Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “materials characterization”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 613 records · Page 34

Development of a Laser Ultrasonics-based Approach for Rapid Screening of High Entropy Alloys

This project utilized a laser ultrasonic technique to systematically study temperature-induced evolution of material properties in a set of interrelated binary alloys and a high entropy alloy (HEA) fabricated using arc-melting and spark plasma sintering processes. This technique involved the use of a nanosecond duration, high-intensity pulsed laser to thermo-elastically generate ultrasonic waves that propagate in the bulk of the metal alloy. Sub-nanometer-scale displacements associated with the propagating bulk ultrasonic waves were detected along the epicenter on the opposite surface of the sample using a 1 GHz bandwidth photorefractive interferometer. Phase transformations and microstructural changes were inferred from the temperature-dependent trends in the bulk acoustic velocities and features in the ultrasonic epicentral waveforms measured in the binary alloys. These inferences were then correlated with electron/optical microscopy observations and predictions using calculations of phase diagrams (CALPHAD). The results showed that the laser-generated ultrasonic pulses were strongly influenced by changes in material microstructure and could accurately track thermally driven phase transformations and detect the presence of microscale heterogeneities (grain boundaries, dendritic structures, etc.) in the set of binary alloy samples. The measurement approach was then applied to a quinary HEA sample for estimating phase transition temperature and determining microstructural heterogeneity. The rapid, non-contact and non-destructive ultrasonic testing approach demonstrated here is amenable to high throughput combinatorial investigations that can be applied to graded composition HEAs produced using advanced manufacturing methods. When paired with atomistic simulations and CALPHAD modeling, this approach can overcome the bottlenecks faced by current material characterization methods in efficiently screening the vast discovery space of HEAs that spans over a hundred million unique quinary alloy compositions.

36 MATERIALS SCIENCE↗

Applications of synchrotron radiation to materials science: Diffraction imaging (topography) and microradiography

Synchrotron radiation sources are now available throughout the world. The use of hard X-ray radiation from these sources for materials science is described with emphasis on diffraction imaging for material characterization. With the availability of synchrotron radiation, real-time in situ measurements of dynamic microstructural phenomena have been started. This is a new area where traditional application of X-rays has been superseded. Examples are chosen from limited areas and are by no means exhaustive. The new emerging information will, no doubt, have great impact on materials science and engineering.

Kuriyama, Masao↗

An Assessment of Nondestructive Evaluation Capability for Complex Additive Manufacturing Aerospace Components

The primary focus of this work is to investigate some of the fundamental relationships between processing, mechanical testing, materials characterization, and NDE for additively manufactured (AM) components using the powder bed fusion direct melt laser sintered process. The goal is to understand the criticality of defects unique to the AM process and then how conventional nondestructive evaluation methods as well as some of the more non-traditional methods such as computed tomography, are effected by the AM material. Specific defects including cracking, porosity and partially/unfused powder will be addressed. Besides line-of-site NDE, as appropriate these inspection capabilities will be put into the context of complex AM geometries where hidden features obscure, or inhibit traditional NDE methods.

Walker, James↗

Quantitative Characterization of Structural and Mechanical Properties of Boron Nitride Nanotubes in High Temperature Environments

The structural stability and mechanical integrity of boron nitride nanotubes (BNNTs) in high temperature environments are of importance in pursuit of their applications that are involved with extreme thermal processing and/or working conditions, but remain not well understood. In this paper, we perform an extensive study of the impacts of high temperature exposure on the structural and mechanical properties of BNNTs with a full structural size spectrum from nano- to micro- to macro-scale by using a variety of in situ and ex situ material characterization techniques. Atomic force microscopy (AFM) and high resolution transmission electron microscopy measurements reveal that the structures of individual BNNTs can survive at up to 850 °C in air and capture the signs of their structural degradation at 900 °C or above. In situ Raman spectroscopy measurements reveal that the BN bonds in BNNT micro-fibrils undergo substantial softening at elevated temperatures of up to 900 °C. The AFM-based nanomechanical compression measurements demonstrate that the mechanical integrity of individual BNNTs remain intact after being thermally baked at up to 850 °C in air. The studies reveal that BNNTs are structurally and mechanically stable materials in high temperature environments, which enables their usages in high temperature applications.

