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ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogeneities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogeneities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogeneities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogenities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

A REDUCED ORDER MODELING APPROACH TO PROBABILISTIC CREEP-DAMAGE PREDICTIONS IN FINITE ELEMENT ANALYSIS

This paper introduces a computationally efficient Reduced Order Modeling (ROM) approach for the probabilistic prediction of creep-damage failure. Component-level probabilistic simulations are needed to assess the reliability and safety of high-temperature components. Full-scale probabilistic creep-damage modeling in finite element (FE) approach is computationally expensive requiring many hundreds of simulations to replicate the uncertainty of component failure. To that end, ROM is proposed to minimize the elevated computational cost while controlling the loss of accuracy. It is proposed that full-scale probabilistic simulations can be completed in 1D at a reduced cost, the extremum conditions extracted, and those conditions applied for lower-cost 2D/3D probabilistic simulations of components that capture the mean and uncertainty of failure. The probabilistic Sine-hyperbolic (Sinh) model is selected which in previous work was calibrated to alloy 304 stainless steel. The Sinh model includes probability density functions (pdfs) for test condition (stress and temperature), initial damage (i.e. microstructure), and material properties uncertainty. The Sinh model is programmed into ANSYS finite element software using the USERCREEP.F material subroutine. First, the Sinh model and FE code are subject to verification and validation to ensure the accuracy of the simulations. Numerous Monte Carlo simulations are executed in a 1D model to generate probabilistic creep deformation, damage, and rupture data. This data is analyzed and the probabilistic parameters corresponding to extreme creep response are extracted. The ROM concept is applied where only the extreme conditions are applied in the 2D probabilistic prediction of a component. The probabilistic predictions between the 1D and 2D geometry is compared to assess ROM for creep. The accuracy of the probabilistic prediction employing the ROM approach will potentially reduce the time and cost of simulating complex engineering systems. Future studies will introduce multi-stage Sinh, stochasticity, and spatial uncertainty for improved prediction.

36 MATERIALS SCIENCE↗

Experimental Fabrication of Porous Additive Manufactured Material

Nuclear industries can benefit from materials that can perform well mechanically and thermally in high temperature and corrosion environments. Functionally graded materials (FGM) are materials manufactured with complex spatial, structural, and chemical compositions, creating components predesigned with tailored microstructural and mechanical properties. Porosity-graded FGMs are designed to introduce pores into a component’s structure as a mechanism to increase bulk or surface material performance, such as stress accommodation and negative thermal conductivity. Additive manufacturing (AM) techniques such as laser energy net shape (LENS) and wire arc additive manufacturing (WAAM), excel in high energy density, point-to-point metal deposition, and present in combination with other combinatorial approaches, exciting methods to manufacture porous FGM components. This project is also examining plasma jet printing as another means for method evaluations for smaller scale graded components. This study explores AM FGM process parameters and combinatorial fabrication methodologies for stainless steel components functionally graded in porosity levels. Preliminary characterization results are provided to attest the feasibility of the combinational fabrication techniques.

36 MATERIALS SCIENCE↗

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogenities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Report on FY 2023 Experimental Results in Developing the Fabrication Parameters for Alloy 709 in Different Product Forms

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 construction in the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code, Section III, Division 5, High Temperature Reactors (ASME 2023). 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, pipes, and forgings using the available ART A709 materials. The objective of this A709 development work in FY 2023 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, which was reported in Y. Wang et al., 2023. This report summarizes the results of the high-speed dilatometry project to develop the CCP diagram using the commercial heat 58776-3RB fabricated by G. O. Carlson and heat 529900-02 fabricated by Allegheny Technologies Incorporated (ATI) Specialty Rolled Products.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Characterization of Intrinsic Fiber Optic Temperature Sensors by In-core and Furnace Testing

Increased research and development in nuclear technology has raised the demand for novel sensors and instrumentation to meet data objectives, and survive in different conditions and environments, beyond conventional light water reactor (LWR) environments. Expediting the deployment of advanced nuclear technologies by developing, demonstrating, and qualifying advanced reactor fuel forms necessitates a deeper understanding of how irradiation affects fuels and materials' performance. To achieve a more comprehensive understanding of fuels and materials performance, researchers require more specialized experiments and measurements. The demand for innovative sensors to support nuclear fuel development arises from the complexity of materials' behavior under irradiation and the challenges of deploying instrumentation in Material Test Reactors (MTRs) for irradiation tests. Additionally, measurements of material properties require integrated measurement systems to characterize thermal properties, mechanical properties, chemistry, and microstructure [1]. Among the potential measurement techniques, optical fiber-based sensors have been identified as potential sensors to measure different physical phenomena such as temperature, strain, pressure, and fluid level. Optical fiber sensors have the capability to provide multi-sensing and multiplexing instrumentation, allowing the measurement of different physical parameters within a single sensor configuration, and transmitting data collected at multiple locations through a single fiber. They offer immunity to electromagnetic interference, electrical passivity, compatibility with various sensing methodologies, and cost-effectiveness. Beyond their widespread use in telecommunications, silica fiber-based instruments are utilized in industrial applications, even at temperatures reaching 300?400°C, such as distributed temperature sensing in oil and gas recovery. The Department of Energy (DOE) is interested in using fiber optics to support fuel cycle development [2]. Fiber optics are an excellent candidate for harsh environment sensing, including sensing at very high temperatures (1900oC for sapphire optical fibers). Distributed fiber optic sensing has been deployed in other harsh environments like coal gasification plants [3]. Distributed strain sensing, which operates similarly to distributed temperature sensing, has been deployed to monitor underground mines and fibers have been imbedded in soil to monitor sink-hole development [4][5]. The application of fiber optic sensors to advanced reactor development is a promising area of research.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Design and Development of Novel Equiatomic Refractory Multi Principal elemental Alloys Based on MoNbTi System for Use in Irradiation Environments

