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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 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
NASA NTRS2017

Experimental Hypervelocity Dust Impact in Olivine: FIB/TEM Characterization of Micron-Scale Craters with Comparison to Natural and Laser-Simulated Small-Scale Impact Effects

The space weathering of regoliths on airless bodies and the formation of their exospheres is driven to a large extent by hypervelocity impacts from the high relative flux of micron to sub-micron meteoroids that comprise approximately 90 percent of the solar system meteoroid population. Laboratory hypervelocity impact experiments are crucial for quantifying how these small impact events drive space weathering through target shock, melting and vaporization. Simulating these small scale impacts experimentally is challenging because the natural impactors are both very small and many have velocities above the approximately 8 kilometers-per-second limit attainable by conventional chemical/light gas accelerator technology. Electrostatic "dust" accelerators, such as the one recently developed at the Colorado Center for Lunar Dust and Atmospheric Studies (CCLDAS), allow the experimental velocity regime to be extended up to tens of kilometers-per-second. Even at these velocities the region of latent target damage created by each impact, in the form of microcraters or pits, is still only about 0.1 to 10 micrometers in size. Both field-emission analytical scanning electron microscopy (FE-SEM) and advanced field-emission scanning transmission electron microscopy (FE-STEM) are uniquely suited for characterizing the individual dust impact sites in these experiments. In this study, we have used both techniques, along with focused ion beam (FIB) sample preparation, to characterize the micrometer to nanometer scale effects created by accelerated dust impacts into olivine single crystals. To our knowledge this work presents the first TEM-scale characterization of dust impacts into a key solar system silicate mineral using the CCLDAS facility. Our overarching goal for this work is to establish a basis to compare with our previous results on natural dust-impacted lunar olivine and laser-irradiated olivine.

Christoffersen, R.↗
DOE OSTI2026

Flash electropolishing for TEM: Reducing FIB‐induced defects in tungsten with protocols for new materials

Focused ion beam (FIB) milling has become the dominant approach for site-specific transmission electron microscopy (TEM) specimen preparation; however, FIB damage remains a critical limitation for reliable microstructural characterisation, particularly in radiation effects studies. Tungsten is especially susceptible to FIB damage due to its high nuclear stopping power, which promotes the formation and strong diffraction contrast of FIB-induced ‘black spot’ defects that are indistinguishable from very fine irradiation-induced loops/defects resulting from low to intermediate temperature neutron irradiation. In this work, flash electropolishing is systematically evaluated as a post-FIB treatment for minimising preparation-induced artefacts for TEM analysis of tungsten-based alloys. Using a range of non-, ion-, and neutron-irradiated tungsten materials, the effectiveness of flash electropolishing has been assessed through direct comparison with conventional FIB and plasma-FIB preparation including low-energy Ga, Ar, Xe ion cleaning. The results demonstrate that flash electropolishing effectively removes FIB-damaged layers and ‘black spot’ defects, thereby enabling reliable observation of irradiation-induced dislocation structures. Key processing parameters governing flash electropolishing quality – including lamella thickness, applied voltage, polishing duration, electrolyte chemistry, and cathode geometry – have been systematically evaluated, and clear criteria were established for determining when flash electropolishing is required to ensure reliable microstructural analysis. This work also provides practical guidance for implementing flash electropolishing as an artefact-controlled specimen-preparation approach for TEM characterisation of FIB-produced specimens. The systematic protocol can be extended to other, non-tungsten materials.

TEM sample preparation↗
DOE OSTI2022

Using Xe Plasma FIB for High-Quality TEM Sample Preparation

Here, a direct comparison between electron transparent transmission electron microscope (TEM) samples prepared with gallium (Ga) and xenon (Xe) focused ion beams (FIBs) is performed to determine if equivalent quality samples can be prepared with both ion species. We prepared samples using Ga FIB and Xe plasma focused ion beam (PFIB) while altering a variety of different deposition and milling parameters. The samples’ final thicknesses were evaluated using STEM-EELS $\textit{t/λ}$ data. Using the Ga FIB sample as a standard, we compared the Xe PFIB samples to the standard and to each other. We show that although the Xe PFIB sample preparation technique is quite different from the Ga FIB technique, it is possible to produce high-quality, large area TEM samples with Xe PFIB. We also describe best practices for a Xe PFIB TEM sample preparation workflow to enable consistent success for any thoughtful FIB operator. For Xe PFIB, we show that a decision must be made between the ultimate sample thickness and the size of the electron transparent region.

