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DOE OSTI2022

Improving Structural Integrity of Direct Laser-Deposited Ni – Co – Cr – Al – Y Superalloys by Alloy Modification

Abstract Ni- and Co-based M–Cr–Al–Y (M = Ni and/or Co), dual phase β and γ/γ′, β—Ni–Al, γ—Ni(Co, Cr), and γ′—Ni3–Al superalloys exhibit several beneficial high-temperature (>1000 °C) (2012 °F) strength and corrosion resistance properties. Our study investigates the feasibility of fabricating a commercially available Ni–Co–Cr–AlY alloy (tradename “Amdry 386”) using laser directed energy deposition (laser-DED). A significant challenge for laser fabrication of bulk Amdry 386 (A386) structures stems from the presence of relatively higher amounts of the β phase than γ/γ′ phases. While prior studies report laser fabrication of these materials in coating and cladding configurations, bulk structures have not been realized. To investigate these challenges, this study was developed to systematically evaluate the effects of modifying the A386 alloy by adding 10, 20, and 30% by weight of a Ni–20%Cr (Ni–Cr) alloy (mainly γ/γ′). Laser-DED-fabricated A386 coupons exhibited a metastable, rapidly solidified β-rich microstructure typical to laser processes. The A386 + Ni–Cr mixtures were processed using laser-DED, and small coupons from each composition were evaluated using SEM, XRD, and microhardness to characterize the as-processed microstructure. Thermodynamic modeling was performed to determine the phase evolution as a function of the alloy composition. The dominating phase switches from β to γ/γ’ between the A386 and A386 + 10% Ni–Cr mixtures, but the increase in structural integrity is not observed until the Ni–Cr additions reach a minimum of 20%. Our results show that the alloy chemistry can be successfully modified to improve the structural integrity of laser-processed structures.

Engineering↗

DOE OSTI2023

Development of process parameters and post-build conditions for qualification of LPBF 316 SS

To harness the potential of laser powder bed fusion (LPBF) 316H stainless steel (SS) for use in advanced nuclear reactors, extensive research efforts are needed to develop optimal laser processing parameters and appropriate heat treatments, taking into account various manufacturing platforms and locations. Furthermore, it is crucial to assess the material properties in environments relevant to reactor operating conditions. In collaboration with Oak Ridge National Laboratory (ORNL) and Los Alamos National Laboratory (LANL), Argonne National Laboratory (ANL) is dedicated to gaining insights into how the manufacturing process and post-build treatments impact the performance of LPBF 316H SS. This report provides an overview of ANL's research findings for FY23, focusing on LPBF 316H SS produced using a Renishaw AM400 laser system. Specifically, our research has concentrated on three key areas: 1) Optimum laser processing parameters: Leveraging the high-throughput printing technology, we systematically varied the laser power, exposure time and point distance within the same build. By measuring the as-printed porosity, we identified an optimum printing parameter window that produced materials with near-complete density; 2) Post-built treatment development: Materials printed with the optimum laser parameters underwent treatments including stress relief, solution annealing, and hot isostatic pressing. Subsequently, we fabricated tension, creep, and fatigue specimens from materials subjected to these different conditions. Over the next year, a series of scoping tests will be conducted to facilitate the selection of the most suitable post-build treatment condition; 3) Thermal aging effects on microstructure and properties: thermal aging at 550°C, 650°C and 750°C was conducted on LPBF 316H SS specimens up to 2500 h. Microstructural characterization was performed with electron microscopy, and the evolution of the dislocation cell structures and secondary phases was studied. Microhardness tests and tension tests were conducted to quantify changes in mechanical properties. The results revealed that the aged LPBF 316H SS exhibited a high density of Cr-rich and Mo-rich fine precipitates within grains due to the presence of a high density of dislocations and the globally distributed dislocation cell structures, which served as heterogeneous nucleation sites for secondary phases. Along grain boundaries, a Mo-Cr-rich phase, observed in 750°C-aged conditions, displayed significant thermal coarsening. Throughout the aging process, various mechanisms, including stress relaxation, dislocation cell structure recovery, solution hardening, and precipitation hardening, competed to influence materials strength. These results contribute towards establishing the technical basis for qualifying LPBF 316H SS for advanced nuclear reactor applications.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Characterization of Build Parameters and Microstructure in Low Heat Input WAAM of Ni-Based Superalloy Haynes 282

