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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
NASA NTRS1996

TEM Study of Precipitation in a NiAl-3Ti-0.5Hf Single-Crystal Alloy

Samples for transmission electron microscopy (TEM) were prepared from 3 mm diameter cylinders electro-discharge machined from the heat-treated ingots. Slices sectioned from the cylinders were mechanically ground and electrochemically thinned in a twinjet Tenupol-3 polisher. Microstructural and energy-dispersive X-ray spectroscopy (EDXS) studies were conducted in a Philips 400T TEM equipped with a double tilt goniometer and a KEVEX Si/Li X-ray detector.

Garg, A.↗
NASA NTRS2005

TEM and NanoSIMS Study of Hydrated/Anhydrous Phase Mixed IDPs: Cometary or Asteroidal Origin?

Chondritic interplanetary dust particles (IDPs) are subdivided into (1) particles that form highly porous aggregates (chondritic porous "CP" IDPs), and (2) smooth particles ("CS" IDPs). Infrared (IR) spectroscopy has been a valuable tool for non-destructively determining the bulk mineralogy of IDPs. Most IDPs fall within three distinct IR groups: (1) olivine-rich particles, (2) pyroxene-rich particles, and (3) phyllosilicate-rich particles. From the IR studies, IDPs dominated by anhydrous minerals tend to be fine grained (CP), while phyllosilicate-rich IDPs are mostly CS. CP IDPs have been linked to cometary sources based on their compositions, spectral properties, and atmospheric entry velocities. Since no spectral signatures of hydrated minerals have been detected in comets, CS IDPs are thought to derive from primitive asteroids. Transmission electron microscopy (TEM) studies have revealed that the mineralogical distinctions between CP and CS IDPs are not always clear. Previous investigators have reported trace amounts of hydrous minerals in dominantly anhydrous particles. A better understanding of these particles will help to elucidate whether there is a genetic relationship between anhydrous and hydrated IDPs, provide insight into the earliest stages of aqueous alteration of primitive materials, and may help to determine whether comets have experienced any aqueous processing. Here we report a combined TEM and isotopic imaging study of an unusual anhydrous IDP with hydrated phases. Additional information is included in the original extended abstract.

Nakamura, K.↗
NASA NTRS2007

Space Plasma Ion Processing of Ilmenite in the Lunar Soil: Insights from In-Situ TEM Ion Irradiation Experiments

Space weathering on the moon and asteroids results largely from the alteration of the outer surfaces of regolith grains by the combined effects of solar ion irradiation and other processes that include deposition of impact or sputter-derived vapors. Although no longer considered the sole driver of space weathering, solar ion irradiation remains a key part of the space weathering puzzle, and quantitative data on its effects on regolith minerals are still in short supply. For the lunar regolith, previous transmission electron microscope (TEM) studies performed by ourselves and others have uncovered altered rims on ilmenite (FeTiO3) grains that point to this phase as a unique "witness plate" for unraveling nanoscale space weathering processes. Most notably, the radiation processed portions of these ilmenite rims consistently have a crystalline structure, in contrast to radiation damaged rims on regolith silicates that are characteristically amorphous. While this has tended to support informal designation of ilmenite as a "radiation resistant" regolith mineral, there are to date no experimental data that directly and quantitatively compare ilmenite s response to ion radiation relative to lunar silicates. Such data are needed because the radiation processed rims on ilmenite grains, although crystalline, are microstructurally and chemically complex, and exhibit changes linked to the formation of nanophase Fe metal, a key space weathering process. We report here the first ion radiation processing study of ilmenite performed by in-situ means using the Intermediate Voltage Electron Microscope- Tandem Irradiation facility (IVEM-Tandem) at Argonne National Laboratory. The capability of this facility for performing real time TEM observations of samples concurrent with ion irradiation makes it uniquely suited for studying the dose-dependence of amorphization and other changes in irradiated samples.

