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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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All sourcesNASA NTRSDOE OSTI
NASA NTRS2016

A Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for In-Situ Mars Surface Sample Analysis

The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) project, funded by the NASA Planetary Instrument Concepts for the Advancement of Solar System Observations (PICASSO) Research Opportunities in Space and Earth Sciences (ROSES), will build upon previous miniaturized SEM designs and recent advancements in variable pressure SEM's to design and build a SEM to complete analyses of samples on the surface of Mars using the atmosphere as an imaging medium. This project is a collaboration between NASA Marshall Space Flight Center (MSFC), the Jet Propulsion Laboratory (JPL), electron gun and optics manufacturer Applied Physics Technologies, and small vacuum system manufacturer Creare. Dr. Ralph Harvery and environmental SEM (ESEM) inventor Dr. Gerry Danilatos serve as advisors to the team. Variable pressure SEMs allow for fine (nm-scale) resolution imaging and micron-scale chemical study of materials without sample preparation (e.g., carbon or gold coating). Charging of a sample is reduced or eliminated by the gas surrounding the sample. It is this property of ESEMs that make them ideal for locations where sample preparation is not yet feasible, such as the surface of Mars. In addition, the lack of sample preparation needed here will simplify the sample acquisition process and allow caching of the samples for future complementary payload use.

Microscope↗
DOE OSTI2022

Perspective: Biochemical and Physical Constraints Associated With Preparing Thin Specimens for Single-Particle Cryo-EM

While many aspects of single-particle electron cryo-microscopy (cryo-EM) of biological macromolecules have reached a sophisticated level of development, this is not yet the case when it comes to preparing thin samples on specimen grids. As a result, there currently is considerable interest in achieving better control of both the sample thickness and the amount of area that is useful, but this is only one aspect in which improvement is needed. This Perspective addresses the further need to prevent the macromolecular particles from making contact with the air-water interface, something that can result in preferential orientation and even structural disruption of macromolecular particles. This unwanted contact can occur either as the result of free diffusion of particles during the interval between application, thinning and vitrification of the remaining buffer, or—when particles have been immobilized—by the film of buffer becoming too thin prior to vitrification. An opportunity now exists to apply theoretical and practical insights from the fields of thin-film physical chemistry and interfacial science, in an effort to bring cryo-EM sample preparation to a level of sophistication that is comparable to that of current data collection and analysis.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

A New Method for Polishing Laminated Dissimilar Metals

Here, this paper presents a novel method for preparing metallographic samples of laminated dissimilar metals, specifically a layered structure of zirconium (Zr), vanadium (V), and tungsten (W), which pose a challenge due to their differing crystal structures and hardness levels. The work was motivated by the need to develop a cladding for tungsten targets in spallation neutron sources, where a zirconium face is applied over an interlayer of either vanadium or titanium to prevent the formation of brittle intermetallic compounds such as ZrW 2 . Traditional polishing techniques prove inadequate because each constituent metal requires a different polishing approach based on its unique material properties. The methodology outlined includes a sequential process involving conductive epoxy mounting, successive grinding and polishing with specific abrasives, and a final chemical-mechanical polish using a colloidal silica-based solution. Optical microscopy confirmed that this multi-step process successfully produced scratch-free surfaces and minimized surface relief across the different metal interfaces. Although developed for refractory metals, this approach shows promise for other layered structures comprised of transition metals, offering a meticulous yet effective technique for high-quality metallographic sample preparation.

Newberry, Daniel [Oak Ridge National Laboratory (O↗
DOE OSTI2025

Geometric control of magnetic domain morphology in electrodeposited Ni rich NiPt mesoscopic wires

In this paper, we study the electrodeposited Ni—Pt magnetic wires, exploring the mechanisms by which changes in geometry and composition influence the local magnetic structure. The samples were prepared by electrodeposition, their elemental composition was analyzed by energy dispersive X-ray spectroscopy, and phase analysis was carried out by an X-ray diffraction measurement. Magnetic force microscopy measurements, and magnetic force microscopy measurements in magnetic field were carried out to study the domain morphology of the prepared samples. Magnetization characteristics were measured via vibrating sample magnetometry mode of a superconducting quantum interference device. Here, the results were analyzed and compared with micromagnetic simulations. It is shown that a strong perpendicular magnetic anisotropy is responsible for the characteristic checkerboard-like surface magnetization patterns, which can be tuned by geometrical constriction and Ni content. Understanding these relationships provides insights into the design of magnetic materials with tailored properties for advanced applications, like magnetic sensors.

