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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 1,639 records · Page 91
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Subgrain geometrically necessary dislocation density mapping in spalled Ta in three dimensions

Here, in this work, the intragranular distributions of the densities of geometrically necessary dislocations (GNDs) generated in a polycrystalline tantalum (Ta) sample loaded in shock compression to spall are investigated. The sample studied is a highly resolved three-dimensional (3D) map of the orientations, grain boundary morphology, and voids across a 0.276mm 3 (with sample dimensions of 688.5µm x 669µm x 600µm) region of the microstructure about the spall plane obtained by TriBeam tomography. We present a formulation for calculating the crystallographic screw and edge character GND densities at a material point within body centered cubic (BCC) crystals when provided any number of potential slip systems or modes. Combining the 3D characterization, GND formulation, and a sample containing ≈ 6000 grains, we sought statistically relevant correlations between GND density per grain with grain size, grain orientation, void formation, and proximity from the spall plane. We show that GND density per grain increases with decreasing distance from the spall plane. Most grains had heterogeneously distributed GND densities but were free of any detectable voids, at least within the ≈ 1.5µm resolution of the characterization technique. It is found that the GND density for most grains is insensitive to grain size and grain orientation. Only the fraction of grains with the highest GND densities tended to have a [001] parallel to shock-direction orientation. Intragranular 3D maps of GNDs reveals that grains that contain voids have high GND density concentrations in the intragranular region immediately surrounding the void. The local intragranular GND mapping also showed voids that are connected to grain boundaries preferred to grow into the grain with the larger size, regardless of orientation.

36 MATERIALS SCIENCE↗
DOE OSTI2020

An image-driven machine learning approach to kinetic modeling of a discontinuous precipitation reaction

Micrograph quantification is an essential component of several materials science studies. Machine learning methods, in particular convolutional neural networks, have previously demonstrated performance in image recognition tasks across several disciplines (e.g. materials science, medical imaging, facial recognition). Here, we apply these well-established methods to develop an approach to microstructure quantification for kinetic modeling of a discontinuous precipitation reaction in a case study on the uranium-molybdenum system. Prediction of material processing history based on image data (classification), calculation of area fraction of phases present in the micrographs (segmentation), and kinetic modeling from segmentation results were performed. Results indicate that convolutional neural networks represent microstructure image data well, and segmentation using the k-means clustering algorithm yields results that agree well with manually annotated images. Classification accuracies of original and segmented images are both 94% for a 5-class classification problem. Kinetic modeling results agree well with previously reported data using manual thresholding. The image quantification and kinetic modeling approach developed and presented here aims to reduce researcher bias introduced into the characterization process, and allows for leveraging information in limited image data sets.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Hybrid fiber metal composite laminate interlaminar reinforcement through metal interlocks

Aircraft and automobile industries are continually seeking high-performance and lightweight solutions. Fiber-reinforced composites in conjunction with metals are being considered in the form of hybrid materials. There is a continuous need for improvement of interfacial bonding between composite layers and metal constituents. In this study, an innovative hybrid fiber interlocking metal hooks laminate (FIMHL) system was developed in which fiber-reinforced thermoset composite, and metal sheets are mechanically bonded together using out of plane hooks stamped in the metal. Process optimization was performed to gain the full benefit of the through-thickness reinforcement. Microstructural analysis showed improved interaction between the metal hooks and the fiber layers which reduced porosity and resin richness. This was reflected in mechanical properties, as tensile and flexural strength of FIMHL was enhanced by 38.5 and 18.8%, respectively, after process optimization. Furthermore, normalized weight fraction (76.4%) properties of FIMHL also confirmed that the increase in mechanical properties of optimized panel were not only due to increased reinforcement (glass fiber + aluminum) volume fraction but also because of improved metal hooks and fibers interaction. There was no significant effect on lap shear and fracture toughness, as they depend on bend back behavior of the hooks. A bilinear traction-separation model was used to characterize mode-I interlaminar fracture toughness properties, and 4.5% variation was recorded when modeling and experimental values were compared.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microstructural and compositional evolutions in $γ$-LiAlO 2 pellets during ion irradiation at an elevated temperature