Christoffersen, R.↗
NASA NTRS2008

TEM Cell Testing of Cable Noise Reduction Techniques From 2 MHz to 200 MHz - Part 1

This paper presents empirical results of cable noise reduction techniques as demonstrated in a TEM cell operating with radiated fields from 2 - 200 MHz. It is the first part of a two-paper series. This first paper discusses cable types and shield connections. In the second paper, the effects of load and source resistances and chassis connections are examined. For each topic, well established theories are compared to data from a real-world physical system. Finally, recommendations for minimizing cable susceptibility (and thus cable emissions) are presented. There are numerous papers and textbooks that present theoretical analyses of cable noise reduction techniques. However, empirical data is often targeted to low frequencies (e.g. <50 KHz) or high frequencies (>100 MHz). Additionally, a comprehensive study showing the relative effects of various noise reduction techniques is needed. These include the use of dedicated return wires, twisted wiring, cable shielding, shield connections, changing load or source impedances, and implementing load- or source-to-chassis isolation. We have created an experimental setup that emulates a real-world electrical system, while still allowing us to independently vary a host of parameters. The goal of the experiment was to determine the relative effectiveness of various noise reduction techniques when the cable is in the presence of radiated emissions from 2 MHz to 200 MHz. The electronic system (Fig. 1) consisted of two Hammond shielded electrical enclosures, one containing the source resistance, and the other containing the load resistance. The boxes were mounted on a large aluminium plate acting as the chassis. Cables connecting the two boxes measured 81 cm in length and were attached to the boxes using standard D38999 military-style connectors. The test setup is shown in Fig. 2. Electromagnetic fields were created using an HP8657B signal generator, MiniCircuits ZHL-42W-SMA amplifier, and an EMCO 5103 TEM cell. Measurements were taken using an Agilent E4401B spectrum analyzer and HP1141a differential probes.

Bradley, Arthur T.↗
NASA NTRS2009

Effectiveness of Shield Termination Techniques Tested with TEM Cell and Bulk Current Injection

This paper presents experimental results of the effectiveness of various shield termination techniques. Each termination technique is evaluated by two independent noise injection methods; transverse electromagnetic (TEM) cell operated from 3 MHz 400 MHz, and bulk current injection (BCI) operated from 50 kHz 400 MHz. Both single carrier and broadband injection tests were investigated. Recommendations as to how to achieve the best shield transfer impedance (i.e. reduced coupled noise) are made based on the empirical data. Finally, the noise injection techniques themselves are indirectly evaluated by comparing the results obtained from the TEM Cell to those from BCI.

Bradley, Arthur T.↗
NASA NTRS2020

Coordinated NanoSIMS and TEM Analysis of a Large 26Mg-Rich AGB Silicate from the Meteorite Hills 00426 CR2 Chondrite

Silicates are one of the most abundant presolar phases around evolved stars, in the inter-stellar medium (ISM), and in our Solar System. These grains afford the opportunity for O, Si, Mg, Fe, and Ca isotopic analyses to constrain stellar nucleosynthetic and mixing processes, and Galactic chemical evolution (GCE). While Mg and Fe isotopic studies have been successfully conducted on presolar silicates, isotopic analyses beyond O and Si are often hampered by the small grain sizes (average ~250 nm). This also makes coordinated mineral and chemical characterization challenging. These studies provide insight into the dust condensation conditions as well as subsequent alteration in the ISM and/or the Solar System. TEM studies of presolar silicates have shown that they are much more mineralogically and chemically diverse than other presolar phases [1 and references therein]. Large (>500nm) presolar silicate grains are rare, but they allow for detailed isotopic, mineral, and chemical characterization. We identified a large presolar silicate grain in the MET 00426 CR2 chondrite and report the O, Si, Mg, and Fe isotopic compositions and TEM study of this grain.

