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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
All sourcesNASA NTRSDOE OSTI
NASA NTRS1985

Ellipsometric surface analysis of wear tracks produced by different lubricants

Ellipsometric analyses of wear tracks in berings of M-50 steel were carried out after operation under severe conditions with different lubricant additives. The base lubricant was a synthetic ester. It was found that the surface and wear additives benzotirazole and tricresylyphosphate produced very patchy oxide layers. Dioctyldiphenylamine, a common antioxidant, on the other hand produced smoother films. The analyses were performed with a specially designed and constructed ellipsometer of very high (20 micron) spatial resolution. The results are consistent with data obtained by Auger electron spectroscopy.

Lauer, J. L.↗
DOE OSTI2020

Multi-modal surface analysis of porous films under operando conditions

Practical catalysts with a porous framework, such as zeolites, host catalytic reactions at active sites engrained in the pores and channels of the scaffold. The mechanism of interaction at these active sites, defining catalyst performance, remains elusive, in large part, due to the lack of surface characterization methods available for thick films or powders. Here, we present thin film analogs of practical catalysts that allow for the implementation of surface characterization tools, including advanced microscopy and operando spectroscopy methodologies. Specifically, we investigated bilayer silica, MFI nanosheets, and UiO-66 thin films using a multi-modal approach addressing film growth, characterization, and gas adsorption aimed at understanding catalytic activity, reactivity, and selectivity properties, as defined by molecular-level changes in the reaction mechanism.

36 MATERIALS SCIENCE↗
NASA NTRS2002

Surface Analysis and Tools

This article is a chapter of the book entitled, "Tribology of Mechanical Systems," to be published by ASME Press, New York, NY. It describes selected analytical techniques, which are being used in understanding phenomena and mechanisms of oxidation, adhesion, bonding, friction, erosion, abrasion, and wear, and in defining the problems. The primary emphasis is on microanalytical approaches to engineering surfaces.

Miyoshi, Kazuhisa↗
DOE OSTI2023

Surface Analysis Insight Note: Observations relating to photoemission peak shapes, oxidation state, and chemistry of titanium oxide films

It is common practice to describe the coordination of metal atoms in a binding configuration with their nearest neighbors in terms of oxidation state, a measure by which the number of electrons redistributed between atoms forming chemical bonds. In XPS terms, change to an oxidation state is commonly inferred by correlating photoemission signal with binding energy. The assumption, when classifying photoemission signals into distinct spectral shapes, is that a distribution of intensities shifted to lower binding energy is evidence of a reduction in oxidation state. In this Insight note, we raise the prospect that changes in photoemission peak shape may occur without obvious changes, determined by XPS in stoichiometry for a material. It is well known that TiO 2 measured by XPS yields reproducible Ti 2p photoemission peaks. However, on exposing TiO 2 to ion beams, Ti 2p photoemission evolves to complex distributions in intensity, which are particularly difficult to analyze by traditional fitting of bell-shaped curves to these data. For these reasons, in this Insight note, a thin film of TiO 2 deposited on a silicon substrate is chosen for analysis by XPS and linear algebraic techniques. Alterations in spectral shapes created from modified TiO 2 , which might be interpreted as the change in oxidation state, are assessed in terms of relative proportions of titanium to oxygen. It is found through detailed analysis of spectra that quantification by XPS, using procedures routinely used in practice, is not in accord with the typical interpretations of photoemission shapes. The data processing methods used and results presented in this work are of particular relevance to elucidating fundamental phenomena governing the surface evolution of materials-enabled energy processes where cyclic/non-steady usage changes the nature of bonding, especially in the presence of contaminants.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1977

A fundamental approach to adhesion: Synthesis, surface analysis, thermodynamics and mechanics

The effects of composites as adherends was studied. Several other variables were studied by fractography: aluminum powder adhesive filler, fiber glass cloth scrim or adhesive carrier, new adhesives PPQ-413 and LARC-13, and strength-test temperature. When the new results were juxtaposed with previous work, it appeared that complex interactions between adhesive, adherend, bonding, and testing conditions govern the observed strength and fracture-surface features. The design parameters likely to have a significant effect upon strength-test results are listed.

