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NASA NTRS2014

Fabrication of Turbine Disk Materials by Additive Manufacturing

Precipitation-strengthened, nickel-based superalloys are widely used in the aerospace and energy industries due to their excellent environmental resistance and outstanding mechanical properties under extreme conditions. Powder-bed additive manufacturing (AM) technologies offer the potential to revolutionize the processing of superalloy turbine components by eliminating the need for extensive inventory or expensive legacy tooling. Like selective laser melting (SLM), electron beam melting (EBM) constructs three-dimensional dense components layer-by-layer by melting and solidification of atomized, pre-alloyed powder feedstock within 50-200 micron layers. While SLM has been more widely used for AM of nickel alloys like 718, EBM offers several distinct advantages, such as less retained residual stress, lower risk of contamination, and faster build rates with multiple-electron-beam configurations. These advantages are particularly attractive for turbine disks, for which excessive residual stress and contamination can shorten disk life during high-temperature operation. In this presentation, we will discuss the feasibility of fabricating disk superalloy components using EBM AM. Originally developed using powder metallurgy forging processing, disk superalloys contain a higher refractory content and precipitate volume fraction than alloy 718, thus making them more prone to thermal cracking during AM. This and other challenges to produce homogeneous builds with desired properties will be presented. In particular, the quality of lab-scale samples fabricated via a design of experiments, in which the beam current, build temperature, and beam velocity were varied, will be summarized. The relationship between processing parameters, microstructure, grain orientation, and mechanical response will be discussed.

oxidation↗

DOE OSTI2025

3D nanolithography with metalens arrays and spatially adaptive illumination

The growing demand for advanced materials, miniaturized devices and integrated microsystems calls for the reliable fabrication of complex, multiscale, three-dimensional (3D) architectures, a need increasingly addressed through light-based and laser-based processes. However, owing to the field-of-view (FOV) limitations of conventional imaging optics, existing 3D laser nanofabrication techniques face fundamental challenges in throughput, proximity error and stitching defects on the path to scaling. Here, in this study, we present a scalable 3D nanofabrication platform that uses a metalens-generated focal spot array to parallelize two-photon lithography (TPL) beyond centimetre-scale write field areas. Metalenses are ideally suited for producing submicron-scale focal spots for high-throughput nanolithography, as they uniquely feature large numerical apertures (NAs), immersion media compatibility and large-scale manufacturability. We experimentally demonstrate a printing system that uses a 12-cm 2 metalens array to produce more than 120,000 cooperative focal spots, corresponding to a throughput exceeding 10 8 voxels s −1 . By programmatically patterning the focal spot array using a spatial light modulator (SLM), an adaptive parallel printing strategy is developed for precise greyscale linewidth modulation and choreographed printing of semiperiodic and fully aperiodic 3D geometries. We demonstrate parallel printing of replicated microstructures (>50 M microparticles per day), centimetre-scale 3D architectures with feature sizes down to 113 nm, and photonic and mechanical metamaterials. This work demonstrates the potential of 3D nanolithography towards wafer-scale production, showing how TPL could be used at scale for applications in microelectronics, biomedicine, quantum technology and high-energy laser targets.

Materials science↗

DOE OSTI2021

3D imaging techniques for characterising microcracks in cement-based materials

Concrete inherently contains pores and microcracks that can adversely impact its mechanical properties and long-term durability. However, characterising microcracks is difficult due to their complex, multiscale and three-dimensional (3D) nature. This paper presents an evaluation of 3D imaging techniques for characterising microcracks induced by different mechanisms. Seven cement pastes, mortars and concretes subjected to drying shrinkage, autogenous shrinkage and freeze-thaw cycles were investigated using focused ion beam nanotomography (FIB-nt), broad ion beam serial section tomography (BIB-SST), laser scanning confocal microscopy (LSCM) combined with serial sectioning and X-ray microtomography (μCT). The study shows that the characteristics of microcracks vary significantly depending on exposure conditions. Yet there is no single technique that can capture the entire size range of microcracks from sub to tens of μm within a sufficiently representative sampling volume. The achievable image volume and resolution, and the advantages and disadvantages of each technique are compared and discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Seeing through nuclear fuel: Three-dimensional, nondestructive X-ray microscopy and volumetric analyses of neutron-irradiated TRISO-coated fuel kernels