This study reports on the microstructural, phasic and compositional evolutions of γ-LiAlO 2 during ion irradiation. Polycrystalline γ-LiAlO 2 pellets were irradiated sequentially with He + and D 2 + ions to the same combined fluences of up to 3 × 10 17 (He + +D + )/cm 2 at 773 K. The irradiated pellets were characterized using scanning transmission electron microscopy and atom probe tomography. Surface amorphization likely due to radiolysis and planar defects as a possible precursor for formation of precipitates are created at 5 × 10 16 (He + +D + )/cm 2 , followed by the formation of nano-sized precipitates and fractures at higher doses. Spinel-like precipitates of non-stoichiometric LiAl 5 O 8 and gas-filled cavities are observed to grow with increasing dose. Faceted precipitates and rounded cavities appear at 2 × 10 17 (He + +D + )/cm 2 . With further increasing ion fluence to 3 × 10 17 (He + +D + )/cm 2 , amorphization of the precipitates takes place and micron-sized fractures appear. Surface exfoliation could occur at an extremely high ion fluence. There are compositional changes in the γ-LiAlO 2 pellets during the microstructural evolution. In the precipitate and amorphized regions, Li concentrations decrease to ~7 and 3.7 at.% from 25 at.% in γ-LiAlO 2 , respectively. This study reveals a full-cycle microstructural evolution with corresponding compositional changes in γ-LiAlO 2 pellets during ion irradiation at 773 K. In conclusion, the data could help model, assess, and predict the material performance during neutron irradiation in reactors.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2022

Physical characterization of fault rocks within the Opalinus Clay formation

Near-surface disposal of radioactive waste in shales is a promising option to safeguard the population and environment. However, natural faults intersecting these geological formations can potentially affect the long-term isolation of the repositories. This paper characterizes the physical properties and mineralogy of the internal fault core structure intersecting the Opalinus Clay formation, a host rock under investigation for nuclear waste storage at the Mont Terri Laboratory (Switzerland). We have performed porosity, density, microstructural and mineralogical measurements in different sections of the fault, including intact clays, scaly clays and fault gouge. Mercury intrusion porosimetry analysis reveal a gouge that has a pore network dominated by nanopores of less than 10 nm, yet a high-porosity (21%) and low grain density (2.62 g/cm 3 ) when compared to the intact rock (14.2%, and 2.69 g/cm 3 ). Thus, a more permeable internal fault core structure with respect to the surrounding rock is deduced. Further, we describe the OPA fault gouge as a discrete fault structure having the potential to act as a preferential, yet narrow, and localized channel for fluid-flow if compared to the surrounding rock. Since the fault gouge is limited to a millimetres-thick structure, we expect the barrier property of the geological formation is almost not affected.

58 GEOSCIENCES↗
DOE OSTI2021

Structural and chemical evolution in layered oxide cathodes of lithium-ion batteries revealed by synchrotron techniques

Abstract Rechargeable battery technologies have revolutionized electronics, transportation and grid energy storage. Many materials are being researched for battery applications, with layered transition metal oxides (LTMO) the dominating cathode candidate with remarkable electrochemical performance. Yet, daunting challenges persist in the quest for further battery developments targeting lower cost, longer lifespan, improved energy density and enhanced safety. This is, in part, because of the intrinsic complexity of real-world batteries, featuring sophisticated interplay among microstructural, compositional and chemical heterogeneities, which has motivated tremendous research efforts using state-of-the-art analytical techniques. In this research field, synchrotron techniques have been identified as a suite of effective methods for advanced battery characterization in a non-destructive manner with sensitivities to the lattice, electronic and morphological structures. This article provides a holistic overview of cutting-edge developments in synchrotron-based research on LTMO battery cathode materials. We discuss the complexity and evolution of LTMO’s material properties upon battery operation and review recent synchrotron-based research works that address the frontier challenges and provide novel insights in this field. Finally, we formulate a perspective on future directions of synchrotron-based battery research, involving next-generation X-ray facilities and advanced computational developments.