Multi Principal Elemental Alloys (MPEA) have emerged as promising materials for next-generation nuclear reactors due to their exceptional irradiation resistance. Eight equiatomic MPEA based on the MoNbTi system, comprising of elements with low thermal neutron absorption cross-sections were explored using a combined approach employing empirical parameter estimations, and CALPHAD simulations by which the phases and elemental segregation observed in all the alloys in the as-cast state were predicted. Solution heat treatment at 1500°C transformed five alloys into single-phase matrix materials, enhancing homogeneity and reducing hardness. The densities of the alloys ranged between 6.47 to 7.68 g/cm3, hardness between 472 and 656 VHN, Young’s modulus between 142 GPa to 169 GPa, shear modulus between 54 GPa and 62 GPa, bulk modulus between 117 GPa to 194 GPa and Poisson’s ratio between 0.3 to 0.35. The in-situ high temperature Xray diffraction results, differential scanning calorimetry and dilatometry results up to 1000°C suggested the high temperature phase stability of the MPEA. Subsequent ageing heat treatment at 800 and 1000 oC for 96 hours revealed significant secondary phase precipitation in MoNbTiZr, MoNbTiZrV, and MoNbTiCrA. Oxidation studies at 800 oC for 24 hours in air revealed superior oxidation resistance and cubic rate law dependence in Cr containing MPEA especially in MoNbTiCrAl, while severe mass gain resulting in total disintegration and exfoliation in MoNbTiZr and MoNbTiZrV. This comprehensive study underscores the potential of novel MPEA as promising materials for advanced nuclear reactor applications, shedding light on their microstructural control, mechanical properties, thermal stability, and oxidation resistance.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Creep Performance of Novel Composite Heating Elements for Reheat Furnace Electrification

The iron and steel industry is critical for the modern world but is also very energy intensive and is a low margin industry. Hot rolling requires reheating steel slabs to ~1250 °C for hot rolling and involves yield loss due to scale formation. Electrification of this process using resistive heating could improve yield but is currently not possible due to the poor creep resistance of MoSi2 heating elements, which need to be operated well below their maximum temperatures when mounted horizontally. To solve this problem, novel MoSi2 composite heating elements with SiBCN ceramic reinforcements are being developed using high energy ball milling and spark plasma sintering. The creep performance of different heating elements and their corresponding microstructures and electrical properties will be presented.

36 - MATERIALS SCIENCE↗

INFLUENCE OF SUPPLEMENTARY ARGON GAS SHIELDING ON THE MICROSTRUCTURE AND MECHANICAL BEHAVIOR OF SS316L ADDITIVELY MANUFACTURED BY DIRECTED ENERGY DEPOSITION

The dissolution of atmospheric gases into parts additively manufactured by directed energy deposition (DED) has long been of concern, and stock shielding solutions have usually proven inadequate at fully removing atmospheric gases from weld beads. The objective of this work was to design a new supplementary argon gas shroud for a specific DED printer and evaluate its effect on microstructure and macroscopic properties of SS316L and the potential for printing more reactive metals such as Ti-6Al-4V. This was investigated by printing four SS316L sample blocks, two with and two without the shroud, each printed in two different orientations. These samples were subsequently evaluated with inert gas fusion (IGF), SEM/EDS imaging, and tensile tests. The shroud reduced oxygen content by 0.019-0.031%, and SEM imaging revealed fewer oxide inclusions. A more dramatic reduction of 0.13% oxygen and 0.171% nitrogen was observed by the inert gas fusion of Ti-6Al-4V samples. Overall, the results indicated the shroud was successful at reducing atmospheric gas uptake within the print region and may enable the printing of reactive metal powders in DED systems.

