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At least 55 records · Page 3

Interfaces in polymer, ceramic, and metal matrix composites; Proceedings of the Second International Conference on Composite Interfaces (ICCI-II), Cleveland, OH, June 13-17, 1988

The present conference on interfacial factors in advanced composite materials discusses such topics in their development status and properties as silane coupling, the electrochemical and plasma-surface treatment of carbon fibers, fiber surface-analytical techniques, polymer molecular scale characterization by atom-probe field-ion microscopy, the study of carbon fiber-epoxy resin interface interactions by means of labeling techniques, and the surface tailoring of SiC by ion implantation. Also discussed are developments in laser light-scattered photoelasticity, microstructural evolutions under heat treatment and radiation damage, TEM for composites, the interfaces of carbon fiber-reinforced Al composites, the influence of the interface on macroscopic composite properties, and the status of the theoretical understanding of composite interfaces.

Ishida, Hatsuo

LDEF polymeric materials: A summary of Langley characterization

The NASA Long Duration Exposure Facility (LDEF) enabled the exposure of a wide variety of materials to the low earth orbit (LEO) environment. This paper provides a summary of research conducted at the Langley Research Center into the response of selected LDEF polymers to this environment. Materials examined include graphite fiber reinforced epoxy, polysulfone, and additional polyimide matrix composites, films of FEP Teflon, Kapton, several experimental high performance polyimides, and films of more traditional polymers such as poly(vinyl toluene) and polystyrene. Exposure duration was either 10 months or 5.8 years. Flight and control specimens were characterized by a number of analytical techniques including ultraviolet-visible and infrared spectroscopy, thermal analysis, scanning electron and scanning tunneling microscopy, x-ray photoelectron spectroscopy, and, in some instances, selected solution property measurements. Characterized effects were found to be primarily surface phenomena. These effects included atomic oxygen-induced erosion of unprotected surfaces and ultraviolet-induced discoloration and changes in selected molecular level parameters. No gross changes in molecular structure or glass transition temperature were noted. The intent of this characterization is to increase our fundamental knowledge of space environmental effects as an aid in developing new and improved polymers for space application. A secondary objective is to develop benchmarks to enhance our methodology for the ground-based simulation of environmental effects so that polymer performance in space can be more reliably predicted.

Young, Philip R.

Mars Geochemical Instrument (MarGI): An instrument for the analysis of the Martian surface and the search for evidence of life

The Mars Geochemical Instrument, MarGI, was developed to provide a comprehensive analysis of the rocks and surface material on Mars. The instrument combines Differential Thermal Analysis (DTA) with miniature Gas Chromatography-Ion Mobility Spectrometry (GC-IMS) to identify minerals, the presence and state of water, and organic compounds. Miniature pyrolysis ovens are used to both, conduct DTA analysis of soil or crushed rocks samples, and pyrolyze the samples at temperatures up to 1000 degrees C for GC-IMS analysis of the released gases. This combination of analytical processes and techniques, which can characterize the mineralogy of the rocks and soil, and identify and quantify volatiles released during pyrolysis, has applications across a wide range of target sites including comets, planets, asteroids, and moons such as Titan and Europa. The MarGI analytical approach evolved from the Cometary Ice and Dust Experiment (CIDEX) selected to fly on the Comet Rendezvous Asteroid Flyby Mission (CRAF).

Kojiro, Daniel R.

Infrared Spectroscopy as a Chemical Fingerprinting Tool

Infrared (IR) spectroscopy is a powerful analytical tool in the chemical fingerprinting of materials. Any sample material that will interact with infrared light produces a spectrum and, although normally associated with organic materials, inorganic compounds may also be infrared active. The technique is rapid, reproducible and usually non-invasive to the sample. That it is non-invasive allows for additional characterization of the original material using other analytical techniques including thermal analysis and RAMAN spectroscopic techniques. With the appropriate accessories, the technique can be used to examine samples in liquid, solid or gas phase. Both aqueous and non-aqueous free-flowing solutions can be analyzed, as can viscous liquids such as heavy oils and greases. Solid samples of varying sizes and shapes may also be examined and with the addition of microscopic IR (microspectroscopy) capabilities, minute materials such as single fibers and threads may be analyzed. With the addition of appropriate software, microspectroscopy can be used for automated discrete point or compositional surface area mapping, with the latter providing a means to record changes in the chemical composition of a material surface over a defined area. Due to the ability to characterize gaseous samples, IR spectroscopy can also be coupled with thermal processes such as thermogravimetric (TG) analyses to provide both thermal and chemical data in a single run. In this configuration, solids (or liquids) heated in a TG analyzer undergo decomposition, with the evolving gases directed into the IR spectrometer. Thus, information is provided on the thermal properties of a material and the order in which its chemical constituents are broken down during incremental heating. Specific examples of these varied applications will be cited, with data interpretation and method limitations further discussed.

