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At least 91 records · Page 5

Determination of Trace Silicone Contamination on Composites by Quantitative XPS and LIBS

Surface treatment and surface characterization techniques are critical to ensure that adherends are chemically activated and free of contaminants prior to adhesive bonding. Silicone contamination from mold-release agents and other sources can interfere with interfacial bonding, decreasing the durability and performance of bonded composite structures. Tools and methods are needed that can be used in a production environment to reliably detect low levels of contaminants in a rapid, simple, and cost-effective manner to improve bond reliability. In this work, surface characterization of carbon fiber reinforced polymer (CFRP) composites was performed using laser induced breakdown spectroscopy (LIBS) and the results were compared with those obtained from X-ray photoelectron spectroscopy (XPS). The objective was to investigate the ability to quantify the surface species measured by LIBS since it offers many advantages over XPS in terms of ease of use, sample preparation, and real-time results. The as-processed CFRP panels had trace surface silicone contamination from the fabrication process, the source of which was not investigated. The composites were laser treated at select average laser power levels, resulting in varying levels of contamination reduction. The Si atomic percentage measurements using XPS were conducted both before and after laser ablation. The XPS results were compared with those obtained from LIBS to assess the reliability of each technique for surface contaminant characterization. The results showed an excellent correlation in Si atomic concentration between the two techniques.

Ledesma, Rodolfo↗

Optimization of Picosecond Laser Parameters for Surface Treatment of Composites Using a Design of Experiments (DOE) Approach

Based on guidelines from the Federal Aviation Administration, research supported by the NASA Advanced Composites Project is investigating methods to improve process control for surface preparation and pre-bond surface characterization on aerospace composite structures. The overall goal is to identify high fidelity, rapid, and reproducible surface treatments and surface characterization methods to reduce the uncertainty associated with the bonding process. The desired outcome is a more reliable bonded airframe structure, and to reduce time to achieve certification. In this work, a design of experiments (DoE) approach was conducted to determine optimum laser ablation conditions using a pulsed laser source with a nominal pulse width of 10 picoseconds. The laser power, frequency, scan speed, and number of passes (1 or 2) were varied within the laser system operating boundaries. Aerospace structural carbon fiber reinforced composites (Torayca® 3900-2/T800H) were laser treated, then characterized for contamination, and finally bonded for mechanical testing. Pre-bond characterization included water contact angle (WCA) using a handheld device, ablation depth measurement using scanning electron microscopy (SEM), and silicone contamination measurement using laser induced breakdown spectroscopy (LIBS). In order to accommodate the large number of specimens in the DoE, a rapid-screening, double cantilever beam (DCB) test specimen configuration was devised based on modifications to ASTM D5528. Specimens were tested to assess the failure modes observed under the various laser surface treatment parameters. The models obtained from this DoE indicated that results were most sensitive to variation in the average laser power. Excellent bond performance was observed with nearly 100% cohesive failure for a wide range of laser parameters. Below about 200 mW, adhesive failure was observed because contamination was left on the surface. For laser powers greater than about 600 mW, large amounts of fiber were exposed, and the failure mode was predominately fiber tear.

Palmieri, Frank L.↗

The Characterization of Surface Variegation Effects on Remote Sensing

Improvements in remote sensing capabilities hinge very directly upon attaining an understanding of the physical processes contributing to the measurements. In order to devise new measurement strategies and to learn better techniques for processing remotely gathered data, it is necessary to understand and to characterize the complex radiative interactions of the atmosphere-surface system. In particular, it is important to understand the role of atmospheric structure, ground reflectance inhomogeneity and ground bidirectional reflectance type. The goals, then, are to model, analyze, and parameterize the observable effects of three dimensional atmospheric structure and composition and two dimensional variations in ground albedo and bidirectional reflectance. To achieve these goals, a Monte Carlo radiative transfer code is employed to model and analyze the effects of many of the complications which are present in nature.

