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Parameter, Post-Processing Sensitivities, and Qualification Approach of Laser Powder Bed Fusion Hydrogen Resistant Alloy NASA HR-1

Metal additive manufacturing (AM) processes are being used to enable economical manufacturing of legacy alloys as well as advancing new alloys. Laser powder bed fusion (L-PBF) is a metal AM process that has high maturity and being used to produce a variety of parts for space applications including complex propulsion components. The National Aeronautics and Space Administration (NASA) has identified the need to develop and advance new materials in unique space applications such as high-pressure hydrogen environments. NASA HR-1 is a high strength Fe-Ni based superalloy designed to resist high pressure hydrogen environment embrittlement (HEE), oxidation, and corrosion that has been successfully adapted to laser powder directed energy deposition (LP-DED). Insights gained from the NASA HR-1 development for LP-DED have guided the development process for L-PBF. However, adapting NASA HR-1 to L-PBF posed new challenges due to the distinct differences between the additive manufacturing processes. During parameter development, sensitivities were observed in post-processing that necessitated additional optimization of heat treatments. Additionally, the variations in thickness and how it influenced the microstructural response during heat treatment was characterized. Understanding these sensitivities is important to qualification of the material in a L-PBF machine. This ensures that the microstructures and properties of the material maintain consistency in production. This presentation will cover parameter development along with post-processing challenges and solutions will be discussed in addition to key material properties as it pertains to application performance and qualification per NASA-STD-6030. Improvements made by developing a derivative alloy, NASA HR-2, will be highlighted through preliminary small scale parameter development, material characterization, and initial property testing.

NASA HR-1↗
DOE OSTI2020

A FEASIBILITY STUDY ON CRACK REPAIR IN AUSTENITIC STAINLESS STEEL DRY STORAGE CANISTERS USING ISOTHERMAL FRICTION STIR WELDING

In recent time, solid state crack repair techniques in spent nuclear fuel dry storage canisters (SNF-DSC) have garnered significant interest. Plates of austenitic stainless steels are usually arc welded to fabricate the cylindrical canisters which are prone to chloride-induced stress corrosion cracking. Friction stir welding (FSW) is considered to be a potential candidate for damage repair. In this work, electrical discharge machining was used to simulate cracks in 304L stainless steel plates of 12.7 mm thickness. Subsequently, isothermal FSW was carried out at two different temperatures (725 and 825°C) in order to repair the simulated crack. Microstructure-mechanical property correlations in FSWed plates were studied in detail. Significant grain refinement observed in the stir zone (SZ) was attributed to dynamic recrystallization occurring during FSW. A comparison of Vickers microhardness showed higher hardness and homogeneity in the 725°C SZ than its 825°C counterpart. The fraction of S3 boundary is found to be low in the SZ as compared to base metal (BM). Yield strength of the joints was found to be approximately 100 MPa higher than that of the BM accompanied by a drop in ductility by a factor of 2. Residual stress profile across 825°C weld was measured using x-ray diffraction.

Bhattacharyya, Madhumanti↗
DOE OSTI2022

Creep behavior of $\gamma$-TiAl fabricated via electron beam additive manufacturing

$\gamma$-TiAl is a desirable structural engineering alloy with excellent high temperature specific strength. This material system has been shown to be processable at industrial scales via additive manufacturing. In this work we investigate the microstructure and properties of Ti48Al2Cr2Nb fabricated via electron beam melting. No significant anisotropy was observed from during creep testing under the considered conditions. Creep deformation resistance and rupture strength are comparable to material synthesized via traditional routes.

Fernandez-Zelaia, Patxi↗
DOE OSTI2023

Fundamental Superconductivity of Nb films for Quantum Computing Application

Niobium is a widely accepted material for quantum computing device as well as superconducting radio frequency (SRF) technology. Superconducting niobium is a marginal type II superconductor which has a very narrow gap (~20-30 mT) of the mixed state at 2K, even showing the intermediate state (IMS) at the early stage of magnetic vortex penetration. Tremendous progress has been made in understanding the impact of the Nb surface and bulk superconductivities on SRF resonator performance. However, the effect of thin superconducting Nb films for quantum computing applications requires further examination. In this study, we explore the fundamental superconducting properties of various thin Nb films and compare them with respect to the energy relaxation time, T1, measured from superconducting qubit fabricated with these films. The Nb films are fabricated both with or without a surface protective layer that prevents the formation of lossy Nb2O5. Electromagnetic properties are characterized by means of bulk magnetization, electromagnetic transport, and dynamics of surface superconductivity. In addition, analytical electron microscopy is implemented to further connect the superconducting properties to microstructure.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Mechanical Properties and Strain-Induced Martensite Transformation in Cold Rolling of 304L Stainless Steel Plate

