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At least 217 records · Page 12

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NASA NTRS2023

Preliminary Examination of Returned Samples From Bennu Using Quantitative Particle Analysis in the Scanning Electron Microscope

The sample of regolith collected from asteroid Bennu by NASA’s OSIRIS-REx spacecraft will land in Utah on September 24, 2023. A 100-mg aliquot of fine Bennu dust adhering to the internal surfaces of the sample return capsule and associated hardware will be collected by curation staff during disassembly and analyzed immediately by members of the sample analysis team in a “Quick-Look” (Q-L) procedure. The Q-L objectives are (1) to provide images for release to the public to inform on the nature of the returned sample, and (2) to perform a reconnaissance investigation of the mineralogic characteristics of the returned material for science purposes. We will determine the minerals that occur in the dust, assess their diversity, and determine relative abundances at the >5% level using a combination of optical microscopy, Fourier-transform infrared spectroscopy, X-ray powder diffraction, and field-emission scanning electron microscopy (SEM). Here we describe the procedures and techniques developed for the Q-L analyses using analog samples analyzed by SEM equipped with energy dispersive X-ray spectroscopy (EDX). To test these techniques, we have applied them to several samples, including powders of the Murchison (Fig. 1) and Orgueil meteorites, as well as simulant samples prepared by the mission.

OSIRIS-REx↗

NASA NTRSDate not supplied

Increasing Flexibility of Polymers in the Application of Complex Space Craft Heat Shield Geometries

Highly crosslinked polymers, commonly utilized in spacecraft component fabrication, especially for heatshields, have historically encountered challenges due to their inherent brittleness. To overcome this issue, researchers have explored the incorporation of additives into the polymer backbone to enhance flexibility and durability. This study aims to improve the flexibility and durability of highly crosslinked polymers by introducing long-chain aliphatic silicon-based additives with varying molecular weights into the polymer backbone. By increasing the flexibility of these brittle polymers, they can be effectively employed in constructing intricate curvatures for heatshields, eliminating the need for gap fillers. In this study, we investigated six different additives, comparing them to a highly crosslinked high-temperature polymer used as a baseline. Various characterization techniques, including thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), dilatometry, dynamic mechanical analysis (DMA), nuclear magnetic resonance (NMR), and Fourier transform infrared spectroscopy (FTIR), were employed to assess the properties of the materials. The FTIR and NMR results indicated the successful incorporation of the silicon-based additives into the polymer backbone. Furthermore, thermal characterization results demonstrated that certain additives exhibited superior flexibility and lower densities compared to the baseline polymer.

Tane Boghozian↗

NASA NTRSDate not supplied

Increasing Flexibility of Polymers in the Application of Complex SpaceCraft Heat Shield Geometries

In this study, six additives were investigated, comparing them to a phenolic baseline. Various characterization techniques, including thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), nuclear magnetic resonance (NMR), and Fourier transform infrared spectroscopy (FTIR), were employed to assess the properties of the materials.

flexible polymers↗

NASA NTRSDate not supplied

Additive Manufacturing and Working Fluid Characterization of Ceramic Heat Pipes

In this work, additively manufactured (AM) aluminum nitride (AlN) ceramic heat pipes were developed to improve spacecraft heat rejection capabilities beyond the current state-of-the-art metal systems. A low sintering temperature aluminum nitride slurry is developed for digital light processing printing (DLP) and the optimal debinding curves are examined. Printed AlN parts are characterized via SEM and optical profilometry. AlN 3D-printed parts are also tested for compatibility with aluminum bromide, aluminum chloride, and iodine, among other proposed working fluids at 350-600 K in an inert atmosphere, with reactivity measured via SEM and Fourier transform infrared spectroscopy (FTIR).