47 OTHER INSTRUMENTATION↗
NASA NTRS2007

Probing the Depths of Space Weathering: A Cross-sectional View of Lunar Rock 76015

The term "space weathering" refers to the cumulative effects of several processes operating at the surface of any solar system body not protected by a thick atmosphere. These processes include cosmic and solar ray irradiation, solar wind implantation and sputtering, as well as melting and vaporization due to micrometeorite bombardment. Space weathering discussions have generally centered around soils but exposed rocks will also incur the effects of weathering. Rocks have much longer surface lifetimes than an individual soil grain and thus record a longer history of exposure. By studying the weathering products which have built up on a rock surface, we can gain a deeper perspective on the weathering process and better assess the relative importance of various weathering components. The weathered coating, or patina, of the lunar rock 76015 has been previously studied using SEM and TEM. It is a noritic breccia with both "glazed" (smooth glassy) and "classic" (microcratered and pancake-bearing) patina coatings. Previous TEM work on 76015 relied on ultramicrotomy to prepare cross sections of the patina coating, but these sections were limited by the "chatter" and loss of material in these brittle samples. Here we have used a focused ion beam (FIB) instrument to prepare cross sections in which the delicate stratigraphy of the patina coating is beautifully preserved.

Noble, Sarah K.↗
NASA NTRS2012

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Kim, Hyun Jung↗
DOE OSTI2024

In-Plane Liftout and Push-to-Pull for In Situ Mechanical Testing of Irradiated Inconel X-750

A streamlined sample preparation method for nanomechanical testing is needed to improve the quality of specimens, reduce the cost, and increase the versatility of specimen fabrication. This work outlines an in-plane liftout focused ion beam (FIB) fabrication procedure to prepare electron-transparent specimens for in situ transmission electron microscopy (TEM) nanomechanical testing. Ion etching and electron backscatter diffraction (EBSD) techniques were used to lift out a [110] oriented grain from a neutron-irradiated bulk X-750 alloy. Careful control of voltages and currents ensured precision. Top surface thinning sweeps prevented resurfacing and redeposition while dog-bone geometries were shaped with a 1:4 gauge width-to-milling pattern diameter ratio. Nanotensile testing in the TEM with a picoindenter allowed for the estimation of an ultimate tensile strength of 2.41 GPa, and inspection revealed a high density of bubbles in the X-750 matrix. The proposed fabrication procedure is significant for preparing samples from radioactive materials, studying complex structures that are orientation-dependent, and analyzing desired planar areas.

36 MATERIALS SCIENCE↗
NASA NTRS2004

Focused Ion Beam Recovery and Analysis of Interplanetary Dust Particles (IDPs) and Stardust Analogues

Meteoritics research is a major beneficiary of recent developments in analytical instrumentation [1,2]. Integrated studies in which multiple analytical techniques are applied to the same specimen are providing new insight about the nature of IDPs [1]. Such studies are dependent on the ability to prepare specimens that can be analyzed in multiple instruments. Focused ion beam (FIB) microscopy has revolutionized specimen preparation in materials science [3]. Although FIB has successfully been used for a few IDP and meteorite studies [1,4-6], it has yet to be widely utilized in meteoritics. We are using FIB for integrated TEM/NanoSIMS/synchrotron infrared (IR) studies [1].

Graham, G. A.↗
DOE OSTI2020

A lathe system for micrometre-sized cylindrical sample preparation at room and cryogenic temperatures

A simple two-spindle based lathe system for the preparation of cylindrical samples intended for X-ray tomography is presented. The setup can operate at room temperature as well as under cryogenic conditions, allowing the preparation of samples down to 20 and 50 µm in diameter, respectively, within minutes. Case studies are presented involving the preparation of a brittle biomineral brachiopod shell and cryogenically fixed soft brain tissue, and their examination by means of ptychographic X-ray computed tomography reveals the preparation method to be mainly free from causing artefacts. Since this lathe system easily yields near-cylindrical samples ideal for tomography, a usage for a wide variety of otherwise challenging specimens is anticipated, in addition to potential use as a time- and cost-saving tool prior to focused ion-beam milling. Fast sample preparation becomes especially important in relation to shorter measurement times expected in next-generation synchrotron sources.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Thermal conductivity measurement of the interaction layer between UMo and Al produced by high-energy heavy ion irradiation

