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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 NTRS2002

Thermal and Chemical Characterization of Non-Metallic Materials Using Coupled Thermogravimetric Analysis and Infrared Spectroscopy

Thermogravimetric analysis (TGA) is widely employed in the thermal characterization of non-metallic materials, yielding valuable information on decomposition characteristics of a sample over a wide temperature range. However, a potential wealth of chemical information is lost during the process, with the evolving gases generated during thermal decomposition escaping through the exhaust line. Fourier Transform-Infrared spectroscopy (FT-IR) is a powerful analytical technique for determining many chemical constituents while in any material state, in this application, the gas phase. By linking these two techniques, evolving gases generated during the TGA process are directed into an appropriately equipped infrared spectrometer for chemical speciation. Consequently, both thermal decomposition and chemical characterization of a material may be obtained in a single sample run. In practice, a heated transfer line is employed to connect the two instruments while a purge gas stream directs the evolving gases into the FT-IR. The purge gas can be either high purity air or an inert gas such as nitrogen to allow oxidative and pyrolytic processes to be examined, respectively. The FT-IR data is collected realtime, allowing continuous monitoring of chemical compositional changes over the course of thermal decomposition. Using this coupled technique, an array of diverse materials has been examined, including composites, plastics, rubber, fiberglass epoxy resins, polycarbonates, silicones, lubricants and fluorocarbon materials. The benefit of combining these two methodologies is of particular importance in the aerospace community, where newly developing materials have little available data with which to refer. By providing both thermal and chemical data simultaneously, a more definitive and comprehensive characterization of the material is possible. Additionally, this procedure has been found to be a viable screening technique for certain materials, with the generated data useful in the selection of other appropriate analytical procedures for further material characterization.

Huff, Timothy L.↗
NASA NTRS1992

Synthesis and characterization of fine grain diamond films

A fine grain diamond film has been developed by microwave plasma assisted chemical vapor deposition. Various analytical techniques, including Rutherford backscattering, proton recoil analysis, Raman spectroscopy, and X-ray diffraction, were utilized to characterize the diamond films. The grain size of the film was determined from bright and dark field electron micrographs, and found to be 200-1000 A. The films exhibited good optical transmission between 2.5 and 10 microns, with a calculated absorption coefficient of 490/cm. The friction coefficients of this film were found to be 0.035 and 0.030 at dry nitrogen and humid air environments, respectively, and the films had low wear rates.

Wu, Richard L. C.↗
NASA NTRS1977

The role of light microscopy in aerospace analytical laboratories

Light microscopy has greatly reduced analytical flow time and added new dimensions to laboratory capability. Aerospace analytical laboratories are often confronted with problems involving contamination, wear, or material inhomogeneity. The detection of potential problems and the solution of those that develop necessitate the most sensitive and selective applications of sophisticated analytical techniques and instrumentation. This inevitably involves light microscopy. The microscope can characterize and often identify the cause of a problem in 5-15 minutes with confirmatory tests generally less than one hour. Light microscopy has and will make a very significant contribution to the analytical capabilities of aerospace laboratories.

Crutcher, E. R.↗
DOE OSTI2025

A Novel Solid Form of Erlotinib: Synthesis by Heterogeneous Complexation and Characterization by NMR Crystallography

We describe the synthesis of a novel complex of the anticancer "active pharmaceutical ingredient erlotinib (ERL) via heterogeneous nucleation on polished zinc tiles. The resulting product, ERL 2 ·ZnCl 2 , is characterized by single-crystal X-ray diffraction, multinuclear solid-state NMR (ssNMR) spectroscopy, and density functional theory (DFT) calculations. Also characterized are the hydrochloride salt (ERL·HCl) and monohydrate free base (ERL·H 2 O) forms of erlotinib. 13 C ssNMR spectroscopy is useful for site-by-site assignment and rapid fingerprinting, while also providing preliminary structural interpretations, such as the number of molecules in the asymmetric unit. 35 Cl ssNMR can readily differentiate between the chloride ions in ERL·HCl and the covalently bonded chlorine in ERL 2 ·ZnCl 2 . 15 N ssNMR proves to be critical here because of the large isotropic chemical shift differences between ERL·H 2 O, ERL·HCl, and ERL 2 ·ZnCl 2 . The 15 N chemical shift tensors are linked directly to differences in structure and bonding with the aid of DFT calculations. Together, these results demonstrate the utility of multinuclear NMR crystallography for the characterization of solid forms of APIs, especially when other analytical techniques face significant challenges.