Thermal Management↗

NASA NTRS2024

High Yield Exfoliation of a Sub-Micron Hexagonal Boron Nitride Using a Solvent Free Method

Sodium fluoride (NaF) has been found to be an activation agent in exfoliating a hexagonal boron nitride (hBN) platelet, using solvent free method. The procedure was carried out by enhancing the intercalation of ferric chloride (FeCl3) in an intermediate step, up to 330 °C, followed by removal of the by-product at room temperature. In this research, five additional common salts including lithium fluoride, potassium fluoride, lithium chloride, sodium chloride, and potassium chloride, were examined and compared to NaF for their effectiveness in producing the most exfoliation of a commercially available sub-micron-size hBN. It was found that, all fluoride and chloride salts significantly activated the intercalation of FeCl3 into this hBN. Analyses and characterization from X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscoy revealed NaCl to be one of most effective agents without further heat treatment and the least expensive salt in the intercalating reaction and exfoliation process. The synthetic route of this solvent free method is straightforward with 89% yield and above which can be produced on a large scale.

boron nitride↗

NASA NTRSDate not supplied

Variable Emittance Coatings

Variable emittance coatings (VECs) can reduce thermal control system mass and power by passively changing radiator heat rejection according to spacecraft and environment heat loads. VECs make establishing a lunar presence easier since this technology helps overcome challenges with harsh thermal environments on the lunar surface and in transit. This CIF focuses on creating testing capabilities to assess VECs from collaborators in academia and industry. Two main testing capabilities were created. First, a set of temperature dependent Fourier Transform Infrared Spectroscopy (FTIR) measurement accessories were designed, fabricated, and used to measure samples received from collaborators. These accessories are capable of measuring the transmittance and reflectance of semi transparent and opaque samples. Second, a vacuum calorimetry experiment was designed and built to assess the variable heat rejection of larger coupons.

Sydney Taylor↗

NASA NTRS2026

Biobased Polybenzoxazine Derived from Furfurylamine and Piceol with Low Cure Temperature and Advanced Properties for Composite Matrices

A novel benzoxazine made from furfurylamine, paraformaldehyde, and piceol, Bz-FA-HA, is assessed for applications in fiber reinforced (FR) composites. Piceol is a biobased phenolic compound derived from the roots of Norwegian spruce trees and contains a methyl ketone group at the para position. Bz-FA-HA is a liquid at room temperature, has a viscosity of < 1 Pa.s at temperatures above 90 °C, and a Tonset of cure at 132 °C. The carbonyl is found to react with the furan ring, yielding a crosslinking reaction, when cured above 180 °C as indicated by differential scanning calorimetry and thermogravimetric analysis coupled with Fourier transform infrared spectroscopy. Poly(Bz-FA-HA) has a Tg > 350 °C, attributed to the crosslinking reaction. Furthermore, the storage modulus is > 3 GPa, regardless of cure temperature. Poly(Bz-FA-HA) has a char yield at 800 °C of 65.0 % (62.3 % at 1000 °C), and a Tonset of decomposition of 357 °C in nitrogen. The resulting carbon formed during pyrolysis shrinks during the carbonization reaction and scanning electron microscopy imaging shows a cross-section with micro cracks. The high processability, advanced mechanical properties, and exceptional char yield make it a promising candidate as the matrix for FR composites.

Benzoxazine↗

NASA NTRSDate not supplied

Evaluating Crystallinity in Thermoplastic composites

Thermoplastics↗

NASA NTRSDate not supplied

Evaluating Crystallinity in Thermoplastic Composites for Aerospace Applications

Polymer matrix composites (PMCs) offer many benefits for the aerospace industry due to their potential for weight reduction when compared to metal or ceramic based materials. Most PMCs currently in flight use thermoset matrices, however, thermoplastic resins are being explored as alternatives due to their ability to be remelted, which is of particular interest due to the potential for in-situ repair and faster production. Most thermoplastic resins are semicrystalline polymers. The properties of semicrystalline thermoplastics are directly influenced by their crystallinity, which can vary due to many factors including thermal treatments, environmental conditions, and mechanical deformation. Within thermoplastic PMC parts, crystallinity gradients can arise due to variations in part geometry, across part thicknesses, and along bonded joints. Monitoring the crystallinity of thermoplastic composites is key to ensuring these materials meet the high demands required for aerospace. Several different analytical techniques exist that can be used to characterize the bulk crystallinity of thermoplastic materials. However, many existing methods lack the specificity required to identify the subtle variations in crystallinity that may play a significant role in the performance and durability of PMC parts. Because of this, a significant amount of work is still required to fully characterize and understand the crystallinity profiles of thermoplastic PMCs and the resulting impact to material properties. This talk discusses the use of multiple techniques such as Differential Scanning Calorimetry, Polarized Light Optical Microscopy, and Fourier-Transform Infrared Spectroscopy to characterize the crystallinity in carbon fiber/thermoplastic composites. Samples of different crystallinity profiles were manufactured using various cooling procedures. This work aims to provide the fundamental data necessary to understand the effects of crystallinity on thermoplastic PMCs, which is key to advancing their use in aerospace applications.

