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At least 667 records · Page 37

Investigation on temporal evolution of the grain refinement in copper under high strain rate loading via in-situ synchrotron measurement and predictive modeling

Synchrotron X-rays are integrated with a modified Kolsky tension bar to conduct in situ tracking of the grain refinement mechanism operating during the dynamic deformation of metals. Copper with an initial average grain size of 36 μm is refined to 6.3 μm when loaded at a constant high strain rate of 1200 s -1 . The synchrotron measurements revealed the temporal evolution of the grain refinement mechanism in terms of the initiation and rate of refinement throughout the loading test. A multiscale coupled probabilistic cellular automata based recrystallization model has been developed to predict the microstructural evolution occurring during dynamic deformation processes. The model accurately predicts the initiation of the grain refinement mechanism with a predicted final average grain size of 2.4 μm. As a result, the model also accurately predicts the temporal evolution in terms of the initiation and extent of refinement when compared with the experimental results.

36 MATERIALS SCIENCE↗

Microstructure, texture and mechanical properties of 6061 aluminum laser beam welded joints

Highlights: • Strong cube texture ({001}<100>) is observed in columnar dendrites. • The ratio of equiaxed dendrites shows proportional relationship with the strength. • The relations between process-microstructure-property are accurately established. - Abstract: In the present study, laser beam welding was carried out with 6061 Al alloy plate to study the microstructural evolution under various welding heat input (ηP/v = 30 J/mm, 38 J/mm, 46 J/mm, and 58 J/mm). The width of the weld metals increased continuously with the heat input values. Quantitatively correlation of the microstructure distribution with welding parameters was developed based on the EBSD results. The weld metals mainly consisted of coarse columnar dendrites and equiaxed dendrites. The ratio of equiaxed dendrites which were controlled by constitutional supercooling and heterogeneous nuclei showed directly proportional relationship with the weld strength. Strong cube texture ({001}<100>) was observed in columnar dendrites, which showed harmful effect on the weld strength. Slight softening in heat affected zone due to recrystallization was identified by nanoindentation tests. All specimens failed in weld metal and the fracture surfaces showed the characteristics of ductile fracture.

36 MATERIALS SCIENCE↗

Laser Additive Manufacturing of F/M Steels for Radiation Tolerant Nuclear Components

According to the Nuclear Energy R&D Roadmap Report submitted to Congress in 2010, one the key challenges facing the nuclear energy industry involves development of new reactor designs with reduced capital costs. Two related R&D objectives outlined in the report include: 1) Making improvements in the affordability of new reactors; and 2) Development of structural materials to withstand irradiation for longer periods. Laser additive manufacturing (LAM) is particularly well suited for more rapid and economical fabrication of reactor components relative to current fabrication methods. The proposed work involving LAM directly addresses the two R&D objectives outlined above relevant to the pertinent mission problems. The classical Materials Science approach involving development of Process/Structure/Property/Performance (P/S/P/P) relations was employed in this project. Processing included LAM and heat-treating. Thermal cycling during LAM is discussed here, and phase diagrams and continuous cooling transformation (CCT) diagrams are used to rationalize microstructural evolution. Structures were characterized including grain size & morphology, volume fraction, morphology, composition and location of carbides in as-deposited and heat-treated conditions. In the simplest sense, the goal was to control microstructures through process manipulation with a view toward optimizing properties and performance in service.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Microstructure Validation of Graph Theory Model-Derived Cooling Rates in the Wire Arc Additive Manufacturing of ER70S-6 Steel

Wire arc additive manufacturing (WAAM) enables high-rate fabrication of large metallic components, but spatial variations in thermal history can lead to microstructural heterogeneity that requires efficient process models to evaluate. This study evaluates whether cooling rates extracted from a graph theory model (GTM)-based thermal simulation are consistent with the microstructural evolution observed in an ER70S-6 WAAM wall. Thermal histories from the model were analyzed at selected build heights, and cooling rates were extracted from the final thermal excursion through the austenite phase field. Microstructures at corresponding locations were characterized using electron backscatter diffraction (EBSD) to quantify grain size distributions, and pearlite interlamellar spacing was used as an additional indicator of cooling behavior. The modeled cooling rates were highest near the substrate and generally decreased with build height, consistent with the observed reduction in the fine grain fraction and the progressive shift in the grain size distribution as build height increased. Pearlite spacing trends also supported the modeled cooling rate variation. These results indicate that GTM-derived thermal histories can be post-processed into metallurgically meaningful cooling rate estimates for WAAM steel builds and linked to dataset specific empirical grain size distribution relationships for process–thermal history–microstructure assessment.