Ni-based superalloy Haynes® 282® is being targeted for various applications in advanced power generation systems for its superior fabricability, weldability, and excellent high temperature creep and corrosion performance. This process optimization study aims to use a low heat-input, high deposition rate, controlled Gas Metal Arc Welding (GMAW) process, Cold Metal Transfer (CMT) by Fronius, attempting to achieve fully dense fabrication and possibly avoid the need for HIP. Twenty-one multilayer blocks (~25x100x40 mm3) were deposited to explore a large set of build parameters variations that focused on varying the travel speed from 14 to 42 inches per minute (ipm) and wire feed speed from 150 to 450 ipm. A strong correlation has been observed between arc energy – controlled primarily by travel and wire feed speed. Initial visual inspection, internal microstructural examination, and computed tomography (CT) have been used to determine the effects of built parameters on evolution of internal porosity and defects. Scanning electron microscopy techniques enabled structural and compositional imaging of heterogeneity and changes in microstructural properties.

additive manufacturing↗

DOE OSTI2025

Characterization of Build Parameters and Microstructure in Low Heat Input WAAM of Ni-Based Superalloy Haynes 282

additive manufacturing↗

DOE OSTI2024

Phase Composition and Phase Transformation of Additively Manufactured Nickel Alloy 718 AM Bench Artifacts

Additive manufacturing (AM) technologies offer unprecedented design flexibility but are limited by a lack of understanding of the material microstructure formed under their extreme and transient processing conditions and its subsequent transformation during post-build processing. As part of the 2022 AM Bench Challenge, sponsored by the National Institute of Standards and Technology, this study focuses on the phase composition and phase evolution of AM nickel alloy 718, a nickel-based superalloy, to provide benchmark data essential for the validation of computational models for microstructural predictions. Here, we employed high-energy synchrotron X-ray diffraction, in situ synchrotron X-ray scattering, as well as high-resolution transmission electron microscopy for our analyses. The study uncovers critical aspects of the microstructure in its as-built state, its transformation during homogenization, and its phase evolution during subsequent aging heat treatment. Specifically, we identified secondary phases, monitored the dissolution and coarsening of microstructural elements, and observed the formation and stability of γ ’ and γ ” phases. The results provide the rigorous benchmark data required to understand the atomic and microstructural transformations of AM nickel alloy 718, thereby enhancing the reliability and applicability of AM models for predicting phase evolution and mechanical properties.

36 MATERIALS SCIENCE↗

DOE OSTI2021

In situ synchrotron diffraction and modeling of non-equilibrium solidification of a MnFeCoNiCu alloy

The solidification mechanism and segregation behavior of laser-melted Mn 35 Fe 5 Co 20 Ni 20 Cu 20 was firstly investigated via in situ synchrotron x-ray diffraction at millisecond temporal resolution. The transient composition evolution of the random solid solution during sequential solidification of dendritic and interdendritic regions complicates the analysis of synchrotron diffraction data via any single conventional tool, such as Rietveld refinement. Therefore, a novel approach combining a hard-sphere approximation model, thermodynamic simulation, thermal expansion measurement and microstructural characterization was developed to assist in a fundamental understanding of the evolution of local composition, lattice parameter, and dendrite volume fraction corresponding to the diffraction data. This methodology yields self-consistent results across different methods. Via this approach, four distinct stages were identified, including: (I) FCC dendrite solidification, (II) solidification of FCC interdendritic region, (III) solid-state interdiffusion and (IV) final cooling with marginal diffusion. It was found out that in Stage I, Cu and Mn were rejected into liquid as Mn 35 Fe 5 Co 20 Ni 20 Cu 20 solidified dendritically. During Stage II, the lattice parameter disparity between dendrite and interdendritic region escalated as Cu and Mn continued segregating into the interdendritic region. After complete solidification, during Stage III, the lattice parameter disparity gradually decreases, demonstrating a degree of composition homogenization. The volume fraction of dendrites slightly grew from 58.3 to 65.5%, based on the evolving composition profile across a dendrite/interdendritic interface in diffusion calculations. Postmortem metallography further confirmed that dendrites have a volume fraction of 64.7 ± 5.3% in the final microstructure.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Microstructure Clones