The three-dimensional (3D) characterization of nuclear fuel with X-ray microscopy has historically proven difficult, due to uranium’s high attenuation of easily accessible X-rays, both in a laboratory setting and at a synchrotron user facility. However, this imaging modality provides nondestructive information that can be used to investigate morphological changes arising from external stimuli (e.g., neutron irradiation, high-temperature testing). Using an appropriate X-ray energy spectrum and an adequate X-ray filter, suitable transmissions through properly sized nuclear fuel specimens can be achieved. Here, in this study, we present the methods and results of using a commercially available, laboratory-based X-ray microscope (XRM) to examine the extent of 3D morphological changes of tristructural isotropic (TRISO)-coated fuel particles, specifically uranium oxide/uranium carbide fuel kernels, after high-temperature neutron irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Post-irradiation examination of AGR-3/4 TRISO fuel compacts using three-dimensional X-ray computed tomography

The AGR-3/4 irradiation tests combined the third and fourth planned irradiation experiments in the US Department of Energy’s Advanced Gas Reactor (AGR) testing campaign of tri-structural isotropic (TRISO) fuel compacts. In this article, we present post-irradiation examination (PIE) using X-ray computed tomography (XCT) of two unirradiated and two irradiated compacts from the AGR-3/4 irradiation tests. The irradiated compacts studied (compact 7–1 and compact 12–4) represent the upper and lower limit of burnup within the AGR-3/4 irradiation experiment. This article presents a detailed quantitative analysis on the post-irradiation structure of TRISO fuel compacts. Various quantitative parameters including shape, size, and packing of kernels, and their spatial distribution, were utilized to gain insights into the structural changes caused by irradiation. The equivalent diameter and sphericity were found to increase and decrease, respectively, in irradiated compact 7–1 due to its higher burnup. Nearest neighbor distance between fuel kernels decreased after irradiation, suggesting irradiation-induced shrinkage of graphitic matrix. Furthermore, each compact in AGR-3/4 irradiation tests contained 20 designed-to-fail (DTF) fuel particles that were meant to act as a source of fission product release to the experiment test train. Furthermore, in the present work, all DTF fuel particles in the four compacts studied were identified, and it was found that they exhibited larger kernel swelling in compact 12–4 and smaller kernel swelling in compact 7–1, compared to the driver particles.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Scaling deep learning for material imaging with a pseudo 3D model for domain transfer

The recent introduction of deep learning methods for image processing has greatly advanced the characterization of materials using three-dimensional (3D) X-ray imaging techniques. However, deep learning models often have difficulty performing consistently across images owing to unavoidable variations in imaging conditions, which create inconsistencies even for the same material. As a result, networks must frequently be retrained for new datasets, limiting their applicability and generalization. Thus, it is critical to reduce the variations between images to enable a single model to process multiple datasets. Herein, we introduce P3T-Net, a pseudo-3D domain transfer network that transfers diverse 3D images into a uniform domain before processing using deep learning models. Remarkably, P3T-Net enables the reuse of previously trained networks for processing new images and considerably reduces the computational cost of transferring 3D images across domains. These unique capabilities were demonstrated in the following scenarios: (i) image enhancement of fast scans for geological rock and hydrogen fuel cells, (ii) enhancement of images to match the quality of multi-source imaging for lithium-ion batteries, (iii) accurate segmentation of images captured under different conditions, and (iv) tera-scale 3D transfer (10 11 voxels) on a single GPU. Overall, the proposed approach addresses cross-domain inconsistencies across various materials and conditions, thereby enabling more robust and generalizable deep learning solutions for a wide range of material imaging tasks.

25 ENERGY STORAGE↗

DOE OSTI2023

Influence of Potassium Metal-Support Interactions on Dendrite Growth

We report combined synchrotron X-ray nanotomography imaging, cryogenic electron microscopy (cryo-EM) and modeling elucidate how potassium (K) metal-support energetics influence electrodeposit microstructure. Three model supports are employed: O-functionalized carbon cloth (potassiophilic, fully-wetted), non-functionalized cloth and Cu foil (potassiophobic, nonwetted). Nanotomography and focused ion beam (cryo-FIB) cross-sections yield complementary three-dimensional (3D) maps of cycled electrodeposits. Electrodeposit on potassiophobic support is a triphasic sponge, with fibrous dendrites covered by solid electrolyte interphase (SEI) and interspersed with nanopores (sub-10 nm to 100 nm scale). Lage cracks and voids are also a key feature. On potassiophilic support, the deposit is dense and pore-free, with uniform surface and SEI morphology. Mesoscale modeling captures the critical role of substrate-metal interaction on K metal film nucleation and growth, as well as the associated stress state.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Nanoscale defect evaluation framework combining real-time transmission electron microscopy and integrated machine learning-particle filter estimation

