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At least 1,711 records · Page 95

Observation of columnar microstructure in lattice-matched InAlN/GaN grown by plasma assisted molecular beam epitaxy

Nominally lattice matched InAlN/GaN was grown by plasma-assisted molecular beam epitaxy, and the intrinsic microstructure was investigated via x-ray diffraction, transmission electron microscopy, and atom probe tomography. The InAlN showed a cellular structure, which was comprised of ~10 nm wide Al-rich cores and ~1 nm In-rich InAlN intercellular boundaries. Despite the strong laterally non-uniform In distribution, both vertical and lateral lattices are unperturbed by the cellular structure, as evidenced by strong thickness fringes in on-axis ω-2θ high resolution x-ray diffraction scans, coherence lengths derived from on-axis (0002) and off-axis (10{anti 1}2) ω-2θ high resolution x-ray diffraction scans, and a modified Williamson-Hall analysis for on-axis reflections.

36 MATERIALS SCIENCE↗

Hot corrosion behavior of 304 & P91 graded composite transition joint under molten sulfate salts

A novel graded composite transition joint (GCTJ) between AISI 304 stainless steel and ASTM A335 P91 steel, has been demonstrated remarkablely superior creep performance compared to the conventional dissimilar metal weldment (DMW) under equivalent conditions. However, this advance is challenged by hot corrosion under salt deposition at elevated temperatures. Here, this study investigates the hot corrosion behavior of 304&P91 GCTJ exposed to sulfate salts at 700°C. Compared to the 304 steel, corrosion attacks initiate in the P91 triangle, where the dual-phase microstructure of ferrite and tempered martensite significantly influences pitting initiation. Anodic dissolution mainly occurs within the tempered martensite due to more vulnerable sites within the tempered martensite. With prolonged exposure, corrosion propagates across both phases, and the corrosion depth within the P91 triangle is related to the exposed surface area ratio between 304 and P91. Electrochemical analysis reveals the occurrence of galvanic corrosion between the 304 and P91, with a positive linear relationship between anodic dissolution current density (I a ) and the exposed surface area ratio between 304 and P91 in molten salts, further emphasizing the critical impact of this ratio on the corrosion severity in the P91 triangle. These findings underscore the importance of transition zone design optimization in mitigating localized corrosion.

Galvanic corrosion↗

Discovery, Design, Synthesis and Testing of High Performance Structural Alloys (Final Technical Report)

The overarching goal of this project is to understand the phase stability and mechanical behavior of non-stoichiometric multi-principal element alloy (MPEA) materials. In order to identify suitable alloys, we plan to use a combinatorial thin film screening approach, in collaboration with scientists at Lawrence Berkeley National Laboratory who are performing computational work as well as complementary experimental work. Specific tasks within the scope of this project include the fabrication, using thin film deposition from six sputtering targets, of combinatorial samples with multi-dimensional gradients in composition and microstructure. These samples are studied to screen MPEA systems for promising candidate alloys with specific composition(s), based on characterization of composition, structure and mechanical behavior across the thin film. We want to produce single-phase MPEAs with chemical homogeneity in a given thin film region, simple grain structures, and no intermetallic phases present. Gradient films facilitate first-pass screening for desirable characteristics and inform the next stage of work that involves fabrication of bulk MPEA specimens for (tensile) mechanical testing and characterization. To make the bulk alloys, metal (elemental) pieces are melted to form MPEAs, followed by heat treatment to homogenize the composition and microstructure. A subset of alloys is also cast, using vacuum arc melting, to yield larger samples (diameter ~1 cm and length ~5-10 cm) and these allow us to assess viability of scale-up for the alloys in structural applications. Further processing plans include rolling and heat treatment to recrystallize selected bulk MPEAs and grow grains to different extents, in order to investigate size effects in the mechanical behavior of MPEAs. Microspecimen testing will be performed (primarily in tension) to assess the mechanical behavior over a range of temperatures. The deformation microstructure of mechanically tested alloys will be characterized using transmission electron microscopy (TEM) to provide a scientific basis for understanding the structure-property relationships in MPEA mechanical behavior.

