfico para a melhoria da limpeza e lingotabilidade do aço, apesar de mais testes serem necessários para a validação das hipóteses levantadas. / The steel cleanliness is directly associated to its inclusion content. The different kind of non-metallic inclusion can harm from the manufacturing and forming processes up to the demanding characteristics for the final products. The inclusions are formed and modified along the steel manufacturing process, and they are related mainly to the secondary refining and casting of steel. These inclusions are always present in the steel, so it is hardly possible to produce steels completely free of them. Nowadays, there are several fields of research concerning with the development of practices and processes to improve steel cleanliness. The development of new lining materials which are suitable for each melting shop step is one of these fields. With special importance over the steel cleanliness issue, the practices and technologies applied to the continuous casting process can be cited. In this work, the influence of nitrogen injection though the pores of the submerged entry nozzle over the castability and cleanliness of rolled products was evaluated. For this study, different gas flows were tested and then measured its effects. The techniques used for the evaluation were: stopper rod opening; rejection index during the inspection lines; severity in immersion ultra-sonic inspection; total oxygen and nitrogen content analysis and largest inclusion diameter estimated by extreme values distribution. The practical results for each lot of steel were then compared. It was verified from, the collected data, good compatibility between these different variables and coherency of the results with the experiences reported in the literature. The use of nitrogen gas showed itself to be potentially good for the improvement of cleanliness and castability of steel, though more trials are necessary for the validation of the considered hypothesis.

Sulfide Stress Cracking (SSC) resistance of the newly developed API-X100 High Strength Low Alloy (HSLA) steel was investigated in the NACE TM0177 "A" solution. The NACE TM0177 "A" solution is a hydrogen sulfide (H2S) saturated solution containing 5.0 wt.% sodium chloride (NaC1) and 0.5 wt.% acetic acid (CH3COOH). The aim of this thesis was to study the effect of microstructure, non-metallic inclusions and alloying elements of the X100 on H2S corrosion and SSC susceptibility. The study was conducted by means of electrochemical polarization techniques and constant load (proof ring) testing. Microstructural analysis and electrochemical polarization results for X100were compared with those for X80, an older generation HSLA steel. Uniaxial constant load SSC testing was conducted using X100 samples and the results were compared with those reported for older generation HSLA steels. Addition of H2S to the NACE TM0177 "A" solution increased the corrosion rate of X100from 51.6 to 96.7 mpy. The effect of H2S on the corrosion rate was similar for X80. The corrosion rate for X80 increased from 45.2 to 80.2 mpy when H2S was added to the test solution. Addition of H2S enhanced the anodic kinetics by forming a catalyst (FeHSads) on the metal surface and as a result, shifted the anodic polarization curve to more current densities. Moreover, the cathodic half cell potential increased due to the decrease in pH, from 2.9 to 2.7, which shifted the cathodic polarization curve to more current densities. The increase in both the anodic and cathodic currents, after H2S addition, caused the rise in the corrosion current density. In H2S saturated NACE TM-0177 "A" solution, the X100 steel corrosion rate was higher than the X80 steel by 20%. Longer phase boundaries and larger nonmetallic inclusions in the X100 microstructure generated more areas with dissimilar corrosion potentials and therefore, a stronger driving force for corrosion. Higher density of second phase regions and larger nonmetallic inclusions acted as an increased cathode area on the X100 surface which increased the cathodic current density and consequently, increased the corrosion current density. Proof ring tests on the X100 gave a threshold stress value, C5th, of 46% YS, 343.1 MPa(49.7 ksi). The main failure was caused by SSC cracking. SSC nucleated at corrosion pits on the metal surface and microcracks in the metal body and propagated perpendicular to the applied stress. Hydrogen Induced Cracking (HIC) was observed in the X100. HIC cracks nucleated at banded martensite-ferrite interfaces and propagated along the rolling direction parallel to the applied tensile stress through the softer ferrite phase. When compared to older HSLA grades, the X100 tested in this study had a high SSC susceptibility and therefore, is not be recommended for H2S service applications. The high X100 SSC susceptibility was caused by the material high corrosion rates in H2Smedia which formed corrosion pits that acted as crack initiation sites on the metal surface and provided more hydrogen that migrated into the steel. In addition, the X100 inhomogeneous microstructure provided a high density of hydrogen traps in front of the main crack tip which promoted SSC microcrack formation inside the metal. Microcracks in the metal body connected with the main crack tip that originated from corrosion pits which assisted SSC propagation. / Applied Science, Faculty of / Materials Engineering, Department of / Graduate