25 ENERGY STORAGE↗
NASA NTRS1985

Role of Hydrogen and Structure on CMSX-2

The goal was to characterize and understand the detailed effect of hydrogen on the tensile and fatigue behavior of single crystals of CMSX-2. Specimens were solutionized, air cooled, and then aged in one of two ways. The resultant macro and microstructure included a pronounced dendritic structure with numerous low angle boundaries in the interdendritic region and on the average a high level of porosity with a large variation in size and distribution. Hydrogen permeability and diffusivity in this material was found to be very low at room temperature. Hydrogen concentration studies on thin samples yielded values significantly higher than found for similar charging conditions in nickel and stainless steels. The tensile mechanical properties were found to depend on hydrogen concentration. SEM observations of the brittle subsurface zone revealed a strong correlation between crack initiation sites and voids just beneath the surface. The hollow and solid samples were compared to better understand the influence of increased charged volume on the fatigue behavior.

Baker, C. L.↗
NASA NTRS1991

The effect of copper, chromium, and zirconium on the microstructure and mechanical properties of Al-Zn-Mg-Cu alloys

The present study evaluates the effect of the systematic variation of copper, chromium, and zirconium contents on the microstructure and mechanical properties of a 7000-type aluminum alloy. Fracture toughness and tensile properties are evaluated for each alloy in both the peak aging, T8, and the overaging, T73, conditions. Results show that dimpled rupture essentially characterize the fracture process in these alloys. In the T8 condition, a significant loss of toughness is observed for alloys containing 2.5 pct Cu due to the increase in the quantity of Al-Cu-Mg-rich S-phase particles. An examination of T8 alloys at constant Cu levels shows that Zr-bearing alloys exhibit higher strength and toughness than the Cr-bearing alloys. In the T73 condition, Cr-bearing alloys are inherently tougher than Zr-bearing alloys. A void nucleation and growth mechanism accounts for the loss of toughness in these alloys with increasing copper content.

Wagner, John A.↗
NASA NTRS1993

Preliminary AEM study of the microstructure and composition of metal particles in ordinary chondrites

The purpose of this study is to examine the microstructure and composition of the metal particles in ordinary chondrites using analytical electron microscopy (AEM) techniques. Since the phases produced within the metal particles are very fine, the application of various AEM techniques for structural and chemical characterization is critical. However, thin specimen preparation for AEM study has proven very difficult because of the matrix silicate which is present. This is the first AEM study of the metal particles in chondrites. A type 6 chondrite, Saint Severin (LL6), was selected for examination because the metal phases have been reheated into the single phase taenite region (greater than 700 C), and cooled slowly to lower temperatures. A combination of electron optical instruments was employed including a field emission gun (FEG) JEOL 840F high resolution scanning electron microscope (HRSEM), a JEOL 6300F FEG-HRSEM, a Philips 400T AEM, and a JEOL 733 electron probe microanalyzer (EPMA).

Yang, C. W.↗
NASA NTRS2015

Materials Characterization of Electron Beam Melted Ti-6Al-4V

An in-depth material characterization of Electron Beam Melted (EBM) Ti-6Al-4V material has been completed. Hot Isostatic Pressing (HIP) was utilized to close porosity from fabrication and also served as a material heat treatment to obtain the desired microstructure. The changes in the microstructure and chemistry from the powder to pre-HIP and post-HIP material have been analyzed. Computed tomography (CT) scans indicated porosity closure during HIP and high-density inclusions scattered throughout the specimens. The results of tensile and high cycle fatigue (HCF) testing are compared to conventional Ti-6Al-4V. The EBM Ti-6Al-4V had similar or superior mechanical properties compared to conventionally manufactured Ti-6Al-4V.