Background: A material’s microstructure drives its material performance. Contemporary crystal plasticity experiments compare full-field strain measurements of polycrystal specimens to models. Because each specimen is unique, it is impossible to know which features of the observed deformation are deterministic vs statistical; thus, differences between model and experiment may or may not be significant. Objective: This paper introduces the invention of microstructure clones. Microstructure clones are 2D oligocrystal specimens that have nearly identical microstructures to remedy the aforementioned experimental limitations. Having specimens with nearly identical microstructures will allow for multiple destructive tests of a microstructure (either as repeats or intentionally different experiments), an ability to “see the future” by providing insight into how a specimen will deform, variability quantification, and experimental investigations of response to small microstructural changes. Methods: This work introduces microstructure clones. Repeatability of these clones is demonstrated in tensile bars of pure nickel. Local strain measurements from digital image correlation are compared between clone specimens and compared to results from a crystal plasticity finite element model. Results: Two sets of microstructure clones were tested in this study and displayed very consistent deformation responses within each clone set. Small observed differences in deformation invite investigation into microstructure stochasticity and the effect of small microstructural and loading differences. Conclusions: Microstructure clones represent a significant shift in understanding structure–property relationships. This work reshapes experimental crystal plasticity to allow for experiments that control for specific variables, quantification of microstructural stochasticity (and other sources of stochasticity), and opportunities for replicating experiments.

Crystal Plasticity↗

DOE OSTI2022

Measurement of Transport Properties of Woody Biomass Feedstock Particles Before and After Pyrolysis by Numerical Analysis of X-Ray Tomographic Reconstructions

Lignocellulosic biomass has a complex, species-specific microstructure that governs heat and mass transport during conversion processes. A quantitative understanding of the evolution of pore size and structure is critical to optimize conversion processes for biofuel and bio-based chemical production. Further, improving our understanding of the microstructure of biochar coproduct will accelerate development of its myriad applications. This work quantitatively compares the microstructural features and the anisotropic permeabilities of two woody feedstocks, red oak and Douglas fir, using X-ray computed tomography (XCT) before and after the feedstocks are subjected to pyrolysis. Quantitative analysis of the three-dimensional (3D) reconstructions allows for direct calculations of void fractions, pore size distributions and tortuosity factors. Next, 3D images are imported into an immersed boundary based finite volume solver to simulate gas flow through the porous structure and to directly calculate the principal permeabilities along longitudinal, radial, and tangential directions. The permeabilities of native biomass are seen to differ by three to four orders of magnitude in the different principal directions, but we find that this anisotropy is substantially reduced in the biochar formed during pyrolysis. The quantitative transport properties reported here enhance the ability of pyrolysis simulations to account for feedstock-specific effects and thereby provide a useful touchstone for the biorefining community.

09 BIOMASS FUELS↗

DOE OSTI2020

Strain rate sensitivity, microstructure variations, and stress-assisted β → α" phase transformation investigation on the mechanical behavior of dual-phase titanium alloys

In this study, the microstructures of three widely used dual-phase titanium alloys: Ti-6Al-4V, Ti-6Al-2Sn-4Zr-2Mo, and Ti-6Al-2Sn-4Zr-6Mo are characterized using backscatter electron imaging and the deformation behaviors in their individual α and β phases are investigated using in situ high-energy X-ray diffraction during uniaxial tension experiments. This is accompanied by calculation of the strain rate sensitivity (SRS) in these alloys, as a function of applied loading. The results of the calculated SRS and the mechanical response (in terms of lattice strains and hardening behaviors) are rationalized based on the local microstructure, composition, and texture of the alloy. A stress-induced β (BCC) to α" (orthorhombic) phase transformation is observed during the in-situ diffraction experiment, which permitted analysis of the lattice strain evolution during the phase transformation. Results from this study provide insights into the relationship between microstructure, composition, applied loading, and the deformation behavior, including effects on loading with time holds. Specifically, the results show that the microstructure, and not necessarily the chemical composition (Mo content), along with the applied loading have a dominant role in the observed SRS variation in titanium alloys. Further, the evolution of the α" (orthorhombic) phase is observed for the first time during deformation of an industrially relevant titanium alloy, Ti-6246.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Coupled phase field damage and crystal plasticity analysis of intragranular fracture: The role of crystallographic orientation and voids