This thesis covers some aspects of hard part turning of carburised steels using a poly‑crystalline cubic boron nitride (PCBN) cutting tool during fine machining. The emphasis is on the influence of the steel cleanliness and the characteristics of non‑metallic inclusions in the workpiece on the active wear mechanisms of the cutting tool. Four carburising steel grades suitable for automotive applications were included, including one that was Ca‑treated. A superior tool life was obtained when turning the Ca-treated steel. The superior machinability is associated with the deposition of lubricating (Mn,Ca)S and (CaO)x-Al2O3-S slag layers, which are formed on the rake face of the cutting tool during machining. Moreover, the transfer of work material to the rake face crater is characteristic in hard part turning of clean steels. It can be because of the lack of sulfides that protect the cutting edge when turning machinability treated steels. This corresponds to the more pronounced crater wear caused by the low‑sulfur steels than that of the steels with higher sulfur contents. It was also concluded that the composition of the non‑metallic inclusions in the Ca‑treated steel is a more important factor than the inclusion number and size, in hard part turning using a PCBN cutting tool. Also, a 3D analysis after electrolytic extraction was found to give a more precise characterisation of non‑metallic inclusions than the conventional 2D analysis by SEM‑EDS. In turn, better correlations to machinability and mechanical properties can be obtained. Hence, the use of this technique is beneficial for future material development. Finally, the challenge for future metallurgy is to manufacture high‑performance steels with improved combined properties of mechanical strength and machinability. / <p>QC 20150422</p>

The inclusions have a different chemical composition and give the steel different mechanical properties. These inclusions affect several properties of steel. In order to understand how the inclusions will affect the steel properties, the electrolytic extraction of 3D investigate method is applied on the steel grade of 42CrMo4. Then follow with Scanning Electron Microscope (SEM) observation. Steel samples from both ingot and rolling with and without heat treatment are observed and compared with different ratios. The result shown that, heat treatment can be applied for removing carbides successfully. And most inclusions are belonging to Type RS which is rod like MnS. The percentage of broken particles can be up to 80%, which means that the reason for the inclusions broken should be find. And heat treatment can affect the characteristics of elongated MnS.

Heterogeneous mixtures have the potential to be used as synthetic substrates for antenna applications giving the antenna designer new degrees of freedom to control the permittivity and/or permeability in three dimensions such as by a smooth variation of the density of the inclusions, the height of the substrate and the manufacture the whole antenna system in one process. Electromagnetic, fabrication, environmental, time and cost advantages are potential especially when combined with nano-fabrication techniques. Readily available and cheap materials such as Polyethylene and Copper can be used in creating these heterogeneous materials. These advantages have been further explained in this thesis. In this thesis, the research presented is on canonical, numerical and measurement analysis on heterogeneous mixtures that can be used as substrates for microwave applications. It is hypothesised that heterogeneous mixtures can be used to design bespoke artificial dielectric substrates for say, patch antennas. The canonical equations from published literature describing the effective permittivity, ε_eff and effective permeability, μ_eff of heterogeneous mixtures have been extensively examined and compared with each other. Several simulations of homogenous and heterogeneous media have been carried out and an extraction/inversion algorithm applied to find their ε_eff and μ_eff. Parametric studies have been presented to show how the different variables of the equations and the simulations affect the accuracy of the results. The extracted results from the inversion process showed very good agreement with the known values of the homogenous media. Numerically and canonically computed values of ε_eff and μ_eff of various heterogeneous media were shown to have good agreement. The fabrication techniques used in creating the samples used in this research were examined, along with the different measurement methods used in characterising their electromagnetic properties via simulations and measurements. The challenges faced with these measurement methods were explained including the possible sources of error. Patch antennas were used to investigate how the performance of an antenna may be affected by heterogeneous media with metallic inclusions. The performance of the patch antenna was not inhibited by the presence of the metallic inclusions in close proximity. The patch measurement was also used as a measurement technique in determining the ε_eff of the samples.

Foram tomadas amostras de aço líquido referentes a três grupos de aço, a saber: (I) aços baixo-carbono (0,02 %C 0,08), acalmados ao alumínio; (II) aços peritéticos (0,09 %C 0,15), acalmados ao alumínio e silício; (III) aços ultrabaixo carbono ( C<35 ppm), acalmados ao alumínio.Os aços foram produzidos em aciaria do tipo LD e foram, a seguir, tratados em equipamentos de refino secundário, adequados a cada um dos casos.As amostras forma colhidas no distribuidor de uma máquina de lingotamento contínuo de placas, segundo critério que minimiza a possibilidade da ocorrência de interferências que pudessem mascarar o resultado do tratamento de refino secundário tais como re-oxidação do aço e coleta simultânea de escória. As amostras foram submetidas à análise de inclusões utilizando-se técnicas de microscopia óptica, microscopia eletrônica e micro-análise. Foi possível caracterizar as inclusões presentes em cada tipo de aço segundo a morfologia, o tamanho, a quantidade e a composição química. / Non-metallic inclusions in liquid samples of (I) low-carbon aluminium killed steel (0,02wpct C 0,08wpct), (II) peritetic aluminium and silicon killed steel (0,09wpct C 0,15wpct); (III) extra-low-carbon, aluminium killed steel (C<35 ppm) were taken from the tundish distributor of a continuous casting caster for steel plates according to a procedure that minimizes re-oxidation of steel and/or pick up of liquid slag. The samples were inspected through the following microstructural techniques: optical microscopy, electronic microscopy, and electron microprobe. Were possible to feature present inclusion in each kind of steel according to morphology, size, amout and chemical composition.