Chen, Xiaoming↗

Generation of macro- and microplastic databases by high-throughput FTIR analysis with microplate readers

Abstract FTIR spectral identification is today’s gold standard analytical procedure for plastic pollution material characterization. High-throughput FTIR techniques have been advanced for small microplastics (10–500 µm) but less so for large microplastics (500–5 mm) and macroplastics (> 5 mm). These larger plastics are typically analyzed using ATR, which is highly manual and can sometimes destroy particles of interest. Furthermore, spectral libraries are often inadequate due to the limited variety of reference materials and spectral collection modes, resulting from expensive spectral data collection. We advance a new high-throughput technique to remedy these problems using FTIR microplate readers for measuring large particles (> 500 µm). We created a new reference database of over 6000 spectra for transmission, ATR, and reflection spectral collection modes with over 600 plastic, organic, and mineral reference materials relevant to plastic pollution research. We also streamline future analysis in microplate readers by creating a new particle holder for transmission measurements using off-the-shelf parts and fabricating a nonplastic 96-well microplate for storing particles. We determined that particles should be presented to microplate readers as thin as possible due to thick particles causing poor-quality spectra and identifications. We validated the new database using Open Specy and demonstrated that additional transmission and reflection spectra reference data were needed in spectral libraries. Graphical abstract

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

FY 2024 Multidimensional Data Correlation Platform Data Management Infrastructure Progress: Materials Laboratory

This report provides an inventory of the equipment available at the ORNL Manufacturing Demonstration Facility (MDF) for sample preparation and material characterization, including both destructive and non-destructive techniques that generate critical data to support the development of the Multi-Dimensional Data Correlation (MDDC) framework. The success of the MDDC framework depends heavily on the quality and completeness of the data it can access. Therefore, it is essential to establish a comprehensive inventory of the technologies available to the Advanced Materials and Manufacturing Technologies (AMMT) multi-laboratory team. This starts by gathering information about the types of data they produce, the data collection and transfer protocols used, file formats, and data storage requirements for experiments. This information is then carefully evaluated to create the operations and trackables elements of the Damara Tern platform, which is the foundation of the MDDC framework.

36 MATERIALS SCIENCE↗

Sodium trithiocarbonate cathode for high-performance sodium–sulfur batteries

The high abundance and low cost of sodium and sulfur make room-temperature sodium-sulfur (RT Na-S) batteries an attractive technology compared to the current lithium-ion batteries for large-scale grid-storage applications. However, the commercialization of RT Na-S batteries is impeded by the slow kinetics of Na-S chemistry, severe sodium polysulfide shuttling, and uncontrollable growth of dendritic Na. Herein, sodium trithiocarbonate (Na 2 CS 3 ) is applied as a cathode material to facilitate concurrent improvement in both electrodes, leading to a high-rate performance with extended cycle life. The conductive characteristic of the carbon-sulfur resonance bond provides fast ion and electron transfer throughout the cathode, resulting in superior electrochemical reactivity. At the cathode, the presence of Na2CS3 forms an oligomer-structured layer to suppress the dissolution and shuttling of active materials. Meanwhile, when small portions of Na 2 CS 3 intermediates migrate to the anode, a stable solid electrolyte interphase (SEI) layer with uniform Na-ion flux is formed, enabling improved Na stripping and plating performance. A series of electrochemical and materials characterization, accompanied by density functional theory calculations demonstrate that Na 2 CS 3 is a promising candidate to realize high-rate performance long cycle life RT Na-S batteries.

25 ENERGY STORAGE↗

Mixed Ionic Electronic Conducting Quaternary Perovskites: Materials by Design for Solar Thermochemical Hydrogen