Binary alloy↗
DOE OSTI2020

Understanding the Structure and Dynamics of Complex Biomembrane Interactions by Neutron Scattering Techniques

The membrane is one of the key structural materials of biology at the cellular level. Composed predominantly of a bilayer of lipids with embedded and bound proteins, it defines the boundaries of the cell and many organelles essential to life and therefore is involved in almost all biological processes. Membrane-specific interactions, such as drug binding to a membrane receptor or the interactions of an antimicrobial compound with the lipid matrix of a pathogen membrane, are of interest across the scientific disciplines. Herein we present a review, aimed at nonexperts, of the major neutron scattering techniques used in membrane studies: small-angle neutron scattering, neutron membrane diffraction, neutron reflectometry, quasielastic neutron scattering, and neutron spin echo. Neutron scattering techniques are well suited to studying biological membranes. The nondestructive nature of cold neutrons means that samples can be measured for long periods without fear of beam damage from ultraviolet, electron, or X-ray radiation, and neutron beams are highly penetrating, thus offering flexibility in samples and sample environments. Most important is the strong difference in neutron scattering lengths between the two most abundant forms of hydrogen, protium and deuterium. Changing the relative amounts of protium/deuterium in a sample allows the production of a series of neutron scattering data sets, enabling the observation of differing components within complex membrane architectures. This approach can be as simple as using the naturally occurring neutron contrast between different biomolecules to study components in a complex by changing the solution H 2 O/D 2 O ratio or as complex as selectively labeling individual components with hydrogen isotopes. This review presents an overview of each experimental technique with the neutron instrument configuration, related sample preparation and sample environment, and data analysis, highlighted by a special emphasis on using prominent neutron contrast to understand structure and dynamics. This review gives researchers a practical introduction to the often enigmatic suite of neutron beamlines, thereby lowering the barrier to taking advantage of these large-facility techniques to achieve new understandings of membranes and their interactions with other molecules.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2020

Surface and bulk characterization of reservoir and cap-rocks: Past, present, and future

Geologic formations provide potentially some of the largest volume capacities for CO 2 storage or sequestration. Potential storage sites can be deep saline aquifers, depleted oil reservoirs, and coal seams, surrounded by sealing layers to prevent CO 2 from leaking. It is therefore critical to understand mechanisms contributing to CO 2 trapping and CO 2 leaks. Both phenomena are governed by reactions at the interfaces of the reservoir and cap-rocks and are controlled by the complex chemistry and pore structures of rocks. Mechanisms at the macroscale are affected by the processes occurring at the nanoscale. This review highlights the necessity of multitechnique, multiscale characterization of rocks and points to the importance of surface analysis and surface science studies. Two shale rocks (seals) from Niobrara and Agardhfjellet formations with complex surface chemistry are used as examples throughout the paper. Typically, evaluation of rocks with x-ray diffraction, thermogravimetric analysis, Rock-Eval pyrolysis, gas adsorption, and electron microscopy combined with energy dispersive x-ray spectroscopy is conducted to provide valuable information about the bulk mineralogy, elemental composition, pore volume, and adsorbed species on the sample surface. These studies are necessary prior to designing surface sensitive experiments with x-ray photoelectron spectroscopy (XPS), guiding both sample preparation and sample analysis. XPS has been widely used to study the surface composition of rocks during the investigations of their fine-scale wettability, and the main findings are highlighted here. This paper also reviews the existing literature on ambient-pressure XPS, which provides new opportunities to study in situ chemical alteration due to interactions with CO 2 and offers recommendations for adapting this technique to study rock-fluid interactions, allowing for the identification of fundamental interactions during CO 2 sequestration and guide selection of formation sites for improved storage.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1981

