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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 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
NASA NTRS2003

Effect of Alignment on Transport Properties of Carbon Nanotube/Metallic Junctions

Ballistic and spin coherent transport in single walled carbon nanotubes (SWCNT) are predicted to enable high sensitivity single-nanotube devices for strain and magnetic field sensing. Based upon these phenomena, electron beam lithography procedures have been developed to study the transport properties of purified HiPCO single walled carbon nanotubes for development into sensory materials for nondestructive evaluation. Purified nanotubes are dispersed in solvent suspension and then deposited on the device substrate before metallic contacts are defined and deposited through electron beam lithography. This procedure produces randomly dispersed ropes, typically 2 - 20 nm in diameter, of single walled carbon nanotubes. Transport and scanning probe microscopy studies have shown a good correlation between the junction resistance and tube density, alignment, and contact quality. In order to improve transport properties of the junctions a technique has been developed to align and concentrate nanotubes at specific locations on the substrate surface. Lithographic techniques are used to define local areas where high frequency electric fields are to be concentrated. Application of the fields while the substrate is exposed to nanotube-containing solution results in nanotube arrays aligned with the electric field lines. A second electron beam lithography layer is then used to deposit metallic contacts across the aligned tubes. Experimental measurements are presented showing the increased tube alignment and improvement in the transport properties of the junctions.

Wincheski, Buzz↗
NASA NTRS1984

Study of factors determining the radiation sensitivity of quartz crystal oscillators (A0189)

The correlation between defect cluster concentrations observed for different grades of quartz examined by transmission electron microscopy (TEM) and the electrical stability of quartz resonators exposed to complex radiation in an orbital LDEF was determined. It is demonstrated that the technique TEM provides a powerful method for studying the effect of radiation on crystalline quartz. Two factors suggest that the observed clusters may be responsible for the radiation-induced frequency drift and acoustic absorption effects associated with irradiated quartz resonators: (1) the clusters are expected to be very effective in modifying the piezoelectric properties of quartz because of the large strain fields associated with them; (2) both phenomena appear to be sensitive to the impurity concentration. It is suggested that TEM can be used to classify grades of quartz according to their suitability for use in radiation-hard resonators. This technique may identify the impurities that are responsible and thereby effect an improvement in the stability of quartz oscillators.

Venables, J. D.↗
NASA NTRS2015

A Fully Nonmetallic Gas Turbine Engine Enabled by Additive Manufacturing of Ceramic Composites: Additive Manufacturing and Characterization of Ceramic Composites - Part III

This publication is the third part of a three part report of the project entitled "A Fully Nonmetallic Gas Turbine Engine Enabled by Additive Manufacturing" funded by NASA Aeronautics Research Institute (NARI). The objective of this project was to conduct additive manufacturing to produce ceramic matrix composite materials and aircraft engine components by the binder jet process. Different SiC powders with median sizes ranging from 9.3 to 53.0 microns were investigated solely and in powder blends in order to maximize powder packing. Various infiltration approaches were investigated to include polycarbosilane (SMP-10), phenolic, and liquid silicon. Single infiltrations of SMP-10 and phenolic only slightly filled in the interior. When the SMP-10 was loaded with sub-micron sized SiC powders, the infiltrant gave a much better result of filling in the interior. Silicon carbide fibers were added to the powder bed to make ceramic matrix composite materials. Microscopy showed that the fibers were well distributed with no preferred orientation on the horizontal plane and fibers in the vertical plane were at angles as much as 45deg. Secondary infiltration steps were necessary to further densify the material. Two to three extra infiltration steps of SMP-10 increased the density by 0.20 to 0.55 g/cc. However, the highest densities achieved were 2.10 to 2.15 g/cc. Mechanical tests consisting of 4 point bend tests were conducted. Samples from the two CMC panels had higher strengths and strains to failure than the samples from the two nonfiber reinforced panels. The highest strengths were from Set N with 65 vol% fiber loading which had an average strength of 66 MPa. Analysis of the fracture surfaces did not reveal pullout of the reinforcing fibers. Blunt fiber failure suggested that there was not composite behavior. The binder jet additive manufacturing method was used to also demonstrate the fabrication of turbine engine vane components of two different designs and sizes. The binder jet method has benefits over the conventional manufacturing of CMCs in that prototype and production parts can be fabricated quickly and economically with no tooling and extensive hand layup.