36 MATERIALS SCIENCE↗

Implementation of disruptive designs for gas turbine components using direct energy deposition additive manufacturing

This research aims to develop a framework for establishing the correlation between in-situ monitoring data, process parameters, and microstructure evolution in blown-powder laser-directed energy deposition (DED) additive manufacturing (AM). To achieve this, a comprehensive manufacturing framework has been developed, spanning from in-situ data acquisition, melt-pool simulation, microstructure modeling, and statistical microstructure quantification. A machine learning-based surrogate model is constructed to predict melt pool geometry directly from in-situ coaxial camera data. The surrogate model is trained using outputs from a high-fidelity melt pool simulation, which provides accurate melt pool dimension data under varying process conditions. The predicted melt pool geometry is then used as input to a microstructure model to predict microstructural features. To rigorously compare and analyze microstructures, the project introduces statistical metrics that quantify differences based on key features such as morphology and texture. Microstructures are represented using advanced statistical descriptors including angular chord length distribution, two-point spatial statistics, orientation distribution function, and global spherical harmonic. These representations are used to compute four distinct “dissimilarity scores” that quantitatively capture differences in texture and morphology. This framework is demonstrated to enable automated calibration of simulation parameters by minimizing discrepancies between simulated and target microstructures. The technology developed in this project enables direct correlation between in-situ monitoring data and resulting microstructure, paving the way for adaptive microstructure control in metal AM. This capability strengthens the connection between process parameters and final material properties, facilitating more precise and reliable material design.

36 MATERIALS SCIENCE↗

Evolution of grain boundary character distributions in alloy 825 tubes during high temperature annealing: Is grain boundary engineering achieved through recrystallization or grain growth?

Grain boundary engineering (GBE) of nickel-based alloy 825 tubes was carried out with different cold drawing deformations by using a draw-bench on a factory production line and subsequent annealing at various temperatures. The microstructure evolution of alloy 825 during thermal-mechanical processing (TMP) was characterized by means of the electron backscatter diffraction (EBSD) technique to study the TMP effects on the grain boundary network and the evolution of grain boundary character distributions during high temperature annealing. The results showed that the proportion of ∑ 3{sup n} coincidence site lattice (CSL) boundaries of alloy 825 tubes could be increased to > 75% by the TMP of 5% cold drawing and subsequent annealing at 1050 °C for 10 min. The microstructures of the partially recrystallized samples and the fully recrystallized samples suggested that the proportion of low ∑ CSL grain boundaries depended on the annealing time. The frequency of low ∑ CSL grain boundaries increases rapidly with increasing annealing time associating with the formation of large-size highly-twinned grains-cluster microstructure during recrystallization. However, upon further increasing annealing time, the frequency of low ∑ CSL grain boundaries decreased markedly during grain growth. So it is concluded that grain boundary engineering is achieved through recrystallization rather than grain growth. - Highlights: •The grain boundary engineering (GBE) is applicable to 825 tubes. •GBE is achieved through recrystallization rather than grain growth. •The low ∑ CSL grain boundaries in 825 tubes can be increased to > 75%.

36 MATERIALS SCIENCE↗

Effect of Heat Treatment on Microstructure and Mechanical Properties of Stellite 12 Fabricated by Laser Additive Manufacturing

Microstructure evolution and wear resistance of Stellite 12 produced by laser additive manufacturing were studied in untreated and heat-treated conditions. In untreated conditions, cobalt matrix dendrites and inter-dendritic eutectic carbides were the primary microstructure, blocky and lamellar eutectic carbides can be found, and M{sub 7}C{sub 3} and M{sub 23}C{sub 6} are the primary carbides. Heat treatment can modify the microstructure of this alloy. Primary carbides were dissolved into the cobalt matrix after solution treatment. Aging treatment resulted in the precipitation of carbides, the transformation of M{sub 7}C{sub 3} into M{sub 23}C{sub 6} carbides, and the increase in microhardness. Solution and aging treatment can also cause the precipitation of carbides, but the morphology and distribution of carbides were absolutely different. The wear resistance of untreated samples at room temperature (RT) and 600 °C is better than that at 200 and 400 °C due to the high hardness at RT and the formation of oxide film at 600 °C. The wear resistance of heat-treated samples was tested at 600 °C; it was dominated by the formation and flake-off of oxide film. The sample that underwent solution plus aging treatment has a superior wear resistance.