In this work, cold rolling behavior of stainless steel 304L is investigated and the effects of different process parameters on the occurrence of strain-induced martensite and mechanical properties are studied. The rolling experiments are conducted under different rolling speeds and reductions in which a set of samples is deformed at room temperature and the other set is first cooled to the temperature of − 10 °C and then rolled. Afterward, the developed microstructures and mechanical properties of the rolled steel are evaluated employing different testing techniques. In order to justify the results, mathematical modeling of cold rolling operation is also performed using Abaqus/Explicit to estimate the distribution of equivalent plastic strain and temperature rise during rolling. The results show that strain-induced martensite may occur during cold rolling and it efficiently alters microstructure and mechanical performance of the rolled plate. The amount of reduction, initial temperature, rolling layout, and, to a lesser extent, rolling speed can affect the kinetics of martensite transformation as well as microstructure and mechanical properties of the rolled steel.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Fracture Toughness and Fatigue Crack Growth Rate Testing of Baffle-Former Bolts Harvested from a Westinghouse Two-Loop Downflow Type PWR

As one of the pressurized water reactor (PWR) internal components, baffle-former bolts (BFBs) are subjected to significant mechanical stress and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and reduced load-carrying capacity of the bolts. In support of evaluating long-term operational performance of materials used in core internal components, the Oak Ridge National Laboratory (ORNL), through the Department of Energy (DOE), Light Water Reactor Sustainability (LWRS) Program, Materials Research Pathway (MRP) has harvested two high fluence BFBs from a commercial Westinghouse two-loop downflow type PWR. The two bolts of interest, i.e. bolts # 4412 and 4416, were withdrawn from service in 2011 as part of a preventative replacement plan. No identification of cracking or potential damage was found for these bolts during their removal in 2011. However, the bolts required a lower torque for removal from the baffle structure than the original torque specified during installation. Irradiation displacement damage levels in the bolts range from 15 to 41 displacements per atom. The goal of this project is to perform detailed microstructural and mechanical property characterization of BFBs following in-service exposures. The information from these bolts will be integral to the LWRS program initiatives in evaluating end of life microstructure and properties. Furthermore, valuable data will be obtained that can be incorporated into model predictions of long-term irradiation behavior and compared to results obtained in high flux experimental reactor conditions.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2023

Microstructural Characterizations of Two High Fluence Baffle-Former Bolts Retrieved from a Westinghouse Two-loop Downflow Type PWR

As one of the pressurized water reactor (PWR) internal components, baffle-former bolts (BFBs) are subjected to significant mechanical stress and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and reduced load-carrying capacity of the bolts. In support of evaluating long-term operational performance of materials used in core internal components, the Oak Ridge National Laboratory (ORNL), through the Department of Energy (DOE), Office of Nuclear Energy, Light Water Reactor Sustainability (LWRS) Program, Materials Research Pathway (MRP), has harvested two high fluence BFBs from a commercial Westinghouse two-loop downflow type PWR. The two bolts of interest, i.e. bolts # 4412 and 4416, were withdrawn from service in 2011 as part of a preventative replacement plan. No identification of cracking or potential damage was found for these bolts during their removal in 2011. However, the bolts required a lower torque for removal from the baffle structure than the original torque specified during installation. Irradiation damage levels in the bolts range from 15 to 41 displacements per atom. The goal of this project is to perform detailed microstructural and mechanical property characterization of BFBs following in-service exposures. The information from these bolts will be integral to the LWRS program initiatives in evaluating end of life microstructure and properties. Furthermore, valuable data will be obtained that can be incorporated into model predictions of long term irradiation behavior and compared to results obtained from experimental reactor conditions

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2024

ZnO-Au Hybrid Metamaterial Thin Films with Tunable Optical Properties

ZnO-Au nanocomposite thin films have been previously reported as hybrid metamaterials with unique optical properties such as plasmonic resonance properties and hyperbolic behaviors. In this study, Au composition in the ZnO-Au nanocomposites has been effectively tuned by target composition variation and thus resulted in microstructure and optical property tuning. Specifically, all the ZnO-Au nanocomposite thin films grown through the pulsed laser deposition (PLD) method show obvious vertically aligned nanocomposite (VAN) structure with the Au nanopillars embedded in the ZnO matrix. Moreover, the average diameter of Au nanopillars increases as Au concentration increases, which also leads to the redshifts in the surface plasmon resonance (SPR) wavelength and changes in the hyperbolic behaviors of the films. As a whole, this work discusses how strain-driven tuning of optical properties and microstructure resulted through a novel Au concentration variation approach which has not been previously attempted in the ZnO-Au thin film system. These highly ordered films present great promise in the areas of sensing, waveguides, and nanophotonics to name a few.

