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3D Tunable, Multiscale, and Multistable Vibrational Micro-Platforms Assembled by Compressive Buckling

Microelectromechanical systems remain an area of significant interest in fundamental and applied research due to their wide ranging applications. Most device designs, however, are largely 2D and constrained to only a few simple geometries. Achieving tunable resonant frequencies or broad operational bandwidths requires complex components and/or fabrication processes. The work presented here reports unusual classes of 3D micromechanical systems in the form of vibratory platforms assembled by controlled compressive buckling. Such 3D structures can be fabricated across a broad range of length scales and from various materials, including soft polymers, monocrystalline silicon, and their composites, resulting in a wide scope of achievable resonant frequencies and mechanical behaviors. Platforms designed with multistable mechanical responses and vibrationally decoupled constituent elements offer improved bandwidth and frequency tunability. Furthermore, the resonant frequencies can be controlled through deformations of an underlying elastomeric substrate. Systematic experimental and computational studies include structures with diverse geometries, ranging from tables, cages, rings, ring-crosses, ring-disks, two-floor ribbons, flowers, umbrellas, triple-cantilever platforms, and asymmetric circular helices, to multilayer constructions. These concepts form the foundations for engineering designs that complement those supported by conventional, micro-electromechanical systems, with capabilities that could be useful in systems for biosensing, energy harvesting, and others.

36 MATERIALS SCIENCE↗

An innovative and alternative approach toward gear fabrication

In this paper, we present the first demonstration of single-step gear manufacturing via an innovative in-situ friction stir forging approach. This novel process is a natural extension to the friction stir processing technique and relies on shear and normal stresses to form the complex shapes. Friction stir welding pin tool with shoulder is plunged at high revolutions per minute (rpm) into the sample to heat it to the desired temperature and enable plastic flow. Then, the tool is forged at high plunge rate to form the desired structurally-sound and defect free complex shapes. To better visualize the process the experiments are complemented by a 3D thermomechanically coupled, smoothed particle hydrodynamics (SPH) model to understand the material flow pattern both radially and through thickness in the gear teeth, plastic strain distribution, and temperature profile. We have demonstrated application of I-FSF to inherently poor formable AZ31 Mg, AA 7075-T6, and AA5083–10 vol% TiB 2 composite and fabricated 14-tooth spur gears from these materials with minimal farther machining. In conclusion, microstructure of the forged gears exhibited a directional material flow pattern due to the normal forging action and refinement of grains to 6–13 μm through dynamically recrystallization across the radial, through-thickness direction, which is in good agreement with the corresponding SPH simulation results.

42 ENGINEERING↗

Survey of Modeling and Simulation Techniques for Advanced Manufacturing Technologies Volume I – Predicting Initial Microstructures

This report summarizes the current state of modeling and simulation methods for predicting the initial structure and properties of material in components assembled using advanced manufacturing technologies (AMTs). The report is the first volume in a two-volume series. This first volume focuses on predicting initial microstructures of AM material. The second volume discusses predicting material properties given the initial microstructure. The focus is on technologies of particular relevance to the design and manufacture of nuclear reactor components. The purpose of the report is to help develop the technical knowledge base to support regulatory decisions that will be needed to assess nuclear components manufactured with AMTs as these components are installed at nuclear power plants (NPPs). The report develops a list of AMTs of particular interest to the NRC and summarizes the key microstructural features and corresponding processing parameters relevant to each technology. Further sections describe available physically-based and data-driven prediction methods and survey widely available software tools. The report concludes with a summary of gaps that may be of particular interest to the NRC when evaluating modeling and simulation methods for AMTs.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Microstructural Underpinnings of Giant Intrinsic Exchange Bias in Epitaxial NiCo 2 O 4 Thin Films

Understanding intrinsic exchange bias in nominally single-component ferromagnetic or ferrimagnetic materials is crucial for simplifying related device architectures. However, the mechanisms behind this phenomenon and its tunability remain elusive, which hinders the efforts to achieve unidirectional magnetization for widespread applications. Inspired by the high tunability of ferrimagnetic inverse spinel NiCo 2 O 4 , the origin of intrinsic exchange bias in NiCo 2 O 4 (111) films deposited on Al 2 O 3 (0001) substrates are investigated. The comprehensive characterizations, including electron diffraction, X-ray reflectometry and spectroscopy, and polarized neutron reflectometry, reveal that intrinsic exchange bias in NiCo 2 O 4 (111)/Al 2 O 3 (0001) arises from a reconstructed antiferromagnetic rock-salt Ni x Co 1-x O layer at the interface between the film and the substrate due to a significant structural mismatch. Remarkably, by engineering the interfacial structure under optimal growth conditions, it can achieve exchange bias larger than coercivity, leading to unidirectional magnetization. Such giant intrinsic exchange bias can be utilized for realistic device applications. This work establishes a new material platform based on NiCo 2 O 4 , an emergent spintronics material, to study tunable interfacial magnetic and spintronic properties.