Dwight, D. W.↗
DOE OSTI2022

Surface analysis insight note: Synthetic line shapes, integration regions and relative sensitivity factors

Here, methods for estimating photoemission intensity from X-ray photoelectron spectroscopy data are examined. The role played by “synthetic” bell-shaped curves, integration intervals, background curves, and the use of relative sensitivity factors (RSFs) in reporting percentage atomic concentration for a sample is presented. In particular, photoemission lines with differing energy distributions obtained from the NaCl sample surface are used to demonstrate how a comparison of photoemission intensities is dependent on the line shapes, background curves, and appropriate use of RSFs.

42 ENGINEERING↗
NASA NTRS1985

Fracture surface analysis in composite and titanium bonding: Part 1: Titanium bonding

Fractured lap shear Ti 6-4 adherends bonded with polyphenyquinoxaline (PPQ) and polysulfone were analyzed. The effects of adherend pretreatment, stress level, thermal aging, anodizing voltage, and modified adhesive of Ti 6-4 adherend bonded with PPQ on lap shear strength were studied. The effect of adherend pretreatment on lap shear strength was investigated for PS samples. Results of scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) used to study the surface topography and surface composition are also discussed.

Sanderson, K. A.↗
DOE OSTI2021

Nickel(ii) complexes based on dithiolate–polyamine binary ligand systems: crystal structures, hirshfeld surface analysis, theoretical study, and catalytic activity study on photocatalytic hydrogen generation

To ascertain the influence of binary ligand systems [1,1-dicyanoethylene-2,2-dithiolate (i-mnt -2 ) and polyamine {tetraen = tris(2-aminoethyl)amine, tren = diethylene triamine and opda = o-phenylenediamine}] on the coordination modes of the Ni(II) metal center and resulting supramolecular architectures, a series of nickel(II) thiolate complexes [Ni(tetraen)(i-mnt)](DMSO) (1), [Ni 2 (tren) 2 (i-mnt) 2 ] (2), and [Ni 2 (i-mnt) 2 (opda) 2 ] n (3) have been synthesized in high yield in one step in water and structurally characterized by single crystal X-ray crystallography and spectroscopic techniques. X-ray diffraction studies disclose the diverse i-mnt -2 coordination to the Ni +2 center in the presence of active polyamine ligands, forming a slightly distorted octahedral geometry (NiN 4 S 2 ) in 1, square planar (NiS 4 ) and distorted octahedral geometries (NiN 6 ) in the bimetallic co-crystallized aggregate of cationic [Ni(tren) 2 ] +2 and anionic [Ni(i-mnt) 2 ] -2 in 2, and a one dimensional (1D) polymeric chain along the [100] axis in 3, having consecutive square planar (NiS 4 ) and octahedral (NiN 6 ) coordination kernels. The N–H···O, N–H···S, N–H···N, N–H···S, N–H···N, and N–H···O type hydrogen bonds stabilize the supramolecular assemblies in 1, 2, and 3 respectively imparting interesting graph-set-motifs. The molecular Hirshfeld surface analyses (HS) and 2D fingerprint plots were utilized for decoding all types of non-covalent contacts in the crystal networks. Atomic HS analysis of the Ni +2 centers reveals significant Ni–N metal–ligand interactions compared to Ni–S interactions. We have also studied the unorthodox interactions observed in the solid state structures of 1–3 by QTAIM and NBO analyses. Moreover, all the complexes proved to be highly active water reduction co-catalysts (WRC) in a photo-catalytic hydrogen evolution process involving iridium photosensitizers, wherein 2 and 3 having a square planar arrangement around the nickel center(s) – were found to be the most active ones, achieving 1000 and 1119 turnover numbers (TON), respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1977