In this work, we report the first direct thermal conductivity measurement results for Al-UMo interaction layer (IL), which is typically observed in UMo/Al dispersion fuel plates under irradiation. The investigated IL was formed by irradiating Al coated UMo substrate using 80 MeV iodine ions at 180 degrees C up to 3.03 x 10 17 ions/cm 2 fluence. Microstructural characterization indicated that the induced IL is amorphous with an approximately (U 0.8 ,Mo 0.2 )Al 5.3 stoichiometry, which is similar to that formed under in-pile irradiation. Focused ion beam (FIB) was used to prepare nine specimens of various lengths from the IL that could be suspended across a microfabricated device for thermal conductivity measurement. The measured thermal conductivity values of the IL were significantly lower than the values for both the original UMo fuel and the Al. The successful measurement of the Al-UMo IL provides valuable information for the development and qualification of UMo/Al dispersion fuels for research and test reactor conversion applications, and further demonstrates the promising capabilities of utilizing the suspended bridge method in nuclear fuel research.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2015

Characterization of Meteorites by Focused Ion Beam Sectioning: Recent Applications to CAIs and Primitive Meteorite Matrices

Focused ion beam (FIB) sectioning has revolutionized preparation of meteorite samples for characterization by analytical transmission electron microscopy (TEM) and other techniques. Although FIB is not "non-destructive" in the purest sense, each extracted section amounts to no more than nanograms (approximately 500 cubic microns) removed intact from locations precisely controlled by SEM imaging and analysis. Physical alteration of surrounding material by ion damage, fracture or sputter contamination effects is localized to within a few micrometers around the lift-out point. This leaves adjacent material intact for coordinate geochemical analysis by SIMS, microdrill extraction/TIMS and other techniques. After lift out, FIB sections can be quantitatively analyzed by electron microprobe prior to final thinning, synchrotron x-ray techniques, and by the full range of state-of-the-art analytical field-emission scanning transmission electron microscope (FE-STEM) techniques once thinning is complete. Multiple meteorite studies supported by FIB/FE-STEM are currently underway at NASA-JSC, including coordinated analysis of refractory phase assemblages in CAIs and fine-grained matrices in carbonaceous chondrites. FIB sectioning of CAIs has uncovered epitaxial and other overgrowth relations between corundum-hibonite-spinel consistent with hibonite preceding corundum and/or spinel in non-equilibrium condensation sequences at combinations of higher gas pressures, dust-gas enrichments or significant nebular transport. For all of these cases, the ability of FIB to allow for coordination with spatially-associated isotopic data by SIMS provides immense value for constraining the formation scenarios of the particular CAI assemblage. For carbonaceous chondrites matrix material, FIB has allowed us to obtain intact continuous sections of the immediate outer surface of Murchison (CM2) after it has been experimentally ion processed to simulate solar wind space weathering. The surface amorphization and loss of OH produced by the irradiation provides important clues regarding space weathering on primitive asteroids such as the OSIRIS-Rex target 101955 Bennu.

Christoffersen, Roy↗
DOE OSTI2021

4D Imaging of ZnO-Coated Nanoporous Al 2 O 3 Aerogels by Chemically Sensitive Ptychographic Tomography: Implications for Designer Catalysts

The 3D chemical structure (4D spectromicroscopy) of nanoporous Al 2 O 3 aerogels coated with ZnO by atomic layer deposition (ALD) was studied by multienergy scanning transmission X-ray microscopy. These materials are representative of a class of designer catalysts in which the nanoporous support is prepared separately from the active catalyst material, which is subsequently introduced by ALD, thereby allowing independent optimization of the morphology, chemistry, and spatial distribution of the support and catalyst. The samples studied were prepared by Ga ion and Xe plasma focused ion beam (FIB) milling as well as drop casting from water suspension. Zn L and Al K edge spectra of six samples with three different ZnO loadings were measured to investigate how loading and different sample preparation methods affect the 3D distribution of the ZnO and Al 2 O 3 . Scanning transmission X-ray microscopy (STXM) and ptychographic imaging at two energies each at the Zn L 3 and Al K edge were measured. The ptychography data were analyzed by using the SHARP reconstruction code to generate quantitative 2D chemical maps of the Al 2 O 3 and the ZnO. The STXM and ptychography maps were then measured at a sequence of tilt angles, covering up to 160° of rotation. The 3D structure of the ZnO and Al 2 O 3 was derived from the tilt series data by tomographic reconstruction using a compressed sensing algorithm. A twodimensional spatial resolution (half-period) of 6 nm, measured by Fourier ring correlation, and a 3D spatial resolution (half-period) of 9 nm, measured by Fourier shell correlation, were achieved when using the COSMIC beamline at the Advanced Light Source (ALS). The results show that for all of the ZnO loadings studied there is nonuniform coverage of the ZnO on the Al 2 O 3 aerogel framework. In addition, we found that both FIB methods create sample artifacts, although the distortion was less with Xe plasma than Ga ion FIB.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Novel Focused Ion Beam Liftouts for Spatial Characterization of Spherical Biominerals With Transmission Electron Microscopy