Investigations related to evaluation of ultramicrofluorometer

High resolution emission and excitation fluorescent spectra were obtained for several samples in an effort to determine the optimum operational design for the instrument. The instrument was used to determine the required nature of a sample which could be detected, and in so doing, several different sample preparation techniques were considered. Numerous experiments were performed to determine the capabilities of the instrument with regard to the detection of suitably prepared virus specimens. Significant results were obtained in several areas. The fluorescent spectra indicated that substantial changes in the laser might be used advantageously to greatly improve the performance of the instrument. In the existing configuration, the instrument was shown to be capable of detecting the presence of suitably prepared virus samples.

Whitcomb, B.↗
NASA NTRS2001

Microbial detection with low molecular weight RNA

The need to monitor microorganisms in the environment has increased interest in assays based on hybridization probes that target nucleic acids (e.g., rRNA). We report the development of liquid-phase assays for specific bacterial 5S rRNA sequences or similarly sized artificial RNAs (aRNAs) using molecular beacon technology. These beacons fluoresce only in the presence of specific target sequences, rendering as much as a 27-fold fluorescence enhancement. The assays can be used with both crude cell lysates and purified total RNA preparations. Minimal sample preparation (e.g., heating to promote leakage from cells) is sufficient to detect many Gram-negative bacteria. Using this approach it was possible to detect an aRNA-labeled Escherichia coli strain in the presence of a large background of an otherwise identical E. coli strain. Finally, by using a longer wavelength carboxytetramethylrhodamine beacon it was possible to reduce the fraction of the signal due to cellular autofluorescence to below 0.5%.

NASA Discipline Life Sciences Technologies↗
NASA NTRS2021

Amino Acid Abundances and Compositions in Iron and Stony-Iron Meteorites

The organic compositions of carbonaceous chondrite meteorites have been extensively studied; however, there have been fewer reports of other meteorite classes, and almost none from iron meteorites, which contain much less carbon than carbonaceous chondrites but make up ~4% of observed meteorite falls. Here, we report the bulk amino acid content of three iron meteorites (Campo del Cielo, IAB; Canyon Diablo, IAB; and Cape York, IIIAB) and both the metal and silicate portions of a pallasite (Imilac). We developed a novel method to prepare the samples for analysis, followed by hot water extraction and analysis via liquid chromatography‐mass spectrometry. Free amino acid abundances ranging from 301 to 1216 pmol/g were observed in the meteorites, with the highest abundance in the silicate portion of the pallasite. Although some of the amino acid content could be attributed to terrestrial contamination, evidence suggests that some compounds are indigenous. A suite of C(5) amino acids was observed with a distinct distribution favoring a straight chain (n‐pentanoic acid) structure; this straight chain dominance is suggestive of that observed in thermally altered stony meteorites. Amino acids were also observed in terrestrial iron granules that were milled and analyzed in the same way as the meteorites, although the distribution of detected amino acids was different. It is possible that similar formation mechanisms existed in both the meteorites and the terrestrial iron, or that observed amino acids resulted from reactions of precursors during sample preparation. This work suggests that iron meteorites should not be overlooked for contributions of amino acids and likely other soluble organic molecules to the early Earth. Future studies of iron–nickel meteorites and asteroids, such as Psyche, may provide further insights into their potential organic inventory.

Jamie E. Elsila↗
NASA NTRSDate not supplied

From Apollo to Artemis: How Processing ANGSA Core Samples 73001/2 Can Help to Prepare for Future Sample Return Missions to the Moon and Beyond.

