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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 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS2011

Carbon Isotope Systematics in Mineral-Catalyzed Hydrothermal Organic Synthesis Processes at High Temperature and Pressures

Observation of methane in the Martian atmosphere has been reported by different detection techniques. Reduction of CO2 and/or CO during serpentization by mineral surface catalyzed Fischer-Tropsch Type (FTT) synthesis may be one possible process responsible for methane generation on Mars. With the evidence a recent study has discovered for serpentinization in deeply buried carbon rich sediments, and more showing extensive water-rock interaction in Martian history, it seems likely that abiotic methane generation via serpentinization reactions may have been common on Mars. Experiments involving mineral-catalyzed hydrothermal organic synthesis processes were conducted at 750 C and 5.5 Kbars. Alkanes, alcohols and carboxylic acids were identified as organic compounds. No "isotopic reversal" of delta C-13 values was observed for alkanes or carboxylic acids, suggesting a different reaction pathway than polymerization. Alcohols were proposed as intermediaries formed on mineral surfaces at experimental conditions. Carbon isotope data were used in this study to unravel the reaction pathways of abiotic formation of organic compounds in hydrothermal systems at high temperatures and pressures. They are instrumental in constraining the origin and evolution history of organic compounds on Mars and other planets.

Fu, Qi↗
DOE OSTI2024

Synthesis, Processing, and Use of Isotopically Enriched Epitaxial Oxide Thin Films

Isotopic engineering has emerged as a key approach to study the nucleation, diffusion, phase transitions, and reactions of materials at an atomic level. It aims to uncover mass transport pathways, kinetics, and operational and failure mechanisms of functional materials and devices. Understanding these phenomena leads to deeper insights into important physical processes, such as the transport of ions in energy conversion and storage devices and the role of active sites and supports during heterogeneous catalytic reactions. Likewise, isotopic engineering is being pursued as a means of modifying functionality to enable future technological applications. In this Account, we summarize our recent work employing isotope labeling (e.g., 18 O 2 and 57 Fe) during thin film synthesis and postgrowth processing to reveal growth mechanisms, defect chemistry, and elemental diffusion under working and extreme conditions. Isotope-resolved analysis techniques with nanometer-scale spatial resolution, such as time-of-flight secondary ion mass spectrometry and atom probe tomography, facilitate the accurate quantification of isotopic placement and concentration in our well-defined heterostructures with precisely positioned, isotope-enriched layers. By measuring the nanometer-scale redistribution between natural abundance and isotopically enriched oxygen layers during the deposition of Fe 2 O 3 and Cr 2 O 3 by molecular beam epitaxy, we identified intermixing processes driven by surface adatoms occurring both at the film growth surface and within the first few layers below the surface. Further insights into synthesis mechanisms were gained by studying the tungsten oxide thin films grown by evaporating WO 3 powder in the presence of background 18 O 2 , revealing minimal incorporation of background oxygen during the film formation process. Thermal and radiation-enhanced diffusion in epitaxial Fe and Cr oxides were precisely tracked using 18 O and 57 Fe tracer layers incorporated into model epitaxial oxide thin films. This approach has allowed us to access thermal diffusion behavior at lower temperatures than previously measured, revealing a potential changeover in diffusion mechanism. Understanding radiation-enhanced diffusion in model oxides that represent the surface layers on the structural components of nuclear reactors informs our understanding of their corrosion behavior under irradiation. Isotopic labeling can also provide unique insights into the surface exchange reactions and defect chemistry of electrocatalysts. For instance, tracking the change in 18 O concentration at the surface of an epitaxial LaNiO 3 thin film after the electrocatalytic oxygen evolution reaction revealed the participation of lattice oxygen, confirming a hypothesis that had been proposed previously. Lastly, we highlight a new direction wherein we perform in situ processing studies utilizing isotopic tracers in conjunction with model epitaxial thin films within the atom probe tomography instrument. Additionally, this Account illustrates the great potential of isotopic engineering to enable fundamental mechanistic insights into physical processes and engineer functional properties in epitaxial films, heterostructures, and superlattices.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Automation of Nanoparticle Synthesis Processes in a Plasma Environment Using LabVIEW