Pearce, W. A.↗

Image-Based Fracture Surface Defect Characterization Methods for Additively Manufactured Ti-6Al-4V Tested in Fatigue

Abstract Fatigue initiation in additively manufactured samples/parts often occurs at processed-induced defects such as lack-of-fusion (LoF), keyhole, or other morphological/microstructural defects that have unique characteristics and measurable qualities. Attempts at identifying and minimizing such defects have utilized optimized processing conditions along with in situ and ex situ characterization that includes metallography and/or X-ray computed tomography (XCT). This paper highlights the benefits of using fracture surface analyses to detect and quantify defects that may not be detected by metallography/XCT due to sectioning and resolution limits. In addition to using manual quantification of fatigue initiating LoF and keyhole defects on fracture surfaces, image-based machine learning using convolutional neural networks such as U-Net were also used to automate the process. Statistical analyses were used to identify the extreme cases of defects that initiated and accelerated fatigue and to model the distribution of defect size and shape characteristics to distinguish the type of defect. Initial results show agreement between trained machine learning models and ground truth data in defect segmentation, and the distributions of defect characteristics are distinguishable to particular process-induced defect types.

Materials Science↗

Preparation and evaluation of advanced electrocatalysts for phosphoric acid fuel cells

Alloy electrocatalysts on carbon supports were developed for hydrogen oxidation in the presence of carbon monoxide. These electrocatalysts match the best platinum on carbon catalysts for performance yet cost half as much. The results demonstrate that a significant reduction in anode electrocatalyst material cost can be achieved by replacing the platinum. Since surface characterization of this catalyst is important to explain its performance, several approaches and pitfalls to the elucidation of the surface characterization are presented.

Stonehart, P.↗

XPS analysis of molecular contamination and sp 2 amorphous carbon on oxidized (100) diamond

The efficacy of oxygen (O) surface terminations on diamond is an important factor for the performance and stability for diamond-based quantum sensors and electronics. Given the wide breadth of O-termination techniques, it can be difficult to discern which method would yield the highest and most consistent O coverage. Furthermore, the interpretation of surface characterization techniques is complicated by surface morphology and purity, which if not accounted for will yield inconsistent determination of the oxygen coverage. We present a comprehensive approach to consistently prepare and analyze oxygen termination of surfaces on (100) single-crystalline diamond. We report on x-ray photoelectron spectroscopy (XPS) characterization of diamond surfaces treated with six oxidation methods that include various wet chemical oxidation techniques, photochemical oxidation with UV illumination, and steam oxidation using atomic layer deposition (ALD). Our analysis entails a rigorous XPS peak-fitting procedure for measuring the functionalization of O-terminated diamond. The findings herein have provided molecular-level insights on oxidized surfaces in (100) diamond, including the demonstration of clear correlation between the measured oxygen atomic percentage and the presence of molecular contaminants containing nitrogen, silicon, and sulfur. We also provide a comparison of the sp 2 carbon content with the O1s atomic percentage and discern a correlation with the diamond samples treated with dry oxidation which eventually tapers off at a max O1s atomic percentage value of 7.09 ± 0.40%. Given these results, we conclude that the dry oxidation methods yield some of the highest oxygen amounts, with the ALD water vapor technique proving to be the cleanest technique out of all the oxidation methods explored in this work.

XPS↗

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↗

Experimental Characterization of Surface Roughness and Geometric Evaluations of Thin-Wall Laser Powder Directed Energy Deposition

Additive Manufacturing (AM) has offered many new design and manufacturing opportunities for components across various industries. As AM evolves there is a need to better understand outputs of the process including geometric limitations and surface roughness based on specific application requirements. One possible application area of AM are components using thin-wall (<2 mm) microchannel heat exchangers for subsystems across aerospace, and industrial applications. AM offers the opportunity to significantly reduce the cost and lead time associated with fabricating these complex parts with internal features such as an array of cooling channels. Laser Powder Bed Fusion (L-PBF) has been continuously demonstrated as a technique to fabricate heat exchangers with internal geometric complexities. However, L-PBF is limited in the scale at which parts can be fabricated. Laser Powder Directed Energy Deposition (LP-DED) has been demonstrated as an AM technology to significantly increase the scale of which thin-wall microchannel heat exchangers could be manufactured. Successful deployment of the LP-DED technology requires critical understanding of the resulting features from the build process. Surface roughness is one of the critical areas that effects the friction factor and pressure drop within a heat exchanger and must be well understood. This presentation will provide an overview of the characterization work completed to understand the LP-DED process for thin-walls representative of hydrogen resistant alloy NASA HR-1 that would be used in a Hydrogen-environment application. An overview of the experiments conducted with varying LP-DED parameters, evaluation of various geometric channel and geometric build features and resulting surface finish will be provided along with a summary of conclusions from these experiments. Results indicate that powder size is a major contributor and surface roughness varies between closed channel shapes and external surfaces.