Observation of dynamic processes by transmission electron microscopy (TEM) is an attractive technique to experimentally analyze materials’ nanoscale phenomena and understand the microstructure-properties relationships in nanoscale. Even if spatial and temporal resolutions of real-time TEM increase significantly, it is still difficult to say that the researchers quantitatively evaluate the dynamic behavior of defects. Images in TEM video are a two-dimensional projection of three-dimensional space phenomena, thus missing information must be existed that makes image’s uniquely accurate interpretation challenging. Therefore, even though they are still a clustering high-dimensional data and can be compressed to two-dimensional, conventional statistical methods for analyzing images may not be powerful enough to track nanoscale behavior by removing various artifacts associated with experiment; and automated and unbiased processing tools for such big-data are becoming mission-critical to discover knowledge about unforeseen behavior. We have developed a method to quantitative image analysis framework to resolve these problems, in which machine learning and particle filter estimation are uniquely combined. The quantitative and automated measurement of the dislocation velocity in an Fe-31Mn-3Al-3Si autunitic steel subjected to the tensile deformation was performed to validate the framework, and an intermittent motion of the dislocations was quantitatively analyzed. The framework is successfully classifying, identifying and tracking nanoscale objects; these are not able to be accurately implemented by the conventional mean-path based analysis.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Three-dimensional photoluminescence imaging of threading dislocations in GaN by sub-band optical excitation

GaN is rapidly gaining attention for implementation in power electronics but is still impacted by its high density of threading dislocations (TDs), which have been shown to facilitate current leakage through devices limiting their performance and reliability. Here, we discuss a novel implementation of photoluminescence (PL) imaging to study TDs in regions within vertically structured p-i-n GaN (PIN) diodes consisting of metalorganic chemical vapor deposition (MOCVD) epitaxial layers grown on ammonothermal GaN (am-GaN) substrates. PL imaging with a sub-bandgap excitation energy (3.1 eV) reveals TDs with excellent clarity in three dimensions within the am-GaN substrate. Galvanometric-driven PL imaging allows the microstructure of hundreds of devices to be characterized in a single session, enhancing the screening process through the addition of device specific TD location tracking and density mapping. The visibility, structural characteristics, luminescent nature and evolution of TDs through the GaN growth process are described, potentially providing the ability to define TD structures associated with leakage current.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Mechanical design of the highly porous cuttlebone: A bioceramic hard buoyancy tank for cuttlefish

Cuttlefish, a unique group of marine mollusks, produces an internal biomineralized shell, known as cuttlebone, which is an ultra-lightweight cellular structure (porosity, ~93 vol%) used as the animal’s hard buoyancy tank. Although cuttlebone is primarily composed of a brittle mineral, aragonite, the structure is highly damage tolerant and can withstand water pressure of about 20 atmospheres (atm) for the species Sepia officinalis . Currently, our knowledge on the structural origins for cuttlebone’s remarkable mechanical performance is limited. Combining quantitative three-dimensional (3D) structural characterization, four-dimensional (4D) mechanical analysis, digital image correlation, and parametric simulations, here we reveal that the characteristic chambered “wall–septa” microstructure of cuttlebone, drastically distinct from other natural or engineering cellular solids, allows for simultaneous high specific stiffness (8.4 MN∙m/kg) and energy absorption (4.4 kJ/kg) upon loading. We demonstrate that the vertical walls in the chambered cuttlebone microstructure have evolved an optimal waviness gradient, which leads to compression-dominant deformation and asymmetric wall fracture, accomplishing both high stiffness and high energy absorption. Moreover, the distribution of walls is found to reduce stress concentrations within the horizontal septa, facilitating a larger chamber crushing stress and a more significant densification. Overall, the design strategies revealed here can provide important lessons for the development of low-density, stiff, and damage-tolerant cellular ceramics.