Huff, Timothy L.

Marine Algae Polysaccharides: An Overview of Characterization Techniques for Structural and Molecular Elucidation

Polysaccharides make up a large portion of the organic material from and in marine organisms. However, their structural characterization is often overlooked due to their complexity. With many high-value applications and unique bioactivities resulting from the polysaccharides’ complex and heterogeneous structures, dedicated analytical efforts become important to achieve structural elucidation. Because algae represent the largest marine resource of polysaccharides, the majority of the discussion is focused on well-known algae-based hydrocolloid polymers. The native environment of marine polysaccharides presents challenges to many conventional analytical techniques necessitating novel methodologies. We aim to deliver a review of the current state of the art in polysaccharide characterization, focused on capabilities as well as limitations in the context of marine environments. This review covers the extraction and isolation of marine polysaccharides, in addition to characterizations from monosaccharides to secondary and tertiary structures, highlighting a suite of analytical techniques.

09 BIOMASS FUELS

Real-time neutron multiplicity and source localization for criticality safety during fuel debris removal

Advancing neutron detection and analysis techniques for complex radiation environments is an ongoing focus in nuclear instrumentation and monitoring. This proposal presents research and development of a generalized real-time neutron monitoring and analysis system, applicable to any detector capable of producing time-tagged neutron count data. While the work is demonstrated using the Neutron Multiplication Analysis Detector (NoMAD), a modular 15-tube helium-3 (He-3) array, due to its availability, spatial resolution, and flexible deployment, the methods developed are extensible to other systems, including organic scintillators and fast digital detectors. This research investigates two complementary analytical techniques for real-time characterization of neutron emitting sources: neutron multiplicity estimation based on the Hage-Cifarelli formalism and spatial localization using supervised machine learning applied to spatial count rate patterns. These methods are designed to operate under dynamic, evolving conditions such as fuel debris retrieval or reactor startup, where neutron-emitting material geometries may be partially unknown or changing over time. By integrating statistical neutron emission data with spatial localization, this research aims to develop and evaluate methods for real time neutron monitoring, source characterization, and material verification. Key contributions include implementation of a low-latency data pipeline for continuous neutron multiplicity analysis, development and validation of machine learning models for spatial inference, and experimental evaluation of system performance under variable measurement conditions. The outcomes are intended to support applications in nuclear safeguards, verification, emergency response, and reactor startup.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND

Tribological evaluation and analysis of coating materials

A physical characterization of coating materials by analytical techniques such as XPS, AES, ellipsometry, and nuclear reaction analysis can contribute to the understanding of adhesion and friction of the coatings and can partially predict the tribological properties of the coatings. This two-part paper describes the tribological properties and physical characteristics of (1) diamondlike carbon (DLC) films and (2) silicon nitride (SiN(x)) films. Emphasis is to relate plasma deposition conditions to the film chemistry and composition and to the adhesion and friction of the films. With the DLC films, the higher the plasma deposition power, the less the hydrogen concentration and the greater the film density and the hardness. The friction behavior of DLC films deposited at higher deposition powers (200 to 300 W) is similar to that of bulk diamond. Even in a vacuum, the DLC films effectively lubricate ceramic surfaces (Si3N4) at temperatures to 500 C. With SiN(x) films, the silicon to nitrogen ratios and the amount of amorphous silicon depend on deposition frequency. The presence of rich amorphous silicon in the high-frequency plasma-deposited SiN(x) films increases their adhesion and friction above 500 C in vacuum.