This work presents an automated control system for the synthesis of nanomaterials by plasma-enhanced chemical vapor deposition (PECVD), implemented using the LabVIEW software environment. The main objective of the study is to develop an integrated hardware-software platform that enables sequential control of the key stages of the PECVD process, including vacuum chamber preparation, pressure monitoring, working gas supply, plasma ignition, power matching, cyclic nanomaterial growth, and optical monitoring of nanoparticles in the plasma environment. The use of LabVIEW made it possible to integrate actuator control, experimental parameter acquisition, and realtime process visualization within a single automated system. The automated cycle begins with evacuation of the reaction chamber to a predefined base pressure. Transition to the next stage is permitted only after the specified pressure threshold has been reached, ensuring reproducible initial conditions for each experiment. The program then controls the supply of the working gas through mass flow controllers (MFCs). In this work, two gas-flow control modes were considered: analog control using a 0-5 V voltage signal and digital communication via RS-232 interface. It was shown that the analog approach requires accurate scaling of the control voltage, since applying 5 V corresponds to full-scale opening of the controller and results in the maximum gas flow. In contrast, the RS232 interface enables the gas flow rate to be specified directly in sccm, improving the accuracy, flexibility, and convenience of gas-environment control. After pressure stabilization, LabVIEW initiates RF plasma ignition and executes the RF matching algorithm aimed at minimizing reflected power and improving the stability of the plasma process. A separate software module implements the cyclic nanomaterial growth mode, in which the plasma-on time, plasma duration, and total number of synthesis cycles are predefined. This approach makes it possible to control material accumulation on the substrate and to correlate the process parameters with the morphological characteristics of the resulting nanostructures. The final module of the system is designed for optical monitoring of the nanoparticle cloud density in dusty plasma. For this purpose, the change in the intensity of laser radiation passing through the plasma region is recorded using a photodetector and a Keithley 2401 measuring unit connected to LabVIEW via RS-232 interface. The difference between the initial and modified optical signal intensity is used as a diagnostic parameter characterizing the formation and temporal evolution of nanoparticles. The developed system demonstrates that LabVIEW can be effectively applied not only for the automation of individual instruments, but also for the implementation of a complete digital control cycle for PECVD-based nanomaterial synthesis.

PECVD↗
NASA NTRS2010

Carbon Isotopes of Alkanes in Hydrothermal Abiotic Organic Synthesis Processes at High Temperatures and Pressures: An Experimental Study

Observation of methane in the Martian atmosphere has been reported by different detection techniques [1-4]. With more evidence showing extensive water-rock interaction in Martian history [5-7], abiotic formation by Fischer-Tropsch Type (FTT) synthesis during serpentization reactions may be one possible process responsible for methane generation on Mars [8, 9]. While the experimental studies performed to date leave little doubt that chemical reactions exist for the abiotic synthesis of organic compounds by mineral surface-catalyzed reactions [10-12], little is known about the reaction pathways by which CO2 and/or CO are reduced under hydrothermal conditions. Carbon and hydrogen isotope measurements of alkanes have been used as an effective tool to constrain the origin and reaction pathways of hydrocarbon formation. Alkanes generated by thermal breakdown of high molecular weight organic compounds have carbon and hydrogen isotopic signatures completely distinct from those formed abiotically [13-15]. Recent experimental studies, however, showed that different abiogenic hydrocarbon formation processes (e.g., polymerization vs. depolymerization) may have different carbon and hydrogen isotopic patterns [16]. Results from previous experiments studying decomposition of higher molecular weight organic compounds (lignite) also suggested that pressure could be a crucial factor affecting fractionation of carbon isotopes [17]. Under high pressure conditions, no experimental data are available describing fractionation of carbon isotope during mineral catalyzed FTT synthesis. Thus, hydrothermal experiments present an excellent opportunity to provide the requisite carbon isotope data. Such data can also be used to identify reaction pathways of abiotic organic synthesis under experimental conditions.

