Made available in DSpace on 2014-10-09T12:43:27Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:57:46Z (GMT). No. of bitstreams: 1 06630.pdf: 9701259 bytes, checksum: 3a0ddeea466df64d4d1c1cf28780f43d (MD5) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

Made available in DSpace on 2014-10-09T12:54:28Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:07:42Z (GMT). No. of bitstreams: 0 / Este trabalho tem como objetivo principal investigar o comportamento frente à corrosão de aços inoxidáveis avançados em meios fisiológicos. Foram selecionados para o estudo quatro aços inoxidáveis visando avaliar o potencial destes para aplicações em implantes cirúrgicos: um aço superferrítico (DIN W. Nr. 1.4575), a Incoloy MA 956, contendo alumínio e óxido de ítrio, um aço austenítico DIN W. Nr. 1.4970 e um aço superaustenítico obtido por meio da adição de 0,87% de nitrogênio ao aço dúplex DIN W. Nr. 1.4460. Os três primeiros aços contêm baixo teor de níquel e suas películas protetoras são ricas em cromo, enquanto a Incoloy MA 956 é isenta de níquel, e rica em alumínio, o que influencia o seu filme passivo. Os materiais foram analisados usando técnicas de espectroscopia de impedância eletroquímica (EIE), polarização potenciodinâmica, técnica do eletrodo vibrante, microscopia eletroquímica de varredura, microscopia eletrônica de varredura de emissão de campo, microscopia ótica e microscopia eletrônica de varredura. Os meios escolhidos para avaliação da resistência à corrosão foram a solução de Hanks, um meio de cultura e uma solução tamponada com fosfato. Os resultados de EIE foram interpretados usando circuitos elétricos equivalentes que simularam uma camada passiva dúplex em todos os materiais analisados. Todos os materiais analisados apresentaram resistência à corrosão superior à do aço inoxidável AISI 316L, correspondente ao ASTM F-138, que é o mais utilizado na fabricação de implantes metálicos. Também foi destacada a importância do tratamento de solubilização nos aços com alto teor de nitrogênio. O DIN W. Nr. 1.4970 foi considerado citotóxico e sua potencialidade para uso como biomaterial, rejeitada. O DIN W. Nr. 1.4575 e Incoloy MA 956 podem ser usados como biomateriais, mas somente em próteses odontológicas ou de fácil remoção, devido ao seu comportamento ferromagnético. O DIN W. Nr. 1.4460 com 0,87% de nitrogênio foi o que apresentou as condições mais apropriadas para uso como biomaterial, inclusive para próteses ortopédicas. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energéticas e Nucleares - IPEN/CNEN-SP