Miyoshi, Kazuhisa

A parametric study of single-wall carbon nanotube growth by laser ablation

Results of a parametric study of carbon nanotube production by the double-pulse laser oven process are presented. The effect of various operating parameters on the production of single-wall carbon nanotubes (SWCNTs) is estimated by characterizing the nanotube material using analytical techniques, including scanning electron microscopy, transmission electron microscopy, thermo gravimetric analysis and Raman spectroscopy. The study included changing the sequence of the laser pulses, laser energy, pulse separation, type of buffer gas used, operating pressure, flow rate, inner tube diameter, as well as its material, and oven temperature. It was found that the material quality and quantity improve with deviation from normal operation parameters such as laser energy density higher than 1.5 J/cm2, pressure lower than 67 kPa, and flow rates higher than 100 sccm. Use of helium produced mainly small diameter tubes and a lower yield. The diameter of SWCNTs decreases with decreasing oven temperature and lower flow rates.

Nanotubes, Carbon/chemistry

The Preliminary Examination of Organics in the Returned Stardust Samples from Comet Wild 2

The primary objective of STARDUST is to collect coma samples from comet 8lP/Wild 2. These samples were collected by impact onto aerogel tiles on Jan 2, 2004 when the spacecraft flew through the comet's coma at a relative velocity of about 6.1 km/sec. Measurements of dust impacts on the front of the spacecraft suggest that the aerogel particle collector was impacted by 2800 +/- 500 particles larger than 15 micron in diameter. Following recovery of the Sample Return Capsule (SRC) on Jan 15, 2006, the aerogel collector trays will be removed in a clean room at JSC. After documentation of the collection, selected aerogel tiles will be removed and aerogel and cometary samples will be extracted for study. A number of different extraction techniques will be used, each optimized for the analytical technique that is to be used. The STARDUST Mission will carry out a 6 month preliminary examination (PE) of a small portion of the returned samples. The examination of the samples will be made by a number of subteams that will concentrate on specific aspects of the samples. One of these is the Organics PE Team (see the author list above for team members). These team members will use a number of analytical techniques to produce a preliminary characterization of the abundance and nature of the organics (if any) in the returned samples.

Sandford, S. A.

Parametric Study of Carbon Nanotube Production by Laser Ablation Process

Carbon nanotubes form a new class of nanomaterials that are presumed to have extraordinary mechanical, electrical and thermal properties. The single wall nanotubes (SWNTs) are estimated to be 100 times stronger than steel with 1/6th the weight; electrical carrying capacity better than copper and thermal conductivity better than diamond. Applications of these SWNTs include possible weight reduction of aerospace structures, multifunctional materials, nanosensors and nanoelectronics. Double pulsed laser vaporization process produces SWNTs with the highest percentage of nanotubes in the output material. The normal operating conditions include a green laser pulse closely followed by an infrared laser pulse. Lasers ab late a metal-containing graphite target located in a flow tube maintained in an oven at 1473K with argon flow of 100 sccm at a 500 Torr pressure. In the present work a number of production runs were carried out, changing one operating condition at a time. We have studied the effects of nine parameters, including the sequencing of the laser pulses, pulse separation times, laser energy densities, the type of buffer gas used, oven temperature, operating pressure, flow rate and inner flow tube diameters. All runs were done using the same graphite target. The collected nanotube material was characterized by a variety of analytical techniques including scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman and thermo gravimetric analysis (TGA). Results indicate trends that could be used to optimize the process and increase the efficiency of the production process.

Arepalli, Sivaram

Compound Specific Hydrogen Isotope Composition of Type II and III Kerogen Extracted by Pyrolysis-GC-MS-IRMS