36 MATERIALS SCIENCE↗

A Comparative Study of the Efficacy of Local/Global and Parametric/Nonparametric Machine Learning Methods for Establishing Structure–Property Linkages in High-Contrast 3D Elastic Composites

Reduced-order structure–property (S-P) linkages play a pivotal role in the tailored design of materials for advanced engineering components. There is a critical need to distill these from the simulation datasets aggregated using sophisticated, computationally expensive, physics-based numerical tools (e.g., finite element methods). The recent emergence of materials data science approaches has opened new avenues for addressing this challenge. In this paper, we critically compare the relative merits of the application of four distinct machine learning approaches for their efficacy in extracting microstructure-property linkages from the finite element simulation data aggregated on high-contrast elastic composites with different microstructures. The machine learning approaches selected for the study have included different combinations of local/global and parametric/nonparametric approaches. Furthermore, the nonparametric approaches selected for this study are based on Gaussian Process (GP) models that allow for a formal treatment of uncertainty quantification in the predicted values. The predictive performances of these different approaches have been compared against each other using rigorous cross-validation error metrics. Furthermore, their sensitivity to both the dataset size and dimensionality has been investigated.

36 MATERIALS SCIENCE↗

Dissipation of radiation energy in concentrated solid-solution alloys: Unique defect properties and microstructural evolution

The effort to develop metallic alloys with increased structural strength and improved radiation performance has focused on the incorporation of either solute elements or microstructural inhomogeneities to mitigate damage. The recent discovery and development of single-phase concentrated solid-solution alloys (SP-CSAs) has prompted fundamental questions that challenge established theories and models currently applicable to conventional alloys. Here, the current understanding of electronic and atomic effects, defect evolution, and microstructure progression suggests that radiation energy dissipates in SP-CSAs at different interaction strengths via energy carriers (electrons, phonons, and magnons). Modification of electronic- and atomic-level heterogeneities and tailoring of atomic transport processes can be realized through tuning of the chemical complexity of SP-CSAs by the selection of appropriate elements and their concentrations. Fundamental understanding of controlling energy dissipation via site-to-site chemical complexity reveals new design principles for predictive discovery and guided synthesis of new alloys with targeted functionalities, including radiation tolerance.

36 MATERIALS SCIENCE↗

Deep Learning-Based Hardness Prediction of Novel Refractory High-Entropy Alloys with Experimental Validation

Hardness is an essential property in the design of refractory high entropy alloys (RHEAs). This study shows how a neural network (NN) model can be used to predict the hardness of a RHEA, for the first time. We predicted the hardness of several alloys, including the novel C0.1Cr3Mo11.9Nb20Re15Ta30W20 using the NN model. The hardness predicted from the NN model was consistent with the available experimental results. The NN model prediction of C0.1Cr3Mo11.9Nb20Re15Ta30W20 was verified by experimentally synthesizing and investigating its microstructure properties and hardness. This model provides an alternative route to determine the Vickers hardness of RHEAs.

36 MATERIALS SCIENCE↗

Design and development of equi-atomic refractory High Entropy Alloys for use in radiation environments

Development of new structural materials that can withstand the extreme environments of nuclear reactors where the materials are exposed to high dose rate of ~ 30 200 dpa, high temperatures of the order of 500 1000 o C and tens of years of operation is vital for exploiting the “smallest carbon footprint energy source” to its fullest, in order to deal with the energy crisis worldwide. Recently, HEAs have shown superior irradiation properties over conventional alloys like higher resistance to defect formation, lower void swelling, limited irradiation hardening and higher microstructural stability under irradiation, making them potential structural material candidates for reactors. Proper characterization and testing of these materials are essential before they can replace the conventional alloys.