42 ENGINEERING↗

DOE OSTI2025

Niobium hydride formation in superconducting qubit thin films

The formation of nonsuperconducting hydrides in 160–170-nm-thick films of niobium is examined. We identify six elastically distinct orientation relationships ɛ−Nb 4 ⁢H 3 takes within the matrix, solid-solution 𝛼−NbH 𝑥 phase. We employ a phase field model to assess the impact of elastic energy induced by the strain of phase transformation on the morphology and transformation dynamics of ɛ precipitates within a thin film. We consider the dimensions of the thin film, crystallographic growth direction, and diffusion rates to predict the timescale of hydride evolution. Leveraging the finite element method, we predict two-dimensional and three-dimensional equilibrium shapes of ɛ-hydrides within a bulk sample and in a thin film that has a traction-free surface. Our results suggest that niobium hydrides migrate to the free surface of the film. Precipitates which reach the free surface coarsen, while precipitates within the film dissolve. Precipitates in both two dimensions and three dimensions experience a repulsive interaction force at the free surface, that is attractive in the bulk, shown in experiment and theory of previous studies.

36 - MATERIALS SCIENCE↗

DOE OSTI2022

A cellulose-derived supramolecule for fast ion transport

Supramolecular frameworks have been widely synthesized for ion transport applications. However, conventional approaches of constructing ion transport pathways in supramolecular frameworks typically require complex processes and display poor scalability, high cost, and limited sustainability. Here, we report the scalable and cost-effective synthesis of an ion-conducting (e.g., Na + ) cellulose-derived supramolecule (Na-CS) that features a three-dimensional, hierarchical, and crystalline structure composed of massively aligned, one-dimensional, and ångström-scale open channels. Using wood-based Na-CS as a model material, we achieve high ionic conductivities (e.g., 0.23 S/cm in 20 wt% NaOH at 25 °C) even with a highly dense microstructure, in stark contrast to conventional membranes that typically rely on large pores (e.g., submicrometers to a few micrometers) to obtain comparable ionic conductivities. This synthesis approach can be universally applied to a variety of cellulose materials beyond wood, including cotton textiles, fibers, paper, and ink, which suggests excellent potential for a number of applications such as ion-conductive membranes, ionic cables, and ionotronic devices.

36 MATERIALS SCIENCE↗

NASA NTRS2003

Evolution of Local Microstructures of Clusters Undergoing 2-Dimensional Diffusion

A primary objective of our current work is to study the details of evolving microstructures through a study of "island" formation in heteroepitaxial film/substrate systems. Such systems could be of direct relevance to so-called mixed-dimensional coarsening and to the study of heterostructures grown by thin-film techniques. The spontaneous formation of three-dimensional islands in strained-layer heteroepitaxy, e.g., has emerged as a new technique for the synthesis of self-assembled quantum dots. This work focuses on coarsening by two-dimensional diffusion of three-dimensional droplets on a flat surface.

Frazier, Donald O.↗

NASA NTRS2003

Evolution of Local Microstructures: Spatial Instabilities in Coarsening Clusters

Diffusion-limited capillarity-driven coarsening of precipitates is an important and intensively studied phenomenon. The classic coarsening theory developed by Lifshitz and Syozov and Wagner (LSW theory) is limited to infinitesimally small volume fractions, V(sub nu), therefore neglects all direct interparticle interactions. This work uses modeling and holographic imaging to compare coarsening rates in "high" volume fraction versus low volume fraction microstructures by observing mixed-dimensional droplets (spherical caps on a surface coarsening by two-dimensional diffusion) during ground-based investigations. The method involves filling a cell with selected homogeneous parent phase, and cooling below the consolute temperature to the isopycnic temperature in the two-phase region of a monotectic system. A microgravity holographic experiment is required for three-dimensional observations to minimize sedimentation during long-term coarsening. Determination of sizes and positions of the many droplets in the holographic images requires automation. We have developed software for automated data analysis, and demonstrated good agreement between regenerated maps and scaled photographs of the original holograms for mixed dimensional coarsening. The results of these experiments were presented in a formal microgravity Science Concept Review (SCR) on December 18, 2000.

Source record↗

NASA NTRS2003

High-Fidelity Micromechanics Model Enhanced for Multiphase Particulate Materials

This 3-year effort involves the development of a comprehensive micromechanics model and a related computer code, capable of accurately estimating both the average response and the local stress and strain fields in the individual phases, assuming both elastic and inelastic behavior. During the first year (fiscal year 2001) of the investigation, a version of the model called the High-Fidelity Generalized Method of Cells (HFGMC) was successfully completed for the thermo-inelastic response of continuously reinforced multiphased materials with arbitrary periodic microstructures (refs. 1 and 2). The model s excellent predictive capability for both the macroscopic response and the microlevel stress and strain fields was demonstrated through comparison with exact analytical and finite element solutions. This year, HFGMC was further extended in two technologically significant ways. The first enhancement entailed the incorporation of fiber/matrix debonding capability into the two-dimensional version of HFGMC for modeling the response of unidirectionally reinforced composites such as titanium matrix composites, which exhibit poor fiber/matrix bond. Comparison with experimental data validated the model s predictive capability. The second enhancement entailed further generalization of HFGMC to three dimensions to enable modeling the response of particulate-reinforced (discontinuous) composites in the elastic material behavior domain. Next year, the three-dimensional version will be generalized to encompass inelastic effects due to plasticity, viscoplasticity, and damage, as well as coupled electromagnetothermomechanical (including piezoelectric) effects.