Abstract In this thesis, the hot deformation behavior of stabilized 12–27% Cr ferritic stainless steels was investigated in order to find ways to improve the current hot rolling schedules for enhancing texture structures and deep drawability of the end product. Hot deformation was studied using axial and plane strain compression in two thermomechanical simulators: a Gleeble and a TMC machine. In addition to flow stress measurements, the resultant microstructures and textures were investigated using electron backscatter diffraction (EBSD), and the dislocation structures using transmission electron microscopy (TEM). In the case of 21% Cr steel, industrial multi-pass hot rolling, including low finish rolling temperatures, was simulated in order to investigate the microstructure and texture development under varying deformation conditions. Flow behavior of high-Cr ferritic stainless steels during hot deformation was mainly controlled by intense dynamic recovery. However, the deformation conditions greatly affected the extent of dynamic recovery. Cr increased the flow stress through solid solution hardening, although increasing the Cr content reduced the activation energy for hot deformation. Two modeling approaches for flow stress were successfully applied: an empirical constitutive equation and a dislocation density-based flow stress model. Continuous dynamic recrystallization was identified regardless of the Zener-Hollomon parameter, whereas discontinuous dynamic recrystallization was not observed. Static recrystallization slowed down towards the completion of the process, and especially the α fiber grains were difficult to recrystallize. Static recrystallization was enhanced by lowering the deformation temperature to 800 °C or below due to the accelerating effect of in-grain shear bands on the static recrystallization kinetics. However, an intensifying effect on γ fiber texture development was achieved after deformation at 600 °C or below. Two different improved process routes for hot rolling were proposed based on the results: 1) sufficiently long inter-pass times together with lowering the finish rolling temperature in order to promote static recrystallization during inter-pass times and hot band annealing, and 2) hot band annealing preceded by a warm rolling procedure, in which thin gauge hot band is produced by multiple heavy warm rolling deformation passes. / Tiivistelmä Tässä väitöstyössä tutkittiin stabiloitujen 12–27 % kromia sisältävien ferriittisten ruostumattomien terästen käyttäytymistä kuumamuokkauksessa tavoitteena kehittää nykyisin käytössä olevia kuumamuokkauskäytäntöjä lopputuotteen tekstuurirakenteen ja siten sen syvävedettävyyden parantamiseksi. Kuumamuokkausta simuloitiin sylinteri- ja tasomuodonmuutospuristuskokeilla Gleeble- ja TMC-laitteistoissa. Kokeista saatuja jännitys–venymä-käyriä analysoitiin ja syntyneet mikrorakenteet ja tekstuuri tutkittiin EBSD-menetelmällä pyyhkäisyelektronimikroskoopissa sekä dislokaatio- ja erkaumarakenteet läpäisyelektronimikroskoopilla. Lisäksi 21 % kromia sisältävälle teräkselle tehtiin monipistoista kuumavalssausta simuloivia puristuskokeita, joissa varioitiin myös valssauksen lopetuslämpötilaa ja jäähtymisnopeutta. Jännitys–venymä-käyriä mallinnettiin käyttäen sekä empiirisiä yhtälöitä että dislokaatiotiheyteen perustuvaa fysikaalista mallia. Kromipitoisuus kasvatti muodonmuutosvastusta mutta pienensi deformaation aktivaatioenergiaa. Dynaaminen toipuminen oli erittäin voimakasta kuumamuokkauslämpötiloissa, joskin lämpötila ja muodonmuutosnopeus vaikuttivat merkittävästi sen määrään. Jatkuvan dynaamisen rekristallisaation todettiin tapahtuvan riippumatta Zener-Hollomon -parametrin arvosta, mutta epäjatkuvaa dynaamista rekristallisaatiota ei havaittu. Staattinen rekristallisaatio hidastui, kun rekristallisaatioaste saavutti 90 %, ja erityisesti α-rungon rakeet pyrkivät vain toipumaan. Staattista rekristallisaatiota pystyttiin voimistamaan laskemalla muokkauslämpötila 800 °C:een tai sen alle, jolloin rakeiden sisälle syntyi staattisen rekristallisaation ydintymistä nopeuttavia leikkausnauhoja. γ-rungon intensiteetti voimistui rekristallisaatiossa kuitenkin vasta, kun muokkauslämpötila oli 600 °C tai tätä matalampi. Koetulosten perusteella ehdotettiin kahta erilaista kuumavalssauspraktiikkaa, joiden avulla kuumanauhan ominaisuuksia voidaan parantaa: 1) staattisen rekristallisaation edistäminen sekä pistojen välillä että kuumanauhahehkutuksessa käyttämällä pitkiä pistojen välisiä aikoja sekä laskemalla valssauksen lopetuslämpötilaa, tai 2) kuumanauhahehkutus yhdistettynä edeltävään voimakkaaseen lämminvalssaukseen, jolloin on mahdollista valmistaa ohutta kuumanauhaa.

The structural stability of creep-resistant steels P22, P91 and Eurofer´97 and structural stability of weld joint P22/P91 have been studied. The microstructural changes during annealing at temperatures of 500 – 900°C were examined. The state of equilibrium have been simulated using the ThermoCalc software. The computed results were compared with published data. A good agreement between the simulation and the published data was observed.