A fundamental approach to adhesion: Synthesis, surface analysis, thermodynamics and mechanics

The ability of SEM/EDAX to determine the physical and chemical composition of very small areas was used to study several diverse types of samples representative of NASA-LaRC technology. More systematic investigation was carried out on differences in the results of grit-blasting Ti 6-4 adherends and the presence of extraneous elements, primarily silicon, in some polymer/HT-S fiber composites. Initial results were obtained from a fractured (ILS) short-beam shear specimen, and from Ti 6-4 alloy, before and after a proprietary Boeing anodizing surface preparation for adhesive bonding. Photomicrographs and EDAX spectra were also obtained from new, fractured lap shear strength specimens that employed PPQ and LARC-13 adhesives.

Dwight, D. W.↗
NASA NTRS1985

Surface analysis of space telescope material specimens

Qualitative and quantitative data on Space Telescope materials which were exposed to low Earth orbital atomic oxygen in a controlled experiment during the 41-G (STS-17) mission were obtained utilizing the experimental techniques of Rutherford backscattering (RBS), particle induced X-ray emission (PIXE), and ellipsometry (ELL). The techniques employed were chosen with a view towards appropriateness for the sample in question, after consultation with NASA scientific personnel who provided the material specimens. A group of eight samples and their controls selected by NASA scientists were measured before and after flight. Information reported herein include specimen surface characterization by ellipsometry techniques, a determination of the thickness of the evaporated metal specimens by RBS, and a determination of trace impurity species present on and within the surface by PIXE.

Fromhold, A. T.↗
NASA NTRS1985

Fracture surface analysis in composite and titanium bonding

To understand the mechanical properties of fiber-reinforced composite materials, it is necessary to understand the mechanical properties of the matrix materials and of the reinforcing fibers. Another factor that can affect the mechanical properties of a composite material is the interaction between the fiber and the matrix. In general, composites with strong fiber matrix bonding will give higher modulus, lower toughness composites. Composites with weak bonding will have a lower modulus and more ductility. The situation becomes a bit more complex when all possibilities are examined. To be considered are the following: the properties of the surface layer on the fiber, the interactive forces between polymer and matrix, the surface roughness and porosity of the fiber, and the morphology of the matrix polymer at the fiber surface. In practice, the surface of the fibers is treated to enhance the mechanical properties of a composite. These treatments include anodization, acid etching, high temperature oxidation, and plasma oxidation, to name a few. The goal is to be able to predict the surface properties of carbon fibers treated in various ways, and then to relate surface properties to fiber matrix bonding.

Devilbiss, T. A.↗
DOE OSTI2023

Micro- and Nanoscale Surface Analysis of Late Iron Age Glass from Broborg, a Vitrified Swedish Hillfort

Abstract Archaeological glasses with prolonged exposure to biogeochemical processes in the environment can be used to understand glass alteration, which is important for the safe disposal of vitrified nuclear waste. Samples of mafic and felsic glasses with different chemistries, formed from melting amphibolitic and granitoid rocks, were obtained from Broborg, a Swedish Iron Age hillfort. Glasses were excavated from the top of the hillfort wall and from the wall interior. A detailed microscopic, spectroscopic, and diffraction study of surficial textures and chemistries were conducted on these glasses. Felsic glass chemistry was uniform, with a smooth surface showing limited chemical alteration (<150 nm), irrespective of the position in the wall. Mafic glass was heterogeneous, with pyroxene, spinel, feldspar, and quartz crystals in the glassy matrix. Mafic glass surfaces in contact with topsoil were rougher than those within the wall and had carbon-rich material consistent with microbial colonization. Limited evidence for chemical or physical alteration of mafic glass was found; the thin melt film that coated all exposed surfaces remained intact, despite exposure to hydraulically unsaturated conditions, topsoil, and associated microbiome for over 1,500 years. This supports the assumption that aluminosilicate nuclear waste glasses will have a high chemical durability in near-surface disposal facilities.

