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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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS1993

Thermal-infrared emission spectroscopy of natural surfaces: Application to coated surfaces

Thermal-infrared vibrational spectroscopy has great potential for remotely determining the composition of planetary surface materials by taking advantage of fundamental molecular vibrational modes that produce spectral features in the range from approximately 3 to greater than 50 microns. Much of the current interest in the thermal infrared wavelength region stems from the deployment of multispectral scanners, such as the Thermal Infrared Multispectral Scanner (TIMS) and the Mars Observer Thermal Emission Spectrometer (TES). In order to support these missions, it is necessary to develop an appropriate library of laboratory measurements. The purpose of this work was to develop a technique which, with a very limited set of assumptions, can be used to determine the emissivity of natural surfaces directly by using emitted energy.

Christensen, Philip R.↗
NASA NTRS2017

Contamination and Surface Preparation Effects on Composite Bonding

Results presented here demonstrate the effect of several prebond surface contaminants (hydrocarbon, machining fluid, latex, silicone, peel ply residue, release film) on bond quality, as measured by fracture toughness and failure modes of carbon fiber reinforced epoxy substrates bonded in secondary and co-bond configurations with paste and film adhesives. Additionally, the capability of various prebond surface property measurement tools to detect contaminants and potentially predict subsequent bond performance of three different adhesives is also shown. Surface measurement methods included water contact angle, Dyne solution wettability, optically stimulated electron emission spectroscopy, surface free energy, inverse gas chromatography, and Fourier transform infrared spectroscopy with chemometrics analysis. Information will also be provided on the effectiveness of mechanical and energetic surface treatments to recover a bondable surface after contamination. The benefits and drawbacks of the various surface analysis tools to detect contaminants and evaluate prebond surfaces after surface treatment were assessed as well as their ability to correlate to bond performance. Surface analysis tools were also evaluated for their potential use as in-line quality control of adhesive bonding parameters in the manufacturing environment.

Kutscha, Eileen O.↗
NASA NTRS1974

Auger spectroscopy of fracture surfaces of ceramics

Results of Auger electron spectroscopy (AES) studies of fracture surfaces in a series of ceramic materials, including Al2O3, MgO, and Si3N4, which were formed using different processing techniques. AES on the fractured surface of a lunar sample is also discussed. Scanning electron micrograph fractography is used to relate the surface chemistry to the failure mode. Combined argon ion sputtering and AES studies demonstrate the local variations in chemistry near the fracture surface. The problems associated with doing AES in insulators are also discussed, and the experimental techniques directed toward solving them are described.

Marcus, H. L.↗
DOE OSTI2024

Time-resolved photoelectron spectroscopy via trajectory surface hopping

Time-resolved photoelectron spectroscopy is a powerful pump-probe technique which can probe nonadiabatic dynamics in molecules. Interpretation of the experimental signals however requires input from theoretical simulations. Advances in electronic structure theory, nonadiabatic dynamics, and theory to calculate the ionization yields, have enabled accurate simulation of time-resolved photoelectron spectra leading to successful applications of the technique. Here, we review the basic theory and steps involved in calculating time-resolved photoelectron spectra, and highlight successful applications.

Chakraborty, Pratip↗
NASA NTRSDate not supplied

Examination of Lunar Regolith Simulants By SEM-EDS and Imaging Raman Spectroscopy

The Artemis series lunar missions will include sample returns from the lunar south pole. Lunar regolith simulants (RS) generated in the lab provide opportunities to compare two surface science techniques: scanning electron microscopy (SEM-EDS) and Raman induced surface spectroscopy. The results will also be applicable for supporting future commercial lunar payload services (CLPS) and Artemis surface. Surface characterization contributes to continued development of lunar regolith studies and adds to various regolith databases. In characterizing various lunar regolith simulants, part of the aim should be to standardize techniques and utilize anticipated methods available for astromaterials studied during, or returned from, upcoming missions, particularly samples collected from the Moon’s south pole and permanently shadowed regions (PSRs).. An initial survey of available simulants has been started with Raman scanning process for particle counting the results of which will enrich the NASA-JSC Simulant Development Lab (SDL) simulant properties database and the Colorado School of Mines Planetary Simulant Data Base. An SEM-EDS dataset of raw regolith simulant materials are collected.

