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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 73 records · Page 4

Meteoritic ablation and fusion spherules in Antarctic ice

In the course of two Antarctic expeditions in 1980/1981 and 1982/1983 approximately 4 metric tons of documented ice samples were collected from the Atka Bay Ice Shelf, Antarctica, and subsequently shipped for cosmic dust studies. After filtration of the melt water, approximately 700 Antarctic spherules (AAS) in the size range of 5 to 500 microns were handpicked from the filter residue under optical microscopes. For the chemical investigation of single dust grains the following techniques were applied: scanning electron microscopy (SEM), X-ray analysis (EDAX), instrumental neutron activation analysis (INAA), laser microprobe mass analysis (LAMMA), and accelerator mass spectroscopy (AMS). For more than 95% of the total mass the bulk and trace elements were determined in single grain analyses using EDAX, INAA, and LAMMA. The element pattern of the dust particles was compared with that of typical terrestrial material and meteoritic matter. The majority of the spherules exhibited elemental compositions compatible with meteoritic element patterns.

Thiel, K.↗

Image and compositional characteristics of the LDEF Big Guy impact crater

A 5.2 mm crater in Al-metal represents the largest found on LDEF. We have examined this crater by field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS) and time-of-flight/secondary ion mass spectroscopy (TOF-SIMS) in order to determine if there is any evidence of impactor residue. Droplet and dome-shaped columns, along with flow features, are evidence of melting. EDS from the crater cavity and rim show Mg, C, O and variable amounts of Si, in addition to Al. No evidence for a chondritic impactor was found, and it hypothesized that the crater may be the result of impact with space debris.

Bunch, T. E.↗

Carbon Nanotubes/Nanofibers by Plasma Enhanced Chemical Vapour Deposition

Plasma enhanced chemical vapour deposition (PECVD) has been recently used for the production of vertically aligned carbon nanotubedfibers (CN) directly on substrates. These structures are potentially important technologically as electron field emitters (e.g. microguns, microwave amplifiers, displays), nanoelectrodes for sensors, filter media, superhydrophobic surfaces and thermal interface materials for microelectronics. A parametric study on the growth of CN grown by glow discharge dc-PECVD is presented. In this technique, a substrate containing thin film Ni catalyst is exposed to C2H2 and NH3 gases at 700 C. Without plasma, this process is essentially thermal CVD which produces curly spaghetti-like CN as seen in Fig. 1 (a). With the plasma generated by biasing the substrate at -6OOV, we observed that the CN align vertically during growth as shown in Fig. l(b), and that the magnitude of the applied substrate bias affects the degree of alignment. The thickness of the thin film Ni catalyst was found to determine the average diameter and inversely the length of the CN. The yield and density of the CN were controlled by the use of different diffusion barrier materials under the Ni catalyst. Patterned CN growth [Fig. l(c)], with la variation in CN diameter of 4.1% and 6.3% respectively, is achieved by lithographically defining the Ni thin film prior to growth. The shape of the structures could be varied from very straight nanotube-like to conical tip-like nanofibers by increasing the ratio of C2H2 in the gas flow. Due to the plasma decomposition of C2H2, amorphous carbon (a-C) is an undesirable byproduct which could coat the substrate during CN growth. Using a combination of depth profiled Auger electron spectroscopy to study the substrate and in-situ mass spectroscopy to examine gas phase neutrals and ions, the optimal conditions for a-C free growth of CN is determined.

Teo, K. B. K.↗

Elucidating the corrosion mechanism of Ni-based superalloys in the presence of uranium-containing chloride molten salt

The United States Department of Energy (DOE) is committed to the advancement of nuclear reactor technology through initiatives such as the Advanced Reactor Development Program (ARDP), in an effort to diversify the United States energy portfolio towards more sustainable energy options. The ARDP includes demonstration by industry partners of molten chloride fast reactors (MCFRs). Construction of MCFRs requires qualified nuclear structural materials. Unfortunately, there are no current materials that are fully qualified by the Nuclear Regulatory Commission for the construction of molten salt reactors, including MCFRs. Adapting current structural material qualifications requires expansion of our current knowledgebase on the property-performance relationships regarding corrosion performance. In this investigation, we assess microstructural changes in a Ni-based superalloy after exposure to a UCl3¬-containing chloride salt eutectic mixture through a correlated multi-modal approach combining several advanced characterization techniques, including scanning electron microscopy/focused ion beam (SEM/FIB) and transmission electron microscopy (TEM). SEM/FIB analysis will illustrate changes in elemental composition, microstructure, and isotopic information acquired from energy x-ray dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and secondary ion mass spectroscopy (SIMS), respectively. This information will then aid in identifying localized regions to elucidate the corrosion mechanism with TEM through a combination of electron diffraction, electron energy loss spectroscopy (EELS), and additional EDS. The findings from this investigation will further expand our assessment of the corrosion performance of structural materials in molten salt chloride systems, aiding to developing fully qualified materials for construction of MCFRs.