Abstract Focused ion beam (FIB) is frequently used to prepare electron- and X-ray-beam-transparent thin sections of samples, called lamellae. Typically, lamellae are prepared from only a subregion of a sample. In this paper, we present a novel approach for FIB lamella preparation of microscopic samples, wherein the entire cross-section of the whole sample can be investigated. The approach was demonstrated using spherical, porous, and often hollow microprecipitates of biologically precipitated calcium carbonate. The microprecipitate morphology made these biogenic samples more fragile and challenging than materials commonly investigated using FIB lamellae. Our method enables the appropriate orientation of the lamellae required for further electron/X-ray analyses after attachment to the transmission electron microscopy (TEM) grid post and facilitates more secure adhesion onto the grid post. We present evidence of autofluorescence in bacterially precipitated vaterite using this lamella preparation method coupled with TEM selected area diffraction. This innovative approach allows studying biomineralization at the micro to nano scales, which can provide novel insights into bacterial responses to microenvironmental conditions.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Evidence of lithium mobility under neutron irradiation

Understanding the evolution of intermetallic materials in high-radiation environments is of great importance for fusion science and national security. Tritium ( 3 H) and lithium ( 6 Li, 7 Li) transport within neutron irradiated claddings coated with aluminide (FeAl3) has been investigated using state-of-the-art multimodal imaging. Specifically, scanning electron microscopy – focused ion beam (SEM-FIB) was used to prepare irradiated coating lift-out samples for follow-on microanalysis. Here, scanning transmission electron microscopy (STEM) was used to acquire atomic-scale information on the carbonaceous structure and elemental mapping. Atomic force microscopy (AFM) was used to determine lift-out dimensions nondestructively. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) spectral and depth profiling show unexpected lithium isotopic distributions in the irradiated cladding, raising an important evidence of possible light isotope mobility within the cladding under elevated temperature and irradiation. ToF-SIMS three-dimensional chemical mappings of mid- and bottom-cladding coatings show light isotopic (e.g., 3 H, 6 Li, 7 Li) distributions in the irradiated coating and give new insights into the fundamental mechanism related to transport mechanisms within the cladding. Multimodal imaging is power to link microstructure, chemistry, and nanoscale defects that impact reliability of these materials. Furthermore, chemical mapping offers observations of the microstructural evolution due to irradiation and provides insights into unexpected material transport under extreme conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Speciation mapping of the oxidation layer on aged uranium dioxide using scanning transmission x-ray spectromicroscopy

In this study, UO 2 was aged in humid air and prepared as a thin section using a focused ion beam (FIB) instrument. The specimen was measured using synchrotron radiation spectromicroscopy techniques at the Beamline 11.0.2 STXM end station of the Advanced Light Source (ALS). Non-negative matrix factorization (NMF) methods were used to identify and map three component x-ray absorption near-edge structure (XANES) spectra in the oxygen K-edge data, revealing a surface layer of U 4 O 9 with a thickness of 206 ± 21 nm, and the bulk of the sample remaining as UO 2 . Uranium N 4,5 -edge XANES spectromicroscopy supports these results. The diffusion-controlled parabolic rate constant for UO 2 oxidation to U 4 O 9 was calculated from the observed layer thickness and compared to literature values. Complementary transmission electron microscopy (TEM) was used to image the sample and identify the phases present in various regions, confirming the STXM results.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Correlating dislocation structures to basal and prismatic slip bands near grain boundaries in tensile-tested Mg–4Al using a multiscale electron microscopy approach