La fragilisation des aciers de cuve des réacteurs nucléaires sous irradiation aux neutrons est le facteur limitant la durée de vie des centrales nucléaires françaises. Ceci est dû au mouvement des dislocations qui se trouve être entravé par des amas de Cu, P, Si, Mn et Ni. Plus particulièrement, les amas induits de Mn et de Ni sont à l'origine d'un durcissement significatif à forte dose. Afin de prédire la dégradation des propriétés mécaniques, les expériences sont généralement réalisées à l'aide d'accélérateurs de particules. Cependant, les flux d'irradiation atteints sont compris entre 10⁻⁴ 10 ⁻ ⁶ dpa/s⁻ ¹, tandis qu'il est limité à 10⁻ ¹ ⁰ dpa/s⁻ ¹ dans les réacteurs de puissance actuels. Ce point est essentiel étant donné que le dommage d'irradiation dépend du flux de particules incidentes. La transférabilité ion/neutron constitue donc la problématique centrale. Celle-ci a été étudiée dans les alliages austénitiques seulement. Ce travail de thèse se propose donc d'étudier, dans des alliages ferritiques, l'effet du flux d'irradiation sur l'endommagement dans deux alliages différents : le Fe-Ni et le Fe-Mn, dans le but d'évaluer également l'effet de chaque soluté sur la microstructure obtenue après irradiation.Les alliages ont été analysés expérimentalement par Microscopie Electronique en Transmission (TEM), Microscopie Electronique à Balayage par Transmission (STEM) couplée à l'Analyse Dispersive en Energie des Rayons-X (EDS) et à la Spectroscopie de Perte d'énergie des Electrons (EELS), ainsi que par Sonde Atomique Tomographique (APT).Les irradiations ont été réalisées avec des ions Fe³⁺ de 2 MeV et des ions Fe⁹⁺ de 27 MeV, à 400°C, à des taux de dommage de 10⁻⁴ et 10⁻ ⁶ dpa/s⁻ ¹ respectivement, jusqu'à un même dommage de 1.2 dpa.Les résultats obtenus montrent que le Ni et le Mn ont des comportements sous irradiation très différents en termes de nature de nano-défauts créés.Des irradiations aux particules légères ont également été réalisées de manière à apprécier l'effet des cascades de déplacement.Enfin, une irradiation séquentielle, en deux étapes, a été effectuée à l'aide d'ions Fe⁹⁺ à température ambiante, puis de protons à 400°C, dans le but d'isoler la contribution au durcissement des amas de défauts ponctuels de celle des zones enrichies en soluté. / Reactor pressure vessel (RPV) steel embrittlement under neutron irradiation is the main lifetime limiting factor of nuclear reactors. This is due to the impeding of dislocation glide by nanometric clusters composed of Cu, P, Si, Mn and Ni. More specifically, radiation induced Mn and Ni enriched clusters cause a significant hardening at high dose. To predict this change in mechanical properties, particle accelerator based experiments are conducted. However, the achieved flux ranges between 10⁻⁴ and 10 ⁻ ⁶ dpa/s⁻ ¹, whereas it is limited to 10⁻ ¹ ⁰ dpa/s⁻ ¹ in modern nuclear power technologies. This point is of high importance since radiation damage highly depends on irradiation flux. The reproducibility ion-neutron is thus the key point. It has been studied in austenitic steels but little is known regarding any dose rate dependence in ferritic alloys. Therefore, this thesis focuses on the effect of ion fluxes on radiation damage in two different alloys : Fe-Ni and Fe-Mn in order to investigate, additionally, the effects of each solute on the microstructure after irradiation.The alloys were experimentally investigated using conventional Transmission Electron Microscopy, Scanning Transmission Electron Microscopy coupled to Energy Dispersive X-ray Spectroscopy and Electron Energy Loss Spectroscopy and by Atom Probe Tomography.Irradiations were performed with 2 MeV Fe³⁺ ions and 27 MeV Fe⁹⁺ ions at 400°C at a nominal damage rate of 10⁻⁴ and 10⁻ ⁶ dpa/s respectively, up to a nominal displacement damage of 1.2 dpa. The detailed analysis shows that Ni and Mn behave in a very different way in terms of nano-defects formed under irradiation.Besides, light particle irradiations were also performed in order to ascertain the cascade effects.Finally, a two-series irradiation was carried out using Fe ions at room temperature and protons at 400°C, to isolate the contribution of point defect clusters to hardening from that of solute enriched zones.

The purpose of this research is to investigate the mechanical, microstructural and corrosion performance of the ferritic stainless steel coarse powders, used in Metal Injection Molding (MIM) process. Three coarser powders made by Höganäs AB, were examined along with a commercially available fine MIM powder and samples from sheet metal. The studied powders were individually mixed with binders and then injection molded in the shape of dog bone shaped tensile bars. These green samples were then debinded and sintered to examine under different characterization methods. The methods used for examining the samples were tensile test, hardness test, metallography, SEM, chemical analysis, and salt spray test. After a comparative study of these different materials, it turns out that the chemical composition and the process parameters have more effect on materials properties compared to only particle size distribution in studied materials. After this study, 434 coarse powder was preferred upon the PolyMIM 430 fine powder, because of its lower price and same performance as that of PolyMIM 430.

This project was ordered by Sandvik Materials Technology and was performed by a group of students at Uppsala university. The purpose of the project was to study precipitation behavior and structure stability in six advanced heat resistant alloys. Each sample were subjected to a creep rupture test in 600 or 700°C depending on the alloy type. Two parts of each alloy where examined; one part which had been affected by creep and another part which was unaffected by creep. A literature study was performed first to gain knowledge of the scientific theory utilized in this project, namely creep, precipitation hardening, and about the different materials which were analyzed. Preliminary results for the phase composition of the materials were obtained from a Thermo-Calc (TC) simulation. The SEM-images showed nothing noteworthy for any sample due to the roughness of the sample surfaces. The EDS-analysis showed chromium depletion in the centers of the aged samples of HT9 and Sanicro® 75X. Other minority phases such as Cr23C6 in Sanicro®70, P-phase and a titanium nitride phase in sanicro® 60X, VB in Esshete 1250 and Sigma-phase in 4C54 were identified using EDSmapping. It was found that when using XRD to analyze the phase compositions of small samples it is impractical to have the samples cast in bakelite beforehand. The XRD-results obtained in this project showed that more than 90% of the XRD diffractogram for every sample was graphite, which made the identification of minority phases impossible. The quality of the LOM-images varied greatly between samples, for 4C54 grain sizes were measured in all images, for Esshete 1250 grain sizes were measured for the crept sample, and for Sanicro® 60X measurements could only be taken from one image. Most of the sample preparation was insufficient to achieve the test results necessary for complete microstructural analysis and phase analysis of the samples. The mistakes in the practical steps of the project were noted and improvements for these mistakes are presented in the conclusion.