The use of Hydrogen (H) isotopes in understanding oil and gas resource plays is in its infancy. Described here is a technique for H isotope analysis of organic compounds pyrolyzed from oil and gas shale-derived kerogen. Application of this technique will progress our understanding. This work complements that of Pernia et al. (2013, this meeting) by providing a novel method for the H isotope analysis of specific compounds in the characterization of kerogen extracted by analytically diverse techniques. Hydrogen isotope analyses were carried out entirely "on-line" utilizing a CDS 5000 Pyroprobe connected to a Thermo Trace GC Ultra interfaced with a Thermo MAT 253 IRMS. Also, a split of GC-separated products was sent to a DSQ II quadrupole MS to make semi-quantitative compositional measurements of the extracted compounds. Kerogen samples from five different basins (type II and III) were dehydrated (heated to 80 C overnight in vacuum) and analyzed for their H isotope compositions by Pyrolysis-GC-MS-TC-IRMS. This technique takes pyrolysis products separated via GC and reacts them in a high temperature conversion furnace (1450 C) which quantitatively forms H2, following a modified method of Burgoyne and Hayes, (1998, Anal. Chem., 70, 5136-5141). Samples ranging from approximately 0.5 to 1.0mg in size, were pyrolyzed at 800 C for 30s. Compounds were separated on a Poraplot Q GC column. Hydrogen isotope data from all kerogen samples typically show enrichment in D from low to high molecular weight compounds. Water (H2O) average deltaD = -215.2 (V-SMOW), ranging from -271.8 for the Marcellus Shale to -51.9 for the Polish Shale. Higher molecular weight compounds like toluene (C7H8) have an average deltaD of -89.7 0/00, ranging from -156.0 for the Barnett Shale to -50.0 for the Monterey Shale. We interpret these data as representative of potential H isotope exchange between hydrocarbons and sediment pore water during formation within each basin. Since hydrocarbon H isotopes readily exchange with water, these data may provide some useful information on gas-water or oil-water interaction in resource plays, and further as a possible indicator of paleo-environmental conditions. Alternatively, our data may be an indication of H isotope exchange with water and/or acid during the kerogen isolation process. Either of these interpretations will prove useful when deciphering H isotope data derived from kerogen analysis. More experiments are planned to discern these two or other possible scenarios.

Socki, Richard A.

XPS Protocol for the Characterization of Pristine and Functionalized Single Wall Carbon Nanotubes

Recent interest in developing new applications for carbon nanotubes (CNT) has fueled the need to use accurate macroscopic and nanoscopic techniques to characterize and understand their chemistry. X-ray photoelectron spectroscopy (XPS) has proved to be a useful analytical tool for nanoscale surface characterization of materials including carbon nanotubes. Recent nanotechnology research at NASA Johnson Space Center (NASA-JSC) helped to establish a characterization protocol for quality assessment for single wall carbon nanotubes (SWCNTs). Here, a review of some of the major factors of the XPS technique that can influence the quality of analytical data, suggestions for methods to maximize the quality of data obtained by XPS, and the development of a protocol for XPS characterization as a complementary technique for analyzing the purity and surface characteristics of SWCNTs is presented. The XPS protocol is then applied to a number of experiments including impurity analysis and the study of chemical modifications for SWCNTs.

Sosa, E. D.

Resin transfer molding of textile preforms for aircraft structural applications

The NASA LaRC is conducting and supporting research to develop cost-effective fabrication methods that are applicable to primary composite aircraft structures. One of the most promising fabrication methods that has evolved is resin transfer molding (RTM) of dry textile material forms. RTM has been used for many years for secondary structures, but has received increased emphasis because it is an excellent method for applying resin to damage-tolerant textile preforms at low cost. Textile preforms based on processes such as weaving, braiding, knitting, stitching, and combinations of these have been shown to offer significant improvements in damage tolerance compared to laminated tape composites. The use of low-cost resins combined with textile preforms could provide a major breakthrough in achieving cost-effective composite aircraft structures. RTM uses resin in its lowest cost form, and storage and spoilage costs are minimal. Near net shape textile preforms are expected to be cost-effective because automated machines can be used to produce the preforms, post-cure operations such as machining and fastening are minimized, and material scrap rate may be reduced in comparison with traditional prepreg molding. The purpose of this paper is to discuss experimental and analytical techniques that are under development at NASA Langley to aid the engineer in developing RTM processes for airframe structural elements. Included are experimental techniques to characterize preform and resin behavior and analytical methods that were developed to predict resin flow and cure kinetics.

Hasko, Gregory H.