36 MATERIALS SCIENCE↗

AREVA NP MR Cladding benefits for proposed US NRC RIA and LOCA requirements

M5 is the reference alloy of AREVA NP for PWR cladding applications. It is a zirconium-based alloy containing 1% niobium, no tin, and well-controlled oxygen, iron, and sulfur contents. It has a fully recrystallized microstructure. The absence of tin in M5 results in a very low corrosion rate and hydrogen pick-up during normal operation, even at high burn-up and in high duty irradiation conditions. Due to this low hydrogen pick-up under irradiation (typically less than 100 ppm, End of Life), M5 retains a very good strength and an exceptional residual ductility during and after the accident. This allows utilities implementing M5 to simplify the safety analysis and to demonstrate significant margins regarding fuel related criteria. Simplified methods are easier for plants to implement and maintain for future plant operations and core design management. This paper specifically presents 3 examples on the safety improvement brought by M5 cladding. First, during a reactivity-induced accident (RIA), the properties of M5 are such that bounding analyses for future cycles are significantly simplified, in particular by demonstrating that fuel dispersal will not occur. The major aspects of the AREVA NP RIA methodology are presented. A second focus is made on the low hydrogen embrittlement of M5 and on its high ductility after quenching during a loss-of-coolant accident (LOCA). In a third part, the breakaway oxidation testing program currently under development in Paimboeuf (France) is described, including details about the testing devices and qualification. The tests have demonstrated that M5 cladding does not have breakaway at least up to 5000 s oxidation duration at 1000 C. degrees, which is much higher than the LOCA duration.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

High-resolution characterization of ceramic-metal interface of TiN coating on ferritic-steels for nuclear application

Advanced fuel cladding is critical for fast reactors, offering sufficient thermal conductivity, mechanical and dimensional stability and radiation tolerance of the cladding base material. Additionally, it must provide corrosion resistance and high temperature coolant compatibility on the cladding outer surface, as well as chemical stability on the cladding inner wall against fuel cladding chemical interaction (FCCI). TiN ceramic coating has been considered an effective diffusion barrier for inner and outer cladding-walls for enhanced performance. The TiN-metal interface microstructure and chemistry play a critical role in coating bond strength and integrity under harsh conditions. High-resolution transmission electron microscopy characterization of ceramic-metal interface at atomic resolution in unirradiated, irradiated and thermal cycled conditions were performed. The interface remained intact after irradiation up to 200 dpa or thermal cycling five times up to 550 °C. In conclusion, this work discusses the potential impact of these results on coating performance and design for advanced claddings.

36 - MATERIALS SCIENCE↗

Postirradiation Examination of the ATF-1 Experiments - 2018 Status

The Advanced Fuels Campaign in collaboration with industry are working to develop enhanced accident tolerant fuels for light water reactors. The initial irradiations of these concepts were performed in the Idaho National Laboratory Advanced Test Reactor using simple drop-in style irradiations. These irradiations are collectively referred to as ATF 1. The postirradiation examination of ATF 1 has begun and some concepts have now completed initial examination. This report describes the results of examinations on ATF 1 irradiations designed to test the feasibility of enhancing UO 2 thermal conductivity with additives, ATF 1 irradiations of uranium silicide, and the current status of ATF 1 irradiations that are in process at the hot cell. Enhanced thermal conductivity uranium dioxide composites containing silicon carbide (UO 2 SiC) and diamond (UO 2 diamond) have been irradiated to low burnup. The conditions of this irradiation test and subsequent postirradiation examinations are discussed. These irradiations evaluate fuel microstructure and potential fuel cladding interaction under representative light water reactor power conditions. Both non destructive and destructive techniques have been used to evaluate fuel integrity, fission gas release, fission product distribution, burnup, fuel swelling and cladding strain. Examination of the UO 2 SiC pellets revealed enhanced cracking when compared to a UO 2 rodlet also irradiated under similar conditions. Additionally, instability of the SiC whiskers in the uranium dioxide matrix was observed in the pellet central region, where the local temperatures exceeded 1300 °C. The microstructure of the diamond added UO 2 was severely disrupted during irradiation, resulting in local migration of cesium along the fuel stack and increased fission gas release when compared with the expected release from the Vitanza curve at corresponding values of burnup and irradiation temperature. The postirradiation examination results cast doubt on the suitability of these additives to improve UO 2 fuel performance in a way that would lead to enhanced accident tolerance. Additionally, postirradiation examination data of U 3 Si 2 fuels at low burnup (i.e., < 20 GWd/tHM) for application in advanced Light Water Reactor (LWR) is presented. The U 3 Si 2 pellets show limited cracking in comparison to the expected behavior of UO 2 at same power level. In addition, gamma scanning data did not reveal migration of fission products. Minor homogeneous hardening along the pellet radius due to accumulation of fission products and radiation damage was measured by microindentation. The fission gas release and swelling remains very low. Formation of fission gas bubbles resolvable with optical microscopy occurs from the pellets center outward to approximately 60% of the fuel pellet radius. The overall data suggest a good performance of this accident tolerant fuel candidate at low burnup. Finally, the current status of postirradiation examination on other ATF 1 irradiations will be discussed. These irradiations include UO 2 clad in an FeCrAl alloy, an alternative uranium silicide compound U 3 Si 5 also clad in a FeCrAl alloy, and an interaction test between UO 2 and different FeCrAl alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