Matthews, Bethany E. (ORCID:0000000171932583)↗
NASA NTRS1992

Multidisciplinary design optimization using response surface analysis

Aerospace conceptual vehicle design is a complex process which involves multidisciplinary studies of configuration and technology options considering many parameters at many values. NASA Langley's Vehicle Analysis Branch (VAB) has detailed computerized analysis capabilities in most of the key disciplines required by advanced vehicle design. Given a configuration, the capability exists to quickly determine its performance and lifecycle cost. The next step in vehicle design is to determine the best settings of design parameters that optimize the performance characteristics. Typical approach to design optimization is experience based, trial and error variation of many parameters one at a time where possible combinations usually number in the thousands. However, this approach can either lead to a very long and expensive design process or to a premature termination of the design process due to budget and/or schedule pressures. Furthermore, one variable at a time approach can not account for the interactions that occur among parts of systems and among disciplines. As a result, vehicle design may be far from optimal. Advanced multidisciplinary design optimization (MDO) methods are needed to direct the search in an efficient and intelligent manner in order to drastically reduce the number of candidate designs to be evaluated. The payoffs in terms of enhanced performance and reduced cost are significant. A literature review yields two such advanced MDO methods used in aerospace design optimization; Taguchi methods and response surface methods. Taguchi methods provide a systematic and efficient method for design optimization for performance and cost. However, response surface method (RSM) leads to a better, more accurate exploration of the parameter space and to estimated optimum conditions with a small expenditure on experimental data. These two methods are described.

Unal, Resit↗
DOE OSTI2025

Material Extrusion Printing of Poly(Acrylonitrile‐Styrene‐Acrylate) and Poly(Acrylonitrile‐Butadiene‐Styrene) Structures Reinforced with Poly(Phenylene Oxide) Additives for Improved Thermomechanical Properties and their Surface Analysis by Time‐of‐Flight Secondary Ion Mass Spectrometry

Fused filament fabrication offers the ability to 3D print complex geometries made from plastic filament materials; however, these parts are mechanically outperformed by parts created by traditional fabrication methods. To overcome this challenge, a high-performance polymer poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) is incorporated as an additive into two common engineering thermoplastics, poly(acrylonitrile-styrene-acrylate) (ASA) and poly(acrylonitrile-butadiene-styrene) (ABS). Structures printed from these polymer blends are more mechanically robust compared to those prepared from the parent polymers, with low loading levels (1–5 wt%) of PPO improving the elastic strength by up to ≈30% relative to the parent terpolymers. Even at higher loading levels (10 and 20 wt% PPO), there is no evidence of additive aggregation in the model thin films, which is supported by compositional analysis of the copolymers and chemical analysis via time-of-flight secondary ion mass spectrometry. The enhancements in mechanical properties of ASA and ABS blends appear to be a consequence of homogeneous incorporation of the PPO additive. In conclusion, this work explores expanding materials-property space using miscible blends of engineering thermoplastics to improve mechanical performance as a general approach to overcoming challenges with parts created by melt-based material extrusion printing.

additive manufacturing↗
DOE OSTI2022

Surface analysis insight note: Differentiation methods applicable to noisy data for determination of sp2‐ versus sp3‐hybridization of carbon allotropes and AES signal strengths