Additive Manufacturing↗
DOE OSTI2024

Atomic-Scale Scanning of Domain Network in the Ferroelectric HfO 2 Thin Film

Ferroelectric HfO 2 -based thin films have attracted much interest in the utilization of ferroelectricity at the nanoscale for next-generation electronic devices. However, the structural origin and stabilization mechanism of the ferroelectric phase are not understood because the film is typically nanocrystalline with active yet stochastic ferroelectric domains. Here, in this study, electron microscopy is used to map the in-plane domain network structures of epitaxially grown ferroelectric Y:HfO 2 films in atomic resolution. The ferroelectricity is confirmed in free-standing Y:HfO 2 films, allowing for investigating the structural origin for their ferroelectricity by 4D-STEM, high-resolution STEM, and iDPC-STEM. At the grain boundaries of <111>-oriented Pca2 1 orthorhombic grains, a high-symmetry mixed-(R3m, Pnm2 1 ) phase is induced, exhibiting enhanced polarization due to in-plane compressive strain. Nanoscale Pca2 1 orthorhombic grains and their grain boundaries with mixed-(R3m, Pnm2 1 ) phases of higher symmetry cooperatively determine the ferroelectricity of the Y:HfO 2 film. It is also found that such ferroelectric domain networks emerge when the film thickness is beyond a finite value. Furthermore, in-plane mapping of oxygen positions overlaid on ferroelectric domains discloses that polarization is suppressed at vertical domain walls, while it is active when domains are aligned horizontally with subangstrom domain walls. In addition, randomly distributed 180° charged domain walls are confined by spacer layers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

FY24 Integrated Results for High-Temperature Mechanical Testing of LPBF 316H Stainless Steel

This report provides the mechanical test data of laser powder bed fusion (LPBF) 316H stainless steel (SS) collected during Fiscal Year 2024 (FY 24) under the US Department of Energy, Office of Nuclear Energy’s Advanced Materials and Manufacturing Technologies program, along with the current state of microstructural-based understandings of the behaviors. Materials with variabilities in manufacturing site, machine, laser parameters, powder chemistry, porosity, specimen geometry and heat treatment were tested in high-temperature tension, creep, fatigue and creep-fatigue. Electron microscopy and optical microscopy were performed on selected materials before and after the tests to provide microstructural-based understandings to the mechanical behavior. It was discovered that the as-built (AB) and stress-relieved (SR) materials exhibit similar behaviors in tension and creep, as do the solution-annealed (SA) and hot-isostatic pressed (HIP) materials. The AB and SR materials are softer but more ductile than the SA and HIP materials in tension. In creep, the LPBF materials have comparable rupture times but lower rupture strains compared to the wrought materials. The AB and SR materials have low creep rupture strains (<10%) when tested at 720°C and 800°C, while the SA and HIP materials are much more ductile. The LPBF materials exhibit large scatter in fatigue and creep-fatigue lives. The cyclic lives of creep-fatigue tests are lower than those of fatigue tests. In fatigue and creep-fatigue, SR materials outperform SA materials. A common observation from the cyclic tests is that, given the same post-build heat treatment, a lower initial peak stress generally results in a longer cyclic life regardless of hold time. It was also discovered that the batch variation can be more impactful than heat treatment, as demonstrated by the overall better performance of one batch of material than another, regardless of the heat treatment. The results provided insights into how different factors impact the behaviors of LPBF 316H SS. An outlook to FY 25 work scope is provided.

36 MATERIALS SCIENCE↗
NASA NTRS1973

Correlation of creep rate with microstructural changes during high temperature creep

The techniques of electron microscopy were used to examine the microstructural changes which occur during primary creep for two important types of engineering alloys: (1) alloys strengthened by solid-solution additions, and (2) dispersion-strengthened alloys. The metals chosen for study are unalloyed titanium, Ti-6Al-4V, and the cobalt-base alloy, Haynes 188. Results to date on NGR 47-004-108 show that development of prior dislocation substructure in Haynes 188 by 10% prestrain and annealing for one hour at 1800 F increases the time to reach 0.5% creep strain at 1600 F by more than an order of magnitude for creep stresses from 3 to 20 ksi. For creep at 1800 F, similar results were obtaind for stresses above 7 ksi, but the prior substructure decreases creep resistance below 7 ksi. This effect appears to be related to instability of grain structure at 1800 F in prestrained material.