36 MATERIALS SCIENCE↗

A Study of Tensile Flow and Work-Hardening Behavior of Alloy 617

The simple power relationship σ = Κε{sub p}{sup n} satisfactorily expresses the tensile flow behavior of many metals and alloys in their uniform plastic strain regime. However, many FCC materials with low stacking fault energy have opposed such power law relationship. Alloy 617, an age-hardenable Ni-based superalloy is also observed not to obey the simple power law relationship neither in its solution-treated nor in its aged conditions. Various flow relationships were used to obtain the best fit for the tensile data, and different relationships were identified for the different aged conditions. The work-hardening rate (θ) demonstrates three distinct regions for all aged conditions, and there is an obvious change in the trend of θ versus σ. In the initial portion, θ decreases rapidly followed by a gradual increase in the second stage and again a decrease in its third stage is perceived in the Alloy 617. These three-stage characteristics are attributed to a commonly known precipitate, γ′: Ni{sub 3}(Ti, Al) which evolves during aging treatment and well recognized under transmission electron microscopy (TEM) observation. TEM results also reveal a slight degree of coarsening in γ′ over aging. The tensile flow and the work-hardening behavior are well correlated with other microstructural evolution during the aging treatments.

36 MATERIALS SCIENCE↗

Microstructure and texture evolution of deformed Mg-Zn alloy during recrystallization

Highlights: • The texture intensity in the Mg-Zn alloy relied on the microstructure. • Fine DRXed grains showed a fiber texture distributing between <10.0> and <11.0>. • Coarse DRXed grains mainly exhibited <11.0> fiber texture. • The preferred growth of <11.0> oriented grains resulted in texture evolution. - Abstract: The microstructure and texture evolution of Mg-Zn alloy during recrystallization was investigated by EBSD in the present study. Deformed region, fine DRXed region and coarse DRXed region were obtained in Mg-Zn alloy during deformation. It was found that the texture intensity in DRXed region was weaker compared with the deformed region. The second phase at grain boundaries resulted in the formation of fine DRXed grains with weaker texture compared with the coarse DRXed region. Additionally, a remarkable grain-size driven textural transition from <10.0>–<11.0> texture to <11.0> texture were detected with the growth of DRXed grains. The recrystallized grains with small grain size showed a fiber texture distributing homogeneously between <10.0> and <11.0>, while <11.0> fiber texture was predominant for the large recrystallized grains. It is suggested that <11.0> oriented grains grew faster than other oriented grains, which was ascribed to larger misorientation between <11.0> oriented grains and their neighboring grains.

36 MATERIALS SCIENCE↗

Transmission electron microscopy investigation of phase transformation and fuel constituent redistribution in neutron irradiated U-10wt.%Zr fuel

Uranium-10wt.%zirconium (U-10wt.%Zr) is a primary candidate for fast reactor nuclear fuels. However, there is a lack of data characterizing neutron irradiated crystallographic phases and chemistry. In the current study, the microstructural evolution of a U-10wt.%Zr fuel neutron irradiated to a burnup of 5.7 at.% was investigated by scanning transmission electron microscopy, energy dispersive spectroscopy, and selected area electron diffraction to determine the major phases, alterations in microstructure, and variations in local chemical composition at different localities of a fuel cross-section. The current study revealed that the irradiated U-10wt.%Zr fuel was comprised of various major phases, including a-U, ß-U, and d-UZr2, as well as amorphous and crystalline solid fission product (FP) precipitates within different regions of the fuel cross-section. Regions A and A/B in the center of the fuel were comprised of U-rich, U-intermediate, and U-lean localities with a-U and d-UZr 2 composing the major phases. Regions B and C in the intermediate and peripheral fuel localities, respectively, were comprised of a-U grains, U-rich (ß-U) grains with Zr-rich precipitates, U-intermediate grains (d-UZr2), and solid FP precipitates. The major phases identified were associated with the nanoscopic chemical concentrations, the phase diagram, and the as-characterized specimen temperature, with the exception of the non-equilibrium ß-U phase identified in region B. The U-lean localities in regions A, A/B, B, and C were Zr-enriched pathways along subgrain/grain boundaries. This phenomenon suggests that Zr is susceptible to radiation-induced segregation in U-Zr fuels and indicates a new mechanism for constituent redistribution.