The innovative research conducted by Arizona State University and Princeton University in the project "Mixed Ionic-Electronic Conducting Quaternary Perovskites: Materials by Design for Solar Thermochemical Hydrogen" marks a significant stride forward in thermochemical water splitting. Through an intricate blend of computational design and experimental validation, the project delved into the promising potential of Mixed Ionic Electronic Conducting (MIEC) perovskites. These complex materials, characterized by their unique redox-active nature and adaptability in stoichiometry, present a promising frontier for efficient solar thermochemical hydrogen production. Firstly, the research enhanced the science by utilizing state-of-the-art computational methodologies to unravel the nuanced chemical potentials of MIEC perovskites. By simulating various off-stoichiometric scenarios and redox conditions, the team was able to predict material behaviors under diverse environmental conditions, a feat unachievable through conventional experimental methodologies alone. This approach not only fast-tracks the material screening process, significantly reducing the time from laboratory re-search to practical application, but also uncovers trends and correlations that are pivotal for future materials innovation. Regarding technical effectiveness, the project stands out in its economic feasibility. Traditional methods of materials discovery are often marred by high costs and extensive timeframes, owing to the iterative nature of experimental processes. However, by employing theoretical computations and validating these findings with targeted experiments, the project introduced a cost-effective paradigm for materials discovery and the first ever prediction, synthesis, and preliminary validation of a material solely from computational and theoretical considerations. This synergy between computation and experimentation expedites the discovery of optimal materials conducive to high-efficiency solar-to-hydrogen conversion processes. Furthermore, the public stands to benefit substantially from this research. The success of MIEC perovskites in solar thermochemical applications heralds a shift towards lower cost and lower electricity input for clean hydrogen production, hence potentially impacting climate and energy resilience. By improving the efficiency of solar-to-hydrogen conversions, the research paves the way for reduced dependency on fossil fuels, addressing the urgent global need for accessible and renewable energy sources. Moreover, the project's advancements contribute to scientific literacy in renewable energy technologies, empowering society through knowledge and spurring future innovations. In essence, this research project demonstrates significant progress in the realm of advanced water splitting through solar thermochemistry. Through its groundbreaking approaches in computational materials science and its implications for real-world applications, it holds the promise of a cleaner, more energy-resilient future.

08 HYDROGEN↗

A New Test Method for Material Flammability Assessment in Microgravity and Extraterrestrial Environments

The standard oxygen consumption (cone) calorimeter (described in ASTM E 1354 and NASA STD 6001 Test 2) is modified to provide a bench-scale test environment that simulates the low velocity buoyant or ventilation flow generated by or around a burning surface in a spacecraft or extraterrestrial gravity level. The Equivalent Low Stretch Apparatus (ELSA) uses an inverted cone geometry with the sample burning in a ceiling fire (stagnation flow) configuration. For a fixed radiant flux, ignition delay times for characterization material PMMA are shown to decrease by a factor of three at low stretch, demonstrating that ignition delay times determined from normal cone tests significantly underestimate the risk in microgravity. The critical heat flux for ignition is found to be lowered at low stretch as the convective cooling is reduced. At the limit of no stretch, any heat flux that exceeds the surface radiative loss at the surface ignition temperature is sufficient for ignition. Regression rates for PMMA increase with heat flux and stretch rate, but regression rates are much more sensitive to heat flux at the low stretch rates, where a modest increase in heat flux of 25 kW/m2 increases the burning rates by an order of magnitude. The global equivalence ratio of these flames is very fuel rich, and the quantity of CO produced in this configuration is significantly higher than standard cone tests. These results [2] demonstrate the ELSA apparatus allows us to conduct normal gravity experiments that accurately and quantifiably evaluate a material s flammability characteristics in the real-use environment of spacecraft or extra-terrestrial gravitational acceleration. These results also demonstrate that current NASA STD 6001 Test 2 (standard cone) is not conservative since it evaluates materials flammability with a much higher inherent buoyant convective flow.

Olson, S. L.↗

Trace Fe activates perovskite nickelate OER catalysts in alkaline media via redox-active surface Ni species formed during electrocatalysis

The accurate description of activity trends among perovskite-oxide oxygen-evolution-reaction (OER) catalysts using electronic-structure descriptors requires that the bulk structure of the catalyst is comparable to that of the surface. Few studies have addressed the dynamic nature of the catalyst's structure during the OER and the consequential implications for understanding activity. Here, we use a combination of electrochemical and materials-characterization techniques to study the surface reconstruction and the associated formation of a new redox-active phase on LaNiO 3 particles, LaNiO 3 epitaxial films, and an analogous Ruddlesden-Popper phase, La 2 NiO 4 . Small, but characteristic, redox features corresponding to Ni redox in nominally amorphous NiO x H y are observed during cyclic voltammetry of these initially fully crystalline materials. The size of these redox features grows with prolonged cycling and contributes to an increased surface area as determined from electrochemical impedance spectroscopy (EIS). Here we find the OER activity is strongly dependent on soluble Fe species in the electrolyte, common impurities in alkaline media. These observations are consistent with the reconstruction of the crystalline surface to form NiO x H y species and subsequent activation by adsorption of Fe forming the well-known and extremely active NiFeO x H y OER catalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Post weld heat treatment and operating temperature effect on tribological behavior of laser cladded stellite 21 coating

This study intends to investigate the feasibility of using laser cladding as a potential process to repair hot working tools by a hardfacing process. A Stellite 21 alloy coating was printed on a 350 maraging steel via laser cladding and the coating microstructure and tribological performance were characterized in as printed conditions and after heat treatment. Such a laser-processed coating showed a high integrity with little porosity and good bonding with the substrate. The Stellite coating produced substantially lower friction and a smoother contact area but had inferior wear resistance compared with the maraging steel substrate. Post process heat treatment at 650 °C for 20 h led to significant amount of strain-induced FCC to HCP phase transformation but had little improvement in wear resistance. Detailed materials characterization using X-ray diffraction and electron microscopy provided fundamental insights to the underlying mechanisms. This study opens the door for future R&D for tool surface repair by laser cladding.