In-situ monitoring of atomically dispersed Pt sites supported on OMS-2 during CO 2 activation

Atomically dispersed catalysts have drawn great interest lately, as they showcase a high density of active sites, selectivity, and high turnover frequencies in oxidation chemistry due to labile oxygen activation. In contrast, the applications of these catalysts have lagged in reduction reactions due to the ambiguity caused by the sintering and restructuring of active sites. To bridge this gap, the evolution of Pt 4+ isomorphically substituted into an octahedral molecular sieve structure (OMS-2) under reductive conditions was correlatively characterized using multiple in-situ analytical techniques such as ambient pressure X-ray photoelectron spectroscopy, environmental transmission electron microscopy, and solid-state nuclear magnetic resonance. The surface dynamics of the Pt single atoms were revealed during the Reverse Water Gas Shift (RWGS) reaction, where the active sites were identified as two-coordinated platinum single atoms. Under reaction, we show nonbinding atoms adjacent to the single atoms restructured the motif of the single atoms to Pt 2+ via ion mobility of potassium, increasing the activation energy by 25.6 kJ/mol. Here, this work also highlights the potential for increased stability of the single atom sites via isomorphic substitution of the metal oxide support, since the Pt-OMS-2 catalyst retained activity for about 33 h before deactivation, after which nanoparticles were observed in TEM images. This work offers a new perspective in single atom synthesis using the metal oxide as the host for the single atom site, instead of adatoms on the surface

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Metasurfaces with Multipolar Resonances and Enhanced Light–Matter Interaction

Metasurfaces, composed of engineered nanoantennas, enable unprecedented control over electromagnetic waves by leveraging multipolar resonances to tailor light–matter interactions. This review explores key physical mechanisms that govern their optical properties, including the role of multipolar resonances in shaping metasurface responses, the emergence of bound states in the continuum (BICs) that support high-quality factor modes, and the Purcell effect, which enhances spontaneous emission rates at the nanoscale. These effects collectively underpin the design of advanced photonic devices with tailored spectral, angular, and polarization-dependent properties. This review discusses recent advances in metasurfaces and applications based on them, highlighting research that employs full-wave numerical simulations, analytical and semi-analytic techniques, multipolar decomposition, nanofabrication, and experimental characterization to explore the interplay of multipolar resonances, bound and quasi-bound states, and enhanced light–matter interactions. A particular focus is given to metasurface-enhanced photodetectors, where structured nanoantennas improve light absorption, spectral selectivity, and quantum efficiency. By integrating metasurfaces with conventional photodetector architectures, it is possible to enhance responsivity, engineer photocarrier generation rates, and even enable functionalities such as polarization-sensitive detection. The interplay between multipolar resonances, BICs, and emission control mechanisms provides a unified framework for designing next-generation optoelectronic devices. This review consolidates recent progress in these areas, emphasizing the potential of metasurface-based approaches for high-performance sensing, imaging, and energy-harvesting applications.

Kerker effect

Analyses of spacecraft polymeric materials

Partial analytical characterizations are made by four different techniques of three polymeric materials used in conjunction with the Space Telescope for samples flown on mission STS-8. The polymers were Tedlar, Kapton H, and Kapton F. The surfaces of the three polymers were attacked and oxidized by atomic oxygen, and fluorine is lost from the surface of Kapton F, largely due to displacement by atomic oxygen.

Worley, S. D.

Functionalization of Carbon Nanotubes

These project will explore the functionalization of carbon nanotubes via the formation of molecular complexes with perylene diimide based systems. It is anticipated that these complexes would be soluble in organic solvent and enable the homogenous dispersion of carbon nanotubes in polymer films. Molecular complexes will be prepared and characterized using standard spectroscopic and thermal analytical techniques. Polymer films will be prepared with these complexes and their properties (electrical and thermal conductivity, mechanical properties, stability) evaluated.

Webber, Stephen E.

Reduction of chromium in Ni-base superalloys through element substitution and rapid solidification processing

The reduction in the use of Cr in Ni base superalloys by the combined approaches of both elemental substitution and rapid solidification processing is studied. The elements Si, Zr, Y and Hf were chosen as potential partial substitutes for Cr in Waspaloy and IN 713LC sine their separate addition to other alloys has previously resulted in enhanced oxidation resistance. The roles of Cr and these replacement elements in determining the microstructure and properties are evaluated. The elements Si, Zr, and Y and Hf are used as partial replacements for Cr in the base superalloys and these resultant alloys are processed using rapid solidification techniques. The mechanical properties and oxidation resistance of the processed materials are evaluated. The microstructure is characterized using state of the art techniques (e.g. analytical transmission electron microscopy), and the mechanism by which these structures are produced is determined.

Fraser, H. D.