Directed Energy Deposition↗

Unsteady Surface Pressure Characterization on Launch Vehicle in Liftoff Configuration

Acquisition of unsteady pressure using remote scanners can provide practical advantages over making the same measurements directly using flush-mounted pressure transducers. However, pneumatic distortion of the signal is introduced by the tubing between the sensing module and surface port. This typically limits the usefulness of such measurements to averaged, steady data only, restricting the application of pressure scanners for unsteady pressure measurements in the wind tunnel and flight-testing applications. In this work, unsteady pressure on the surface of a 1.75%-scale model of the NASA Space Launch System Block 1B Cargo vehicle was remotely measured at the NASA Langley Research Center 14- by 22-Foot Subsonic Tunnel using an ESP pressure scanner. Subsequent reconstruction using an empirically-tuned, Wiener-filtered inverse transfer function produced excellent agreement compared to nearby surface-mounted transducers within a usable bandwidth of approximately 500 Hz. Interactions between the launch vehicle and the support tower produced strong oscillations that were absent in the vehicle-alone configuration, and it is likely that the wake interaction leads to a resonant flow response when the launch tower is immediately downstream of the vehicle.

Unsteady pressure↗

High-Resolution Near-Surface Imaging at the Basin Scale Using Dark Fiber and Distributed Acoustic Sensing: Toward Site Effect Estimation in Urban Environments

Near-surface seismic structure, particularly the shear wave velocity (V s ), can strongly affect local site response, and should be accurately estimated for ground motion prediction during seismic hazard assessment. The Imperial Valley (California), occupying the southern end of the Salton Trough, is a seismically active basin with thick surficial lacustrine sedimentary deposits. In this study, we utilize ambient noise records and local earthquake events for high-resolution near-surface characterization and site effect estimation with an unlit fiber-optic telecommunication infrastructure (dark fiber) in Imperial Valley by using the distributed acoustic sensing (DAS) technique. We apply ambient noise interferometry to retrieve coherent surface waves from DAS records, and evaluate performances of three different surface wave methods on DAS ambient noise dispersion imaging. We develop a quality control workflow to improve the dispersion measurement of noisy portions of the DAS data set by using a data selection strategy. Using the joint inversion of both the fundamental mode and higher overtones of Rayleigh waves, a high resolution two-dimensional (2D) V s structure down to 70 m depth is obtained. We successfully achieve an improved V s 30 (the time-averaged shear-wave velocity in the top 30 m) model with higher spatial-resolution and reliability compared to the existing community model for the area. We also explore the potential for utilizing DAS earthquake events for site amplification estimation. The preliminary results reveal a clear anti-correlation between the approximated site response and the V s 30 profile. In conclusion, our results indicate the potential utility of DAS deployed on dark fiber for near-surface characterization in appropriate contexts.

58 GEOSCIENCES↗

Tribological Evaluation of Candidate Coatings

This SPP project with Novus was to investigate tribological properties of candidate ceramic composites. Systematic tribological bench tests and surface characterization were performed to determine composition-property relationships of several Zr-Ti-B based ceramic composites of different compositions. The lowest friction coefficient was measured with Ti0.6Zr0.4B2 composition tested in the hydraulic oil. Surface characterization suggests a formation of ZDDP tribofilm in the worn region when tested with a hydraulic oil. In all experiments, the ceramic composites did not have measurable wear, but caused material loss of the steel countersurface.

36 MATERIALS SCIENCE↗

Biophysical characterization and surface radiation balance

The Kursk 1991 Experiment (KUREX-91) was conducted as one of a suite of international studies to develop capabilities to monitor global change. The studies were designed specifically to understand the earth's land-surface vegetation and atmospheric boundary layer interaction. An intensive field campaign was conducted at a site near Kursk, Russia during the month of July in 1991 by a team of international scientists to aid in the understanding of land-surface-atmosphere interactions in an agricultural/grassland setting. We were one of several teams of scientists participating at KUREX-91 at the Streletskaya Steppe Researve near Kursk, Russia. The main goals of our research were to: (1) characterize biophysical properties of the prairie vegetation; and (2) to characterize radiation regime through measurements and from estimates derived from canopy bidirectional reflectance data. Four objectives were defined to achieve these goals: (1) determine dependence of leaf optical properties on leaf water potential of some dominant species in discrete wavebands in the visible, near-infrared, and mid-infrared (spanning 0.4-2.3 microns range); (2) characterize the effective leaf area index (LAI) and leaf angle distribution of prairie vegetation; (3) characterize the radiation regime of the prairie vegetation through measures of the radiation balance components; and (4) examine, develop, and test methods for estimating albedo, APAR, and LAI from canopy bidirectional reflectance data. Papers which were the result of the research efforts are included.