Damage evolution in engineering metal alloys at the grain scale exhibits significant microstructural heterogeneity and anisotropy. These heterogeneities create local hotspots for stress and strain localization, leading to void nucleation. Crystal orientation influences the active slip systems around voids, affecting lattice rotation and potentially forming discontinuities. At low triaxiality, voids may change shape due to lower stress, rotation, elongation, and coalescence. At high triaxiality, the correlation between crystal orientation and void growth rate becomes stronger, resembling the behavior observed in isolated single crystals. Therefore, understanding the effects of crystal orientation, heterogeneous strain, and defect evolution is crucial for single crystal fracture characterization. Here, in this work, a coupled phase-field damage (PFD) and crystal plasticity (CP) model is implemented within a finite element framework to analyze crystal deformation and failure. The CP method employs a dislocation density-based constitutive model, while intragranular failure is modeled using an anisotropic PFD method. The PFD model considers both the stored energy due to elastic stretching and the energy release due to defect formation and crack formation. A single crystal Al2219 with an intracrystalline spherical void is chosen to analyze fracture. The study finds that fracture propagation is strongly correlated with crystal orientations. This coupled CP-PFD model provides accurate failure prediction in crystalline materials by incorporating the effects of crystal orientations and existing voids. This study demonstrates how the local microstructure and defects influence plastic deformation and failure mechanisms in metal alloys.

Aluminum alloy↗

DOE OSTI2022

The complex structural and chemical nature of monolithic U-10Mo fuel and Zr barrier layer

Nanoscale microstructural characterization by advanced transmission electron microscopy techniques on a U-10Mo/Zr barrier layer monolithic fuel plate was performed to evaluate the microstructural evaluation after high burn-up. Gas bubble superlattice evolution, grain restructuring, and evolution of the Zr interaction layer is investigated through detailed electron microscopy characterization. The use of automated crystallographic orientation mapping to irradiated U-10Mo fuel highlights that the restructured ultra-fine grains are separated by high angle grain boundaries at a burn up of 4.42 × 10 21 fissions/cm 3 . Additionally, advanced chemical analysis and multi-variable statistical analysis shows spatial clustering of solid fission product precipitates. Finally, characterization of a newly observed porous nanocrystalline Zr region in the barrier layer is studied. Finally, this work provides insights into the grain subdivision and restructuring process while using advanced microscopy techniques to analyze fission products in neutron-irradiated U-10Mo fuel.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Direct observation of dislocation structure evolution in SRF cavity niobium using electron channeling contrast imaging

Two major goals of superconducting radio frequency cavity research and development are achieving higher accelerating gradient and gaining the highest quality factor, a measure of efficiency. However, the consistent improvement of these performance metrics is restricted by many factors, one of which is microstructural defects, such as dislocation substructures within the material. In this work, dislocation evolution is compared in four samples extracted from a 2.8 mm thick large-grain niobium slice, with tensile axes chosen to generate specific dislocation structures during subsequent deformation. The four samples are (1) as-extracted, (2) extracted and annealed, (3) extracted and then deformed to 40% tensile strain, and (4) extracted, annealed at 800 °C 2 h, and then deformed to 40% strain. Electron channeling contrast imaging was performed on all samples to characterize initial dislocation density and dislocation structure evolution due to annealing and deformation, and related to the mechanical behavior observed in stress-strain curves. A fundamental understanding of dislocation evolution in niobium is necessary to develop computational models to simulate cavity forming, which could enable new processing methods for cavity fabrication to be identified that could lead to improved performance.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2022