Raman Microscopy↗
DOE OSTI2023

Surface Chemistry and Reactions for Bimetallic Au Catalysis (Final Report)

Gold-based catalysts offer tremendous opportunities for developing new technologies for selective oxidation reactions that directly use gas-phase oxygen as a benign reagent and produce either no byproducts or water as the only byproduct. These processes are urgently needed and critical for achieving the sustainable production of chemicals. While recent studies demonstrate that the catalytic properties of gold can be significantly enhanced by addition of other metals, the development of these catalysts with sufficient performance for commercialization is hindered by a lack of fundamental understanding of how the catalytic properties of gold can be controlled and tailored. This project addressed this need by synergistically combining experimental and computational studies to establish fundamental composition-structure-activity relationships for gold-based catalysts for several industrially important reactions. Results from surface spectroscopy, atomic imaging and thermal desorption experiments were combined with molecular models and reaction mechanisms from quantum chemical calculations to link observable reaction rates to the structure and composition of surfaces at the molecular level. The results were used to develop improved catalyst formulations and identify optimized reaction conditions for gold-based catalysts. For broader impacts, the developed methodology was extended to other metallic catalysts, such as silver, platinum-molybdenum and nickel-tin, for improved catalytic efficiency and sustainable production of specialty and commodity chemicals.

36 MATERIALS SCIENCE↗
NASA NTRS1987

Stability and rheology of dispersions of silicon nitride and silicon carbide

The relationship between the surface and colloid chemistry of commercial ultra-fine silicon carbide and silicon nitride powders was examined by a variety of standard characterization techniques and by methodologies especially developed for ceramic dispersions. These include electrokinetic measurement, surface titration, and surface spectroscopies. The effects of powder pretreatment and modification strategies, which can be utilized to augment control of processing characteristics, were monitored with these technologies. Both silicon carbide and nitride were found to exhibit silica-like surface chemistries, but silicon nitride powders possess an additional amine surface functionality. Colloidal characteristics of the various nitride powders in aqueous suspension is believed to be highly dependent on the relative amounts of the two types of surface groups, which in turn is determined by the powder synthesis route. The differences in the apparent colloidal characteristics for silicon nitride powders cannot be attributed to the specific absorption of ammonium ions. Development of a model for the prediction of double-layer characteristics of materials with a hybrid site interface facilitated understanding and prediction of the behavior of both surface charge and surface potential for these materials. The utility of the model in application to silicon nitride powders was demonstrated.

Feke, Donald L.↗
NASA NTRS1972

Thermal effects in equilibrium surface segregation in a copper/10-atomic-percent-aluminum alloy using Auger electron spectroscopy

Equilibrium surface segregation of aluminum in a copper-10-atomic-percent-aluminum single crystal alloy oriented in the /111/ direction was demonstrated by using Auger electron spectroscopy. This crystal was in the solid solution range of composition. Equilibrium surface segregation was verified by observing that the aluminum surface concentration varied reversibly with temperature in the range 550 to 850 K. These results were curve fitted to an expression for equilibrium grain boundary segregation and gave a retrieval energy of 5780 J/mole (1380 cal/mole) and a maximum frozen-in surface coverage three times the bulk layer concentration. Analyses concerning the relative merits of sputtering calibration and the effects of evaporation are also included.

Ferrante, J.↗
NASA NTRS1999

Secondary Electron Emission Spectroscopy of Diamond Surfaces

This report presents the results of the secondary electron emission spectroscopy study of hydrogenated diamond surfaces for single crystals and chemical vapor-deposited polycrystalline films. One-electron calculations of Auger spectra of diamond surfaces having various hydrogen coverages are presented, the major features of the experimental spectra are explained, and a theoretical model for Auger spectra of hydrogenated diamond surfaces is proposed. An energy shift and a change in the line shape of the carbon core-valence-valence (KVV) Auger spectra were observed for diamond surfaces after exposure to an electron beam or by annealing at temperatures higher than 950 C. This change is related to the redistribution of the valence-band local density of states caused by hydrogen desorption from the surface. A strong negative electron affinity (NEA) effect, which appeared as a large, narrow peak in the low-energy portion of the spectrum of the secondary electron energy distribution, was also observed on the diamond surfaces. A fine structure in this peak, which was found for the first time, reflected the energy structure of the bottom of the conduction band. Further, the breakup of the bulk excitons at the surface during secondary electron emission was attributed to one of the features of this structure. The study demonstrated that the NEA type depends on the extent of hydrogen coverage of the diamond surface, changing from the true type for the completely hydrogenated surface to the effective type for the partially hydrogenated surface.