36 MATERIALS SCIENCE↗

Pulse current auxiliary forging of sintered TiAl alloys based on the investigation of dynamic recrystallization and phase transformation

Highlights: • DRX kinetics model of sintered near γ TiAl alloy was established. • DRX process was accompanied by twinning when compressed at 1125 °C/0.1 s{sup − 1}. • Hot deformation has a promotion to the phase transformation of γ → α. - Abstract: Pulse current auxiliary forging is a new and efficient way to fabricate high performance TiAl based alloys. Dynamic recrystallization (DRX) and phase transformation have a pronounced effect on the subsequent deformability of TiAl based alloys. Hence, the dynamic recrystallization kinetics were determined at the temperature range of 1125–1275 °C and strain rate range of 0.1–0.001 s{sup − 1}. In addition, the DRX mechanism and phase transformation of TiAl based alloys were investigated to model the microstructure evolution in order to provide guidance for the pulse current auxiliary forging process. When the specimens were compressed at 1125 °C/0.1 s{sup − 1}, twinning played an important role in the DRX process. With increasing deformation temperature, the microstructure transformed from near gamma into duplex microstructure. In addition, according to the kinetics of dynamic recrystallization and phase transformation, fully DRXed TiAl based alloys were fabricated through pulse current auxiliary forging. The as-forged TiAl-based alloys show good superplastic performance with an elongation over 410%.

36 MATERIALS SCIENCE↗

B2 Grain Growth Behavior of a Ti-22Al-25Nb Alloy Fabricated by Hot Pressing Sintering

Grain growth behavior of a powder metallurgy (P/M) Ti-22Al-25Nb alloy was investigated by applying a series of isothermal treatment tests over a wide range of temperatures and holding times. An isothermal treatment scheme was conducted in the B2 phase region (1070-1110 °C) and α{sub 2} + B2 phase region (1010-1050 °C) at holding times of 10, 30 min, 1, 2, and 3 h, respectively. The effects of temperature and holding time on the microstructure evolution and microhardness of the P/M Ti-22Al-25Nb alloy at elevated temperatures were evaluated using optical microscope, scanning electron microscope, x-ray diffraction, and Vickers hardness test techniques. The results revealed that the alloy’s treated microstructure was closely linked to temperature and holding time, respectively. The change law of B2 grain growth with holding time and temperature can be well interpreted by the Beck equation and Hillert equation, respectively. The B2 grain growth exponent n and activation energy Q were acquired based on experimental data in the α{sub 2} + B2 and B2 phase regions. In addition, the grain growth contour map for the P/M Ti-22Al-25Nb alloy was constructed to depict variations in B2 grain size based on holding time and temperature.

36 MATERIALS SCIENCE↗

Multimodal Analysis of Spatially Heterogeneous Microstructural Refinement and Softening Mechanisms in Three-Pass Friction Stir Processed Al4Si Alloy

Multiple thermally and thermomechanically induced microstructural refinement mechanisms can be activated in metallic alloys when subjected to solid phase processing methods such as friction stir processing (FSP). In this work, we provide detailed descriptions of the relationship between region-specific microstructural refinement mechanisms and the variation in microhardness, through a systematic and multimodal microstructural characterization of an FSP-processed 75% cold-rolled Al-4 at.% Si model binary alloy. Spatially resolved high-energy synchrotron X-ray diffraction, electron backscattered diffraction, and scanning transmission electron microscopy were used to understand the spatially heterogeneous microstructural evolution due to FSP. Results provide insights into how mechanisms such as static recovery, static recrystallization, dynamic recovery and recrystallization, geometric and continuous dynamic recrystallization, and particle-stimulated static or dynamic grain nucleation may occur heterogeneously in the microstructure as a function of the distance from the stir zone in processed alloys, directly influencing the degree of softening. The systematic analysis of microstructures and hardness in the FSP-processed model binary alloy given in this work highlights the rich microstructural domains that can be uniquely harnessed through solid phase processing of metallic alloys.

Al4Si, Friction Stir Processing, Geometric Dynamic↗

Temperature-dependent cyclic response and microstructure of AlSi10Mg(Cu) alloy

Highlights: • The cyclic behavior of AlSi10Mg(Cu) alloy in LCF regime is temperature-dependent. • The transition temperature of the cyclic behavior is about 180 °C. • Microstructure transitions were observed with increasing temperature. - Abstract: In the present work, the cyclic stress response and microstructure evolution of AlSi10Mg(Cu) alloy at high temperature were investigated. Samples were tested at high temperature, under total strain control and tensile-compression loading (R = −1) until failure. The cyclic stress response was analyzed, as well as the microstructures were examined by TEM. The results demonstrated that the cycle stress response of the studied alloy is experimental temperature dependence. Microstructure analysis indicated the precipitated phase was disruptive changed by high temperature compared to the as-received alloy. A lot of coherent β″-Mg{sub 2}Si precipitates and GP zones were observed in the as-received alloy, resulting in sustaining cyclic hardening by pinning effect. At high temperature, the vast majority of the tiny coherency precipitates and clusters transformed to the large semi-coherency Q′ and β′-Mg{sub 2}Si precipitates, leading to the sharp decrease of pinning number and the change of dislocation interaction mechanism, which is believed to be one of the reasons for softening. Another reason is that high temperatures can promote dislocations movement.