36 MATERIALS SCIENCE↗

Thermoreflectance Detection of Point Defects Resulting from Focused Ion Beam Milling

Focused ion beam (FIB) milling is a commonly used tool for nanoscale material processing, such as for transmission electron microscopy (TEM) sample preparation, or the creation of fiducial markers prior to other processes and measurements. During milling, a high energy ion beam is used to remove material via sputtering. The expelled target material may return to the sample surface however, affecting subsequent measurements. Beam spreading or irradiation due to neutral gallium may also irradiate a larger area than intended. Extensive research has explored the effects of FIB milling on the prepared TEM sample, but few have looked at the effects of milling on the properties of the sample surrounding the milled region. We use multiple pump-probe laser-based techniques (time domain thermoreflectance and steady-state thermoreflectance) to measure the spatial extent of FIB-induced surface/subsurface changes on a series of silicon wafers milled at multiple currents and doses. We supplement these measurements with high-resolution scanning transmission electron microscopy, energy dispersive X-ray spectroscopy, stylus profilometry, and time-of-flight secondary ion mass spectroscopy. We find a sample surface affected by the FIB up to 1 mm from where milling occurred, with a notable dependence on the ion beam current. We also note remarkably high sensitivity to surface defects using the thermoreflectance metrologies, including detection where other measurements failed.

defects↗

Integrated material-surface analyzer

These 10 surface-analysis tests can be run without breaking vacuum: secondary-ion mass spectroscopy, ion-scattering spectroscopy, electron-stimulated desorption, residual-gas analysis, auger electron spectroscopy, x-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, characteristic-electron energy-loss spectroscopy, scanning electron microscope, scanning low-energy electron probe. Quadruple mass spectrometer, used in first 4 tests, serves as electron transfer lens in last 6 tests.

Grunthaner, F. J.↗

Large-area silicon sheet task

A set of computer models was used to define a growth system configuration that was then built and used to grow web with lower thermally generated stress. Aspects of research in the edge-defined film-fed growth (EFG) method of making Si ribbon are reported. A technique was developed to determine base resistivity and carrier lifetime in semicrystalline wafers. Automated growth of 150 kg of 15 cm-dia ingot material per crucible is reviewed. Scanning transmisson electron microscopy (STEM) and microprobe investigations of processed EFG ribbon are reported. The chemical composition of the large precipitates was studied. The structural arrangement and the electrical activity of distentions or close to the central twin plane in processed material were studied. The electrical and structural properties of grain boundaries in silicon are discussed. Temperature-dependence measurements of zero-bias conductance, a photoconductivity technique, and deep-level transient spectroscopy (DLTS) were developed. A grooving and staining technique, secondary ion mass spectroscopy, and EBIC measurements in scanning electron microscopy were used to study enhanced diffusion of phosphorus at grain boundaries in polycrystaline silicon. The fundamental mechanisms of abrasion and wear and the deformation of Si by a diamond in various fluid environments are described. The efficiency of solar cells made from EFG ribbon and Semix Inc. material is reported.