Bhatt, Nirali A.↗
DOE OSTI2018

A comprehensive investigation of the strengthening effects of dislocations, texture and low and high angle grain boundaries in ultrafine grained AA6063 aluminum alloy

Highlights: • Evolution of microstructure and mechanical properties of AA6063 after severe plastic deformation was investigated. • Average cell size shows a more solid relationship with mechanical properties rather than the average grain size. • This indicates that in addition to high angle boundaries, cell boundaries play a strengthening role. - Abstract: The effect of equal channel angular pressing (ECAP) on the microstructure and mechanical properties of AA6063 aluminum alloy was investigated. For this purpose, samples of AA6063 aluminum alloy were deformed up to 10 passes using ECAP and the evolution of microstructure, texture and dislocation density was investigated. It was found that the dislocation density increased and cells mostly surrounded by low angle boundaries (LABs) formed after 2 passes ECAP. Increasing the dislocation density continued with further processing and reached a maximum at the 4th ECAP pass. With further deformation to 6 passes, the dislocation density reduced, the fraction of high angle boundaries (HABs) increased and the averages of cell size and grain size reduced, significantly, which indicated the occurrence of grain refinement. However, a slight increase in dislocation density, average cell size (ACS) and average grain size (AGS), indicating coarsening, occurred when 10 passes of ECAP are imposed. Hardness, yield (YS) and ultimate tensile strength (UTS) increased continuously although the most significant enhancement occurred after 2 passes of ECAP. Investigating the correlation between the microstructure and mechanical properties indicated that Hall-Petch relationship was valid for ultrafine grained AA6063 before the coarsening started provided that the property of interest was correlated to average cell size but not the average grain size.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Development of a Novel Magnesium Alloy for Thixomolding® of Automotive Components (Final Report)

Magnesium (Mg) alloy die-castings are increasingly used in the automobile industry to achieve cost effective mass reduction, especially in systems where multiple components can be integrated into a single thin wall die-casting. However, there are several component quality restrictions in thin-walled Mg die castings, including variability in dimensional accuracy, part-to-part variation in mechanical properties, and porosity in the final part, which has limited the continued growth of die-cast components in the automobile industry. An alternative to die-casting is the process of thixomolding®. While the die-casting process relies on filling a mold at high speeds with the alloy in the completely molten state, the thixomolding® process fills a mold with a thixotropic alloy in a semi-solid slurry state at a temperature between the liquidus and solidus temperatures. Ideally, the material should be ~30–65% solid rather than being completely liquid at the beginning of the injection process. Advantages of the thixomolding® process include a finer grain structure, lower porosity, improved dimensional accuracy, improved part-to part consistency, improved mechanical properties, particularly ductility in the component, the ability to reduce wall thickness for mass savings, and longer tool life due to lower process temperatures. The objective of this collaborative project between Oak Ridge National Laboratory, FCA US LLC, and Leggera Technologies was to develop one or more novel Mg alloys more suitable for thixomolding® automotive structural components than the current die-casting alloys used for this process. The primary interest was to improve ductility while maintaining tensile and fatigue strengths, as these are properties that are critical for use in body and chassis structural applications. Since good corrosion resistance is also desirable for this application, this property was also considered when evaluating promising alloy compositions. An initial evaluation of existing components thixomolded® using AM60 was performed and microstructure, and tensile properties were evaluated for the baseline alloy. Targets were established for ease of processing (characterized by the melting range defined as the difference between the liquidus and the solidus), strength, and ductility. Computational modeling was used to identify promising alloys and selected alloys were cast in laboratory scale heats. Properties measured from laboratory scale heats were used to down-select two alloys for further evaluation and component fabrication. Two alloys were prepared in industrial scale heats, cut into small pieces (chips), and thixomolding® trials were initiated. Trial components were successfully fabricated using one alloy composition, but it was concluded that further refinement of the thixomolding® process parameters are required to successfully fabricate component using second alloy. Microstructure and mechanical properties were evaluated on the material removed from the fabricated component and properties were compared to the baseline alloy. Although mechanical properties of the alloys showed improvement over the baseline alloy, it was determined that modifications to the thixomolding® process would result in better microstructure control with further improvement in properties leading to successful commercialization. A provisional patent application has already been filed on the new alloys developed as part of the project.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Properties of Rolled AZ31 Magnesium Alloy Sheet Fabricated by Continuous Variable Cross-Section Direct Extrusion