No description available.

[pt] Pesquisas atuais evidenciam que diversos materiais com aplicação nas indústrias automotiva, ferroviária, aeronáutica e aeroespacial não apresentam um limite de fadiga. Porém, em torno de 1860 Wohler propôs a curva S-N (tensão - número de ciclos), admitindo um conceito que há um limite de fadiga, estipulado na época como 1E5 ciclos e considerado como vida infinita em fadiga. Contudo, com os avanços tecnológicos, inúmeros componentes falham na condição de vida infinita, de maneira contrária ao proposto por Wöhler. Atualmente, se considera 3 regimes distintos de fadiga: fadiga de baixo ciclo, fadiga de alto ciclo e fadiga de altíssimo ciclo. Nas indústrias automotivas há um extensivo uso de chapas de aço para a fabricação de componentes de geometria complexa. Neste contexto, o aço interstitial free (IF – aços com baixa quantidade de átomos intersticiais), é um dos materiais de largo emprego, em função da sua excelente estampabilidade. O aço IF apresenta uma microestrutura ferrítica com uma baixíssima quantidade de elementos intersticiais. Interstícios com carbono e nitrogênio são estabilizados pelo titânio (Ti) ou nióbio (Nb) formando frações de volume extremamente pequenas na matriz ferrítica de carbetos e nitretos. O trabalho baseia-se na investigação experimental dos danos microestruturais no aço IF após carregamentos cíclicos de longa duração. Amostras do aço IF estabilizado pelo Ti foram submetidas a ensaios ultrassônicos de fadiga com carregamentos superiores a 1E7 ciclos. Se observou o aparecimento de danos microestruturais (persistent slip bands, PSB s) após determinado número de ciclos. Por meio de análise no microscópio ótico foi estimado que 97,76 por cento da vida em fadiga foi destinado para nucleação de trinca enquanto 2,23 por cento para a propagação de trinca. Houve o projeto de um novo corpo de prova para a máquina de fadiga de altíssimo, com o intuito de acompanha a superfície do material durante os ensaios. É proposto a equação da curva S-N fadiga de altíssimo ciclo com os dados extraídos dos testes. E por fim, é sugerido um fator de correção na equação de deformação plástica cisalhante nos PSB s formados / [en] Current research shows that several materials with application in the automotive, railway, aeronautical and aerospace industries do not have a fatigue limit. However, around 1860 Wohler proposed the S-N curve (stress - number of cycles), admitting a concept that there is a fatigue limit, stipulated at the time as 1E5 cycles and considered as infinite fatigue life. Although, with technological advances, numerous components fail in the condition of infinite life, contrary to what Wöhler proposed. Currently, 3 different fatigue regimes are considered: low cycle fatigue, high cycle fatigue and very high cycle fatigue. In the automotive industries there is an extensive use of sheet steel for the manufacture of components with complex geometry. In this context, interstitial free steel (IF steel) is one of the widely used materials, due to its excellent stampability. IF steel has a ferritic microstructure with a very low amount of interstitial elements. Interstices with carbon and nitrogen are stabilized by titanium (Ti) or niobium (Nb) forming extremely small volume fractions in the ferritic matrix of carbides and nitrides. The work is based on the experimental investigation of microstructural damage in IF steel after long-term cyclic loading. Samples of Ti-stabilized IF steel were subjected to ultrasonic fatigue tests with loads greater than 1E7 cycles. It was observed the arising of microstructural damage (persistent slip bands, PSB s) after a certain number of cycles. By means of image analysis in the optical microscope, it was estimated that 97.76 percent of the fatigue life was destined for crack nucleation while 2.23 percent for crack propagation in very high cycle fatigue regime. There was the project of a new specimen for the very high fatigue machine, in order to accompany the surface of the material during the tests. It is proposed the equation of the curve S-N fatigue of very high cycle os with data extracted from the tests. Finally, a correction factor is suggested in the plastic shear deformation equation in PSB s based on experimental data.

<p>An investigation of the influence of three alloying elements Chromium, Phosphorus, and Nitrogen with the solute types of oversized substitutional, undersized substitutional, and interstitial on the irradiation induced microstructural evolution and hardening</p>