The derivatives of the spectra are commonly used for quantification in Auger Electron Spectroscopy (AES) spectra, while the derivative of the KLL C Auger line has proven to be valuable in obtaining a measure of the relative proportions of sp 2 ‐ and sp 3 ‐hybridization using the D‐parameter in both AES and X‐ray Photoelectron Spectroscopy (XPS). Differentiation of X‐ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES) spectra by numerical means is presented and illustrated for polymeric, such as PEEK and Nylon, as well as for graphitic materials including highly ordered pyrolytic graphite and graphene oxide. The most commonly available Savitzky–Golay method is explained mathematically and developed through the case of constructing a 5‐point quadratic polynomial convolution kernel suitable for differentiating spectra of adequate signal to noise. The concept of differentiation of spectra where signal to noise is less than adequate is also developed. Two alternative strategies to Savitzky–Golay differentiation are presented, which fit curves to data that allow derivatives to be obtained where Savitzky–Golay would otherwise fail. These alternative methods involve constructing a parametric curve that fits data over the entire energy interval of interest. Derivatives of spectra are then obtained by differentiating these parametric curves directly. A comparison of results for different materials for which specific sp 2 ‐ vs sp 3 ‐hybridized carbon proportions are of interest is used to emphasize the importance of characterizing methods used to differentiate spectra and understanding the characteristics of instrumentation used to measure spectra. The case for using Principal Component Analysis noise reduction with C KLL spectra is made for spectra collected from a heterogeneous graphene oxide sample.

Fairley, Neal↗
DOE OSTI2023

Surface analysis insight note: X‐ray photoelectron spectroscopy analysis of battery electrodes—Challenges with nickel–manganese–cobalt and Li examples using an Al Kα x‐ray source

X‐ray photoelectron spectroscopy (XPS) has become a highly important tool for the analysis of battery materials and components. However, both anecdotal and detailed analysis of selected parts of the literature indicate that many reports of XPS on battery electrodes have significant analysis or data flaws. In this paper, we highlight several of the common challenges that analysts face when using XPS for battery materials, pointing to recent literature that addresses many of the critical issues associated with sample preparation as well as data collection and analysis. A common error for battery materials (and other materials) involves ignoring peak overlaps and interferences. Specifically, when a “minor” peak associated with a component in relatively high concentration overlaps or contributes to the primary peak (or one recommended for quantitative analysis) from a different element in the material. Overlap issues apply to many battery electrodes composed of many elements with complex photoelectron peak structures, as well as those involving peaks with seemingly simpler spectral envelopes such as Li and F. Examples of issues associated with battery systems are highlighted by a discussion of challenges associated with XPS analysis of Li and nickel–manganese–cobalt (NMC) electrodes in battery systems. Lithium analysis has challenges associated with the preparation and an often‐unrecognized peak overlap with F. In our laboratory and in the literature, NMC electrodes are often examined and new XPS users do not always recognize interference of the Auger signal from F KLL (in or on the electrode) with Ni 2p photoelectron spectrum when generated with Al Kα X‐rays. The use of simulated spectra involving both F and NiO demonstrates the extent of F Auger contributions to the Ni 2p signal strength as a function of the F/Ni atom ratio in the material and suggests spectra information that can be used to identify how significant effects will be on the resultant spectra. Our analysis demonstrates that in many cases overlap issues are significant for real electrode materials.

25 ENERGY STORAGE↗
DOE OSTI2023

Surface analysis insight note: Illustrating the effect of adventitious contamination on Pt photoemission peak intensities

Adventitious carbon contaminations are not only omnipresent and used for charge referencing of XPS spectra but also can alter the apparent presence of the element peaks that span over the large spectral window of binding energies. This Insight note describes the effect of an adventitious contamination layer on Pt and presents, in brief, the approach whereby the component spectra are derived for ion beam cleaned Pt samples that can then utilize linear mathematics to peak fit said spectra thus quantifying the amount of each component including that assigned to the contamination itself of Pt metal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Attack Surface Analysis of the Digital Twins interface with Advanced Sensor and Instrumentation Interfaces: Cyber Threat Assessment and Attack Demonstration for Digital Twins in Advanced Reactor Architectures

A digital twin is a virtual representation of a physical system or object using real-time data that can predict and analyze how the system or object performs. This relatively new technology can be applied to the field of nuclear power generation, to aid in the design and development of new nuclear power plants and reduce operation costs using predictive maintenance and other data analytical methods. While there are already companies utilizing simulation software to train operators and technicians in the nuclear industry, some are now transitioning to utilizing their existing technology, software, and methods to develop digital twin solutions for the next generation of nuclear power plants, offering their services to utilities and government organizations around the world.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