Young, C. T.↗
DOE OSTI2026

TEM Approaches for Microstructure-Informed Prediction of Mechanical Properties in Structural Alloys

Predicting the mechanical performance of structural alloys from their evolving microstructure remains a major challenge in materials science, particularly for nuclear structural materials, where irradiation-induced defects span multiple types and length scales and interact through complex mechanisms. The dispersed barrier hardening (DBH) [1] and Friedel–Kroupa–Hirsch (FKH) [2,3] models have been widely used to evaluate the hardening contributions of individual obstacles and to estimate tensile strength from quantified microstructures; however, when multiple size-dependent obstacles coexist and evolve, predicting temperature-dependent tensile strength becomes significantly more complex, and a fully consistent hardening model is still lacking. Transmission electron microscopy (TEM) plays a central role in refining hardening models and enabling predictive assessments of tensile strength evolution by providing quantitative characterization of dislocations, irradiation-induced defects (e.g., dislocation loops and cavities), precipitates, and grain structure (Fig. 1.). These experimentally measured defect densities are incorporated into physically based hardening models with size- and shape- dependent obstacle strengths [4], using root-sum-square superposition for obstacles of comparable strength and linear superposition for dissimilar ones [5]. In addition, recent advances in TEM [6-8], including high-resolution imaging, 4D-STEM strain mapping, EDS/EELS elemental analysis, and flash-polishing-based TEM specimen preparation and extraction-replica methods (Fig. 2), further improve the accuracy of microstructural quantification. By comparison with prior studies as well as our own results, we show that when TEM-derived microstructural information is carefully integrated with physically grounded hardening models, yield strength (or irradiation-induced hardening) measured at room temperature can be predicted with good quantitative agreement across multiple alloy classes. In-situ TEM combined with high-temperature mechanical testing represents an important next step for refining hardening models by directly probing dislocation–obstacle interactions across varying irradiation doses and temperatures [9]. Because the barrier strength factor (α) depends on both temperature and obstacle size, it should not be treated as a constant fitting parameter; rather, it must be explicitly evaluated to achieve physically meaningful predictions of mechanical behaviour at operating temperatures. This presentation therefore discusses why all strengthening contributions (e.g., Peierls stress, solid-solution strengthening, voids, bubbles, dislocation loops, dislocation lines, and grain boundaries) must be considered collectively, why appropriate superposition methods are essential when obstacles possess different barrier strength factors, how hardness measurements can be meaningfully related to tensile properties, and how TEM-derived microstructural information can be systematically incorporated into hardening models. More broadly, it outlines a pathway toward microstructure-informed prediction of mechanical properties and supports the goal of establishing science-based tools for evaluating structural materials in extreme environments [10].

Lin, Yan-Ru [ORNL] (ORCID:0000000339991473)↗
NASA NTRS1989

Chemical profiling of silicon nitride structures

X ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), and scanning electron microscopy (SEM) were used to study structural and chemical inhomogeneities in several electronic materials and device structures of relevance to radiation hard electronics. The systems studied include metal nitride oxide semiconductor (MNOS) structures, silicon oxynitride (SiO(x)N(y)) formed by the thermal nitridation of SiO2, and semiconductor on insulator (SOI) structures. Studies of MNOS structures suggest that the effect of H2 annealing is to make the Si3N4/SiO2 interface less abrupt by causing interdiffusion of silanol and silamine groups with subsequent oxynitride formation. Another effect of the annealing appears to be to relieve the strain at the SiO2/Si interface.

