Causes for the differences in precipitation morphology observed and investigation. / Master of Science

Thesis (M.S. in Mechanical Engineering and Mechanical Engineer)--Naval Postgraduate School, December 1990. / Thesis Advisor(s): Fox, Alan G. "December 1990." Description based on title screen as viewed on April 2. 2010. DTIC Identifier(s): Steel, Microstructure, Mechanical Properties, Copper, Quenching, Tempering, Processing, Naval Vessels, HSLA-100 Steel, Theses, Age Hardening, Modulus of Elasticity, Charpy V Notch Tests. Author(s) subject terms: HSLA-100, Mechanical Properties, Copper Precipitation, Carbide. Includes bibliographical references (p. 66-68). Also available in print.

High entropy alloys (HEAs) is a concept wherein alloys are constructed with five or more elements mixed in equal proportions; these are also known as multi-principle elements (MPEs) or complex concentrated alloys (CCAs). This PhD thesis dissertation presents research conducted to develop precipitation-hardenable high entropy alloys using a much-studied fcc-based equi-atomic quaternary alloy (CoCrFeNi). Minor additions of aluminium make the alloy amenable for precipitating ordered intermetallic phases in an fcc matrix. Aluminum also affects grain growth kinetics and Hall-Petch hardenability. The use of a combinatorial approach for assessing composition-microstructure-property relationships in high entropy alloys, or more broadly in complex concentrated alloys; using laser deposited compositionally graded AlxCrCuFeNi2 (0 < x < 1.5) complex concentrated alloys as a candidate system. The composition gradient has been achieved from CrCuFeNi2 to Al1.5CrCuFeNi2 over a length of ~25 mm, deposited using the laser engineered net shaping process from a blend of elemental powders. With increasing Al content, there was a gradual change from an fcc-based microstructure (including the ordered L12 phase) to a bcc-based microstructure (including the ordered B2 phase), accompanied with a progressive increase in microhardness. Based on this combinatorial assessment, two promising fcc-based precipitation strengthened systems have been identified; Al0.3CuCrFeNi2 and Al0.3CoCrFeNi, and both compositions were subsequently thermo-mechanically processed via conventional techniques. The phase stability and mechanical properties of these alloys have been investigated and will be presented. Additionally, the activation energy for grain growth as a function of Al content in these complex alloys has also been investigated. Change in fcc grain growth kinetic was studied as a function of aluminum; the apparent activation energy for grain growth increases by about three times going from Al0.1CoCrFeNi (3% Al (at%)) to Al0.3CoCrFeNi. (7% Al (at%)). Furthermore, Al addition leads to the precipitation of highly refined ordered L12 (γ′) and B2 precipitates in Al0.3CoCrFeNi. A detailed investigation of precipitation of the ordered phases in Al0.3CoCrFeNi and their thermal stability is done using atom probe tomography (APT), transmission electron microscopy (TEM) and Synchrotron X-ray in situ and ex situ analyses. The alloy strengthened via grain boundary strengthening following the Hall-Petch relationship offers a large increment of strength with small variation in grain size. Tensile strength of the Al0.3CoFeNi is increased by 50% on precipitation fine-scale γ′ precipitates. Furthermore, precipitation of bcc based ordered phase B2 in Al0.3CoCrFeNi can further strengthen the alloy. Fine-tuning the microstructure by thermo-mechanical treatments achieved a wide range of mechanical properties in the same alloy. The Al0.3CoCrFeNi HEA exhibited ultimate tensile strength (UTS) of ~250 MPa and ductility of ~65%; a UTS of ~1100 MPa and ductility of ~30%; and a UTS of 1850 MPa and a ductility of 5% after various thermo-mechanical treatments. Grain sizes, precipitates type and size scales manipulated in the alloy result in different strength ductility combinations. Henceforth, the alloy presents a fertile ground for development by grain boundary strengthening and precipitation strengthening, and offers very high activation energy of grain growth aptly suitable for high-temperature applications.