BISON Capability to Account for Dopant Sensitivity in Relevant UO 2 Material Models

The U.S. Department of Energy’s Nuclear Energy Advanced Modeling and Simulation program aims to develop predictive capabilities using computational methods for the analysis and design of advanced reactor and fuel cycle systems. This program has been supporting the development of BISON, a high-fidelity and high-resolution fuel performance tool at the engineering scale. Incorporation of more physics-based models in BISON for the accident tolerant fuel applications motivated this study. This document details integration of new modeling capabilities in BISON, including: a tensile strength model for uranium dioxide (UO 2 ) fuel to incorporate the microstructural effects (e.g., grain size, fabrication pore size, and porosity), and atomistic-informed creep model for UO 2 fuel that is developed by Los Alamos National Laboratory. Sensitivity analyses are conducted on these models separately as well as a two-dimensional full rod application under normal operating conditions. Lastly, these new modeling capabilities in BISON are exercised in Halden IFA-677.1 and IFA-716.1 assessment cases.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Sintered Cathodes for All-Solid-State Structural Lithium-Ion Batteries

All-solid-state structural lithium ion batteries serve as both structural load-bearing components and as electrical energy storage devices to achieve system level weight savings in aerospace and other transportation applications. This multifunctional design goal is critical for the realization of next generation hybrid or all-electric propulsion systems. Additionally, transitioning to solid state technology improves upon battery safety from previous volatile architectures. This research established baseline solid state processing conditions and performance benchmarks for intercalation-type layered oxide materials for multifunctional application. Under consideration were lithium cobalt oxide and lithium nickel manganese cobalt oxide. Pertinent characteristics such as electrical conductivity, strength, chemical stability, and microstructure were characterized for future application in all-solid-state structural battery cathodes. The study includes characterization by XRD, ICP, SEM, ring-on-ring mechanical testing, and electrical impedance spectroscopy to elucidate optimal processing parameters, material characteristics, and multifunctional performance benchmarks. These findings provide initial conditions for implementing existing cathode materials in load bearing applications.