Morrison, A. D.↗

Co-templating of polyoxoniobates and silicate/germanate trimer-rings in crystals and inorganic gels

Polyoxometalate (POM) supramolecular gels are a growing family of materials, both for understanding fundamental self-assembly and fabricating flexible monolithic materials that retain the function of metal oxides. Here, we exploited the pH-dependent speciation of polyoxoniobates (PONbs), targeting the formation of PONb-containing supramolecular gels that contain other low molecular weight components (silicate, germanate, phosphate, and carbonate). The introduction of gaseous CO 2 into aqueous hexaniobate solutions resulted in the formation of both new crystalline phases and highly transparent gels. The crystalline phases, formulated Cs 24 [Nb 7 O 22 (NbO(CO 3 ) 2 ) 9 (Si 3 O 9 )]·19.6H 2 O and Cs 21 Na 3 [Nb 7 O 22 (NbO(CO 3 ) 2 ) 9 (Ge 3 O 9 )]·33.6H 2 O are templated by a rare planar [X 3 O 9 ] 6− (X = Si, Ge) ring. Crystalline phases were not obtained with phosphate; instead, the gels contain a mixture of phosphate-centred PONbs and network-forming phosphate. POM speciation within the gels, physical properties, and assembly mechanisms were benchmarked by solution and solid-state nuclear magnetic resonance (NMR) spectroscopy, vibrational spectroscopies, small-angle X-ray scattering (SAXS), and thermogravimetry-mass spectroscopy. Optical analysis and dielectric behavior of the gels confirmed that they are highly transparent ionic and electronic conductors. The alkali and hydroxide concentration controls the formation of crystalline materials or supramolecular gels while maintaining the same network building blocks, providing a rare opportunity to describe the molecular-level structure of inorganic amorphous materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

An evaluation: The potential of discarded tires as a source of fuel

The destructive distillation of rubber tire samples was studied by thermogravimetry, differential scanning calorimetry, combustion calorimetry, and mass spectroscopy. The decomposition reaction was found to be exothermic and produced a mass loss of 65 percent. The gas evolution curves that were obtained indicate that a variety of organic materials are evolved simultaneously during the decomposition of the rubber polymer.

Collins, L. W.↗

An evaluation of discarded tires as a potential source of fuel

The destructive distillation of rubber tire samples was studied by thermogravimetry, differential scanning calorimetry, combustion calorimetry, and mass spectroscopy. The decomposition reaction was found to be exothermic and produced a mass loss of 65%. The products from the distillation process were a solid residue with a heating value of about -30 MJ/kg, a liquid with a heating value of about -40 MJ/kg, and a combustible gas of undetermined heating value. The gas evolution curves which were obtained indicate that a variety of organic materials are evolved simultaneously during decomposition of the rubber polymer.

Collins, L. W.↗

High-performance double-focusing mass spectrometer

Double focusing was first employed when mass spectrometers of a simpler design were not capable any longer to satisfy increasing demands in mass spectroscopy. One of the successful instruments of the 1930's was the mass spectrometer designed by Mattauch and Herzog (1934). The compactness of the Mattauch-Herzog geometry became particularly important in connection with studies involving the employment of rockets, satellites, or space probes. Another advantage of the considered spectrometer is related to the capability of measuring several masses of ions simultaneously. The instrument design was, therefore adopted for some rocket flights to the upper atmosphere, the investigation of the upper atmosphere of Mars, and for studying the upper atmosphere of Venus. Attention is given to laboratory applications involving the instrument in a somewhat enlarged version, and aspects of instrument operation and performance.

Nier, A. O.↗

A microwave plasma cleaning apparatus

In a microwave electron cyclotron resonance plasma source, reactive plasmas of oxygen and its mixtures of argon have been used for evaluating plasma cleaning technologies. Small aluminum samples (0.95 x 1.9 cm) were coated with thin films (less than or equal to 20 micrometers in thickness) of Shell Vitrea oil and cleaned with reactive plasmas. The discharge parameters, such as gas pressure, magnetic field, substrate biasing, and microwave power, were varied to change cleaning conditions. A mass spectroscopy (or residual gas analyzer) was used to monitor the status of plasma cleaning. Mass loss of the samples after plasma cleaning was measured to estimate cleaning rates. Measured cleaning rates of low-pressure (0.5-m torr) argon/oxygen plasmas were as high as 2.7 micrometers/min. X-ray photoelectron spectroscopy was used to determine cleanliness of the sample surfaces. In this paper, significant results of the plasma cleaning are reported and discussed.