Rolling is currently a widely used method for manufacturing and processing high-performance magnesium alloy sheets and has received widespread attention in recent years. Here, we combined continuous variable cross-section direct extrusion (CVCDE) and rolling processes. The microstructure and mechanical properties of the resulting sheets rolled at different temperatures from CVCDE extrudate were investigated by optical microscopy, scanning electron microscope, transmission electron microscopy and electron backscatter diffraction. The results showed that a fine-grained microstructure was present with an average grain size of 3.62 μm in sheets rolled from CVCDE extrudate at 623 K. Dynamic recrystallization and a large strain were induced by the multi-pass rolling, which resulted in grain refinement. In the 573-673 K range, the yield strength, tensile strength and elongation initially increased and then declined as the CVCDE temperature increased. The above results provide an important scientific basis of processing, manufacturing and the active control on microstructure and property for high-performance magnesium alloy sheet.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Machine-learning-based, online estimation of ceramic’s microstructure upon the laser spot brightness during laser sintering

The ceramic microstructure strongly influences its properties. During manufacturing, the online monitoring of microstructure is critical to ensure the desired material properties. So far, the microstructure on the relevant scale is usually characterized offline using scanning electron microscopy (SEM), which is time and cost-consuming. In this work, we demonstrate a cost-effective, machine learning (ML)-based approach to simulate the SEM micrographs in real-time from the laser spot brightness. We experimentally observed a strong correlation between the laser spot brightness and the corresponding microstructure at the exact locations. The brightness values obtained from thermal emission images and the corresponding SEM micrographs were used in the training datasets. The ML algorithm was a style-based conditional generative adversarial network (CGAN). After training, the ML model could generate high-fidelity microstructure images within 0.1 seconds based on in-situ captured brightness at the laser sintering spot. We used the average grain sizes as the metric to evaluate the accuracy of the ML-predicted micrographs. Here, the ML-predicted microstructures were in good agreement, with less than 5% in difference from the real SEM images. In conclusion, we demonstrate the cost-effective, online microstructure estimation during laser sintering with a simple setup (a camera, a regular computer, and the ML model).

08 HYDROGEN↗
DOE OSTI2025

Evaluating the bond strength and fracture mechanisms of cold-sprayed zinc coating on AZ91 magnesium substrate via a combined experimental and computational approach

Magnesium (Mg) alloys are ideal candidates for automotive applications due to their high strength to weight ratio, castability, recyclability etc., however, they lack corrosion and oxidation resistance. Solid-state deposition techniques, such as cold spray, have been demonstrated to enhance their corrosion resistance as it relies on the severe plastic deformation of powder particles upon impact with the substrate to form a metallurgical bond with the substrate and within the coating. At cold sprayed interfaces, a heterogeneous microstructure is formed that includes some porosity, oxides and intermetallics which can significantly affect coating performance. Thus, establishing a direct correlation between the interface microstructure and its properties can aid in designing optimal cold spray parameters. In this study, we investigated the microstructure and mechanical properties of a zinc (Zn) coating deposited on a high pressure die cast (HPDC) AZ91 Mg substrate via high resolution scanning transmission electron microscopy, in situ micro-tensile testing, and finite element method (FEM) modeling. Micro-tensile pillars fabricated using the plasma focused ion beam (PFIB) successfully isolates the coating-substrate interface within the gauge length. The average bond strength of Zn-Mg interface was determined to be ∼140 MPa with failure occurring partially at the interface and mostly into the coatings. A detailed microstructural characterization revealed evidence of a strong metallurgical bonding at the Zn-Mg interface and formation of the C14 MgZn 2 laves phase interlayer resulting in a mixed mode of fracture during the micro-tensile experiments. FEM modeling reveals the stress distribution along the interfaces and suggests that a MgZn 2 layer thickness between 200–400 nm is optimum to increase the bond strength and minimize the triaxiality. Such a site-specific interfacial analysis with correlative computational modeling provides crucial insight into the overall performance of cold spray interfaces.