Introduction: Apollo Sample 73001/2 is a ~71cm long double drive tube consisting of an upper part (73002) and a lower part (73001) that contains regolith collected near Lara Crater at the Apollo 17 site, Station 3. The double drive tube is believed to have penetrated a lunar landslide deposit that was transported from the slope of the South Massif into the Taurus-Littrow Valley [1]. As part of the ANGSA (Apollo Next Generation Sample Analyses) initiative, preparing a preliminary examination (PE) catalog of 73001/2 is a crucial first step for the early identification of material types such as rock fragments and potential stratigraphy within the core. Many new curation and scientific tools such as X-ray computed tomography (XCT) [3], multi-spectral imaging [4], and gas extraction manifold with piercing tool [5-7], have been applied to the ANGSA core to benefit curation strategy, PE efforts, sample allocation to the planetary science community, and ultimately help to prepare for future sample return missions like Artemis. 73001/2 Preliminary Examination and Processing: Sample 73002 was successfully opened and extruded in Nov. 2019 and fully dissected at the end of 2021. Sample 73001 (Fig. 1) was successfully extruded in March 2022 after careful planning before opening the Core Sample Vacuum Container (CSVC) that was holding the drive tube of 73001. XCT, as part of PE, was used to scan the bottom and top part of the 73001 core tube within the CSVC prior to opening it to 1) facilitate non-destructive, rapid detection of any contamination potentials due to piercing of the CSVC during gas extraction [7]; and 2) to aid in the Artemis sample tool development and provide data on the knife edge seal of the CSVC. This knowledge will help us connect the mechanics of the implemented design (i.e., XCT data) to the performance of the seal (i.e., data on the gas samples will tell us how well the seal preserved the volatile record of lunar samples). Both type of information will feed forward into Artemis tool and storage strategies for future samples. Results and Lessons learned: The XCT data of the CSVC and core tube within showed that the bottom Teflon cap was not pierced during gas extraction (Fig. 1c) and thus, the sample integrity remained guaranteed during piercing and subsequent gas extraction. However, the XCT scan of the top of the core (Fig. 1b) revealed that the drive tube was overfilled with lunar soil and the tool that keeps the soil constrained within the drive tube was not fully deployed. These preliminary data allowed us to implement the necessary steps to prevent loss of sample integrity, including any potential stratigraphy shifts during extrusion. Processing Apollo core 73001/2, creating an informative PE catalog, and applying new and refined tools and technologies for sample analyses are invaluable activities that will assist in circumventing any potential pitfalls, aid in the characterization of samples, and help in the assessment of how well any lunar material has been collected and preserved in the past. This will aid in designing future sample collections and curation procedures and help to prepare for future human exploration and sampling missions such as Artemis. References: [1] Schmitt H. (2017) Icarus 298, 2-33. [3] Zeigler et al. (2021) LPSC 52nd, #2632; [4] Sun et al. (2021), LPSC 52nd, #1789; [5] Parai et al. (2021), LPSC 52nd #2665; [6] Schild et al. (2021) LPSC 52nd #1888; [7] McDonald (2022) ESL 2022.

ANGSA↗
NASA NTRS1999

Workshop on Mars 2001: Integrated Science in Preparation for Sample Return and Human Exploration

The Workshop on Mars 2001: Integrated Science in Preparation for Sample Return and Human Exploration was held on October 2-4, 1999, at the Lunar and Planetary Institute in Houston, Texas. The workshop was sponsored by the Lunar and Planetary Institute, the Mars Program Office of the Jet Propulsion Laboratory, and the National Aeronautics and Space Administration. The three-day meeting was attended by 133 scientists whose purpose was to share results from recent missions, to share plans for the 2001 mission, and to come to an agreement on a landing site for this mission.

Marshall, John↗
NASA NTRS1991

Microstructure and magnetization of Y-Ba-Cu-O prepared by melt quenching, partial melting and doping

Y-Ba-Cu-O samples prepared by means of a variety of melt-based techniques exhibit high values for their magnetic properties compared with those of samples prepared by solid state sintering. These techniques include single-stage partial melting as well as melt quenching followed by a second heat treatment stage, and they have been applied to the stoichiometric 123 composition as well as to formulations containing excess yttrium or other dopants. The structure of these melt-based samples is highly aligned, and the magnetization readings exhibit large anisotropy. At 77 K and magnetic field intensities of about 2 kOe, diamagnetic susceptibilities as high as -14 x 10(exp -3) emu/g were obtained in the cases of melt-quenched samples and remanent magnetization values as high as 10 emu/g for samples prepared by partial melting.