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

Systematic characterization of unknown compounds via dimensionality reduction of time series

Analysis of ambient aerosols provides valuable insight into particle sources and formation chemistry. However, due to the complexity of atmospheric data and the dynamic nature of aerosol composition, a substantial fraction of data often become discarded by conventional analysis methods. Furthermore, a large fraction of chemical species within those data are unidentifiable due to a lack of matching spectral information, resulting in suboptimal characterization of chemical composition. Previous work has demonstrated techniques for cataloging analytes in a chromatographic dataset by deconvolution of mass spectra, but integration of these analytes throughout a large dataset remains time consuming. Here, we present a method to automatically identify an ion for quantitation for single-ion chromatogram based peak fitting and integration, enabling comprehensive integration of analytes with minimal user interaction. The resulting time series are clustered with a machine-learning based dimensionality reduction technique to systematically investigate the underlying characteristics of the categorized analytes and gain new insights into the chemical composition and physicochemical properties of the unidentifiable analytes. We apply these methods to existing atmospheric datasets collected in Manacapuru, Brazil during the GoAmazon2014/5 campaign to identify new analytes and interpret their variability and transformations in the atmosphere. The analysis results generate 408 time series from cataloged analytes of interest, and the clustering of those time series with spherical k-means results in 8 distinct clusters. We find the analytes form clusters based on their distinct physicochemical properties, demonstrating the method’s ability to systematically identify and selectively filter contaminants and instrumental analytes and characterize the unidentifiable analytes.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS2002

Test and Analysis Capabilities of the Space Environment Effects Team at Marshall Space Flight Center

Marshall Space Flight Center has developed world-class space environmental effects testing facilities to simulate the space environment. The combined environmental effects test system exposes temperature-controlled samples to simultaneous protons, high- and low-energy electrons, vacuum ultraviolet (VUV) radiation, and near-ultraviolet (NUV) radiation. Separate chambers for studying the effects of NUV and VUV at elevated temperatures are also available. The Atomic Oxygen Beam Facility exposes samples to atomic oxygen of 5 eV energy to simulate low-Earth orbit (LEO). The LEO space plasma simulators are used to study current collection to biased spacecraft surfaces, arcing from insulators and electrical conductivity of materials. Plasma propulsion techniques are analyzed using the Marshall magnetic mirror system. The micro light gas gun simulates micrometeoroid and space debris impacts. Candidate materials and hardware for spacecraft can be evaluated for durability in the space environment with a variety of analytical techniques. Mass, solar absorptance, infrared emittance, transmission, reflectance, bidirectional reflectance distribution function, and surface morphology characterization can be performed. The data from the space environmental effects testing facilities, combined with analytical results from flight experiments, enable the Environmental Effects Group to determine optimum materials for use on spacecraft.

Finckenor, M. M.↗
DOE OSTI2026

Fluorescence Signatures of Rare Earth Metals during Precipitation in Various Conditions

Fluorescence spectroscopy is a widely used sensor methodology that analyzes light emitted from a compound or element as it decays from an excited state. This technique is very sensitive and selective, which is ideal to characterize analytes at lower limits of detection. Key example targets of significant industry and research interest include rare earth elements (REEs) such as dysprosium (Dy) and europium (Eu). These are widely used in advanced technologies including semiconductors, electric vehicle motors, lasers, and permanent magnets. Identifying new sources and responsible reutilization of REEs is essential, and new approaches to extract and recycle REEs could be notably enhanced through the integration of on-line sensors. The sensors can support faster process design, informed scale-up, and cost-effective deployment. This study covers the initial exploration of applying fluorescence-based on-line monitoring to REEs within a precipitation process. This study demonstrates the successful scale-up of a fluorescence -based sensing approach, from stationary cuvettes and small-volume microfluidic devices to continuous flow systems operating at the bench scale (10-25mL). This work also provides initial insight into the challenges of signal’s effects and utility within a turbid environment. Using a modular design for monitoring flowing solutions in a flow tube, fluorescence can be characterized for a variety of analytical targets. In this study, detection performance parameters between the cuvette and flow tube system were compared. Additionally, the response of Dy during precipitation by sodium bicarbonate in the two measurement designs was explored. This letter represents a starting point to bridge the gap between traditional fluorescence sensor measurements in a cuvette to future developments that explore the ability to integrate fluorescence sensors into extraction and separation processes at industrially relevant scales.