36 MATERIALS SCIENCE↗

Developing a novel hierarchical approach for multiscale structural reliability predictions for ultra-high consequence applications

Microstructural variabilities are among the predominant sources of uncertainty in structural performance and reliability. We seek to develop efficient algorithms for multiscale calcu- lations for polycrystalline alloys such as aluminum alloy 6061-T6 in environments where ductile fracture is the dominant failure mode. Our approach employs concurrent multiscale methods, but does not focus on their development. They are a necessary but not sufficient ingredient to multiscale reliability predictions. We have focused on how to efficiently use concurrent models for forward propagation because practical applications cannot include fine-scale details throughout the problem domain due to exorbitant computational demand. Our approach begins with a low-fidelity prediction at the engineering scale that is sub- sequently refined with multiscale simulation. The results presented in this report focus on plasticity and damage at the meso-scale, efforts to expedite Monte Carlo simulation with mi- crostructural considerations, modeling aspects regarding geometric representation of grains and second-phase particles, and contrasting algorithms for scale coupling.

36 MATERIALS SCIENCE↗

Robust Joining and Assembly Technologies for Ceramic Matrix Composites: Technical Challenges and Opportunities

Fiber reinforced ceramic matrix composites are under active consideration for use in a wide variety of high temperature applications within the aeronautics, energy, process, and nuclear industries. The engineering designs require fabrication and manufacturing of complex shaped parts. In many instances, it is more economical to build up complex shapes by Joining simple geometrical shapes. Thus, joining and attachment have been recognized as enabling technologies for successful utilization of ceramic components in various demanding applications. In this presentation, various challenges and opportunities in design, fabrication, and testing of high temperature joints in ceramic matrix composites will be presented. Various joint design philosophies and design issues in joining of composites will be discussed along with an affordable, robust ceramic joining technology (ARCJoinT). A wide variety of ceramic composites, in different shapes and sizes, have been joined using this technology. Microstructure and mechanical properties of joints will be reported. Current status of various ceramic joining technologies and future prospects for their applications will also be discussed.

Mrityunjay, Singh↗

Advancement of Novel Additively Manufactured Alloys for Space Applications

NASA has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. Several efforts have focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into development and flight applications. While many common aerospace alloys have been and continue to be a focus of ongoing development, the need for custom-alloy developments for high performance applications enabled by AM processes has been realized. The applications being targeted are liquid rocket engines with high heat fluxes, high pressure, and that utilize propellants such as hydrogen, which can degrade the alloy. NASA has recently focused on the development and advancement of novel alloy advancement using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, and JBK-75. These alloys have been evaluated using the laser powder bed fusion (L-PBF) and laser powder directed energy deposition (LP-DED) processes. The results from these processes have demonstrated that AM can enable rapid development of new alloy systems that can yield higher performances. These alloys have undergone the fundamental metallurgical evaluations, heat treatment study, and microstructure characterization and mechanical testing campaign. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL). This presentation will provide a background and overview of these AM-enabled novel alloys, AM processing development including metallurgical and mechanical property studies. It will also cover the latest advancement in the parallel component development and testing and future developments. The goal of these alloy development is to allow for technology infusion into NASA and commercial spaceflight missions as well as to establish and sustain the needed commercial AM supply chain.

Additive Manufacturing↗

Capturing, Analyzing, Maintaining, and Disseminating Shape Memory Material Data Between Information Management Systems