Nguyen, A. N.↗
NASA NTRSDate not supplied

The Zircon-Reidite Shock Transformation: A Tem Study of Reidite Produced at A Newly Established 21.2 GPa Shock Pressure Threshold

The high-pressure polymorph of zircon (Zr2SiO4) is reidite, a phase with the scheelite structure that was first discovered to form at ca. 12 GPa in static high-pressure experiments [1]. Reidite was subsequently found to occur in naturally shocked zircons from several terrestrial impact localities [2,3], as well as in shock recovery-reverberation experiments performed above 20 GPa [4]. The nature and distribution of reidite occurrences in terrestrial impact localities has pointed to its potential use as a shock pressure indicator, as well as to the importance of understanding its age-reset effects in zircon geochronology [3]. In this study we have used coordinated SEM/Electron Backscatter Diffraction (EBSD) and Field-Emission Scanning Transmission Electron Microscopy (FE-STEM) to study the micro- and nanostructure of reidite and its shocked zircon host produced at 21.2 GPa under experimental shock recovery/reverberation conditions [5]. Our results document the TEM microstructure of reidite formed at a 21.2 GPa experimental shock pressure that is significantly lower than that observed in previous studies [4]. At these conditions the sample developed a diverse set of microstructures that have not been previously documented on the TEM scale.

shock metamorphism↗
NASA NTRS2022

Development of a Loop Antenna Deployment System for TEM-Based Subsurface Mars Water Detection

The subsurface of Mars has the potential to harbor existing deposits of liquid water, which are of great interest both scientifically (in the search for life) and as resources for future astronauts living on the red planet. However, the depth to a potential subsurface aquifer may be kilometers deep, which is well beyond what current surface or orbital approaches can survey while also confirming the unique signature for liquid water. Inspired by critical technology for exploring deep aquifers on Earth, we are developing the Transient H2O Reconnaissance (TH2OR) instrument at NASA’s Jet Propulsion Laboratory (JPL). TH2OR operates on the principle of transient electromagnetics (TEM), which leverages induction and electromotive force to induce a current in a subsurface water body using a loop-shaped antenna that provides both transmit and receive functions when placed on the surface. On Mars, TEM may be even more effective given the relative dryness of the subsurface compared to a more conductive, saline, liquid, water body on Earth. However, to probe deep within the subsurface (below 5 km) a large enclosed antenna is needed – specifically, a 100-m diameter effective loop or a shape with roughly equivalent area that can transmit at low frequencies (kHz-Hz). The deployment of a large-scale structure on the surface is complicated by the fact that the transmit wire must be both lightweight and robust to contact with the surface. Further, TH2OR may be delivered to the surface by a non-mobile vehicle, so it is desired that the deployment can be activated from a static location. This paper provides an overview of the deployment trade study, focusing on our current, favored approach, using a projectile wire launcher. Building on past approaches in the literature, we have developed and fielded an Earth-based, gas-projectile prototype for launching a triangle-shaped antenna onto analogue terrain. Our results compare simulated launch performance to actual field tests conducted under Earth gravity and pressure conditions. We discuss how Earth performance maps to a prospective Mars deployment under reduced gravity and pressure. We also provide lessons learned and next steps towards the development of an integrated TH2OR instrument for finding water on Mars.

Stamenkovic, Vlada↗
DOE OSTI2025

Ex-situ Heat Treatment of TEM Foils in a Custom Titanium Fixture: A Case Study on Ni-based Superalloy

The advancement of microstructural characterization at the nanoscale is critical to understanding the microstructural evolution and performance of engineering materials. Transmission electron microscopy (TEM) plays a vital role in such investigations, particularly when coupled with controlled ex- and in-situ experiments. In this study, we introduce a novel method for ex-situ heat treatment (HT) of TEM foils using a custom-designed fixture, made from pure titanium, and vacuum furnace to inhibit oxidation. This approach ensures precise temperature control and minimal sample contamination during HT, critical for substructural characterization and analysis of metallic materials. The fixture consists of a titanium base with three slits, for three sample foils, and a titanium cap for closure. The entire assembly is placed in a vacuum heat treatment furnace with high vacuum capability to prevent oxidation. To validate the effectiveness of the setup, precipitation behavior and microstructural changes were studied in an IN725 variant heat-treated at 500°C for 1 hour and 282 variant heat-treated at 700°C for 1 hour, as case studies.

electron microscopy↗
DOE OSTI2024

Nanocompression of 20 nm Silver Nanoparticles: In situ Aberration‐Corrected TEM and Atomistic Simulations