Thermoplastics↗

DOE OSTI2026

Chemical and Radiological Compatibility Testing of 3D Printed Materials

To dramatically increase the adaptability, performance, and safety of processes in support of the Defense Waste Processing Facility (DWPF), Savannah River National Lab (SRNL) plans to perform chemical and radiological compatibility testing on a wide variety of 3D printed materials of interest. The 3D printing process provides numerous strategic operational benefits such as rapid prototyping of complex designs and geometry specific to the needs of the nuclear waste disposition process, as well as on-demand rapid prototyping and iteration with materials that aren’t as accessible through traditional manufacturing methods. Reaction chemistry in simulated waste batches can be matched closely to its radioactive counterpart, but glass reactor vessels have limitations. Vessel geometry can play a big factor in mixing transport limitations, process chemistry, and degradation reaction kinetics. In addition, additive manufacturing allows for much more detailed vessel design than traditional alternatives. Waste processing techniques in DWPF also encounter extreme chemical environments including high pH, strong acids, abrasive slurries, and significant irradiation. To meet these challenges, a matrix of various polymer, ceramic, and metal additive manufacturing materials have been exposed to a suite of chemical environments of interest as well as radioactive dose (such as gamma radiation from 60 Co) to properly test their durability under these conditions. Mass change has been monitored over a period of up to a week in these conditions, as well as added characterization for surface modification through Scanning Electron Microscopy/Electron Dispersive X-ray analysis (SEM/EDX). Further chemical characterization has been monitored through Fourier-Transform InfraRed Spectroscopy (FTIR), with planned investigation via thermal and tensile strength degradation. While the direct product of this research is identification of material(s) that can withstand specific hazardous environments encountered by the mercury water wash tank in DWPF process simulation experiments, the reference base of materials will be used for many other nuclear processes in the pursuit of rapidly developed, cost-efficient, and highly specific devices for environmental remediation and much more.

Wilson, Nathan W. [Savannah River National Laborat↗

NASA NTRS1995

Surface contamination analysis technology team overview

A team was established which consisted of representatives from NASA (Marshall Space Flight Center and Langley Research Center), Thiokol Corporation, the University of Alabama in Huntsville, AC Engineering, SAIC, Martin Marietta, and Aerojet. The team's purpose was to bring together the appropriate personnel to determine what surface inspection techniques were applicable to multiprogram bonding surface cleanliness inspection. In order to identify appropriate techniques and their sensitivity to various contaminant families, calibration standards were developed. Producing standards included development of consistent low level contamination application techniques. Oxidation was also considered for effect on inspection equipment response. Ellipsometry was used for oxidation characterization. Verification testing was then accomplished to show that selected inspection techniques could detect subject contaminants at levels found to be detrimental to critical bond systems of interest. Once feasibility of identified techniques was shown, selected techniques and instrumentation could then be incorporated into a multipurpose inspection head and integrated with a robot for critical surface inspection. Inspection techniques currently being evaluated include optically stimulated electron emission (OSEE); near infrared (NIR) spectroscopy utilizing fiber optics; Fourier transform infrared (FTIR) spectroscopy; and ultraviolet (UV) fluorescence. Current plans are to demonstrate an integrated system in MSFC's Productivity Enhancement Complex within five years from initiation of this effort in 1992 assuming appropriate funding levels are maintained. This paper gives an overview of work accomplished by the team and future plans.

Burns, H. Dewitt↗

NASA NTRS2002

Vapor transport growth of organic solids in microgravity and unit gravity: some comparisons and results to date

Thin films of an organic nonlinear optical (NLO) material, N, N-dimethyl-p-(2,2-dicyanovinyl) aniline (DCVA), have been grown in space and on the ground by physical vapor transport in an effusive ampoule arrangement. The thin film growth technique developed on the ground is a direct result of information gleaned from experiments in microgravity. This paper covers the results of our experimental investigations for establishing "ideal" terrestrial conditions for deposition of a DCVA film. The active control during the deposition process was exercised by three deposition variables: the material source temperature, the background pressure external to the growth ampoule and the substrate temperature. Successful growth occurred when the difference in temperature between the source material and the copper substrate was 14 degrees C and the background nitrogen pressure was such that the transport was either diffusive or convective. A qualitative diffusion limited boundary was estimated to occur at a pressure of approximately 20 torr. We have probed the DCVA thin films with visible-near infrared reflection absorption spectroscopy, polarized Fourier transform infrared spectrometry, differential interference contrast optical microscopy, and stylus profilometry.