Dislocation structures where basal and prismatic slip bands meet grain boundaries in tensile-tested Mg with 4 wt% Al (Mg–4Al) were studied using a multiscale electron microscopy approach to explore the assumptions made for the dislocation pileup theory: a) slip bands consist of dislocation arrays piling up near grain boundaries, and b) stress concentration in the adjacent grain is solely caused by dislocation pileup. After post-testing electron backscatter diffraction (EBSD) scans, focused-ion-beam (FIB) lift-out specimens were prepared from regions of interest so that the specimen plane is parallel to the bulk sample surface to allow for direct correlation between mesoscale and microscale characterization. High dislocation density and the dislocation arrays in the slip bands corroborated with the first assumption. Evidence of plastic deformation in all grains, however, showed that the second assumption was false. Additionally, dislocation structures including crystal rotation boundaries and dislocations dissociating to the basal plane provide additional stress relief mechanisms near grain boundaries that are not accounted for in many crystal plasticity models, which requires auxiliary models to more accurately predict the stress and strain distribution in a microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Record of Decision: LEBT Energy Change

The LAMP Conceptual Design (LCD), as described in the LAMP Conceptual Design Report incorporates multiple 100-keV low-energy beam transport (LEBT) lines between the ion sources and the radiofrequency quadrupole (RFQ). The LEBT lines transport H + and H - beams from their respective ion sources to the RFQ entrance, and provide the required manipulations (focusing, steering, chopping, etc.) to the ion beams to prepare them for injection into the RFQ and further acceleration.

43 PARTICLE ACCELERATORS↗
NASA NTRS2018

Novel Applications of Focused Ion Beam Technique for Planetary Sample Analyses

We are using innovative FIB techniques to prepare samples of planetary materials for different types of coordinated analyses using ion microprobes, synchrotron beamlines, and specialized transmission electron microscopy (TEM) techniques. In these cases, the FIB sample preparation is the critical step in enabling these specialized analyses. We discuss several examples below utilizing the FEI Quanta3D instrument at the NASA Johnson Space Center. Trace element analyses utilizing synchrotron x-ray fluorescence. The trace element content of mineral grains in comet dust provides important clues on their formation and processing in the early solar system. We preformed coordinated analyses of a comet dust particle that had been prepared using ultramicrotomy for TEM analysis. Following the TEM analyses, we extracted a 70 nm thick section from a region of the carbon (C) film of the TEM grid, for additional analyses. A carbon ring ~2-3 μm thick was deposited on top of the C film using the FIB. The C film on the outer rim of the ring was milled away using various patterns to uniformly release the stresses on the film, preventing rupture and collapse, and was attached to the micromanipulator needle. We then isolated the ring completely and transferred the section to a silicon sample holder for analysis using the HXN (hard X-ray nanoprobe) beamline at NSLSII at Brookhaven National Lab. Coordinated Analyses of Presolar Grains. Rare sub-m presolar grains that originate in evolved stars and supernovae, occur in primitive astromaterials and are identified by their exotic isotopic compositions. Coordinated analyses of these grains using NanoSIMS, TEM, and other techniques on the same grain is enabled by innovative FIB sample preparation. In order to obtain subsequent isotopic analyses of Mg and Fe, contributions from surrounding grains were minimized. We precisely deposited a protective cap of Pt on top of the grain to preserve the grain of interest and then milled away about 5 μm diameter of the surrounding material. Following the isotopic analyses, the spindle was extracted and thinned to electron transparency for TEM microstructural analyses. In situ heating TEM experiments on lunar samples. We extracted a FIB thin section from Apollo 17 lunar rock 76015. To avoid ion-beam damage, e-beam deposition was used to deposit the first 500 nm of the C strap, followed by ion beam-assisted deposition of ~3 μm carbon. We performed an ex situ lift-out of the section and placed the section on one of the elements of a microelectromechanical systems (MEMS) - specialized heating substrate and attached the section to the substrate by depositing small C straps with the FIB. The heating chips utilize silicon nitride windows to support the samples and provide uniform heating while enabling TEM imaging. The heating chip was loaded into a Hitachi “Blaze” heating holder and analyzed using a Hitachi HF5000 at the University of Arizona.

Rahman, Z.↗