Pindera, Marek-Jerzy↗

NASA NTRS2015

Investigation of Micro-Scale Architectural Effects on Damage of Composites

This paper presents a three-dimensional, energy based, anisotropic, stiffness reduction, progressive damage model for composite materials and composite material constituents. The model has been implemented as a user-defined constitutive model within the Abaqus finite element software package and applied to simulate the nonlinear behavior of a damaging epoxy matrix within a unidirectional composite material. Three different composite microstructures were considered as finite element repeating unit cells, with appropriate periodicity conditions applied at the boundaries. Results representing predicted transverse tensile, longitudinal shear, and transverse shear stress-strain curves are presented, along with plots of the local fields indicating the damage progression within the microstructure. It is demonstrated that the damage model functions appropriately at the matrix scale, enabling localization of the damage to simulate failure of the composite material. The influence of the repeating unit cell geometry and the effect of the directionality of the applied loading are investigated and discussed.

damage↗

NASA NTRS2019

A Three-Dimensional Thermodynamically Based Function for the Progressive Failure of Unidirectional Composites

A thermodynamically-based work potential theory for modeling progressive damage for laminated, unidirectional composites assuming plane stress (2D Schaperystheory) is extended to three dimensioanl (3D). An internal state variable, S, is defined to account for the dissipated energy due to damage evolution in the form of microstructure changes in the matrix. With the stationary of the total work potential with respect to the internal state variable, a thermodynamically-consistent set of evolution equationsis derived. The internal state variable is related to the transverse and shear modulithrough microdamage functions. In the first part of this work, coupon specimensare prepared to conduct experiments to characterize the relations between the internalstate variable and the transverse modulus as well as shear modulus. The informationis subsequent used for the prediction of three point bending test. In the second partof this work, objectivity is studied. Three separate methods utilizing different definitions of a reduced internal state variable or of the order of the polynomials are used to represent the matrix micro-damage functions are employed. The three methods are implemented in a user defined subroutine within a commercial finite element method software package. Results from numerical simulations of a center-notched composites panel are compared. The agreement in the maximum stress predictions among the three methods indicates that objectivity, with respect to the functional form of themicrodamage functions, is satisfied.

carbon fiber reinforced polymer composites↗

NASA NTRSDate not supplied

Three-Dimensional Reconstruction of Defects and Structures in Additively Manufactured Parts with Automated Serial Sectioning

Metal additive manufacturing (AM) processes have been demonstrated to be effective at reducing costs and lead times associated with complex components for space flight applications. Laser powderbed fusion (L-PBF) is a commonly used AM technology due to the ability to produce complex parts with fine feature resolution in a wide variety of alloys and applications. L-PBF, like many other manufacturing processes, can produce minor flaws in parts when in nominal operation as well as process-escape defects when process abnormalities occur. The effects of the flaws and methods of detecting the flaws are a subject of interest to understand the difficulties in detecting these flaws with current technology and how much risk the flaws or defects pose to potential flight parts. Using a RoboMet.3D automated serial sectioning system, seeded defects as well as minor process flaws can be imaged and reconstructed in three dimensions to compare to non-destructive evaluation (NDE) techniques, such as x-ray computed tomography (CT), neutron CT, and in-situ monitoring. The RoboMet automates the metallography process by automatically grinding, polishing, and imaging samples in a single system and providing the control data for NDE comparisons to know the real size of defects built into coupons. These comparisons provide an understanding behind the technological limitations of the NDE techniques for different alloys. The same serial sectioning methods have also been utilized to characterize the surfaces of parts to reconstruct the surfaces and take measurements of internal features not easily examined with non-destructive methods. Using the RoboMet, fine lattice structures built with L-PBF have been characterized to determine the actual thicknesses of struts and density of the lattice structures. These structures have been used as finer build supports for the L-PBF process, designs for fine catalysts, and other design considerations for small components. The RoboMet data helps to inform the modeling and design efforts around these fine components.

additive manufacturing↗