Titanium↗
NASA NTRS1991

Mechanical characterization and modeling of non-linear deformation and fracture of a fiber reinforced metal matrix composite

The nonlinear anisotropic mechanical behavior of an aluminum alloy metal matrix composite reinforced with continuous alumina fibers was determined experimentally. The mechanical behavior of the composite were modeled by assuming that the composite has a periodical microstructure. The resulting unit cell problem was solved with the finite element method. Excellent agreement was found between theoretically predicted and measured stress-strain responses for various tensile and shear loadings. The stress-strain responses for transverse and inplane shear were found to be identical and this will provide a simplification of the constitutive equations for the composite. The composite has a very low ductility in transverse tension and a limited ductility in transverse shear that was correlated to high hydrostatic stresses that develop in the matrix. The shape of the initial yield surface was calculated and good agreement was found between the calculated shape and the experimentally determined shape.

Jansson, S.↗
DOE OSTI2021

Precipitation Hardening in Ferroelectric Ceramics

Domain wall motion in ferroics, similar to dislocation motion in metals, can be tuned by well-concepted microstructural elements. In demanding high-power applications of piezoelectric materials, the domain wall motion is considered as a lossy hysteretic mechanism that should be restricted. Current applications for so-called hard piezoelectrics are abundant and hinge on the use of an acceptor-doping scheme. However, this mechanism features severe limitations due to enhanced mobility of oxygen vacancies at moderate temperatures. By analogy with metal technology, the authors present here a new solution for electroceramics, where precipitates are utilized to pin domain walls and improve piezoelectric properties. Through a sequence of sintering, nucleation, and precipitate growth, intragranular precipitates leading to a fine domain structure are developed as shown by transmission electron microscopy, piezoresponse force microscopy, and phase-field simulation. This structure impedes the domain wall motion as elucidated by electromechanical characterization. As a result, the mechanical quality factor is increased by ≈50% and the hysteresis in electrostrain is suppressed considerably. This is even achieved with slightly increased piezoelectric coefficient and electromechanical coupling factor. This novel process can be smoothly implemented in industrial production processes and is accessible to simple laboratory experimentation for microstructure optimization and implementation in various ferroelectric systems.

36 MATERIALS SCIENCE↗
DOE OSTI2022

NSUF Report EBSD analyses on metallic fuel samples: Tips and improvements in sample preparation

EBSD (Electron Backscatter Diffraction) is an analytic technique used to evaluate the microstructure of a specimen. It can be used to evaluate interesting crystallographic data ranging from grains size to grain orientation, from grain boundaries to stresses. Moreover, in the field of nuclear materials EBSD can aid in estimating properties important for reactor performance, such as dislocation and residual strain [1]. EBSD patterns are generated by focusing a stationary electron gun on the specimen and detecting the backscatter electrons that satisfy Bragg conditions, and thus are diffracted by the crystal planes forming the so called Kikuchi bands. These bands correspond to each of the lattice diffracting crystal planes and are detected on a phosphor screen via a low-light CCD camera [2]. The patterns are generated within a small interaction volume located at a depth of less than 50-100 nm. Because of this, the data quality is extremely sensitive to the integrity of the crystallographic lattice order at the surface of the sample and thus to sample preparation and to oxidation [3]. While conventional sample preparation methods are widely used in materials science, they often do not lead to quality electron backscatter patterns needed for the characterization of nuclear materials [4]. This has been related by many authors to the challenges associated with handling radiological specimens, their rapid oxidation, and artifacts in such samples (e.g. high number of defects, precipitates and/or porosities) [4-8]. EBSD, however, can be an invaluable technique to evaluate microstructural evolution during fabrication and after irradiation at the required mesoscale for model and simulation. It also provides important information on grain structure necessary to understand irradiation effect, such as grain subdivision. Thus, it is of paramount importance to further the application of this technique to nuclear materials and especially irradiated fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1999