A castable alloy, i.e., one that flows easily to fill the entire mold cavity and also has resistance to hot tearing during solidification, must invariably contain a sufficient amount of a eutectic structure. For this reason, most traditional aluminum casting alloys contain silicon because the aluminum-silicon eutectic imparts to the alloy excellent casting characteristics. However, the solidus temperature in the Al-Si system does not exceed 577°C, and the major alloying elements (i.e., zinc, magnesium, and copper) used with silicon in these alloys further lower the solidus temperature. Also, these elements have high diffusivity in aluminum and so, while they enhance the room temperature strength of the alloy, they are not useful at elevated temperatures. Considering nickel-base super alloys, whose mechanical properties are retained up to temperatures that approach 75% of their melting point, it is conceivable that castable aluminum alloys can be developed on the same basis so that they are useful at temperatures approaching 350C. A castable aluminum alloy intended for high temperature applications must contain a eutectic structure that is stable at temperatures higher than 600°C, and must contain second phase precipitate particles that are thermodynamically stable at the service temperature. Transition metal trialuminides with the general chemical formula AlxTMy in which TM is a transition metal, are excellent candidates for both the eutectic structure and the precipitate particles. In this research, the use of transition metals in the constitution of aluminum casting alloys is investigated with emphasis on the morphology, crystallography, and mechanisms of formation of the various phases.

A castable alloy, i.e., one that flows easily to fill the entire mold cavity and also has resistance to hot tearing during solidification, must invariably contain a sufficient amount of a eutectic structure. For this reason, most traditional aluminum casting alloys contain silicon because the aluminum-silicon eutectic imparts to the alloy excellent casting characteristics. However, the solidus temperature in the Al-Si system does not exceed 577°C, and the major alloying elements (i.e., zinc, magnesium, and copper) used with silicon in these alloys further lower the solidus temperature. Also, these elements have high diffusivity in aluminum and so, while they enhance the room temperature strength of the alloy, they are not useful at elevated temperatures. Considering nickel-base super alloys, whose mechanical properties are retained up to temperatures that approach 75% of their melting point, it is conceivable that castable aluminum alloys can be developed on the same basis so that they are useful at temperatures approaching 350 °C. A castable aluminum alloy intended for high temperature applications must contain a eutectic structure that is stable at temperatures higher than 600°C, and must contain second phase precipitate particles that are thermodynamically stable at the service temperature. Transition metal trialuminides with the general chemical formula AlxTMy in which TM is a transition metal, are excellent candidates for both the eutectic structure and the precipitate particles. In this research, the use of transition metals in the constitution of aluminum casting alloys is investigated with emphasis on the morphology, crystallography, and mechanisms of formation of the various phases.

The increasing technological need to push service conditions of structural materials to higher temperatures has motivated the development of several alloy systems. Among them, superalloys are an excellent candidate for high temperature applications because of their ability to form coherent ordered precipitates, which enable the retention of high strength close to their melting temperature. The accelerated kinetics of solute diffusion, with or without an added component of mechanical stress, leads to coarsening of the precipitates, and results in microstructural degradation, limiting the durability of the materials. Hence, the coarsening of precipitates has been a classical research problem for these alloys in service. The prolonged hunt for an alternative of nickel base superalloys with superior traits has gained hope after the recent discovery of Co-Al-W based alloys, which readily form high temperature g precipitates, similar to Ni base superalloys. In the present study, coarsening behavior of g precipitates in Co-10Al-10W (at. %) has been carried out at 800°C and 900°C. This study has, for the first time, obtained critical coarsening parameters in cobalt-base alloys. Apart from this, it has incorporated atomic scale compositional information across the g/g interfaces into classical Cahn-Hilliard model for a better model of coarsening kinetics. The coarsening study of g precipitates in Ni-14Al-7 Cr (at. %) has shown the importance of temporal evolution of the compositional width of the g/g interfaces to the coarsening kinetics of g precipitates. This study has introduced a novel, reproducible characterization method of crystallographic study of ordered phase by coupling of orientation microscopy with atom probe tomography (APT). Along with the detailed analysis of field evaporation behaviors of Ni and Co superalloys in APT, the present study determines the site occupancy of various solutes within ordered g precipitates in both Ni and Co superalloys. This study has explained the role of structural and compositional gradients across the precipitates (g)/matrix (g) interfaces on the coarsening behavior of coherent precipitates in both Ni and Co-base superalloys. The observation of two interfacial widths, one corresponding to a structural order-disorder transition, and the other to the compositional transition across the interface, raises fundamental questions regarding the definition of the interfacial width in such systems. The comparative interface analysis in Co and Ni superalloy shows significant differences, which gives insights to the coarsening behaviors of g precipitates in these alloys. Hence, the principal goal of this work is to compare and contrast the Co and Ni superalloys and also, to accommodate atomic scale information related to transitions across interfaces to coarsening models for a better practical applicability of coarsening laws to various alloys.