Hojaji, Hamid↗
NASA NTRS2016

Community Extreme Tonnage User Service (CETUS): A 5000 Ton Open Research Facility in the United States

Large sample volume 5000 ton multi-anvil presses have contributed to the exploration of deep Earth and planetary interiors, synthesis of ultra-hard and other novel materials, and serve as a sample complement to pressure and temperature regimes already attainable by diamond anvil cell experiments. However, no such facility exists on the North American continent. We propose the establishment of an open user facility for COMPRES members and the entire research community, with the unique capability of a 5000 ton (or more) press, supported by a host of extant co-located experimental and analytical laboratories and research staff. We offer wide range of complementary and/or preparatory experimental options. Any required synthesis of materials or follow up experiments can be carried out controlled atmosphere furnaces, piston cylinders, multi-anvil, or experimental impact apparatus. Additionally, our division houses two machine shops that would facilitate any modification or custom work necessary for development of CETUS, one for general fabrication and one located specifically within our experimental facilities. We also have a general sample preparation laboratory, specifically for experimental samples, that allows users to quickly and easily prepare samples for ebeam analyses and more. A service we can offer to COMPRES community members in general, and CETUS visiting users specifically, is a multitude of analytical instrumentation literally steps away from the experimental laboratories. This year we will be pursuing site funding of our laboratories through NASA's Planetary Science Directorate, which should result in substantial cost savings to all visiting users, and supports our mission of interagency cooperation for the enhancement of science for all (see companion PSAMS abstract). The PI is in a unique position as an employee of Jacobs Technology to draw funding from multiple sources, including those from industry and commerce. We submitted a Planetary Major Equipment proposal to the NASA Emerging Worlds solicitation for the full cost of a press, with competitive bids submitted from Sumitomo, Rockland Research, and Voggenreiter. Additional funding is currently being sought from industry sources through the Strategic Partnerships Office at NASA JSC, External Pursuits Program Office on the JETS contract, and Jacobs corporate in the United States. Internal funding is available for JETS contract personnel to travel to large press locations worldwide to study set-up and operations. We also anticipate a fortuitous cost savings in installation of the large press because plans are already underway for major renovations to the entire experimental petrology suite within the next 2 years in order to accommodate our growing user base. Our focus as contract staff is on serving the scientific needs of our users and collaborators. We are seeking community expert input on multiple aspects of this proposed facility, such as the press type and design, access management, immediate projects, and future innovation initiatives.

Danielson, L.↗
DOE OSTI2023

A streamlined tandem tip-based workflow for sensitive nanoscale phosphoproteomics

Effective phosphoproteome of nanoscale sample analysis remains a daunting task, primarily due to significant sample loss associated with non-specific surface adsorption during enrichment of low stoichiometric phosphopeptide. We develop a tandem tip phosphoproteomics sample preparation method that is capable of sample cleanup and enrichment without additional sample transfer, and its integration with our recently developed SOP (Surfactant-assisted One-Pot sample preparation) and iBASIL (improved Boosting to Amplify Signal with Isobaric Labeling) approaches provides a streamlined workflow enabling sensitive, high-throughput nanoscale phosphoproteome measurements. This approach significantly reduces both sample loss and processing time, allowing the identification of >3000 (>9500) phosphopeptides from 1 (10) µg of cell lysate using the label-free method without a spectral library. It also enables precise quantification of ~600 phosphopeptides from 100 sorted cells (single-cell level input for the enriched phosphopeptides) and ~700 phosphopeptides from human spleen tissue voxels with a spatial resolution of 200 µm (equivalent to ~100 cells) in a high-throughput manner. The new workflow opens avenues for phosphoproteome profiling of mass-limited samples at the low nanogram level.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2026

Automation of Laser Plasma Focused Ion Beam Microscopy for Next-Gen Energy Materials