short duration↗

NASA NTRS2015

On the Use of Fourier Transform Infrared (FT-IR) Spectroscopy and Synthetic Calibration Spectra to Quantify Gas Concentrations in a Fischer-Tropsch Catalyst System

One possible origin of prebiotic organic material is that these compounds were formed via Fischer-Tropsch-type (FTT) reactions of carbon monoxide and hydrogen on silicate and oxide grains in the warm, inner-solar nebula. To investigate this possibility, an experimental system has been built in which the catalytic efficiency of different grain-analog materials can be tested. During such runs, the gas phase above these grain analogs is sampled using Fourier transform infrared (FT-IR) spectroscopy. To provide quantitative estimates of the concentration of these gases, a technique in which high-resolution spectra of the gases are calculated using the high-resolution transmission molecular absorption (HITRAN) database is used. Next, these spectra are processed via a method that mimics the processes giving rise to the instrumental line shape of the FT-IR spectrometer, including apodization, self-apodization, and broadening due to the finite resolution. The result is a very close match between the measured and computed spectra. This technique was tested using four major gases found in the FTT reactions: carbon monoxide, methane, carbon dioxide, and water. For the ranges typical of the FTT reactions, the carbon monoxide results were found to be accurate to within 5% and the remaining gases accurate to within 10%. These spectra can then be used to generate synthetic calibration data, allowing the rapid computation of the gas concentrations in the FTT experiments.

Infrared Spectroscopy↗

DOE OSTI2025

Broadband Fourier-Transform Optical Photothermal Infrared Spectroscopy and Imaging

Infrared (IR) spectroscopy is a powerful method for mapping chemical heterogeneity on the microscale. Synchrotron IR radiation uniquely provides a high brightness and broad bandwidth to further extend the capabilities of IR spectroscopic imaging. However, the diffraction-limited spatial resolution of IR spectroscopy is insufficient for studies requiring submicrometer spatial differentiation. Optical photothermal IR (O-PTIR) microscopy is a powerful, emerging method that overcomes the IR diffraction limit in IR hyperspectral imaging by employing a modulated IR beam and a visible probe laser beam to detect local temperature-induced modulation at the visible diffraction limit. In this work, we extend the spectral range of photothermal infrared measurements by incorporating a synchrotron IR source, demonstrating a combined synchrotron-based O-PTIR modality that enables high spatial resolution far-field chemical imaging spanning the entire mid-IR range. Both optical- and fluorescence-detected photothermal modalities were performed using a step-scan interferometer, demonstrating improved spectral range (541-4000 cm-1) when compared to optical photothermal microscopy with commercial laser sources (800-1800 cm-1 for this particular source) and improved spatial resolution, when compared to synchrotron microspectroscopy measurements. Following these initial validation studies, synchrotron Fourier-transform fluorescence-detected photothermal IR spectroscopy in combination with synchrotron microspectroscopy measurements was used to differentiate cells in mouse brain tissue sections, which requires submicron spatial resolutions beyond those accessible by IR spectroscopy alone.

Razumtcev, Aleksandr↗

DOE OSTI2025

A Reduced-Temperature Process for Preparing Atomically Clean Si(100) and SiGe(100) Surfaces with Vapor HF

Silicon processing techniques such as atomic precision advanced manufacturing (APAM) and epitaxial growth require surface preparations that activate oxide desorption (typically >1000 °C) and promote surface reconstruction toward atomically clean, flat, and ordered Si(100)-2 × 1. Here, in this study, we compare the aqueous and vapor phase cleaning of Si and Si/SiGe surfaces to prepare APAM-ready and epitaxy-ready surfaces at lower temperatures. Angle resolved X-ray photoelectron spectroscopy (ARXPS) and Fourier transform infrared (FTIR) spectroscopy indicate that vapor hydrogen fluoride (VHF) cleans dramatically reduce carbon surface contamination and allow the chemically prepared surface to reconstruct at lower temperatures, 600 °C for Si and 580 °C for a Si/Si 0.7 Ge 0.3 heterostructure, into an ordered atomic terrace structure indicated by scanning tunneling microscopy (STM). After thermal treatment and vacuum hydrogen termination, we demonstrate STM hydrogen desorption lithography (HDL) on VHF-treated Si samples, creating reactive zones that enable area-selective chemistry by using a thermal budget similar to CMOS process flows. We anticipate that these results will establish new pathways to integrate APAM with Si foundry processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Multi-Analytical Investigation of Arsenical Transfer and Remediation on Nineteenth-Century Green Books