Ceramics↗

Microstructure and thermal conductivity of surfactant-free NiO nanostructures

High purity, nanometer sized surfactant-free nickel oxide (NiO) particles were produced in gram scale using a solution combustion method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), gas pycnometry and gas adsorption analysis (BET). The average particle size of the as-synthesized NiO increases significantly with the preheating temperature of the furnace, while the specific surface area decreases. A BET specific surface area of {approx}100 m{sup 2}/g was obtained for NiO nanoparticles with size as small as 3 nm synthesized at 300 Degree-Sign C. The thermal conductivity ({kappa}) of pressed pellets of the synthesized NiO nanoparticles obtained using spark plasma sintering (SPS) and uniaxial hot pressing is drastically decreased ({approx}60%) compared to that of NiO single crystal. This strong reduction in {kappa} with particle size suggests the suitability of the synthesized surfactant-free NiO nanoparticles for use as nanoinclusions when designing high performance materials for waste heat recovery. - Graphical abstract: Highly efficient phonon scattering by surfactant-free NiO nanostructures obtained by solution combustion of a mixture of nickel (II) nitrate hexahydrate (oxidizer) and urea (fuel) at various temperatures. Highlights: Black-Right-Pointing-Pointer Fast synthesis of surfactant-free NiO nanoparticles with controllable size. Black-Right-Pointing-Pointer High specific surface area for NiO nanoparticles with size range from 3 to 7 nm. Black-Right-Pointing-Pointer Strong reduction of the thermal conductivity with decreasing particle size. Black-Right-Pointing-Pointer NiO as nanoinclusions in high performance materials for energy conversion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Origin of Ferroelectric Phase Stabilization via the Clamping Effect in Ferroelectric Hafnium Zirconium Oxide Thin Films

The presence of the top electrode on hafnium oxide-based thin films during processing has been shown to drive an increase in the amount of metastable ferroelectric orthorhombic phase and polarization performance. This “Clamping Effect,” also referred to as the Capping or Confinement Effect, is attributed to the mechanical stress and confinement from the top electrode layer. However, other contributions to orthorhombic phase stabilization have been experimentally reported, which may also be affected by the presence of a top electrode. In this study, it is shown that the presence of the top electrode during thermal processing results in larger tensile biaxial stress magnitudes and concomitant increases in ferroelectric phase fraction and polarization response, whereas film chemistry, microstructure, and crystallization temperature are not affected. Through etching experiments and measurement of stress evolution for each processing step, it is shown that the top electrode locally inhibits out-of-plane expansion in the HZO during crystallization, which prevents equilibrium monoclinic phase formation and stabilizes the orthorhombic phase. This study provides a mechanistic understanding of the clamping effect and orthorhombic phase formation in ferroelectric hafnium oxide-based thin films, which informs the future design of these materials to maximize ferroelectric phase purity and corresponding polarization behavior.

36 MATERIALS SCIENCE↗

One-Shot Synthesis and Melt Self-Assembly of Bottlebrush Copolymers with a Gradient Compositional Profile

Morphological control plays a central role in soft materials design. Herein, we report the synthesis of a gradient bottlebrush architecture and its role in directing molecular packing in the solid state. Bottlebrush copolymers with gradient interfaces were prepared via one-shot ring-opening metathesis polymerization of exo- and endo- norbornene-capped macromonomers. Kinetic studies revealed a gradient compositional profile separating the two blocks along the backbone. Side-chain symmetric gradient bottlebrush copolymers exhibited a strong tendency to assemble into cylindrical microstructures, in contrast to their block copolymer analogs with sharp interfaces. Furthermore such exquisite architectural control of the interfacial composition affords a delicate handle to direct macromolecular assembly.

36 MATERIALS SCIENCE↗

Research Plan and Preliminary Results in Developing the Fabrication Parameters for Alloy 709 in Different Product Forms―Grain Coarsening Temperature Evaluation

The Advanced Reactor Technologies (ART) Program has established a multi-year plan to develop Alloy 709 advanced stainless steel (A709), generate the data package and develop material-specific design parameters in qualifying it as a new structural material for Class A component design in the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code, Section III, Division 5, High Temperature Reactors. In collaboration with material vendors, the Advanced Materials Development activities under ART have successfully scaled the A709 plate form production from a laboratory heat of 500 pounds to commercial heats totaling 133,000 pounds of A709 plate fabricated from three heats. The goal of the overall A709 development program is to establish the necessary microstructural and mechanical properties relationship for A709 to ultimately develop fabrication parameters for other product forms such as bars, piping and forging using the available ART A709 materials. The objective of this A709 development work at ORNL in FY2023 is to experimentally determine grain coarsening behavior for the A709 heats and to experimentally generate the continuous cooling precipitation (CCP) diagram for A709 using the as-rolled commercial heat plate materials. Integral to this work is the characterization of the as-rolled materials and the determination of an effective solution annealing process. This report summarizes the work performed to identify the grain coarsening temperature for commercial heat 58776-3RB fabricated by G. O. Carlson and heat 529900-02 fabricated by Allegheny Technologies Incorporated (ATI) Flat Rolled Products.