fluorescence↗
NASA NTRS1982

Material characterization and specification development for 350 F curing epoxy-graphite materials

New analytical techniques and a processability laminate have been used in the development of a material specification for 350 F curing epoxy-graphite materials. The development of the specification required the evaluation of prepregs which had variations in their processing behavior that were detected only in production. Chemical techniques were used to analyze the prepregs and establish limits on the concentrations of the various chemical constituents. A batch acceptance test laminate was designed to determine suitability of prepregs for production useage. The new specification requires that the processability laminate be ultrasonically and micrographically inspected for voids and porosity. Incorporation of these and other requirements will help to insure material consistency and processability.

Rogers, A. K.↗
NASA NTRS1986

Analytical ultrasonics for characterization of metallurgical microstructures and transformations

The application of contact (piezoelectric) and noncontact (laser generation and detection) ultrasonic techniques for dynamic investigation of precipitation hardening processes in aluminum alloys, as well as crystallization and phase transformation in rapidly solidified amorphous and microcrystalline alloys is discussed. From the variations of the sound velocity and attenuation the precipitation mechanism and kinetics were determined. In addition, a correlation was established between the observed changes in the velocity and attenuation and the mechanical properties of age-hardenable aluminum alloys. The behavior of the elastic moduli, determined ultrasonically, were found to be sensitive to relaxation, crystallization and phase decomposition phenomena in rapidly solidified metallic glasses. Analytical ultrasonics enables determination of the activation energies and growth parameters of the reactions. Therefrom theoretical models can be constructed to explain the changes in mechanical and physical properties upon heat treatment of glassy alloys. The composition dependence of the elastic moduli in amorphous Cu-Zr alloys was found to be related to the glass transition temperature, and consequently to the glass forming ability of these alloys. Dynamic ultrasonic analysis was found to be feasible for on-line, real-time, monitoring of metallurgical processes.

Rosen, M.↗
NASA NTRS1988

Nondestructive evaluation of advanced ceramics

A review is presented of Lewis Research Center efforts to develop nondestructive evaluation techniques for characterizing advanced ceramic materials. Various approaches involved the use of analytical ultrasonics to characterize monolythic ceramic microstructures, acousto-ultrasonics for characterizing ceramic matrix composites, damage monitoring in impact specimens by microfocus X-ray radiography and scanning ultrasonics, and high resolution computed X-ray tomography to identify structural features in fiber reinforced ceramics.

Klima, Stanley J.↗
NASA NTRS2005

Biologically inspired technologies using artificial muscles

One of the newest fields of biomimetics is the electroactive polymers (EAP) that are also known as artificial muscles. To take advantage of these materials, efforts are made worldwide to establish a strong infrastructure addressing the need for comprehensive analytical modeling of their response mechanism and develop effective processing and characterization techniques. The field is still in its emerging state and robust materials are still not readily available however in recent years significant progress has been made and commercial products have already started to appear. This paper covers the current state of- the-art and challenges to making artificial muscles and their potential biomimetic applications.

electroactive↗
NASA NTRS2016

The Search for Surviving Direct Samples of Early Solar System Water

We have become increasingly aware of the fundamental importance of water, and aqueous alteration, on primitive solar-system bodies. All classes of astromaterials studied show some degree of interaction with aqueous fluids. Nevertheless, we are still lacking fundamental information such as the location and timing of the aqueous alteration and the detailed nature of the aqueous fluids. Halite crystals in two meteorite regolith breccias were found to contain aqueous fluid inclusions (brines) trapped approx. 4.5 BYBP. Heating/freezing studies of the aqueous fluid inclusions in these halites demonstrated that they were trapped near 25 C. The initial results of our O and H isotopic measurements on these brine inclusions can be explained by a simple model mixing asteroidal and cometary water. We have been analyzing solids and organics trapped alongside the brines in the halites by FTIR, C-XANES, SXRD and Raman, as clues to the origin of the water. The organics show thermal effects that span the entire range witnessed by organics in all chondrite types. Since we identified water-soluble aromatics, including partially halogenated methanol, in some of the halite, we suspected amino acids were also present, but have thus far found that levels of amino acids were undetectable (which is very interesting). We have also been locating aqueous fluid inclusions in other astromaterials, principally carbonates in CI and CM chondrites. Although we have advanced slowly towards detailed analysis of these ancient brines, since they require techniques right at or just beyond current analytical capabilities, their eventual full characterization will completely open the window onto the origin and activity of early solar system water.