Walter-Shea, Elizabeth A.↗

Characterization of Surface Reflectance Variation Effects on Remote Sensing

The use of Monte Carlo radiative transfer codes to simulate the effects on remote sensing in visible and infrared wavelengths of variables which affect classification is examined. These variables include detector viewing angle, atmospheric aerosol size distribution, aerosol vertical and horizontal distribution (e.g., finite clouds), the form of the bidirectional ground reflectance function, and horizontal variability of reflectance type and reflectivity (albedo). These simulations are used to characterize the sensitivity of observables (intensity and polarization) to variations in the underlying physical parameters both to improve algorithms for the removal of atmospheric effects and to identify techniques which can improve classification accuracy. It was necessary to revise and validate the simulation codes (CTRANS, ARTRAN, and the Mie scattering code) to improve efficiency and accommodate a new operational environment, and to build the basic software tools for acquisition and off-line manipulation of simulation results. Initial calculations compare cases in which increasing amounts of aerosol are shifted into the stratosphere, maintaining a constant optical depth. In the case of moderate aerosol optical depth, the effect on the spread function is to scale it linearly as would be expected from a single scattering model. Varying the viewing angle appears to provide the same qualitative effect as modifying the vertical optical depth (for Lambertian ground reflectance).

Pearce, W. A.↗

Processing LiDAR Data to Predict Natural Hazards

ELF-Base and ELF-Hazards (wherein 'ELF' signifies 'Extract LiDAR Features' and 'LiDAR' signifies 'light detection and ranging') are developmental software modules for processing remote-sensing LiDAR data to identify past natural hazards (principally, landslides) and predict future ones. ELF-Base processes raw LiDAR data, including LiDAR intensity data that are often ignored in other software, to create digital terrain models (DTMs) and digital feature models (DFMs) with sub-meter accuracy. ELF-Hazards fuses raw LiDAR data, data from multispectral and hyperspectral optical images, and DTMs and DFMs generated by ELF-Base to generate hazard risk maps. Advanced algorithms in these software modules include line-enhancement and edge-detection algorithms, surface-characterization algorithms, and algorithms that implement innovative data-fusion techniques. The line-extraction and edge-detection algorithms enable users to locate such features as faults and landslide headwall scarps. Also implemented in this software are improved methodologies for identification and mapping of past landslide events by use of (1) accurate, ELF-derived surface characterizations and (2) three LiDAR/optical-data-fusion techniques: post-classification data fusion, maximum-likelihood estimation modeling, and hierarchical within-class discrimination. This software is expected to enable faster, more accurate forecasting of natural hazards than has previously been possible.

Fairweather, Ian↗

Surface Stress Characterization and Trends in Thermally Strengthened Photovoltaic Module Glass

Simultaneous changes in photovoltaic (PV) module architecture-such as increased area, replacing the polymeric backsheet with a glass backsheet, and reducing glass thickness from 3.2 to 2.0 mm-have resulted in a novel failure called spontaneous glass breakage. Spontaneous glass breakage results in front and/or rear glass failure without any obvious cause. The resulting low-energy fracture patterns have raised concerns about the thermal strengthening in 2.0-mm glass. We present validation of a nondestructive method for measuring the glass surface stress in PV modules. We use a scattered light polariscope to examine the glass properties of 11 modules from 6 solar fields, with and without spontaneous glass breakage. Based on a Mann-Whitney test p-value of 1.4 x 10-6, we conclude that there is a correlation between lower surface stress and susceptibility to spontaneous breakage. A Kendall's Tau test p-value of 2.0 x 10-4 indicates a correlation between increased module area and lower surface stress. We find that 2.0-mm glass can be, and often is, fully tempered (surface stress ≥69 MPa), but inspecting the fracture pattern is not a reliable way to assess the amount of thermal strengthening. A combination of factors, not just surface stress, influences glass breakage.