Bond strength↗
DOE OSTI2024

Comparison of hardening and microstructures of ferritic/martensitic steels irradiated with fast neutrons and dual ions

Ferritic/martensitic steels T91 and HT9 were irradiated with neutrons (BOR-60 reactor) and dual ions (9 MeV Fe 3+ and 3.42 MeV energy degraded He 2+ ) from 369 to 520 °C and damage levels of 16.6 to 72 dpa to quantify the possibility of using ion irradiation to simulate neutron irradiation in terms of microstructures and mechanical properties. Nanoindentation testing was performed to obtain the bulk equivalent hardness of the dual-ion irradiated samples. For the neutron irradiated samples, both nanoindentation and Vickers hardness testing were conducted. Transmission Electron Microscopy (TEM) characterizations of the cavities, dislocation loops and precipitates were conducted to account for the strengthening contribution of each microstructure element. The good agreement between the microstructure-predicted (dispersed barrier hardening) and measured strength of the irradiated specimens demonstrated the accuracy of the strengthening model and the nanoindentation tests. Furthermore, the comparison of mechanical property and microstructure changes in ion and neutron irradiated structural materials indicated that ion irradiation replicated many neutron irradiation features. However, a single 70 °C temperature shift is insufficient to match all complex microstructures of neutron vs. ion irradiation over the irradiation temperature range of 369–520 °C.

36 MATERIALS SCIENCE↗
NASA NTRS2015

Material Characterization of Additively Manufactured Components for Rocket Propulsion

To advance Additive Manufacturing (AM) technologies for production of rocket propulsion components the NASA Glenn Research Center (GRC) is applying state of the art characterization techniques to interrogate microstructure and mechanical properties of AM materials and components at various steps in their processing. The materials being investigated for upper stage rocket engines include titanium, copper, and nickel alloys. Additive manufacturing processes include laser powder bed, electron beam powder bed, and electron beam wire fed processes. Various post build thermal treatments, including Hot Isostatic Pressure (HIP), have been studied to understand their influence on microstructure, mechanical properties, and build density. Micro-computed tomography, electron microscopy, and mechanical testing in relevant temperature environments has been performed to develop relationships between build quality, microstructure, and mechanical performance at temperature. A summary of GRCs Additive Manufacturing roles and experimental findings will be presented.

Additive Manufacturing↗
NASA NTRS2015

Materials Characterization of Additively Manufactured Components for Rocket Propulsion

To advance Additive Manufacturing (AM) technologies for production of rocket propulsion components the NASA Glenn Research Center (GRC) is applying state of the art characterization techniques to interrogate microstructure and mechanical properties of AM materials and components at various steps in their processing. The materials being investigated for upper stage rocket engines include titanium, copper, and nickel alloys. Additive manufacturing processes include laser powder bed, electron beam powder bed, and electron beam wire fed processes. Various post build thermal treatments, including Hot Isostatic Pressure (HIP), have been studied to understand their influence on microstructure, mechanical properties, and build density. Micro-computed tomography, electron microscopy, and mechanical testing in relevant temperature environments has been performed to develop relationships between build quality, microstructure, and mechanical performance at temperature. A summary of GRC's Additive Manufacturing roles and experimental findings will be presented.

Additive Manufacturing↗
DOE OSTI2017

Elaborating the phases and mechanical properties of multiphase alloy: Experimental two-dimensional mapping combined with theoretical calculations

Highlights: • Mechanical modulus and hardness distribution mapping is obtained for the first time by NanoBlitz 3D. • Phases mapping and exact element ratio are characterized for the nano multielement carbides by EPMA. • Carbides types are confirmed by acid etching and XRD refinement. • Young's modulus of multiple carbides is verified by DFT calculations and Voigt-Reuss-Hill model. - Abstract: The relationship between types of phases, microstructure and mechanical properties is always a critical challenge for the research and application of multiphase alloys. We report for the first time that NanoBlitz 3D method implemented in iNano is used to investigate the distribution of micro mechanical modulus and hardness for the entire complex multiphase alloy Fe-6.0W-5.0Mo-4.0Cr-2.0V-0.83C by constructing the two-dimensional mapping. In order to build the correlation between the microstructure and properties, the carbides in this tempering state steel are confirmed to be Fe{sub 3}(W, Mo){sub 3}C, Cr{sub 15.58}Fe{sub 7.42}C{sub 6} and V{sub 8}C{sub 7} by acid etching and XRD refinement. The phases mapping is obtained by electron probe micro-analysis. Exact element ratio is characterized for the nano-scale multielement carbides precipitates. The Young's modulus and hardness of the precipitated carbides are up to 330 GPa and 22 GPa, respectively. The distribution range of Young's modulus and hardness is during 150 to 250 GPa and 2.5 to 7.0 GPa for the matrix phases, respectively. The experimental Young's modulus and hardness results are verified by first-principles calculations combined with Voigt-Reuss-Hill approximation. In fact, this work provides a successful demonstration to three-dimensionally characterize the micro mechanical properties for all the ceramics and alloys.

36 MATERIALS SCIENCE↗