With an increased demand on reducing the time, cost, and effort to develop new materials, Integrated Computational Materials Engineering (ICME) has received widespread attention in various engineering disciplines as a catalyst for significantly reducing experimental testing during the material design process. An ICME approach to design can enable ‘fit-for-purpose’ materials to be realized in engineering applications by incorporating well-understood process-property-performance relationships between the various length and time scales in a material’s structure, enabling material optimization. However, such an approach requires validated multiscale models at the various length scales for a material, which in turn requires a large amount of data, a robust means of storing the data, and the ability to link data to developed material models. The NASA Vision 2040 [1] has identified nine key elements to enabling ICME approaches in system level design, with one being “Data, Information, and Visualization”, thus outlining the importance of a robust information management system for ICME. As the relationship between microstructure, properties, and material performance become better understood and incorporated into multiscale models that can be leveraged in application design, the emergence of new materials with application-driven properties can be realized. One such new material class that has seen growing attention are shape memory materials (SMM), in which a material can transition between a deformed and undeformed state via a reversible phase transformation when subject to a thermal, mechanical, or magnetic load [2]. SMMs have been used widely in aerospace and biomedical industries, including applications such as actuators, low-shock mechanisms, medical staples, braces, and stents [3, 4]. These materials exhibit unique behavior due to their ability to transition between phases, and thus the mechanisms that enable this transition must be captured in a data information management system and incorporated into SMM material models. At NASA Glenn Research Center, the Shape Memory Materials Database (SMMD) Tool has been developed to capture the necessary information that governs SMM material behavior and provide users the ability to select and visualize various SMMs for a specific application [5]. The database contains point-wise data for published SMM materials, along with the pedigree metadata for traceability necessary for a robust information management system. The database is also capable of storing in-house test data performed at NASA GRC by interacting with the developed Shape Memory Alloy (SMA) Analytics tool to extract the necessary point-wise values and populate the database. Although the SMMD Tool offers its users a single, authoritative source for SMM material data that is critical for model development and material design, the full material pedigree of the in-house test data for SMMs is not currently captured and is out of the scope for the SMMD tool. In this work, the schema for capturing SMM test data within the larger NASA GRC ICME Schema [6, 7, 8, 9] will be developed and implemented for thermomechanical tests conducted at NASA GRC. The developed schema will not only store the relevant data needed for the SMMD tool, but also the material pedigree (i.e., production of the bulk material, bulk material analysis, sample cut-out diagrams, sample fabrication procedure, etc.), test pedigree (i.e., test equipment used, measurement systems used, raw test data), and analysis pedigree (i.e., how the data in the SMMD tool is calculated). Furthermore, a Python-based framework will be developed to seamlessly interact between the SMA Analytics and SMMD tools, which will write the full dataset and associated metadata to the GRC Information Management System before passing the required point-wise data to the SMMD tool. Data informatics is a key element of the NASA Vision 2040, which requires not only that data is stored and maintained throughout the material lifecycle, but that the data is also accessible and reusable such that material development efforts can be minimized. Therefore, for an ICME design approach to be realized, a centralized information management system that drives the ICME process must be able to communicate with other databases. The work that will be presented in this presentation will therefore not only demonstrate the ability of NASA GRC’s information management system to capture SMM data, but also its ability to interact with pre-existing tools specialized for such materials.

Data management↗

Creep-rupture behavior of 6 candidate stirling engine iron-base superalloys in high pressure hydrogen. Volume 1: Air creep-rupture behavior

Four wrought alloys (A-286, IN 800H, N-155, and 19-9DL) and two cast alloys (CRM-6D and XF-818) were tested to determine their creep-rupture behavior. The wrought alloys were used in the form of sheets of 0.89 mm (0.035 in.) average thickness. The cast alloy specimens were investment cast and machined to 6.35 mm (0.250 in.) gage diameter. All specimens were tested to rupture in air at different times up to 3000 h over the temperature range of 650 C to 925 C (1200 F to 1700 F). Rupture life, minimum creep rate, and time to 1% creep strain were statistically analyzed as a function of stress at different temperatures. Temperature-compensated analysis was also performed to obtain the activation energies for rupture life, time to 1% creep strain, and the minimum creep rate. Microstructural and fracture analyses were also performed. Based on statistical analyses, estimates were made for stress levels at different temperatures to obtain 3500 h rupture life and time to 1% creep strain. Test results are to be compared with similar data being obtained for these alloys under 15 MPa (2175 psi) hydrogen.

Bhattacharyya, S.↗

Creep fatigue life prediction for engine hot section materials (isotropic)

This Final Report covers the activities completed under the optional program of the NASA HOST Contract, NAS3-23288. The initial effort of the optional program was report-in NASA CR189221, which consisted of high temperature strain controlled fatigue tests to study the effects of thermomechanical fatigue, multiaxial loading, reactive environments, and imposed stresses. The baseline alloy used in the tests included B1900+Hf (with or without coating) and wrought INCO 718. Tests conducted on B1900+Hf included environmental tests using various atmospheres (75 psig oxygen, purified argon, or block exposures) and specimen tests of wrought INCO 718 included tensile, creep, stress rupture, TMF, multiaxial, and mean stress tests. Results of these testings were used to calibrate a CDA model for INCO 718 alloy and to develop modifications or corrections to the CDA model to handle additional failure mechanisms. The Socie parameter was found to provide the best correlation for INCO multiaxial loading. Microstructural evaluations consisting of optical, Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM) techniques, and surface replication techniques to determine crack initiation lives provided data which were used to develop life prediction models.