Single‐crystalline nanoparticles play an increasingly important role in a wide variety of fields including pharmaceuticals, advanced materials, catalysts for fuel cells, energy materials, as well as environmental detection and monitoring. Yet, the deformation mechanisms of very small nanoparticles are still poorly understood, in particular the role played by single dislocations and their interaction with surfaces. Here, in this work, silver nanoparticles with particularly small dimensions (≈20 nanometers in diameter) are compressed in situ in an aberration‐corrected transmission electron microscopy (TEM) and molecular dynamics (MD) simulations. During compression, the emergence of both dislocations and nanotwins are observed. However, these defects prove to be unstable and disappear upon removal of the indenter. Atomistic simulations confirm the role played by image stresses associated with the nearby surfaces and the reduction in dislocation line length as it approaches the free surface, thereby supporting the experimental observations. These results provide justification for the frequent observation of the absence of dislocations in nanoparticles of a few nanometers in size during in situ experiments, even after significant deformation. This phenomenon contributes to the self‐healing of samples through dislocation ejection toward the surfaces.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Large scale polymer toughening of two-dimensional materials revealed by in situ TEM fracture tests and multiscale simulations

Two-dimensional (2D) materials offer significant potential for applications in energy-harvesting devices, batteries, sensors, and transistors. However, their intrinsic brittleness makes them prone to mechanical failure, limiting their practical use. In this work, we perform in situ transmission electron microscopy (TEM) fracture tests on monolayer MoSe2 and uncover an extrinsic toughening effect induced by an ultrathin adsorbed polystyrene adlayer. This adlayer substantially enhances the fracture resistance of the 2D flakes. Through a combination of molecular dynamics simulations and finite element analysis, we elucidate the molecular mechanism behind this toughening effect. Further, it arises from the active crack-bridging behavior of entangled polymer chains and the formation of a fracture process zone that stabilizes crack propagation and increases the energy required for crack extension. The proposed toughening mechanism offers a pathway to improving the mechanical reliability of 2D material-based devices by mitigating the risk of sudden failure.

2D materials↗
DOE OSTI2026

Cross-slip and easy-glide CRSS in titanium: Theoretical predictions and in-situ TEM measurements

This study investigates the mechanics of prismatic and first-order pyramidal $\langle$a$\rangle$ slip in titanium (Ti), elucidating the physics of easy-glide and cross-slip through a combination of theory and experiments. Screw-character prismatic (Pr) dislocations in Ti are of particular interest because their complex cores can be stable or unstable, leading to activation by either cross-slip or planar glide. To investigate these mechanisms, site-specific micro tensile samples were prepared using focused ion beam (FIB) milling and mounted on a push-to-pull (PTP) device for in-situ transmission electron microscopy (TEM) tensile testing. The in-situ experiments provide direct observations of the onset of dislocation motion and the precise determination of the critical resolved shear stress (CRSS) for the activated mechanisms, and its evolution with load cycling. A comprehensive theory has been developed to predict the CRSS values for easy glide, cross-slip, and multiplication of dislocations. Predicted critical stresses for pyramidal (π)-to-Pr and reverse cross-slip agree closely with the experimental measurements. The latter cross-slip stress is a factor of two higher than that of unobstructed planar slip. The model accounts for overlapping dislocation cores and employs a Wigner-Seitz based cell to evaluate misfit energies. By combining ab initio density functional theory (DFT) with anisotropic elasticity, the framework identifies minimum energy pathways for dislocation glide, which can be intermittent and zig-zag. A simplified expression utilizing (π) and Pr Schmid factor ratios is proposed for critical stress corresponding to (π)-to-Pr cross-slip transition. The results are strongly dependent on crystal orientation, underscoring non-Schmid behavior. Overall, this study explores key critical stress parameters essential for informing higher-scale simulations of plasticity in Ti.