Vasquez, R. P.↗
NASA NTRS1999

Fabrication of Pop-up Detector Arrays on Si Wafers

High sensitivity is a basic requirement for a new generation of thermal detectors. To meet the requirement, close-packed, two-dimensional silicon detector arrays have been developed in NASA Goddard Space Flight Center. The goal of the task is to fabricate detector arrays configured with thermal detectors such as infrared bolometers and x-ray calorimeters to use in space fliGht missions. This paper focuses on the fabrication and the mechanical testing of detector arrays in a 0.2 mm pixel size, the smallest pop-up detectors being developed so far. These array structures, nicknamed "PUDS" for "Pop-Up Detectors", are fabricated on I pm thick, single-crystal, silicon membranes. Their designs have been refined so we can utilize the flexibility of thin silicon films by actually folding the silicon membranes to 90 degrees in order to obtain close-packed two-dimensional arrays. The PUD elements consist of a detector platform and two legs for mechanical support while also serving as electrical and thermal paths. Torsion bars and cantilevers connecting the detector platform to the legs provide additional flexures for strain relief. Using micro-electromechanical structure (MEMS) fabrication techniques, including photolithography, anisotropic chemical etching, reactive-ion etching, and laser dicing, we have fabricated PLTD detector arrays of fourteen designs with a variation of four parameters including cantilever length, torsion bar length and width, and leg length. Folding tests were conducted to test mechanical stress distribution for the array structures. We obtained folding yields and selected optimum design parameters to reach minimal stress levels. Computer simulation was also employed to verify mechanical behaviors of PUDs in the folding process. In addition, scanning electron microscopy was utilized to examine the flatness of detectors and the alignment of detector pixels in arrays. The fabrication of thermistors and heaters on the pop-up detectors is under way, preparing us for the next step of the experiment, the thermal test.

Li, Mary J.↗
DOE OSTI2026

Temperature-Dependent Sn Incorporation and Defect Formation in Pseudomorphic SiSn Layers on Si (001) via Molecular Beam Epitaxy

SiSn alloys have attracted growing interest for group-IV bandgap engineering, although their epitaxial growth remains challenging due to the extremely low equilibrium solubility of Sn in Si. In this work, fully strained (pseudomorphic) SiSn epitaxial layers were grown on Si (001) substrates by means of molecular beam epitaxy. A systematic investigation reveals a strong inverse correlation between growth temperature and Sn incorporation efficiency. Despite a constant Sn flux, the incorporated Sn composition decreases from 5.5% to 3.2% as the growth temperature increases, indicating a pronounced temperature dependence of Sn incorporation. Reflection high-energy electron diffraction indicates a gradual transition of the growth from two-dimensional to three-dimensional with increasing film thickness. Structural characterization by means of X-ray diffraction, atomic force microscopy, and transmission electron microscopy confirms the pseudomorphic growth and smooth surface morphology and reveals twins and stacking faults near the surface region. These results establish a quantitative reference for SiSn growth kinetics and provide guidance for future studies of SiSn and SiGeSn alloys in silicon-compatible electronic and optoelectronic applications.

SiSn alloys↗
NASA NTRS1992

Surface morphology of molecular-beam epitaxially grown Si(1-x)Ge(x) layers on (100) and (110) Si

The surface morphology and dislocation structure of Si(1-x)Ge(x) layers grown on (100) and (110) Si substrates have been investigated using atomic force microscopy, and scanning and transmission electron microscopy. The layers, which have up to a 1.2 percent lattice mismatch with the substrates, were grown by molecular-beam epitaxy at 550 C at thicknesses above those required for the introduction of dislocations. Si(1-x)Ge(x) layers grown on (100) show a crosshatch morphology which is correlated to the underlying misfit dislocation network. Annealing greatly enhances the surface roughness producing a partial islanding growing on the preexisting crosshatch morphology. On the (110) substrates no annealing is necessary to produce a roughened surface. The roughened surface morphology is analyzed as a strain-reducing growth mode which enables partial relaxation of the near-surface atomic planes.