36 MATERIALS SCIENCE↗

Trace Compound Analysis in TATB by Liquid Chromatography coupled with Spectroscopic and Spectrometric Detection

Accurate quantitation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) is important because of its strategic use as an energetic material. A purity determination is also needed for the proper assessment of performance. A fast and sensitive method has been developed to measure the purity of TATB in polymer-bonded materials. The target material is extracted with DMSO, and the extract is separated on a reversed-phase chromatography column. The column effluent is monitored by diode array detection (DAD) at 354 nm. The characteristic UV-Vis response and retention time identify the individual components when compared to pure compound standards. The chemical structures of compounds with no pure standards available have been determined by high-resolution mass spectrometry (MS) and MS/MS. The major component, TATB, along with 1-chloro-3,5-dinitro-2,4,6-triaminobenzene (T4A) and mono-benzofuroxan (FX1) were quantitated directly from pure compound standards. Several trace concentration components, mono-benzofurazan (F1), 1-bromo-3,5-dinitro-2,4,6-triaminobenzene (Br-T4A), 2,4,6-triamino-1-nitroso-3,5-dinitrobenzene (MN-TATB), 2,4,6-triamino-1-hydroxyl-3,5-dinitrobenzene (HO-TATB), and 2,4,6-triamino-1-nitrile-3,5-dinitrobenzene (Nitrile-TATB) were also detected and structures verified via MS/MS. Approximate concentrations were determined using calibrations from standards of similar structures. Additional trace components were also detected by MS. Contained herein are the results of analyses of TATB-based materials characterized for polymer-bonded formulations compared to different preparations of TATB. The accuracy, details, and process of developing this method are reported here.

36 MATERIALS SCIENCE↗

Characterization of front contact degradation in monocrystalline and multicrystalline silicon photovoltaic modules following damp heat exposure

Reliability and durability tests play a key role in the photovoltaic (PV) industry by minimizing potential failure risks for both existing and new cell and module technologies. In this work, a detailed study of contact degradation in monocrystalline and multicrystalline PV modules is performed. The modules are subjected to a sequence of damp heat (DH) exposures followed by electrical characterization after each step. Electroluminescence (EL) imaging shows different darkening patterns for monocrystalline modules compared to multicrystalline modules; the former shows darkening near the busbars and the latter shows it across virtually the entire cell surface. The primary loss mechanism is confirmed to be resistive after comparing the current-voltage (I–V) characteristics at each DH exposure step. Representative samples have been cored out from both the degraded modules and controls for materials characterization to gain further insights into the degradation mechanism. Top-down and cross-sectional scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and top-down high-resolution X-ray photoelectron spectroscopy (XPS) analysis performed on the cored samples confirm the degradation is due to metallization corrosion. Our study suggests that the difference in the darkening pattern can most likely be attributed to the different silver paste composition used for contacting each cell technology, particularly the composition of the glass frit.

36 MATERIALS SCIENCE↗

Physics-Based Continuum Modeling for an Aqueous Rechargeable Zn/MnO 2 Battery

This study introduces a framework for modeling the aqueous Zn/MnO 2 rechargeable battery. A reaction system and a physics-based continuum model are proposed based on two reaction types, one involving insertion and the second related to dissolution and deposition of a solid reaction product. The model, fitted to empirical data, predicts voltage behavior and capacity limitations during cycling, identifying electrolytic zinc depletion as a limiting mechanism, depending on the original cell construction. The research suggests the need for further material characterization and reaction analysis, which will advance our understanding and facilitate the development of grid-scale energy storage solutions.

Electrochemistry↗

FNAS materials processing and characterization

Research on melt-sintered high temperature superconducting materials is presented. The vibrating sample magnetometer has become a useful characterization tool for the study of high temperature superconductors. Important information regarding the superconducting properties of a sample can be obtained without actually making contact with the sample itself. A step toward microgravity processing of high temperature superconductors was taken. In the future, the samples need to be optimized prior to this processing of the sample before the specific effects of the microgravity environment can be isolated. A series of melt-sintered samples show that bulk processing of high temperature superconductors is getting better.