Tsai, C. C.↗

2023 Cleanroom Monitoring for OSIRIS-REx

OSIRIS-REx is an asteroid sample return mission that delivered asteroid regolith from Bennu to Earth on 9/24/2023 [1]. Cleanroom monitoring of OSIRIS-REx Curation facilities has been ongoing since 2021 when construction of the OSIRIS-REx lab at Johnson Space Center (JSC) was completed [2]. The monitoring continues inside of the OSIRIS-REx lab in Houston. Monitoring was also conducted on a temporary cleanroom constructed inside a hangar at the Utah Test and Training Range (UTTR) to initially receive the Sample Return Capsule (SRC) upon its landing there. The following reports on cleanroom monitoring that has taken place in the months leading up to as well as after OSIRIS-REx return. Monitoring techniques used include particle counts, deployment of Si wafer witness plates (Balazs, Inc.) and Al foil witness plates, gas sampling (Balazs, Inc.) and microbiological monitoring. We collected particle counts at both the lab at JSC as well as the temporary cleanroom at UTTR. Particle counts were taken monthly from six locations in the lab at JSC. Particle counts were taken from seven locations at UTTR in July, August, and September. The UTTR cleanroom particle counts were taken daily in the five days leading to OSIRIS-REx return as well as consistently the day of return (every 2 minutes and 15 seconds 7:21 am- 6:27 pm) from one location inside the cleanroom. The particle counts at UTTR consistently stayed well within the ranges of its required ISO 7 equivalent classification (352,000 maximum particles/ m3 ≥ 0.5 μm). Most analysis showed that the particle counts were far below ISO 7 requirements (highest measured count was 61,484 particles/ m3 ≥ 0.5 um). but the elevated instances correlated to exterior hangar doors being open. Particle counts were reduced when keeping exterior hangar doors closed. The particle counts at JSC have stayed consistently within their ISO 5 equivalent classification (3,520 maximum particles/ m3 ≥ 0.5 um). In most instances, the counts are much better except in one instance where the count measured 13,381 particles/ m3 ≥ 0.5 um. The high spike in particle counts in the JSC lab correlated with the air handlers being shut down temporarily the previous day. The particle counts taken in the same location quickly reduced and measured 0 when taken a month later with the air handlers on. We deployed 8-inch semiconductor polished Si wafer witness plates for 24-hour periods inside of the OSIRIS-REx Curation lab at JSC (in July, August, September, and November 2023) and the cleanroom at UTTR (July and September 2023) to test for possible organic and inorganic contaminants. We also deployed these wafers inside of the OSIRIS-REx Touch-and-Go sample Acquisition Mechanism (TAGSAM) glovebox (where Bennu sample processing occurs) and desiccator (Bennu sample storage) at JSC in August 2023. These samples were all sent to Balazs for analysis via Thermal Desorption Gas Chromatography Mass Spectroscopy (TD-GC-MS) to quantify organic compounds and vapor phase decomposition inductively coupled plasma mass spectrometry (VPD-ICP-MS) to quantify inorganic contaminants. We collected air samples using an adsorbent tube connected to a pump for six hours (100 mL/minute) inside of both the JSC lab and the UTTR cleanroom. These samples were taken at JSC in July, August, September, November, and December and at UTTR in July and September. Additionally, a sample was taken just outside of the TAGSAM glovebox airlock door in July. These samples were sent to Balazs for analysis of volatile organics in air. Overall, the OSIRIS-REx lab at JSC and cleanroom at UTTR yielded very low organic and inorganic contaminants (similar results to Genesis lab at JSC which is ISO 4 equivalent) except for boron, which is attributed to the borosilicate glass in the fan filter units. We collected monthly surface and air samples inside the JSC lab to monitor potential microbial contamination. We report the recovery rate for each sampling event, which is defined as the number of samples exhibiting bacterial or fungal growth divided by the total number of samples collected. Since the lab was commissioned in 2021 the median recovery rate is 29%. This recovery rate is consistent with other ISO 5 equivalent labs used to curate astromaterials collections. Increases in recovery rate correspond to construction and/or extra activity in the lab. However, increases in recovery rate do not reliably correlate to increases in particle counts, which highlights the need for a dedicated microbial monitoring program for biologically sensitive collections. We sampled the temporary clean room at UTTR in July, August, and September of 2023 to monitor potential microbial contamination. The recovery rate decreased from 80% in August to 29% in September. However, in all instances, the diversity of bacteria and fungi was higher in the UTTR cleanroom than in the JSC lab. We routinely collected more than twenty different organisms from the UTTR cleanroom. In the JSC lab the median diversity is 2 organisms. Based on these results we hypothesize that microbes from UTTR could be transported back to JSC with the Bennu samples. To mitigate this risk, in September of 2023, we implemented additional cleaning procedures in the JSC lab to reduce the bioburden on surfaces that could come into direct contact with hardware used to process Bennu samples. Since adopting these additional cleaning measures, the median recovery rate has decreased to 14%. We did not observe an increase in fungal or bacterial diversity in the lab in the October sampling. We will continue to monitor this trend closely for the next several months. Supported by NASA under Award NNH09ZDA007O and Contract NNM10AA11C.