Pike, W. T.↗
DOE OSTI2025

Examples of X-Ray Characterization Techniques in Energy Storage Research

Lithium-ion batteries have revolutionized the portable electronics and transportation sectors. Their performance is often critically dependent on the crystal structures of the anode and cathode electrode materials, which must enable the transport and reversible storage of lithium ions into and out of the lattice. Because lithium is a low-Z element, characterization of materials for lithium-ion batteries can be particularly challenging. Regardless, X-ray techniques enable analysis of material structures to better understand how battery materials perform and degrade, particularly when combined with other materials characterization and electrochemical characterization techniques. While X-ray techniques are most often used in battery research for phase identification of crystal structures, X-ray characterization techniques are also used for a wide variety of other purposes. I will discuss several examples from my research with various collaborators on several projects that highlight the impact that X-ray characterization techniques can have on battery research. The first example will focus on low-temperature microwave-assisted solvothermal synthesis of vanadium-doped LiFePO4 cathode materials for lithium-ion batteries. (1,2) Through a combination of electrochemical and materials characterization, we determined that low temperature synthesis resulted in metastable phases that enabled incorporation of higher dopant levels than resulting from high-temperature synthesis of thermodynamically stable phases. Rietveld refinement of X-ray diffraction data enabled understanding of how lattice parameters changed with doping levels and synthesis temperature. X-ray absorption near edge spectroscopy enabled understanding of the vanadium and iron oxidation states to confirm how vacancies in the structure caused by doping were charge compensated. This was important to understand because the literature suggests doping can improve LiFePO4 electrical conductivity, which improves battery charge and discharge rates. The second example will focus on understanding residual strain in lithium metal anodes. Lithium-ion batteries typically use graphite anodes, but the charge-storage capacity can be theoretically improved ~10x by using lithium metal as the anode material instead. However, lithium anodes suffer from growth of high-aspect-ratio features, such as dendrites, that can pierce nanoporous polymer separators and lead to short circuits and fires. External pressure is commonly applied to cells to enable better morphological control. We hypothesized that applied pressure may promote strain and possibly work hardening during electrochemical cycling, which motivated us to look for evidence of residual strain in lithium metal cycled under applied pressure using X-ray diffraction and sin2(..psi..) analysis. We found that lithium electrodeposited under high pressure exhibited in-plane compressive strain and that that lithium electrodeposited under low pressure did not. (3) The residual strain that accompanies electrodeposition under high pressure may lead to work hardening, which may explain how a soft metal like lithium can puncture separators and why higher pressure does not always decrease short circuits. (4-6) References: 1) Harrison, K. L.; Manthiram, A. Microwave-Assisted Solvothermal Synthesis and Characterization of Metastable LiFe1- x (VO) x PO4 Cathodes. Inorganic chemistry 2011, 50(8), 3613-3620. 2) Harrison, K. L.; Bridges, C. A.; Paranthaman, M. P.; Segre, C. U.; Katsoudas, J.; Maroni, V. A.; Idrobo, J. C.; Goodenough, J. B.; Manthiram, A. Temperature Dependence of Aliovalent-Vanadium Doping in LiFePO4 Cathodes. Chemistry of Materials 2013, 25(5), 768-781. 3) Rodriguez, M. A.; Harrison, K. L.; Goriparti, S.; Griego, J. J.; Boyce, B. L.; Perdue, B. R. Use of a Be-Dome Holder for Texture and Strain Characterization of Li Metal Thin Films via Sin2 (..psi..) Methodology. Powder Diffraction 2020, 35(2), 89-97. 4) Jungjohann, K. L.; Gannon, R. N.; Goriparti, S.; Randolph, S. J.; Merrill, L. C.; Johnson, D. C.; Zavadil, K. R.; Harris, S. J.; Harrison, K. L. Cryogenic Laser Ablation Reveals Short-Circuit Mechanism in Lithium Metal Batteries. ACS Energy Letters 2021, 6(6), 2138-2144. 5) Harrison, K. L.; Merrill, L. C.; Long, D. M.; Randolph, S. J.; Goriparti, S.; Christian, J.; Warren, B.; Roberts, S. A.; Harris, S. J.; Perry, D. L. Cryogenic Electron Microscopy Reveals That Applied Pressure Promotes Short Circuits in Li Batteries. Iscience 2021, 24(12). 6) Harrison, K. L.; Goriparti, S.; Merrill, L. C.; Long, D. M.; Warren, B.; Roberts, S. A.; Perdue, B. R.; Casias, Z.; Cuillier, P.; Boyce, B. L. Effects of Applied Interfacial Pressure on Li-Metal Cycling Performance and Morphology in 4 M LiFSI in DME. ACS Applied Materials & Interfaces 2021, 13(27), 31668-31679.