Golben, John P.↗

Development and Hotfire Testing of Additively Manufactured Copper Combustion Chambers for Liquid Rocket Engine Applications

NASA and industry partners are working towards fabrication process development to reduce costs and schedules associated with manufacturing liquid rocket engine components with the goal of reducing overall mission costs. One such technique being evaluated is powder-bed fusion or selective laser melting (SLM), commonly referred to as additive manufacturing (AM). The NASA Low Cost Upper Stage Propulsion (LCUSP) program was designed to develop processes and material characterization for GRCop-84 (a NASA Glenn Research Center-developed copper, chrome, niobium alloy) commensurate with powder bed AM, evaluate bimetallic deposition, and complete testing of a full scale combustion chamber. As part of this development, the process has been transferred to industry partners to enable a long-term supply chain of monolithic copper combustion chambers. To advance the processes further and allow for optimization with multiple materials, NASA is also investigating the feasibility of bimetallic AM chambers. In addition to the LCUSP program, NASA’s Marshall Space Flight Center (MSFC) has completed a series of development programs and hot-fire tests to demonstrate SLM GRCop-84 and other AM techniques. MSFC’s efforts include a 4,000 pounds-force thrust liquid oxygen/methane (LOX/CH4) combustion chamber. Small thrust chambers for 1,200 pounds-force LOX/hydrogen (H2) applications have also been designed and fabricated with SLM GRCop-84. Similar chambers have also completed development with an Inconel 625 jacket bonded to the GRCop-84 material, evaluating direct metal deposition (DMD) laser- and arc-based techniques. The same technologies for these lower thrust applications are being applied to 25,000-35,000 pounds-force main combustion chamber (MCC) designs. This paper describes the design, development, manufacturing and testing of these numerous combustion chambers, and the associated lessons learned throughout their design and development processes.

Gradl, Paul R.↗

Biocatalyst discovery and design for plastics deconstruction: A multi‐scale perspective

Plastic waste accumulation poses significant environmental challenges due to a lack of economical solutions for the molecular deconstruction of diverse synthetic polymers. Biological‐based degradation offers promise but is hindered by the crystallinity, hydrophobicity, and additive complexity of plastics, which restrict biocatalyst access and activity. To address these problems, we propose a multi‐scale framework that combines detailed materials characterization, optimization of plastic‐biomolecular interfacial interactions, and enhancement of biocatalytic kinetics to develop effective plastic‐deconstructing enzymes. This approach leverages principles from reaction kinetics, transport and interfacial phenomena, and enzyme engineering to systematically address barriers across diverse plastic types. Our framework aims to accelerate the discovery and optimization of biocatalysts capable of scalable, selective, and efficient deconstruction of plastic waste. These advances hold potential to enable sustainable biological recycling and upcycling pathways, contributing to global efforts in mitigating plastic pollution and promoting circular material economies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Development and Hot-fire Testing of Additively Manufactured Copper Combustion Chambers for Liquid Rocket Engine Applications

NASA and industry partners are working towards fabrication process development to reduce costs and schedules associated with manufacturing liquid rocket engine components with the goal of reducing overall mission costs. One such technique being evaluated is powder-bed fusion or selective laser melting (SLM), commonly referred to as additive manufacturing (AM). The NASA Low Cost Upper Stage Propulsion (LCUSP) program was designed to develop processes and material characterization for GRCop-84 (a NASA Glenn Research Center-developed copper, chrome, niobium alloy) commensurate with powder-bed AM, evaluate bimetallic deposition, and complete testing of a full scale combustion chamber. As part of this development, the process has been transferred to industry partners to enable a long-term supply chain of monolithic copper combustion chambers. To advance the processes further and allow for optimization with multiple materials, NASA is also investigating the feasibility of bimetallic AM chambers. In addition to the LCUSP program, NASA has completed a series of development programs and hot-fire tests to demonstrate SLM GRCop-84 and other AM techniques. NASA's efforts include a 4K lbf thrust liquid oxygen/methane (LOX/CH4) combustion chamber and subscale thrust chambers for 1.2K lbf LOX/hydrogen (H2) applications that have been designed and fabricated with SLM GRCop-84. The same technologies for these lower thrust applications are being applied to 25-35K lbf main combustion chamber (MCC) designs. This paper describes the design, development, manufacturing and testing of these numerous combustion chambers, and the associated lessons learned throughout their design and development processes.

Gradl, Paul R.↗