Helvie, Kyle↗

Assessment of effective elastic constants of U-10Mo fuel: A multiscale modeling and homogenization study

The significant microstructural changes that U-Mo fuel undergoes during operation degrades its mechanical properties and structural integrity. Microstructural evolution entails the formation, evolution, and redistribution of porosity in conjunction with grain refinement. In the present paper, we employ numerical approaches to assess the impact of the various microstructural features—grains, nanoscale intragranular fission gas bubbles, and mesoscale intergranular voids—on the degradation of elastic constants. Phase-field microstructure models are combined with the asymptotic expansion homogenization technique in order to derive the effective elastic constants as a function of porosity and fission density. Here the results are verified and compared against theoretical bounds. Using this approach, elastic degradation in operating nuclear fuels can be quantified when the distributions of microstructural features are known.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

The In Situ Ion Irradiation Toolbox: Time-Resolved Structure and Property Measurements

Abstract The dynamic interactions of ions with matter drive a host of complex evolution mechanisms, requiring monitoring on short spatial and temporal scales to gain a full picture of a material response. Understanding the evolution of materials under ion irradiation and displacement damage is vital for many fields, including semiconductor processing, nuclear reactors, and space systems. Despite materials in service having a dynamic response to radiation damage, typical characterization is performed post-irradiation, washing out all information from transient processes. Characterizing active processes in situ during irradiation allows the mechanisms at play during the dynamic ion-material interaction process to be deciphered. In this review, we examine the in situ characterization techniques utilized for examining material structure, composition, and property evolution under ion irradiation. Covering analyses of microstructure, surface composition, and material properties, this work offers a perspective on the recent advances in methods for in situ monitoring of materials under ion irradiation, including a future outlook examining the role of complementary and combined characterization techniques in understanding dynamic materials evolution.

36 MATERIALS SCIENCE↗

STEM imaging of irradiation induced defects in Eurofer97 steel variants irradiated in the EUROfusion collaboration

Ten exploratory variants of Eurofer97 reduced activation ferritic martensitic (RAFM) steel were irradiated in HFIR to ~2.94 – 32.4 dpa, 300±30 °C as a part of the EUROfusion collaboration. The irradiations were performed in rabbit capsules. ES21-22 capsule were used for irradiating SS-J3 tensile samples while M4CVN bend bar samples were irradiated in ES31-35 capsules. The mechanical properties and multi-length scale characterization of the microstructures of these ten steels, designated as H, I, P, J, K, L, M, N, O, P and reference E, in the nonirradiated form was reported in "Mechanical properties and microstructure characterization of unirradiated Eurofer-97 steel variants for the EUROfusion project, ORNL/SPR-2018/882," while their irradiated properties and some microstructure analysis was reported in "Post-irradiation examination of Eurofer97 steel variants irradiated to 2.5 dpa, ~300 °C in HFIR for the EUROfusion program, ORNL/SPR-2020/1440." Here, additional microstructures using TEM/STEM and STEM-EDX of the irradiated steels is presented. Characterization was performed at the Low Activation Materials Development and Analysis (LAMDA) laboratory.

36 MATERIALS SCIENCE↗

Micro-structural features and material properties impact on adhesive metal joints via computational modeling and machine learning

The quality of structural bonding in practical applications depends on various factors arising from materials, pre-processing conditions, and manufacturing. Understanding how these factors influence bonding performance and determining their relative importance are of significant interest. Thus, this study evaluates the effects of microstructural features and material properties on the structural strength of adhesively-bonded metal joints at the submillimeter scale, utilizing a combination of Finite Element Modeling (FEM) and Machine Learning (ML) with Gradient Boosting Regression (GBR). The microstructural features include adhesive thickness, internal voids within the adhesive, adherend-adhesive interfacial voids, void size and volume fraction, and surface roughness. The material properties include the constitutive behavior of the adhesive, as well as the adherend-adhesive interfacial strength and fracture energy. The changes in structural strength and morphologies of the bonded metal structures with respect to different microstructural features and material properties were clarified by FEM. By further leveraging ML-GBR, the sequence of importance of these factors affecting bonding performance across various scenarios was summarized. This work provides valuable insights into the development of improved structural bonding for adhesive joints in industries such as automotive , aerospace, and beyond.

36 MATERIALS SCIENCE↗

Influence of cementation on the yield surface of rocks numerically determined from digital microstructures

Digital Rock Physics has reached a level of maturity on the characterisation of primary properties that depend on the microstructure – such as porosity, permeability or elastic moduli – by numerically solving field equations on μCT scan images of rock. After small deformations or at depth though, most rocks eventually reach their limit of elasticity and the complementary plastic properties are needed to describe the full mechanical behaviour. Currently, determination of a rock’s yield surface from its microstructure is often restricted to semi-analytical criteria derived by limit analysis or numerical simulations performed on idealised geometries. Such simplification lacks representativeness, particularly for processes that affect directly the pore-grain interface such as the cementation phenomenon, happening during diagenesis. Eventually, only direct numerical simulation of elasto-plasticity performed on digitalised microstructures can be used to assess the strength of different cemented materials and its evolution with the alteration of the microstructure. In this study, we provide a comprehensive parametric study on the impact of cementation on rock strength for real microstructures of cemented granular materials. Compared to most previous studies, the whole yield surface is determined numerically (using Finite Element Method) in order to assess the influence of cementation for different stress-paths. The previously known tendency of rock to strengthen with increasing cementation volume is verified. New results on the influence of cement property namely Young’s modulus, friction and cohesion on the rock’s yield surface are explored. The envelopes obtained are compared to the ones obtained by experimental data and existing models. Finally, the framework presented in this study showcases the wider possibility of determining any rock’s or porous material’s yield surface from its microstructure.

36 MATERIALS SCIENCE↗