14 SOLAR ENERGY↗

Characterization of surfaces

Low gravity biotechnology experiments indicate a need to better understand and control a host of liquid-solid interfacial phenomena which reduce the efficiency of bioseparations methods on earth as well as in space. We have improved and utilized polymeric and silane derivatives, developed in association with MSFC, in order to control such phenomena. The objectives of the proposed research have been obtained. They were to improve NASA-patented coatings capable of controlling macromolecular adsorption, electroosmosis, and particle electrophoresis over a wide range of pH, and to further characterize the ability of polymeric coatings to control wall wetting interactions. To date this research has resulted in six publications and four abstracts. It has also aided researchers at MSFC with studies on the electrophoresis of large DNA molecules in free solution. It will continue to enhance NASA's efforts to exploit the space environment to enhance knowledge of phenomena relevant to biotechnology, and obtain bioseparations currently unobtainable on Earth. Abstracts from the 1994 ACS Meeting in Birmingham are attached.

Vanalstine, James M.↗

Tuning the reactivity of carbon surfaces with oxygen-containing functional groups

Oxygen-containing carbons are promising supports and metal-free catalysts for many reactions. However, distinguishing the role of various oxygen functional groups and quantifying and tuning each functionality is still difficult. Here we investigate the role of Brønsted acidic oxygen-containing functional groups by synthesizing a diverse library of materials. By combining acid-catalyzed elimination probe chemistry, comprehensive surface characterizations, 15N isotopically labeled acetonitrile adsorption coupled with magic-angle spinning nuclear magnetic resonance, machine learning, and density-functional theory calculations, we demonstrate that phenolic is the main acid site in gas-phase chemistries and unexpectedly carboxylic groups are much less acidic than phenolic groups in the graphitized mesoporous carbon due to electron density delocalization induced by the aromatic rings of graphitic carbon. The methodology can identify acidic sites in oxygenated carbon materials in solid acid catalyst-driven chemistry.

Zhou, Jiahua↗

Milestone 1.2.15: Feasibility of In Situ Accelerated Aluminum Coupon Radiolysis by Synchrotron X-Rays

Extended dry storage of aluminum-clad spent nuclear fuel (ASNF) requires an assessment of the radiolytic generation of molecular hydrogen gas (H2) from the ASNF’s corrosion layers. H2 accumulation can potentially lead to storage canister embrittlement/rupture and the accumulation of flammable gas mixtures in accident scenarios. To date, computational models have been developed for the prediction of radiolytic H2 generation from samples exposed to lower absorbed dose regimes (up to ~3 MGy). However, greater accuracy is needed for higher absorbed doses (> 25 MGy) where the concentration of H2 ultimately reaches a steady-state. Data in this area is limited due to the amount of time taken (months) to accumulate such high gamma doses. Furthermore, a recent study observed radiation-induced damage to the surface of pre-corroded aluminum alloy coupons at high absorbed gamma doses. Despite this observation and its implications, there is currently no computational connection between the radiolytic formation of H2 and changes in the composition and morphology of the cladding’s corrosion layers with absorbed dose. To develop a better understanding of the processes and effects described above, the present study aimed to evaluate the feasibility of leveraging synchrotron x-ray capabilities for coupled accelerated irradiation and in situ surface characterization of ASNF alloys. To that end, National Synchrotron Light Source II (NSLS-II) beamtime was secured and a series of aluminum alloy 1100 (AA1100) wires, prepared under a variety of conditions, were interrogated using ex situ x-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques at Idaho National Laboratory (INL) and ex situ and in situ XRD capabilities at the NSLS-II x-ray powder diffraction (XPD) beamline. Results indicated that performing synchrotron XRD using the available XPD beamline configuration can provide sufficient radiation dose but cannot discern changes in the composition and morphology of sample corrosion layers. Additionally, ex situ XRD and SEM data from Idaho National Laboratory (INL) indicated that the pre-corrosion of AA1100 wires did not generate an appreciably thick corrosion layer, as compared with previous aluminum coupon studies. These thinner surface corrosion layers were not sufficient for detection by both ex situ and in situ synchrotron XRD, specifically under consideration of the NSLS-II XPD beamline’s configuration primarily capturing information from the sample’s bulk material, i.e., aluminum metal. In summary, the use of the NSLS-II XPD beamline for promoting accelerated radiolysis and in situ surface characterization is not appropriate for this program’s goals.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