Krainsky, Isay L.↗
DOE OSTI2024

Subsurface Spectroscopy in Heterogeneous Materials Using Self-Healing Laser Beams

Self-healing optical beams are a class of propagation modes that can recover their beam shapes after distortion or partial blockage. This self-healing property makes them attractive for use in applications involving turbid media as they can—in theory—penetrate further into these materials than standard Gaussian beams. In this paper, we characterize the propagation of two different self-healing beams (Bessel and Airy) through a solid scattering material with different scatterer concentrations and find that both beams do recover after scattering for samples below a threshold scatterer concentration. Additionally, we test the applicability of both beam shapes for improved sub-surface spectroscopy in heterogeneous materials using fluorescent particles and find that there is an average fluorescence intensity enhancement of 1.3× using self-healing beams versus a standard Gaussian beam.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Distinct Mechanism of Anti-Corrosion and Swelling-Adhesion Modeling of Low-Dimensional Nylon-Fluoropolymer Composite Coatings

Compared to other polymers, composite coatings with fluoropolymers as the matrix have attracted considerable interest due to their mechanical performance, chemical stability, and low surface energy. Herein, we present an anticorrosion mechanism of fluoropolymer composite coatings achieved by dispersing varying amounts of polyamide 12 (PA-12) particles over a poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) matrix. The choice of PVDF-HFP as a coating matrix was driven by its superior processability and mechanical properties over Teflon, while PA-12 afforded swelling capacity, preventing electrolyte permeation, and inhibiting matrix stress crack propagation. The corrosion resistance of the coatings was assessed mainly by potentiodynamic polarization and impedance measurements while being immersed in a NaCl solution. Our electrochemical measurement findings showed that 0.75% w/w PA-12 in the PVDF-HFP matrix significantly enhanced corrosion protection even after 21 days of immersion. Microscopy, dielectric spectroscopy, surface analysis, and mechanical testing (American Society for Testing and Materials standards) corroborated the results. PVDF-HFP coatings containing a minimum percolation threshold of 0.75 wt % PA-12 with 1 mil thickness on mild steel exhibited a remarkable increase in resistance and film adhesion, and a notable corrosion rate decrease. Finite element analysis simulation with a bilinear traction-separation law confirmed the swelling mechanism and adhesion behavior. Finally, this study highlights the potential of nylon particle dispersion in PVDF-HFP matrices as a practical approach to developing advanced anticorrosion coatings with promising practical applications in various industries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2004

New Material for Surface-Enhanced Raman Spectroscopy

A chemical method of synthesis and application of coating materials that are especially suitable for surface-enhanced Raman spectroscopy (SERS) has been developed. The purpose of this development is to facilitate the utilization of the inherently high sensitivity of SERS to detect chemicals of interest (analytes) in trace amounts, without need for lengthy sample preparation. Up to now, the use of SERS has not become routine because the methods available have not been able to reproduce sampling conditions and provide quantitative measurements. In contrast, the coating materials of the present method enable analysis with minimum preparation of samples, and SERS measurements made using these materials are reproducible and reversible. Moreover, unlike in methods investigated in prior efforts to implement SERS, sampling is not restricted to such specific environments as electrolytes or specific solvents. The coating materials of this method are porous glasses, formed in sol-gel processes, that contain small particles of gold or silver metal. Materials of this type can be applied to the sample-contact surfaces of a variety of sampling and sensing devices, including glass slides, glass vials, fiber-optic probes, and glass tubes. Glass vials with their insides coated according to this method are particularly convenient for SERS to detect trace chemicals in solutions: One simply puts a sample solution containing the analyte(s) into a vial, then puts the vial into a Raman spectrometer for analysis. The chemical ingredients and the physical conditions of the sol-gel process have been selected so that the porous glass formed incorporates particles of the desired metal with size(s) to match the wavelength(s) of the SERS excitation laser in order to optimize the generation of surface plasmons. The ingredients and processing conditions have further been chosen to tailor the porosity and polarity of the glass to optimize the sample flow and the interaction between the analyte(s) and the plasmon field that generates Raman photons. The porous silica network of a sol-gel glass creates a unique environment for stabilizing SERS-active metal particles. Relative to other material structures that could be considered for SERS, the porous silica network offers higher specific surface area and thus greater interaction between analyte molecules and metal particles. Efforts to perform SERS measurements with the help of sampling devices coated by this method have been successful. In tests, numerous organic and inorganic chemicals were analyzed in several solvents, including water. The results of the tests indicate that the SERS measurements were reproducible within 10 percent and linear over five orders of magnitude. One measure of the limits of detectability of chemicals in these tests was found to be a concentration of 300 parts per billion. Further development may eventually make it possible to realize the full potential sensitivity of SERS for detecting some analytes in quantities as small as a single molecule.