[pt] O objetivo deste trabalho é avaliar a estabilidade microestrutural da liga 8090 (Al-Li-Cu-Mg-Zr) submetida a tratamentos térmicos de retrogressão e reenvelhecimento em diferentes condições de tempo e temperatura. Caracterização da morfologia e da estabilidade das fases endurecedoras foi realizada por microscopia eletrônica de varredura (MEV), utilizando a técnica EBSD (Electron Backscattering Diffraction). Microscopia eletrônica de transmissão (MET) foi também usada devido a ordem de grandeza nanométrica das fases precipitadas. Os resultados obtidos foram correlacionados com a propriedades mecânicas através de ensaios de microdureza e tração. Foi observado que a microestrutura da liga 8090 é estável, tanto na sua constituição policristalina quanto na sua microestrutura. O efeito de textura em virtude da deformação sofrida durante o processo de laminação permanece após o tratamento de retrogressão. Além disso, a evolução dos estágios de precipitação é pouco perceptível até o pico de endurecimento. As fases predominantes nesta liga são as fases delta (Al3Li), beta (Al3Zr) e T1 (Al2CuLi). Durante um reenvelhecimento mais prolongado é observado a precipitação da fase S (Al2CuMg) e do precipitado duplex delta/beta. Os ensaios de tração indicam a ocorrência do efeito Portevin-Le Chatelier para as amostras como recebida e envelhecidas a curtos intervalos de tempo. Este fenômeno dinâmico é resultado da interação de discordâncias com átomos de soluto e partículas de segunda fase. / [en] The purpose of this work is to evaluate the microstructural stability of alloy 8090 (Al-Li-Cu-Mg-Zr) when submitted to heat treatments of retrogression and reaging at different temperatures and for different time intervals. Characterization of the morphology and stability of the second phases was carried out by scanning electron microscopy (SEM), making use of the electron backscattering diffraction (EBSD) technique. Transmission electron microscopy (TEM) was also used for this purpose in virtue of the nanometric size of the second phases precipitated in the alloy. The results obtained were correlated with the mechanical properties determined by means of microhardness measurements as well as tensile tests. It was noted that the alloy exhibits a remarkable stability, not only in regard to its polycrystalline composition but also to its microstructure. The deformation texture introduced in the alloy due to its fabrication process (rolling) was found to persist after the retrogression treatment. In addition, the evolution of precipitation stages did not very considerably until the peak aging was reached. The main phases observed in the alloy were the phases delta (Al3Li), beta (Al3Zr) and T1 (Al2CuLi). During extended reaging, one can observe the precipitation of other phases such as S (Al2CuMg) and the duplex phase delta/beta. The tensile results indicated the occurrence of Portevin-Le Chatelier effect for the alloy in the as-received and short time reaged conditions. This dynamic effect, results from the interaction of dislocations with solute atoms as well as second phases particles.

Abstract not available

The laminated system processed using FusionTM technology is reported to contain a compositional gradient between the different layers. The interface region exhibits various precipitation characteristic during the subsequent heat treatment. The precipitation behavior at the interface region and core layer of a laminated AA3xxx-AA6xxx alloy system is investigated and discussed. The precipitation hardening capacity at the interface region is shown to scale with the existing compositional gradient. TEM observations reveal the precipitates at the interface region with a larger size and a lower number density than those at the core layer. A yield strength model developed for bulk AA6xxx series is employed to predict precipitate hardening behavior of the laminated sheet, and the modeling result shows an agreement with the measured values using a mass correction. The annealing behavior of the laminated system is investigated in a wide temperature range and at various deformation levels. The size and aspect ratio of the recrystallized grains are found to be determined by the interaction between recrystallization and precipitation, and by dissolution/coarsening of pre-existing precipitates. Under the condition of a low annealing temperature and a high deformation level, recrystallization initiates first at the interface region and then progresses into the core layer along the compositional gradient. The preferential onset of recrystallization at the interface is attributed to a higher driving pressure and a lower Zener drag pressure due to a low volume fraction of precipitates. Nucleation from large particles and grain boundaries is found to be operative nucleation mechanism in this system.

Thesis (Ph. D.)--Ohio State University, 2007. / Title from first page of PDF file. Includes bibliographical references (p. 172-179).