Zolensky, Michael↗
NASA NTRSDate not supplied

Dynamic Characterization of NASA Armstrong Test Facility Mechanical Vibration Facility

In preparation for Sierra Nevada Corporation’s (SNC) Dream Chaser spacecraft vibration test campaign at NASA Armstrong Test Facility (ATF) in Sandusky, Ohio, a dynamic characterization of the Mechanical Vibration Facility (MVF) is currently ongoing. The Mechanical Vibration Facility is comprised of an 18 ft diameter annulus table that is driven with sixteen hydraulic vertical actuator assemblies and four hydraulic horizontal actuator assemblies. During a test campaign this allows for single axis vibration testing in the vertical axis and in each of the two orthogonal horizontal axes without the need for reconfiguring the test article. The dynamic characterization of the facility was defined to follow a building-block approach requiring three vibration test configurations: (1) MVF bare table (2) MVF table and head expander (3) MVF table, head expander, and a dummy test article. Following the completion of the facility dynamic characterization, a facility finite element model (FEM) will be test-verified allowing for more accurate pretest analysis used for determining response limits and abort levels. To date two of the three test configurations have been completed. Test results have been used to verify the facility FEM that includes both the 18 ft diameter annulus table and the aluminum head expander that fills in the center opening of the annulus to provide a continuous flat mounting surface. Both the MVF table and the head expander models were previously correlated using test results from free-free boundary condition modal tests so model updates to the facility FEM focused on the uncorrelated vertical actuator assemblies and horizontal actuator assemblies. The accuracy of the test-verified facility FEM will be further determined based on comparison of analytical and test results from the vibration test of the dummy test article. Efforts will also be made to determine fixed base modes of the test article attached to the flexible vibration table using fixed base correction techniques. This paper will discuss test and analytical results from the MVF dynamic characterization test sequence and corresponding model updating effort.

Emma L Pierson↗
DOE OSTI2025

Mixed Element Microparticle Characterization by Electron Probe Microanalysis

Abstract Microparticle compositional characterization for nuclear forensics has traditionally been achieved by “gold-standard” destructive analytical techniques such as large geometry-secondary ion mass spectrometry and fission track-thermal ionization mass spectrometry, but long processing times and total sample consumption eliminate the option of subsequent analysis by other methods. Electron probe microanalysis has long been widely employed for rapid, nondestructive, micrometer-scale compositional measurements and imaging in fields such as material science and geology and may therefore need to be reevaluated as an alternative tool for microparticle analysis for the nuclear forensics community. This study presents the use of electron probe microanalysis for imaging and quantitative characterization of homogeneous microparticles utilizing a calibration curve based on high-precision quadrupole-inductively coupled plasma-mass spectrometry analyses. Samples of opportunity synthesized at Savannah River National Laboratory, nickel-doped cerium oxide microparticles, were selected as analogs for plutonium-doped uranium oxide microparticles. Positive detection and accurate quantification of variable amounts of nickel dopant down to trace levels (10s of parts per million) suggest applicability of this technique to other mixed element systems (e.g., actinides). Quantitative single-particle characterization via electron probe microanalyzer may thus provide a high fidelity, nondestructive complement to techniques currently in use.