36 MATERIALS SCIENCE↗

Development of powder metallurgy 2XXX series Al alloy plate and sheet materials for high temperature aircraft structural applications, FY 1983/1984

The objective of this investigation is to fabricate and evaluate PM 2124 Al alloy plate and sheet materials according to NASA program goals for damage tolerance and fatigue resistance. Previous research has indicated the outstanding strength-toughness relationship available with PM 2124 Al-Zr modified alloy compositions in extruded product forms. The range of processing conditions was explored in the fabrication of plate and sheet gage materials, as well as the resultant mechanical and metallurgical properties. The PM composition based on Al-3.70 Cu-1.85 Mg-0.20 Mn with 0.60 wt. pct. Zr was selected. Flat rolled material consisting of 0.250 in. thick plate was fabricated using selected thermal mechanical treatments (TMT). The schedule of TMT operations was designed to yield the extreme conditions of grain structure normally encountered in the fabrication of flat rolled products, specifically recrystallized and unrecrystallized. The PM Al alloy plate and sheet materials exhibited improved strength properties at thin gages compared to IM Al alloys, as a consequence of their enhanced ability to inhibit recrystallization and grain growth. In addition, the PM 2124 Al alloys offer much better combinations of strength and toughnessover equivalent IM Al. The alloy microstructures were examined by optical metallographic texture techniques in order to establish the metallurgical basis for these significant property improvements.

Chellman, D. J.↗

The Prediction of Long-Term Thermal Aging in Cast Austenitic Stainless Steel

Cast austenitic stainless steel (CASS) materials are extensively used for many massive primary coolant system components of light water reactors (LWRs) including coolant piping, valve bodies, pump casings, and piping elbows. Many of these components are operated in complex and persistently damaging environments of elevated temperature, high pressure, corrosive environment, and sometimes radiation for long periods of time. Since a large number of CASS components are installed in every nuclear power plant and replacing such massive components is prohibitively expensive, any significant degradation in mechanical properties that affects structural integrity, cracking resistance in particular, of CASS components will raise a serious concern on the performance of entire power plant. The CASS materials for nuclear components are highly corrosion-resistant Fe-Cr-Ni alloys with 300 series stainless steel compositions and mostly austenite (γ)–ferrite (δ) duplex structures, which result from the casting processes consisting of alloy melting and pouring or injecting liquid metal into a static or spinning mold. Although the commonly used static and centrifugal casting processes enable the fabrication of massive components with proper resistance to environmental attacks, the alloying and microstructural conditions are not highly controllable in actual fabrication, especially in the casting processes of massive components. In the corrosion-resistant Fe-Cr-Ni alloy system, the minor phase (i.e., the δ-ferrite phase) is inevitably formed during the casting process, and is in a non-equilibrium state subject to detrimental changes during exposure to elevated temperature and/or radiation. In general, relatively few critical degradation modes are expected within the current design lifetime of 40 years, given that the CASS components have been processed properly. It has been well known, however, that both the thermal aging and the neutron irradiation can cause degradation of static and impact toughness in the cast stainless steels, and if combined with any flaws formed during the fabrication process or in service, the thermal degradation in CASS components can be a serious concern for the integrity of the power plant. On the integrity of the CASS components during the extended lifetime of 60 years or longer, no conclusive prediction has been possible, primarily because no direct experience with these materials currently exists, and the aging behavior of CASS alloys still remains largely uncertain. The ongoing research for CASS aging, as part of the LWRS Program/Materials Aging and Degradation Pathway, is an integrated research using holistic experimental and modeling means to provide both the scientific understanding on the aging and failure phenomena and the practical models to predict the degree of property degradation.

cast stainless steels↗