Critical stress↗
DOE OSTI2020

The effects of vanadium substitution on one-dimensional tunnel structures of cryptomelane: Combined TEM and DFT study

Rational design of energy storage materials requires mechanistic understanding which relies on atomic scale characterization of structure and defects. In this paper we utilize vanadium (V)-substituted one-dimensional cryptomelane as a model material to study structural features critical to electrochemical reversibility of the cathode in lithium-ion batteries. We found the substitution of manganese (Mn) atoms in the tunnel wall with V enhances structural uniformity in the parent KMn 8 O 16 material by inhibiting formation of irregular (2 × 3 and 2 × 1) manganese oxide tunnel structures. Upon lithiation, both transmission electron microscopy (TEM) and density functional theory (DFT) reveal significant structural evolution, eventually resulting in phase separation and formation of highly reduced manganese oxide. During this process, Mn 4+ accepts electrons donated by intercalated Li, while the V 4+ substituent is not electrochemically reduced but acts to stabilize the tunnel framework structure. As a result, the V substituted material shows higher operating voltage and improved electrochemical reversibility. Our results highlight the benefits of V-substitution in cryptomelane, and the significance of integrating characterization with simulation for understanding and developing design principles for lithium ion battery materials.

25 ENERGY STORAGE↗
DOE OSTI2020

Sweeping potential regulated structural and chemical evolution of solid-electrolyte interphase on Cu and Li as revealed by cryo-TEM

A fundamental understanding of solid-electrolyte interphase (SEI) is paramount importance for controlling the cycling performance of rechargeable lithium metal batteries. The structural and chemical evolution of SEI with respect to electrochemical operating condition remains barely established. Here we develop a unique method for imaging the evolution of SEI formed on the Cu foil under sweeping electrochemical potential. By using cryogenic TEM imaging combined with energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy electronic structure analyses, we reveal that, for the vinylene carbonate (VC)-free electrolyte, the SEI formed at 1.0 V is a monolithic amorphous structure, which evolves to amorphous matrix embedded with Li 2 O particles as the voltage decreases to 0 V. In the case of VC-containing electrolyte, the SEI is featured by an amorphous matrix with Li 2 O particles from 1.0 V to 0 V. The thickness of SEI formed on Cu foil increases with decreasing voltage. Associated with the localized charge modulation by the surface topographic feature and defects in the Cu foil, the SEI layer shows direct spatial correlation with these structural defects in the Cu. In addition, upon Li deposition, the SEI formed on the Li metal has similar thickness with, but different composition from the SEI formed on the Cu foil at 0 V. Furthermore, those results provide insight toward SEI engineering for enhanced cycling stability of Li metal.

25 ENERGY STORAGE↗
DOE OSTI2025

Site-specific plan-view (S)TEM sample preparation from thin films using a dual-beam FIB-SEM

To fully evaluate the atomic structure, and associated properties of materials using transmission electron microscopy, examination of samples from three non-collinear orientations is needed. This is particularly challenging for thin films and nanoscale devices built on substrates due to limitations with plan-view sample preparation. In this work, a new method for preparation of high-quality, site-specific, plan-view TEM samples from thin-films grown on substrates, is presented and discussed. Here, it is based on using a dual-beam focused ion beam scanning electron microscope (FIB-SEM) system. To demonstrate the method, the samples were prepared from thin films of perovskite oxide BaSnO 3 grown on a SrTiO 3 substrate and metal oxide IrO 2 on a TiO 2 substrate, ranging from 20–80 nm in thicknesses using molecular beam epitaxy. While the method is optimized for the thin films, it can be extended to other site-specific plan-view samples and devices build on wafers. Aberration-corrected STEM was used to evaluate the quality of the samples and their applicability for atomic-resolution imaging and analysis.