Nelson, R. S.↗

A Review on Micro- and Nanoscratching/Tribology at High Temperatures: Instrumentation and Experimentation

High-temperature micro-/nanomechanics has attracted much interest over the last decade, primarily because of the urgent need to understand the mechanical and tribological properties of advanced engineering materials at micro-/nanoscale and the underlying physics controlling such properties at operationally relevant conditions. Recent years have subsequently witnessed the swift growth and development of new high-temperature micro- and nanoscratching/tribology instruments. Here, we present an overview of fundamental principles and developments in these instruments, discuss pertinent findings on the topic in detail, and outline current challenges and promising future directions in the field.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

A continuum framework for coupled solid deformation–fluid flow through anisotropic elastoplastic porous media

We present a continuum framework for coupled solid deformation–fluid flow in anisotropic elastoplastic porous media. A thermodynamic formulation of the coupled processes gives rise to an anisotropic Biot tensor that is a function of drained elastic tangent moduli tensor of the solid skeleton and the intrinsic bulk modulus of the solid constituent. Two effective stress measures emerge from the formulation, namely, σ', which is energy-conjugate to the elastic strain, and σ'', which is energy-conjugate to the plastic strain. For the special case of transverse isotropy that is commonly encountered in natural rocks, the Biot tensor can be expressed in terms of its normal and tangential components to the bedding plane, along with a microstructure tensor. Apart from its thermodynamic consistency, an advantage of this new formulation is that standard mixed finite element formulation can be employed to discretize the domain and solve initial boundary-value problems. We conduct plane strain simulations of coupled solid deformation–fluid flow in a transversely isotropic porous medium to demonstrate the impacts of material anisotropy, stress history, and the Biot tensor on the system response.

42 ENGINEERING↗

Linear complexions enable unprecedented ductility retention in neutron irradiated ferritic steel

Herein, the operando formation of Si-enriched linear complexions during neutron irradiation enables Grade 91 ferritic steel to overcome the strength–ductility tradeoff, one of the most critical life-limiting challenges facing nuclear structural alloys. Linear complexions are a distinct yet confined chemical and structural state at a dislocation, which are rarely reported in engineering alloys. Ferritic steels are amongst the most ubiquitous engineering alloys for current and future nuclear components, but they are susceptible to irradiation hardening and embrittlement. Here, exceptional ductility retention exceeding 90% of pre-irradiation levels is obtained in Grade 91 synthesized using powder metallurgy with hot isostatic pressing (PM-HIP). Powder processing artifacts promote a high density of screw dislocation arrays, on which β-FeSi 2 linear complexions form due to Si segregation during irradiation. Screw dislocation dipoles undergo pinning and unpinning on linear complexions, resulting in extended yielding and significant ductility retention post-irradiation. These findings represent a significant advancement toward design of alloys and manufacturing processes that can autonomously self-regulate their microstructural resilience in-operando during irradiation, enabling exceptional ductility rather than embrittlement.

Chatterjee, Arya [University of Illinois, Urbana, ↗

Microstructural Changes and Chemical Analysis of Fission Products in Irradiated Uranium-7 wt.% Molybdenum Metallic Fuel Using Atom Probe Tomography

Understanding the microstructural and phase changes occurring during irradiation and their impact on metallic fuel behavior is integral to research and development of nuclear fuel programs. This paper reports systematic analysis of as-fabricated and irradiated low-enriched U-Mo (uranium-molybdenum metal alloy) fuel using atom probe tomography (APT). This study is carried out on U-7 wt.% Mo fuel particles coated with a ZrN layer contained within an Al matrix during irradiation. The dispersion fuel plates from which the fuel samples were extracted are irradiated at Belgian Nuclear Research Centre (SCK CEN) with burn-up of 52% and 66% in the framework of the SELENIUM (Surface Engineering of Low ENrIched Uranium-Molybdenum) project. The APT studies on U-Mo particles from as-fabricated fuel plates enriched to 19.8% revealed predominantly γ-phase U-Mo, along with a network of the cell boundary decorated with α-U, γ’-U2Mo, and UC precipitates along the grain boundaries. The corresponding APT characterization of irradiated fuel samples showed formation of fission gas bubbles enriched with solid fission products. The intermediate burnup sample showed a uniform distribution of the typical bubble superlattice with a radius of 2 nm arranged in a regular lattice, while the high burnup sample showed a non-uniform distribution of bubbles in grain-refined regions. There was no evidence of remnant α-U, γ’-U2Mo, and UC phases in the irradiated U-7 wt.% Mo samples.