Books containing heavy metals, specifically nineteenth-century green arsenical books, have been identified at Northwestern University Libraries, raising health and safety concerns related to handling. Copper acetoarsenite pigments, such as emerald green, were detected on book covers, decorative page edges, labels, and other components using noninvasive analytical techniques including X-ray fluorescence (XRF), Raman spectroscopy, and Fourier-transform infrared (FTIR) spectroscopy. Further examination of selected volumes using synchrotron radiation (SR) techniques revealed pigment migration, degradation, and arsenic transfer to adjacent books. This paper expands on initial findings through two related experiments. The first explored the transfer of arsenic using mechanical friction; Staedtler Mars® white vinyl erasers rubbed on arsenical books generated crumbs which were analyzed via scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM-EDX). Results confirmed the transfer of arsenic, copper, and lead, with decorative page edges being particularly prone to shedding arsenic onto other materials. The second experiment tested remediation methods on a book contaminated by prolonged exposure to an arsenical neighbor. Surface cleaning using erasers and a vacuum removed flecks of pigment but did not eliminate non-chromophoric arsenic as confirmed by SR analyses, which highlights its presence either as a degradation product embedded within the paper or present in the paper as part of its production process. Findings demonstrate the acute toxicity risk posed by arsenical books and support the need for safe handling protocols. However, materials with only trace levels of arsenic embedded during production may pose a lower risk of transfer. Cross contamination beyond prolonged direct contact appears limited. These results highlight critical considerations for library preservation practices and future research on arsenic in historical materials.

arsenic↗

NASA NTRS2003

Attachment of Single-wall Carbon Nanotubes (SWNTs) on Platinum Surfaces by Self-Assembling Techniques

Single-wall carbon nanotubes (SWNTs) are very interesting materials because of their morphology, electronic and mechanical properties. Its morphology (high length-to-diameter ratio) and electronic properties suggest potential application of SWNTs as anode material for lithium ion secondary batteries. The introduction of SWNTs on these types of sources systems will improve their performance, efficiency, and capacity to store energy. A purification method has been applied for the removal of iron and amorphous carbon from the nanotubes. Unpurified and purified SWNTs were characterized by transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). In order to attach carbon nanotubes on platinum electrode surfaces, a self-assembled monolayer (SAM) of 4-aminothiophenol (4-ATP) was deposited over the electrodes. The amino-terminated SAM obtained was characterized by cyclic voltammetry, X-ray photoelectron spectroscopy (XPS), and Fourier-transforms infrared (FTIR) spectroscopy. Carbon nanotubes were deposited over the amino-terminated SAM by an amide bond formed between SAM amino groups and carboxylic acid groups at the open ends of the carbon nanotubes.This deposition was characterized using Raman spectroscopy and Scanning Electron microscopy (SEM).

Rosario-Castro, Belinda I.↗

NASA NTRS1995

Surface inspection using FTIR spectroscopy

The use of reflectance Fourier transform infrared (FTIR) spectroscopy as a tool for surface inspection is described. Laboratory instruments and portable instruments can support remote sensing probes that can map chemical contaminants on surfaces with detection limits under the best of conditions in the sub-nanometer range, i.e.. near absolute cleanliness, excellent performance in the sub-micrometer range, and useful performance for films tens of microns thick. Examples of discovering and quantifying contamination such as mineral oils and greases, vegetable oils, and silicone oils on aluminum foil, galvanized sheet steel, smooth aluminum tubing, and sandblasted 7075 aluminum alloy and D6AC steel. The ability to map in time and space the distribution of oil stains on metals is demonstrated. Techniques associated with quantitatively applying oils to metals, subsequently verifying the application, and non-linear relationships between reflectance and the quantity oil are described.

Powell, G. L.↗