36 MATERIALS SCIENCE↗

Microstructural Progression of Shear-Induced Mixing in a CuNi Alloy

Shear deformation has been highlighted in multiple research efforts for its ability to impart mechanical properties improvements and unique microstructures. When used to process and densify powdered material, these shear-based consolidation techniques are commonly referred to as friction consolidation (FC). In this paper, we have examined the microstructural evolution from compacted Cu and Ni powders to a consolidated Cu0.5Ni0.5 alloy. We have shown various stages of porosity reduction and preferential deformation being accommodated by the more ductile material early in the process, leading to formation of a tortuous microstructural zone. Porosity reduction was extensive, decreasing from ~65% in the unprocessed powder to ~1% in the fully consolidated alloy. The final consolidated alloy showed roughly a 2X hardness improvement over the unalloyed, compacted material. Unique aspects of this work include demonstration of the ability to use FC processing to produce a submicron and equiaxed grain size in samples within a 0.5 to 2 minute processing time.

Overman, Nicole R.↗

Austenite formation and cementite dissolution during intercritical annealing of a medium-manganese steel from a martensitic condition

In the present study, in situ high-energy X-ray diffraction (HEXRD), dilatometry, and metallography were conducted for the purpose of understanding microstructure evolution during intercritical annealing of a Fe-0.19C-4.39Mn steel from a martensitic initial condition. Three different simulations for austenite growth and solute partitioning during isothermal holding were conducted using the DICTRA™ module of Thermo-Calc®. The microstructures after intercritical annealing exhibit film-like retained austenite; however, in situ HEXRD indicates that retained austenite in the initial martensitic microstructure had decomposed upon heating to the isothermal holding temperature, suggesting that film-like austenite may be generated during intercritical annealing via nucleation and growth of new austenite and without necessarily preserving initial retained austenite films in the martensitic microstructure. Metallography and in situ HEXRD also indicate that cementite had formed upon heating but did not readily dissolve during an 1800 s isothermal hold although considerable growth of austenite had occurred during the isothermal hold, suggesting that austenite nucleation and initial growth during intercritical annealing does not solely occur due to carbon partitioning. A simulation incorporating cementite suggests that the increase in austenite fraction during intercritical annealing initially occurs in association with Mn partitioning followed by austenite growth induced by gradual cementite dissolution.

36 MATERIALS SCIENCE↗

A crystal plasticity framework for modeling the five-dimensional energy landscape of grain boundaries (Final Technical Report)

In this report, we describe our progress in modeling the co-evolution of grain boundaries and bulk dislocations which plays a crucial role in phenomena such as dynamic recovery, recrystallization, and grain growth in polycrystalline materials. The overarching goal of this work is to develop a robust numerical tool to predict microstructure evolution during severe plastic deformation. This work is associated with the project titled, “Computational Modeling and Design of Radiation Tolerant Materials in Fusion Environments” sponsored by the DOE under grant SC0012774.

36 MATERIALS SCIENCE↗

Preliminary results addressing material qualification using combined ion irradiation and modeling data

Additively-manufactured (AM) materials have attracted increasing attention in recent years as a new method to make novel and customized components. While AM and conventionally produced materials are compositionally similar, they do possess different microstructures, necessitating assessment of materials produced via AM for their behavior in reactor environments. Some microstructures unique to AM materials, such as compositional micro-inhomogeneity and dislocation cell structures, are of particular importance since they may lead to different radiation performance. The performance of AM materials for advanced nuclear reactor applications is of interest to the Advanced Materials and Manufacturing Technologies (AMMT) program under the Department of Energy Office of Nuclear Energy. The AMMT program aims to demonstrate its new accelerated development and qualification methods via laser powder bed fusion (LPBF) 316 stainless steel (SS). Focusing on material bearing both 316L and 316H specifications, we integrate ion irradiation and modeling. This year, we focus on answering foundational questions related to process variability, alloy chemistry variation, and microchemical segregation. Experimental results provide information and motivate questions to the modeling effort, which aims to develop the ability to model radiation-driven microstructural evolution in additively-manufactured 316 stainless steel under a variety of advanced reactor conditions, including different temperatures, neutron spectra, and fluxes, in a sort of "virtual experiment". We perform in-situ and ex-situ ion irradiations and microstructural characterizations to support the development of AM materials for reactor applications, develop a phase field model of radiation-induced segregation in additively manufactured material with high angle grain boundaries and dislocation cells, and investigate the effect of carbon and chromium content on point defect behavior.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