Bachhav, Mukesh↗

Metal Additive Manufacturing Developments for Propulsion Applications

NASA has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the 2000’s. Several efforts have focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into development and flight applications. While many common aerospace alloys have been and continue to be a focus of ongoing development, the need for custom-alloy developments for high performance applications enabled by various AM processes has been realized. The applications being targeted are liquid rocket engines with high heat fluxes, high pressure, and that utilize propellants such as hydrogen, which can degrade the alloy. NASA has recently focused on the development and advancement of novel alloy advancement using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, and JBK-75. These alloys have been evaluated using powder bed fusion (PBF), directed energy deposition (DED), and solid-state AM processes. The results from these processes have demonstrated that AM can enable rapid development of new alloy systems that can yield higher performances across various metal AM processes. These alloys have undergone the fundamental metallurgical evaluations, heat treatment study, and microstructure characterization and mechanical testing campaign. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL). This presentation will provide a background and overview of various AM-enabled novel alloys, a comparison across the AM processes, and development including metallurgical and mechanical property studies. It will also cover the latest advancement in the parallel component development and testing and future developments. The goal of these alloy development and use of various AM processes is to allow for technology infusion into NASA and commercial spaceflight missions as well as to establish and sustain the needed commercial AM supply chain.

Additive Manufacturing↗

Synthesis and Properties of Porous Ti-20 wt.% HA Nanocomposites

In the present study, porous titanium-20 wt.% hydroxyapatite nanocomposites were produced by the combination of mechanical alloying and powder metallurgical process with the addition of titanium hydride particles as the blowing agent. The powder mixture of Ti, HA and spacer particles were milled, pressed and heat-treated to decompose the hydride particles and to sinter into highly porous Ti-HA materials. The resulting microstructures were characterized using x-ray diffraction and scanning electron microscope with energy-dispersive spectrometry. The porosity, compressive strength and corrosion resistance of the porous nanocomposites were investigated. The results show that the compressive strength of porous Ti-HA can be tailored between 210 and 497 MPa by changing the content of blowing agent between 25 and 75%. The increase in the weight ratio of titanium hydride (from 25 to 75%) causes almost a twofold increase in the porosity and decreases the corrosion resistance (by almost two orders of magnitude). The present study has demonstrated that the porous Ti-HA nanocomposites are promising scaffold biomaterials for bone tissue engineering by virtue of their appropriate mechanical and corrosion properties and highly porous structure.

36 MATERIALS SCIENCE↗

Bio-inspired strategies for next-generation perovskite solar mobile power sources

Smart electronic devices are becoming ubiquitous due to many appealing attributes including portability, long operational time, rechargeability and compatibility with the user-desired form factor. Integration of mobile power sources (MPS) based on photovoltaic technologies with smart electronics will continue to drive improved sustainability and independence. With high efficiency, low cost, flexibility and lightweight features, halide perovskite photovoltaics have become promising candidates for MPS. Realization of these photovoltaic MPS (PV-MPS) with unconventionally extraordinary attributes requires new ‘out-of-box’ designs. Natural materials have provided promising designing solutions to engineer properties under a broad range of boundary conditions, ranging from molecules, proteins, cells, tissues, apparatus to systems in animals, plants, and humans optimized through billions of years of evolution. Applying bio-inspired strategies in PV-MPS could be biomolecular modification on crystallization at the atomic/meso-scale, bio-structural duplication at the device/system level and bio-mimicking at the functional level to render efficient charge delivery, energy transport/utilization, as well as stronger resistance against environmental stimuli (e.g., self-healing and self-cleaning). In this paper, we discuss the bio-inspired/-mimetic structures, experimental models, and working principles, with the goal of revealing physics and bio-microstructures relevant for PV-MPS. Here the emphasis is on identifying the strategies and material designs towards improvement of the performance of emerging halide perovskite PVs and strategizing their bridge to future MPS.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