BaSnO3↗
DOE OSTI2026

Heterogeneous Corrosion Pathways in Pt–Ni Nanododecahedra Revealed by In Situ Liquid Cell TEM

Unraveling nanoscale corrosion pathways is essential for understanding materials degradation mechanisms and designing corrosion-resistant metal alloys. Here, in this study, we directly visualize the corrosion of Pt–Ni nanododecahedra in 0.1 M HCl using liquid cell TEM. Each nanoparticle features a Ni-rich core and a Pt-rich frame. Our observation reveals that corrosion proceeds in two distinct stages: first the Ni-rich core dissolves without forming porosity, yielding small Pt nanocrystals and transient NiCl 2 ·6H 2 O at the retreating interfaces; then the Pt-rich frame fragments into ∼5 nm Pt 3 Ni nanocrystals that subsequently dissolve uniformly, accompanied by fleeting Pt chlorides. A percolation-based theory explains the observed behaviors: The core’s ∼8% Pt lies below the Pt connectivity threshold, preventing Pt scaffold formation, whereas the frame’s 48% Ni exceeds the Ni percolation threshold and collapses. Ordered Pt 3 Ni suppresses Ni percolation, thereby enforcing uniform dissolution. These findings reveal how composition and structural ordering govern heterogeneous corrosion in Pt–Ni architectured nanoparticles.

Liquid phase TEM↗
NASA NTRSDate not supplied

TEM and XRD Investigation of Impact Glass Alteration Products: Amorphous Materials, Phyllosilicates and Everything in Between

Impact cratering is one of the most ubiquitous geologic processes shaping the surface of all solid bodies in our solar system. Impacts are also a major source of clay minerals and poorly crystalline, clay-like materials on Earth and Mars[1,2].These phyllosilicates and related clay-like phases comprise an incredibly complex group of materials, and their characterization, even in controlled laboratory settings, remains a challenging endeavor. The nature and origin of clay minerals and amorphous materials on Mars, which form a major component (~20-70 wt %) of rock and soil samples in Gale Crater as determined by the CheMin instrument on Curiosity, have remained ambiguous[3]. These amorphous phases likely fall on a spectrum between pristine volcanic and/or impact-produced primary materials and clay minerals and related phases formed from aqueous alteration. Amorphous materials are common weathering products in terrestrial sediments, soils, and paleosols [e.g., 4,5].Primary impact materials (glass, melt rocks)are comparable in some ways to those generated volcanically [6], and so it may be possible that an amorphous component is preserved within altered impactites. There are hundreds of thousands of impact craters on Mars, and Curiosity and Perseverance are currently exploring ancient impact craters. We hypothesize that the sediments and lithologies in Gale and Jezero Craters and elsewhere contain altered impact products; it is therefore important to better understand the composition and structure of these materials. Here we present the first results from a study characterizing materials produced from impact glass alteration–clay minerals, poorly crystalline/amorphous materials–in terrestrial craters using Transmission Electron Microscopy (TEM), powder X-ray diffraction (pXRD)and chemical (EDS) analysis.

Impact crater↗
DOE OSTI2026

In-Situ TEM Molten Salt Corrosion

Molten salt reactors (MSRs) offer a compelling pathway for next-generation nuclear energy, with advantages in thermal efficiency, inherent safety, and flexible fuel management. Yet, halide-based molten salts introduce significant materials challenges, particularly alloy corrosion. Alloy performance in these environments ultimately depends on understanding how corrosion initiates and progresses at the nanoscale, however most existing models rely on post-exposure characterization, leaving degradation mechanisms largely inferred rather than directly observed. NiCr alloys have garnered interest in MSRs applications as the Ni-based matrix provides strength and creep resistance, while Cr content offers oxidation resistance in air. However, NiCr corrosion resistance in chloride salts has proven poor due to preferential chromium dissolution, the formation of Cr-depleted pathways, and grain-boundary attack. This work aims to directly visualize corrosion of Ni-20Cr exposed to LiCl-KCl using in-situ Transmission Electron Microscopy (TEM) to capture real-time microstructural evolution during corrosion. Experiments will be performed at ~800 °C under controlled pressure conditions while utilizing Energy-Dispersive X-ray Spectroscopy (EDS) to analyze elemental redistribution. Observation of chromium depletion fronts, associated surface restructuring, and localized chloride enrichment are expected. Ultimately, this study is expected to provide a link between microscale processes and the macroscopic degradation behaviors relevant to MSR operation in advanced reactor environments. Simultaneously, this approach enables future in-situ investigations regarding alloy composition, salt chemistry, and their influence on corrosion pathways and long-term stability.?

36 - MATERIALS SCIENCE↗