Riche, Alexis T. (ORCID:0009000121978126)↗
DOE OSTI2026

Forensic characterization of surrogate nuclear explosion debris: radiochemical and spectroscopic strategies for method validation

Surrogate nuclear explosion debris (SNED) has emerged as a critical platform for advancing post-detonation nuclear forensic analysis in the absence of readily accessible historic materials. SNED enables controlled investigation and validation of analytical methodologies used to interrogate the chemical, isotopic, radiological, and microstructural signatures preserved in nuclear explosion debris. This review presents an integrated assessment of destructive and non-destructive analytical techniques commonly employed within decision-driven nuclear forensic workflows. Each technique is discussed individually while highlighting how it contributes to different stages of post-detonation analysis. Core methods – including gamma and alpha spectrometry, ICP-MS, TIMS, SIMS, SEM-EDS, XRF, LIBS, vibrational spectroscopy, and X-ray absorption spectroscopy – are critically evaluated with respect to forensic maturity, information content, and matrix limitations. Emphasis is placed on the role of SNED in benchmarking multi-modal workflows and identifying gaps in reproducing heterogeneity, fractionation, and radiation-driven evolution relevant to forensic attribution.

X-ray spectroscopic methods↗
DOE OSTI2025

Development and characterization of an aerosol-generated multi-method analytical particle test material

Ceria (CeO 2 ) particles with low to ultra-low loading of nickel dopant were produced using an aerosol-based, droplet-to-particle synthesis via an in-line calcination technique. This aerosol-based synthesis method enables the production of particles with a monodisperse size distribution. These produced and well-characterized, multi-element, ceria-based particles demonstrate a material exemplar for multi-method analytical testing. They were prepared from a cerium nitrate feedstock where low loading nickel dopant was added at target Ni/(Ni + Ce) atomic percents of 1 %, 0.1 %, and 0.01 %, using a nickel nitrate spike. This methodology proved to produce ceria particles doped with a dynamic range of low to ultra-low loadings of nickel over a 24-h period, with consistent size distribution, morphology, and composition. The successful incorporation of nickel was demonstrated with bulk and single particle inductively coupled plasma mass spectroscopy and revealed notable particle-to-particle elemental homogeneity. X-ray photoelectron spectroscopy demonstrated the presence of a high concentration of nickel dopant incorporated preferentially toward the surface of the particles, and that this dopant aided oxidation of surface Ce(III) atoms to Ce(IV). These particle test materials were then validated through X-ray absorption near edge spectroscopy, comparing the ultra-low 0.01 % Ni and low 1 % Ni-doped ceria samples. This revealed a more-reduced oxidation state of the nickel with an increase in dopant concentration. Finally, this work demonstrates a synthesis and systematic characterization scheme to produce multi-method analytical test particulates.

36 MATERIALS SCIENCE↗
NASA NTRS1993

An advanced test technique to quantify thermomechanical fatigue damage accumulation in composite materials

A mechanical test technique was developed to assist in quantifying the accumulation of damage in composite materials during thermomechanical fatigue (TMF) cycling. This was accomplished by incorporating definitive elastic mechanical property measurements into an ongoing load-controlled TMF test without disturbing the test specimen or significantly altering the test conditions. The technique allows two fundamental composite properties consisting of the isothermal elastic static moduli and the macroscopic coefficient of thermal expansion (CTE) to be measured and collected as functions of the TMF cycles. The specific implementation was incorporated into the commonly employed idealized in-phase and out-of-phase TMF cycles. However, the techniques discussed could be easily implemented into any form of load-controlled TMF mission cycle. By quantifying the degradations of these properties, tremendous insights are gained concerning the progression of macroscopic composite damage and often times the progression of damage within a given constituent. This information should also be useful for the characterization and essential for the verification of analytical damage modeling methodologies. Several examples utilizing this test technique are given for three different fiber lay-ups of titanium metal matrix composites.

Castelli, Michael G.↗
NASA NTRS1975

Systems identification and application systems development for monitoring the physiological and health status of crewmen in space

The use of automated, analytical techniques to aid medical support teams is suggested. Recommendations are presented for characterizing crew health in terms of: (1) wholebody function including physiological, psychological and performance factors; (2) a combination of critical performance indexes which consist of multiple factors of measurable parameters; (3) specific responses to low noise level stress tests; and (4) probabilities of future performance based on present and periodic examination of past performance. A concept is proposed for a computerized real time biomedical monitoring and health care system that would have the capability to integrate monitored data, detect off-nominal conditions based on current knowledge of spaceflight responses, predict future health status, and assist in diagnosis and alternative therapies. Mathematical models could play an important role in this approach, especially when operating in a real time mode. Recommendations are presented to update the present health monitoring systems in terms of recent advances in computer technology and biomedical monitoring systems.

Leonard, J. I.↗