Phase evolution of U-Zr system in a thermal cycling neutron diffraction experiment: as-cast U-35Zr and U-50Zr

Here, phase evolution of as-cast U-35 wt% Zr and U-50 wt% Zr alloys during thermal cycling (303–1073 K) was investigated using in-situ neutron diffraction. Analysis was performed using Rietveld crystal and microstructure refinements from time-of-flight neutron diffraction data, with a focus on evolution of lattice parameter, atom ordering, unit cell volume, and weight fractions during the thermal cycling. Disordered δ-UZr 2 and residual γ-(U,Zr) phase are retained in the field of δ of the U-Zr equilibrium phase diagram for the U-50Zr sample, and in the field between δ and α-U for the U-35Zr sample. The α phase that is present in the reported phase diagrams of U-Zr was not observed in the diffraction patterns. The evolutions of lattice parameter and unit cell volume of δ and γ are affected by both thermal expansion and chemistry.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Performance and properties evolution of near-term accident tolerant fuel: Cr-doped UO 2

Chromium-doped UO 2 fuel has received significant interest due to the ability for chromium to produce pellets with large average grain size (>30 μm), which has shown to increase fission gas retention during operation. Sintering of chromium-doped UO 2 pellets was pursued with oxygen potential and sintering atmosphere controlled to tailor the final microstructure of the material. Chromium additions in this study ranged from 750 to 7800 ppm. Cr concentrations were studied pre and post sintering using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). Effects of chromium content on lattice parameter and microstructure were examined with X-ray diffraction (XRD) and scanning electron microscopy (SEM). Contraction of the UO 2 lattice parameter was observed, as well as enlargement of grain size with increasing chromium content up to 4900 ppm Cr 2 O 3 . In addition, SEM indicated Cr incorporation within the matrix and the formation of chromium oxide precipitates throughout the microstructure at high Cr concentrations. Evaluation of thermophysical properties of Cr-doped UO 2 pellets were conducted up to 1200 °C to illustrate their evolution with increased dopant concentration and microstructural changes. The results show that grain size is maximized at 52 μm with Cr 2 O 3 concentration equal to 4900 ppm; however, grain size decreases at higher Cr 2 O 3 concentrations. No significant changes were observed in specific heat capacity, linear thermal expansion, and coefficient of thermal expansion compared to undoped UO 2 . The thermal conductivity also decreased through the incorporation of Cr 2 O 3 dopants above 750 ppm and is shown to be ~15 % lower than reported UO 2 values.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2019

Microstructure Development of 308L Stainless Steel During Additive Manufacturing

$In$ $situ$ high-energy X-ray diffraction measurements were completed during deposition of 308L stainless steel wire onto a 304L stainless steel substrate. Attempts were made to extract microstructural features such as phase fraction and internal stress, as well as temperature evolution immediately following the deposition. The limited data that could be collected during deposition and rapid solidification are critically examined. High-energy X-rays coupled with relatively slow detectors were utilized to enable determination of orientation-dependent lattice parameters accurately enough to comment on phase strain evolution between austenite and ferrite. Here, information about the hydrostatic and deviatoric stress states of the constituent phases was determined on time scales that are relevant to their development. However, the time resolution of the technique was insufficient to monitor phase evolution during the solid–solid phase transformation and, more so, during solidification. Moreover, the accurate and absolute determination of inherently statistical parameters, such as phase fraction, depends critically on the ability to sample a statistically significant numbers of grains in the microstructure.

36 MATERIALS SCIENCE↗

DOE OSTI2023

In-Situ Transmission Electron Microscopy Study of the Evolution of Extended Defects in Oxide Nuclear Fuels