Automation can revolutionize the use of ultrafast laser ablation and plasma-focused ion beam (PFIB) techniques for high-throughput, reproducible cross-sectioning and various sample preparation in materials characterization. As these methods become essential for analyzing complex energy materials and next-generation devices, efficient, standardized workflows are needed to minimize variability and enhance precision. This work highlights our advancements in developing automated processes for sample preparation that integrates machine learning, workflow optimization, and large-scale data acquisition to improve efficiency and scalability in applications such as electrolyzers, photovoltaic cells, and microelectronics. To streamline cross-sectioning and lamella fabrication, we have implemented fully automated workflows that standardize laser ablation and PFIB milling sequences. These workflows incorporate pre-programmed protocols for material removal, alignment, and thinning, reducing user intervention and ensuring consistency across different sample types. Machine learning algorithms further enhance automation by predicting optimal milling strategies and adapting parameters based on material properties and sectioning requirements. This approach significantly improves throughput while maintaining the structural integrity of prepared samples for high-resolution imaging and analysis, including transmission electron microscopy. Beyond sample preparation, our automation platform enables the acquisition of large, high-resolution datasets through serial sectioning, image alignment, and 3D reconstruction. These automated routines facilitate multi-scale characterization, capturing structural and compositional details from the nanoscale to the device level. By reducing variability and increasing efficiency, our automated approach enhances defect analysis, failure diagnostics, and process optimization, accelerating advancements in materials research and device engineering.

36 MATERIALS SCIENCE↗
DOE OSTI2024

A Tip-based Workflow for Sensitive IMAC-based Low Nanogram Level Phosphoproteomics

Analyzing the phosphoproteome at nanoscale poses a significant challenge, mainly due to the substantial sample loss from non-specific surface adsorption during the enrichment of low stoichiometric phosphopeptides. Here, we describe a tandem tip-based phosphoproteomics sample preparation method capable of sequential sample cleanup and enrichment without the need for additional sample transfer, thereby minimizing sample loss. Integration of this method to our recently developed SOP (Surfactant-assisted One-Pot sample preparation) and iBASIL (improved Boosting to Amplify Signal with Isobaric Labeling) approaches creates a streamlined workflow, enabling sensitive, high-throughput nanoscale phosphoproteomics measurements.

Phosphoproteome, Immobilized metal ion affinity ch↗
DOE OSTI2025

Characterization of Tank 9H Annulus Sample in Support of Residual Material Inventory Determinations

The Savannah River National Laboratory (SRNL) was requested by Savannah River Mission Completion (SRMC) to provide sample preparation and characterization of the Tank 9H annulus sample in support of Residual Material Inventory Determinations. One Tank 9H sample in three vials [HTF-9-25-13, HTF-9-25-14 and HTF-9-25-15], with each vial containing approximately 200 mL of the Tank 9H annulus salt solution, were delivered to the SRNL Shielded Cells for sample preparation and characterizations in February 2025. The density of the “as-received” solution contained in each of the three Tank 9H annulus sample vials were determined followed by a solid-liquid separation on each one using 0.45-micron Nalgene® nylon filter membranes. The resulting filtrates were combined to form the Tank 9H annulus sample with a total volume of about 600 mL. The combined wet solid fractions, about a total of 4.8 grams of salt material, remaining on the filter membranes were air-dried in the Shielded Cells for 72 hours. The total weight of the air-dried solids was 2.1 grams. These air-dried solids were washed with deionized water (DI water) at a phase ratio of 60 mL DI water/gram of solids to recover insoluble solids, if any. No visible or measurable quantity of insoluble solids were recovered after DI water washing of the air-dried solids because the air-dried solids completely dissolved in the DI water. The solid fraction-wash water was not combined with the 600 mL of the filtrate solution, and the resulting solution was not screened or analyzed for radionuclides. Aliquot sample volumes of the undiluted Tank 9H annulus sample were sent to the SRNL analytical services groups for radionuclides, elementals, anions and total mercury analysis by various methods including radiochemical separations/counting methods, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) and special preparations. All sample analyses were performed in triplicate. This report presents the analytical characterization results for the Tank 9H annulus sample. The results are also reported where analytical methods yielded additional analytes, other than those requested by SRMC. In the characterization of the Tank 9H annulus sample, the detection limits for all the analytes, as specified in the Technical Task Request (TTR) and Task Technical and Quality Assurance Plan (TTQAP), were met.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