batteries↗
DOE OSTI2026

Substrate-Directed Dimensional and Phase Control of Peptide Assemblies on Two-Dimensional van der Waals Materials

Understanding and controlling biomolecular self-assembly on van der Waals (vdW) materials has the potential to advance hybrid bioelectronic devices by enabling precise tuning of the interface and modulation of the resulting electronic properties of the biomolecule-vdW heterostructure. However, how surface properties of vdW materials direct biomolecule assembly remains poorly understood. To fill this knowledge gap, we investigated the assembly of a peptide known to assemble into two-dimensional (2D) crystalline films on MoS 2 on three representative vdW surfaces: WS 2 , MoS 2 , and highly oriented pyrolytic graphite (HOPG). Using in situ atomic force microscopy (AFM), we find that assembly is substrate-dependent, resulting in multilayers on WS 2 , monolayers on MoS 2 , and multiple coexisting phases on HOPG. WS 2 exhibits a higher negative charge, strong long-range electrostatic interactions, and extensive hydration layering that may promote multilayer stacking. In contrast, MoS 2 has stronger short-range interactions with the peptides but much weaker long-range interactions and hydration structure, which may favor monolayer formation. Molecular dynamics simulations predict a corresponding switch from monolayer to multilayer aggregates of the adsorbed monomers, reflected in their relative mobilities. On hydrophobic HOPG, the peptides bind most strongly and remain as monomers with high surface mobility. The peptide dimers comprising the basic unit of the crystals are more compact on HOPG, which has a smaller lattice constant than WS 2 or MoS 2 , suggesting strain contributes to stabilizing multiple phases. Our results provide mechanistic insights into how surface charge and hydration structure, and the lattice structure of the substrates governs peptide assembly on vdW materials, offering a framework to rationally control the 2D peptide-vdW heterostructures.

Molecular dynamics simulations↗
DOE OSTI2024

Imaging Ferroelastic Domain Walls in Hybrid Improper Ferroelectric Sr 3 Sn 2 O 7

For this work, we combined synchrotron-based near field infrared spectroscopy and atomic force microscopy to image the properties of ferroelastic domain walls in Sr 3 Sn 2 O 7 . Although frequency shifts at the walls are near the limit of our sensitivity, we can confirm semiconducting rather than metallic character and widths between 20 and 60 nm. The latter is significantly narrower than in other hybrid improper ferroelectrics like Ca 3 Ti 2 O 7 . We attribute this trend to the softer lattice in Sr 3 Sn 2 O 7 , which may enable the octahedral tilt and rotation order parameters to evolve more quickly across the wall without significantly increased strain. These findings are crucial for the understanding of phononic properties at interfaces and the development of domain wall-based devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Gas-mediated defect engineering in earth-abundant Mn-rich layered oxides for non-aqueous sodium-based batteries

Gases are often by-products of battery materials during cell formation and degradation, affecting the cycle life and safety of rechargeable batteries. However, understanding gas-mediated (electro)-chemical reactions and nanoscale structural transformations during the synthesis of battery electrode materials remains challenging because of the lack of suitable characterization routes and the complexity of the interplay between thermodynamics and kinetics. Here, in this study, we use operando synchrotron X-ray diffraction, in situ transmission X-ray microscopy and multiscale modelling to elucidate the reaction pathways and microstructural defect development of earth-abundant Mn-rich layered oxides as positive electrode materials for sodium-based batteries. In particular, we demonstrate the dominant role of CO 2 over O 2 and H 2 O (g) in modulating the competition between entropy and enthalpy during solid-state synthesis. Using Ni 0.25 Mn 0.75 CO 3 as a model precursor, we reveal that CO 2 generation favours the formation of entropy-driven metastable intermediates, suppresses closed pore/nanovoids formation and decreases chemical heterogeneity and residual lattice strain of Mn-rich layered oxides during the synthesis. This result motivates a fast-sintering strategy to promote CO 2 release, which ultimately leads to improved chemo-mechanical and electrochemical stability of the Mn-rich positive electrodes when tested in non-aqueous Na metal coin cells.