Ultrasonic Nondestructive Characterization of Adhesive Bonds

Adhesives and adhesive joints are widely used in various industrial applications to reduce weight and costs, and to increase reliability. For example, advances in aerospace technology have been made possible, in part, through the use of lightweight materials and weight-saving structural designs. Joints, in particular, have been and continue to be areas in which weight can be trimmed from an airframe through the use of novel attachment techniques. In order to save weight over traditional riveted designs, to avoid the introduction of stress concentrations associated with rivet holes, and to take full advantage of advanced composite materials, engineers and designers have been specifying an ever-increasing number of adhesively bonded joints for use on airframes. Nondestructive characterization for quality control and remaining life prediction has been a key enabling technology for the effective use of adhesive joints. Conventional linear ultrasonic techniques generally can only detect flaws (delamination, cracks, voids, etc) in the joint assembly. However, more important to structural reliability is the bond strength. Although strength, in principle, cannot be measured nondestructively, a slight change in material nonlinearity may indicate the onset of failure. Furthermore, microstructural variations due to aging or under-curing may also cause changes in the third order elastic constants, which are related to the ultrasonic nonlinear parameter of the polymer adhesive. It is therefore reasonable to anticipate a correlation between changes in the ultrasonic nonlinear acoustic parameter and the remaining bond strength. It has been observed that higher harmonics of the fundamental frequency are generated when an ultrasonic wave passes through a nonlinear material. It seems that such nonlinearity can be effectively used to characterize bond strength. Several theories have been developed to model this nonlinear effect. Based on a microscopic description of the nonlinear interface binding force, a quantitative method was presented. Recently, a comparison between the experimental and simulated results based on a similar theoretical model was presented. A through-transmission setup for water immersion mode-converted shear waves was used to analyze the ultrasonic nonlinear parameter of an adhesive bond. In addition, ultrasonic guided waves have been used to analyze adhesive or diffusion bonded joints. In this paper, the ultrasonic nonlinear parameter is used to characterize the curing state of a polymer/aluminum adhesive joint. Ultrasonic through-transmission tests were conducted on samples cured under various conditions. The magnitude of the second order harmonic was measured and the corresponding ultrasonic nonlinear parameter was evaluated. A fairly good correlation between the curing condition and the nonlinear parameter is observed. The results show that the nonlinear parameter might be used as a good indicator of the cure state for adhesive joints.

Qu, Jianmin↗
DOE OSTI2020

Characterization of PyC/SiC interfaces with FIB-SEM tomography

Tristructural-isotropic (TRISO) fuel is being considered for multiple reactor designs due to its exceptional performance. This work studies pyrocarbon (PyC) and silicon carbide (SiC) substrates that are near-representative of the inner pyrocarbon (IPyC) and SiC in TRISO fuel. Focused ion beam (FIB)-scanning electron microscopy (SEM) tomography was used to understand the influence of different processing routes on the PyC/SiC interface structure. Additionally, this work outlines a methodology for characterizing the IPyC/SiC interface when considering fission product accommodation and retention in TRISO fuel design. The high-fidelity images collected with FIB-SEM tomography can be used to achieve a more in-depth interpretation of microstructural parameters and pore-shape analysis that can inform simulations and processing.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Structure of the pellet-cladding interaction layer of a high-burnup Zr-Nb-O nuclear fuel cladding