Rachel Comstock Funk↗

Rigor and Reproducibility in Electrocatalysis: Best Practices for Operando Studies

Operando measurements have rapidly expanded the scope of electrocatalysis by enabling direct observation of catalytic interfaces under working conditions and by linking structural, compositional, and spectroscopic observables to activity and selectivity. However, the growth of operando methods has outpaced the adoption of broadly shared experimental standards, creating persistent challenges in reproducibility, interpretation, and comparison across laboratories and platforms. This perspective synthesizes discussions from the 2025 National Science Foundation Workshop on Rigor and Reproducibility in Electrocatalysis and outlines a practical framework for the rigorous use of operando measurements in electrocatalysis. We highlight three recurring needs: careful implementation of complex methods to avoid overinterpretation; recognition that (subtle) differences in reactor architecture, hydrodynamics, and electrical boundary conditions can alter apparent kinetics and selectivity; and transparent reporting standards that enable meaningful cross-comparison without constraining measurement-specific cell innovation. Focusing on widely used techniques (including X-ray and vibrational spectroscopies, mass spectrometry, and electron microscopy), we discuss technique-specific pitfalls, cross-validation strategies, and recurring platform-agnostic considerations such as mass transport, current distribution, temporal-resolution mismatches, and catalyst evolution. This Perspective aims to strengthen the mechanistic inference and improve the reproducibility, comparability, and predictive value of operando electrocatalysis research.

X-ray absorption spectroscopy↗

Optical and Probe Diagnostics Applied to Reacting Flows

We plan to explore three major threads during the fellowship period. The first interrogates the flame synthesis of carbon nanotubes using aerosol catalysts. Laser light scattering will reveal changes in particle size at various heights above the burner. Analysis of the flame gas by mass spectroscopy will reveal the chemical composition of the mixture. Finally, absorption measurements will map the nanotube concentration within the flow. The second thread explores soot oxidation kinetics. Cavity ring-down absorption measurements of the carbonaceous aerosol can provide a measure of the mass concentration with time and, hence, an oxidation rate. Spectroscopic and direct probe measurements will provide the temperature of the system needed for subsequent modeling. The third thread will explore the details of turbulent flame dynamics. Laser induced incandescence will be applied to measurements of soot volume fraction in a 2-d configuration. Analysis of seed tracer particles by planar laser light MIE scattering will reveal the elemental fuel mixture fraction in the flames. Cavity ring-down spectroscopy, a pulsed transient absorption method, will determine the instantaneous mass loading and its fluctuation. Finally, fluorescence measurements will investigate the formation of PAH's in these flames.

Ticich, Thomas M.↗

Non-mass-analyzed ion implantation from a solid phosphorus source

A phosphorus ion beam, extracted from a Freeman ion source charged with elemental phosphorus, has been investigated for use in solar cell fabrication. Mass spectroscopy of the beam indicates the absence of both minority-carrier lifetime degrading impurities and hydrogen. The ion beam, without mass analysis, was used for ion implantation of solar cells, and performance for all cells was found to be equivalent to mass-analyzed controls.

Spitzer, M. B.↗

Determination of the C-12/C-13 and O-16/O-18 ratio in the Martian atmosphere by 10 micron heterodyne spectroscopy

The planetary atmosphere of Mars was studied during the opposition of May, 1984, by means of a 10-micron heterodyne receiver mounted at the Cassegrain focus of a 3-m telescope. On the basis of a model of the Martian atmosphere, the isotopic ratios derived from the fully resolved absorption spectra obtained were compared with the results of Viking probe in situ measurements and terrestrial values; agreement is obtained within statistical errors. It is shown that highly resolving spectroscopy allows for the determination of isotopic ratios in remote sensing with a precision that is comparable to that of in situ mass spectroscopy.

Schrey, U.↗