In-situ transmission electron microscopy (TEM) with simulated extreme environments is an effective tool for understanding and tracking microstructural changes down to the atomic scale. The objective of this research is to study the effect of temperature on the evolution of extended defects in ThO2 and UO2. Here, we present in-situ TEM isochronal thermal annealing experiments using a micro-electro-mechanical-system (MEMS)-based heating holder. ThO2 and UO2 single crystal specimens were grown inside an inert silver ampoule using hydrothermal synthesis. Both samples were irradiated using 2 MeV protons at 600oC up to 0.1 dpa at Texas A&M University’s Accelerator Laboratory. Fig. 1a shows a weak-beam dark field TEM image of ThO2 after irradiation, indicating the presence of faulted 1/3 <111> type dislocation loops. This presentation will discuss the effect of annealing temperature (600oC, 800oC, 1000oC, 1100oC, etc.) on dislocation loop density, size and distribution, loop nature (interstitial/vacancies) and Burgers vector, as well as the formation of voids in both ThO2 and UO2. This work will also discuss the interaction between defects during annealing. The in-situ TEM annealing cycle is shown in Fig 1b. This research significantly improves the understanding of defect behavior in oxide nuclear fuels with temperature and will aid computational modeling efforts. This work was supported as part of the Center for Thermal Energy Transport under Irradiation (TETI) Energy Frontier Research Center, funded by the U.S. Department of Energy Office of Science.

36 MATERIALS SCIENCE↗

DOE OSTI2022

A Coupled Small and Wide-Angle X-Ray Scattering Study of Phase Transformation Mechanisms in U-6Wt Pct Nb

The elevated temperature phase transformation kinetics of U-6wt%Nb in both wrought and cast conditions were investigated using in-situ high energy synchrotron X-ray scattering. The evolution of the phase content, γ-phase composition, and microstructure morphology was determined through the analysis of simultaneously collected wide-angle diffraction and small-angle scattering (SAXS) data. The results of the wide-angle scattering analysis, especially the phase fractions and average composition of the γ-phase, provide model parameters to enable a quantitative analysis using the SAXS data. Greater clarity regarding the kinetics of different precipitation mechanisms, namely the continuous precipitation (CP) of α-U within the γ-phase matrix and the discontinuous (DP) grain boundary precipitation of a lamellar microstructure, consisting of α-U and Nb-rich γ-phase are obtained from the coupled measurement modes. These results indicate that the CP mechanism is responsible for the initial precipitation of α-U at all temperatures considered. Near the nose in the time-temperature-transformation (TTT) diagram at ~798 K, both mechanisms are active during the early stages of phase transformation. However, the DP mechanism has an increasingly long incubation period with decreasing temperature below the TTT nose. In conclusion, the average interlamellar spacing obtained from the SAXS analysis increases with time, providing further evidence of the so-called divergent DP behavior previously observed in U-6wt%Nb alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Understanding interfacial crystallization dynamics on carbon fiber reinforced polypropylene composite manufacturing

Reinforcing polymers with discontinuous fibers improves mechanical properties, such as strength and stiffness, and in some cases achieve isotropic properties, rendering them suitable for various engineering applications. Matrix materials are generally highly engineered thermosets (e.g. crosslinked epoxies), bonded to the fiber periphery by proprietary surface and sizing chemistries. Semicrystalline thermoplastic matrices are less utilized due to poor fiber-matrix bonding resulting in inefficient interfacial load-transfer in reinforced composites. However, flexibility with melt-processing or molding conditions can be leveraged to promote non-covalent interfacial bonding between matrix and fiber via crystallization of the matrix onto fiber surface. In the present study, we utilize a co-mingle chopped carbon and isotactic polypropylene fibers to form isotropic composites, tailoring interfacial immobilized matrix or interphase morphology to optimize performance through precise control of thermal processing/molding windows. Calorimetry and optical microscopy were employed to investigate the impact of carbon fiber at various volume fractions (10, 20, and 30 %) on isotactic polypropylene crystallization and mechanical performance. Variations in mechanical properties correspond to the structural evolution of the interfacial region and are correlated to underlying microstructural attributes using wide-angle X-ray scattering, thermal analysis, and low-field nuclear magnetic resonance spectroscopy. These results provide a practical framework for the manufacturing of thermoplastic matrix composites. In conclusion, the results presented provide a guide for the strategic optimization of interphase design, showcasing tailorable tensile strengths which outperform any isotactic polypropylene carbon fiber composites previously reported in literature.

36 MATERIALS SCIENCE↗