Here, structure of the pellet/cladding-interaction (PCI) layer of a high-burnup nuclear fuel with niobium-bearing cladding was investigated using modern transmission electron microscopy (TEM) techniques. Morphology of the PCI consisted of uniform zirconia layer on the cladding side and finger-like features towards to the ceramic fuel. The PCI layer showed a complex microstructure that constitutes three distinct zirconia layers formed by two zirconia phases. From cladding to fuel, monoclinic, tetragonal, and another tetragonal phase were determined via TEM diffraction patterns and precession electron diffraction (PED) using ASTAR microscopy platform (AMP). Characterizations showed that monoclinic and tetragonal phases close to the cladding were crack-free, but the tetragonal layer adjacent to the fuel contained cracks and pores. Presence of the monoclinic layer suggested that its formation involved the gaseous diffusion of oxygen below threshold dose of fission product damage before the fuel/cladding contact occurred. Furthermore, high-resolution TEM revealed compound phase of (U,Zr)O 2 at fringes of zirconia fingers on the fuel side.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Unraveling the multi-step crystallization mechanism of polytetrafluoroethylene, modified polytetrafluoroethylene, and their nanocomposites with boron nitride nanobarbs: Experimental insights and theoretical analysis

The non-isothermal crystallization behavior and kinetics of polytetrafluoroethylene (PTFE) composites with boron nitride nanobarb (BNNB), a new generation nanostructure with unique surface morphology and mechanical “barbs” have been analyzed, understanding these properties is essential for their high-end applications as thermal interface materials (TIM) for microwave, 5G and microelectronic devices. The analysis of the crystallization parameters includes crystallization onset, peak and end temperatures, crystallization half-life and overall crystallinity of PTFE, modified PTFE and their BNNB composites. The results were further analyzed using theoretical models such as the combined Avrami-Ozawa model. It was found that BNNB supports crystallization in the modified PTFE but shows minimal effect on the crystallization of PTFE. Due to the limitation of the classical theoretical models used above in fully characterizing the multi-step crystallization process of PTFE, an in-depth analysis using the model-free advanced isoconversional computation was used to characterize the PTFE crystallization based on the evolution of activation energy with fractional crystallinity and for the first time with temperature. Three kinetic regions were identified in the crystallization mechanism. Here, this study investigated the molecular organization and microstructural evolution of PTFE, modified PTFE and their composites during non-isothermal crystallization using advanced X-ray scattering measurements. An insight into the changes undergone by the material's microstructural units including crystallite size and morphology, lamellar thickness and lamellar interfacial layer thickness, and crystallographic phase dynamics during non-isothermal cooling from the melt, was provided here in this work. The effect of copolymer modification of PTFE and the inclusion of pristine and functionalized BNNB (a thermally conductive and electrically insulating ceramic) are both new investigations that provide valuable knowledge for the development of materials with strong matrix-nanofiller interaction and guidance for optimizing sintering and cooling cycles, two key steps in PTFE processing that largely affect the material microstructural features. Overall, the result of the three-part investigation demonstrates that BNNB supports crystallization in the modified PTFE up to 20 wt% concentration and at low and high cooling rates typically used in the industrial processing of PTFE.

36 MATERIALS SCIENCE↗
DOE OSTI2021

X-ray computed tomography-based porosity analysis: Algorithms and application for porous woody biomass

The properties of lignocellulosic biomass, such as bulk physical, thermal, and mechanical properties, as well as the mobility of enzymes or catalysts, are largely affected by porosity, pore structures, and pore size distribution. While X-ray computed tomography (CT) has been introduced to effectively produce 3D volumetric images of material microstructure, a quantitative porosity analysis from the 3D images has never been done. This work introduces a first-of-its-kind X-ray CT-based quantitative porosity analysis method and applies the developed toolkit to characterize the internal porosity distribution of loblolly pine. A sample loblolly pine chip was scanned by a nano-resolution X-ray CT system and digitally reconstructed after a sequence of image processing operations. Here, a comprehensive porosity analysis was then performed to quantify the envelope porosity, the spatial distribution of local porosity, and the directional porosity. Solutions to the various challenges in image processing, porosity calculation, and large data handling are provided.

42 ENGINEERING↗