36 MATERIALS SCIENCE↗
NASA NTRS2008

Joining of Zirconium Diboride-Based Ceramic Composites to Metallic Systems for High-Temperature Applications

Three types of hot-pressed zirconium diboride (ZrB2)-based ultra-high-temperature ceramic composites (UHTCC), ZrB2-SiC (ZS), ZrB2-SiC-C (ZSC), and ZrB2-SCS9-SiC (ZSS), were joined to Cu-clad-Mo using two Ag-Cu brazes (Cusil-ABA and Ticusil, T(sub L) approx.1073-1173 K) and two Pd-base brazes (Palco and Palni, T(sub L) approx.1493-1513 K). Scanning Electron Microscopy (SEM) coupled with energy-dispersive spectroscopy (EDS) revealed greater chemical interaction in joints made using Pd-base brazes than in joints made using Ag-Cu based active brazes. The degree of densification achieved in hot pressed composites influenced the Knoop hardness of the UHTCC and the hardness distribution across the braze interlayer. The braze region in Pd-base system displayed higher hardness in joints made using fully-dense ZS composites than in joints made using partially-dense ZSS composites and the carbon-containing ZSC composites. Calculations indicate a small negative elastic strain energy and an increase in the UHTCC's fracture stress up to a critical clad layer thickness . Above this critical thickness, strain energy in the UHTCC is positive, and it increases with increasing clad layer thickness. Empirical projections show a reduction in the effective thermal resistance of the joints and highlight the potential benefits of joining the UHTCC to Cu-clad-Mo.

Asthana, R.↗
DOE OSTI2026

Atomic Evolution of Hydrogen Intercalation Wave Dynamics in Palladium Nanocrystals Revealed by Liquid-Phase Transmission Electron Microscopy

Solute-intercalation-induced phase separation creates spatial heterogeneities in host materials, a phenomenon ubiquitous in batteries, hydrogen storage, and other energy devices. Despite many efforts, probing intercalation processes at the atomic scale has been a significant challenge. By utilizing liquid-phase transmission electron microscopy (TEM), we study hydrogen (de)intercalation in palladium nanocrystals as a model system and have achieved unprecedented atomic-resolution imaging of hydrogen intercalation wave dynamics. Our observations reveal that intercalation wave mechanisms, instead of shrinking-core mechanisms, prevail at ambient temperature for palladium nanocubes ranging from ∼60 nm down to ∼10 nm. Systematic image analysis uncovers the atomic evolution of the hydrogen intercalation wave, transitioning from nonplanar and inclined boundaries to those closely aligned with {100} planes. Our kinetic Monte Carlo simulations demonstrate that the observed intercalation wave dynamics correspond to sorption pathways minimizing the lattice mismatch strain at the phase boundary. In conclusion, unveiling the atomic intercalation pathways holds profound implications for engineering intercalation-mediated devices and advancements in energy sciences.

Lee, Daewon [Lawrence Berkeley National Laboratory↗
DOE OSTI2024

Microstructure Clones

Microstructure drives component behavior. Contemporary crystal plasticity studies compare strain measurements of polycrystal specimens to models. Because each specimen is unique, it is impossible to know which differences are significant. In this project, we invented microstructure clones and explored their use in understanding crystal plasticity. Microstructure clones are specimens with nearly identical microstructures, which allows for multiple destructive tests of a microstructure, insight into how a specimen will deform, variability quantification, and the ability to measure the effects of microstructural changes. Several sets of microstructure clones, pure nickel tensile bars, were tested. The techniques of digital image correlation, crystal plasticity finite element analysis, high resolution electron backscatter diffraction, transmission electron microscopy, and dislocation dynamics were used to understand the structural behavior of these microstructures. This work reshapes the fields of crystal plasticity and structure-property relationships by providing a technique to control for specific variables, quantify microstructural stochasticity, and replicate experiments.

36 MATERIALS SCIENCE↗