Farquharson, Stuart↗
DOE OSTI2025

Water structure and electric fields at the interface of oil droplets

Interfacial water exhibits rich and complex behaviour, playing an important part in chemistry, biology, geology and engineering. However, there is still much debate on the fundamental properties of water at hydrophobic interfaces, such as orientational ordering, the concentration of hydronium and hydroxide, improper hydrogen bonds and the presence of large electric fields. This controversy arises from the challenges in measuring interfacial systems, even with the most advanced experimental techniques and theoretical approaches available. Here we report on an in-solution, interface-selective Raman spectroscopy method using multivariate curve resolution to probe hexadecane-in-water emulsions, aided by a monomer-field theoretical model for Raman spectroscopy. Our results indicate that oil-water emulsion interfaces can exhibit reduced tetrahedral order and weaker hydrogen bonding, along with a substantial population of free hydroxyl groups that experience about 95 cm -1 redshift in their stretching mode compared with planar oil-water interfaces. Given the known electrostatic zeta potential characteristic of oil droplets, we propose the existence of a strong electric field (about 50-90 MV cm -1 ) emanating from the oil phase. This field is inferred indirectly but supported by control experiments and theoretical estimates. These observations are either absent or opposite in the molecular hydrophobic interface formed by small solutes or at planar oil-water interfaces. Instead, water structural disorder and enhanced electric fields emerge as unique features of the mesoscale interface in oil-water emulsions, potentially contributing to the accelerated chemical reactivity observed at hydrophobic-water interfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Lanthanide binding peptide surfactants at air–aqueous interfaces for interfacial separation of rare earth elements

Rare earth elements (REEs) are critical materials to modern technologies. They are obtained by selective separation from mining feedstocks consisting of mixtures of their trivalent cation. We are developing an all-aqueous, bioinspired, interfacial separation using peptides as amphiphilic molecular extractants. Lanthanide binding tags (LBTs) are amphiphilic peptide sequences based on the EF-hand metal binding loops of calcium-binding proteins which complex selectively REEs. We study LBTs optimized for coordination to Tb 3+ using luminescence spectroscopy, surface tensiometry, X-ray reflectivity, and X-ray fluorescence near total reflection, and find that these LBTs capture Tb 3+ in bulk and adsorb the complex to the interface. Molecular dynamics show that the binding pocket remains intact upon adsorption. We find that, if the net negative charge on the peptide results in a negatively charged complex, excess cations are recruited to the interface by nonselective Coulombic interactions that compromise selective REE capture. If, however, the net negative charge on the peptide is −3, resulting in a neutral complex, a 1:1 surface ratio of cation to peptide is achieved. Surface adsorption of the neutral peptide complexes from an equimolar mixture of Tb 3+ and La 3+ demonstrates a switchable platform dictated by bulk and interfacial effects. The adsorption layer becomes enriched in the favored Tb 3+ when the bulk peptide is saturated, but selective to La 3+ for undersaturation due to a higher surface activity of the La 3+ complex.

Ortuno Macias, Luis E. (ORCID:0000000284342192)↗
NASA NTRS1985

Chemical structure of interfaces

The interfacial structure of silicon/dielectric and silicon/metal systems is particularly amenable to analysis using a combination of surface spectroscopies together with a variety of chemical structures of Si/SiO2, Si/SiO2Si3N4, Si/Si2N2O, Si/SiO2/Al, and Si/Native Oxide interfaces using high resolution (0.350 eV FWHM) X ray photoelectron spectroscopy. The general structure of these dielectric interfaces entails a monolayer chemical transition layer at the Si/dielectric boundary. Amorphous Si substrates show a wide variety of hydrogenated Si and Si(OH) sub x states that are not observed in thermal oxidation of single crystal material. Extended SiO2 layers greater than 8 A in thickness are shown to be stoichiometric SiO2, but to exhibit a wide variety of local network structures. In the nitrogen containing systems, an approach to stoichiometric oxynitride compounds with interesting impurity and electron trapping properties are seen. In native oxides, substantial topographical nonuniformity in oxide thickness and composition are found. Analysis of metal/oxide interfacial layers is accomplished by analytical removal of the Si substrate by UHV XeF2 dry etching methods.

Grunthaner, F. J.↗