Fu, Qi↗
DOE OSTI2025

Moderate-temperature solution-processed synthesis of incommensurate Sr 8/7 TiS 3 thin films and rod-shaped nanocrystals

The chalcogenide perovskite family has been steadily gaining increasing attention from the research community due to its optoelectronic properties and potential for diverse applications. While BaZrS 3 and BaTiS 3 have been the most extensively studied, other promising compounds in this family, such as Sr x TiS 3 (1.05 < x < 1.22), are now being explored for various optical, optoelectronic, and energy storage applications. However, challenges remain in achieving the low-temperature synthesis of Sr x TiS 3 . In this study, we report, for the first time, the synthesis of Sr x TiS 3 nanocrystals at temperatures below 400 °C. The synthesized nanocrystals exhibit a rod-like morphology. Additionally, we have developed solution-processing routes to synthesize phase-pure Sr x TiS 3 thin films, marking the first reported instance of such films, at temperatures below 600 °C. We also demonstrate the solid-state synthesis of Sr x TiS 3 powder below 600 °C. Our work paves the way for new and exciting application avenues for Sr x TiS 3 .

36 MATERIALS SCIENCE↗
NASA NTRS2014

Synthesis, Processing, and Characterization of Inorganic-Organic Hybrid Cross-Linked Silica, Organic Polyimide, and Inorganic Aluminosilicate Aerogels

As aerospace applications become ever more demanding, novel insulation materials with lower thermal conductivity, lighter weight and higher use temperature are required to fit the aerospace application needs. Having nanopores and high porosity, aerogels are superior thermal insulators, among other things. The use of silica aerogels in general is quite restricted due to their inherent fragility, hygroscopic nature, and poor mechanical properties, especially in extereme aerospace environments. Our research goal is to develop aerogels with better mechanical and environmental stability for a variety of aeronautic and space applications including space suit insulation for planetary surface missions, insulation for inflatable structures for habitats, inflatable aerodynamic decelerators for entry, descent and landing (EDL) operations, and cryotank insulation for advance space propulsion systems. Different type of aerogels including organic-inorganic polymer reinforced (hybrid) silica-based aerogels, polyimide aerogels and inorganic aluminosilicate aerogels have been developed and examined.

Insulation materials↗
NASA NTRS1990

Synthesis: Intertwining product and process

Synthesis is a proposed systematic process for rapidly creating different members of a program family. Family members are described by variations in their requirements. Requirements variations are mapped to variations on a standard design to generate production quality code and documentation. The approach is made feasible by using principles underlying design for change. Synthesis incorporates ideas from rapid prototyping, application generators, and domain analysis. The goals of Synthesis and the Synthesis process are discussed. The technology needed and the feasibility of the approach are also briefly discussed. The status of current efforts to implement Synthesis methodologies is presented.

Weiss, David M.↗
NASA NTRS2008

State of the Art Assessment of Simulation in Advanced Materials Development

Advances in both the underlying theory and in the practical implementation of molecular modeling techniques have increased their value in the advanced materials development process. The objective is to accelerate the maturation of emerging materials by tightly integrating modeling with the other critical processes: synthesis, processing, and characterization. The aims of this report are to summarize the state of the art of existing modeling tools and to highlight a number of areas in which additional development is required. In an effort to maintain focus and limit length, this survey is restricted to classical simulation techniques including molecular dynamics and Monte Carlo simulations.

Wise, Kristopher E.↗
NASA NTRS1988

Improved synthesis of ceramic superconductors with alkaline earth peroxides - Synthesis and processing of Ba2YCu3O(7-x)

Synthesis processes for the preparation of ceramic conductors Ba2YCu3O(7-x) from BaO2 or BaCO3 in flowing O2 or N2 are described, and the characteristics of the materials produced in these processes are compared. Results of EDAX, XRD, SEM, and dc resistivity analyses demonstrated that superconducting materials made from BaO2 were more homogeneous, denser, and more metallic than materials produced from BaCO3, because of the higher reactivity of BaO2. Potential applications of this processes are discussed.

Hepp, A. F.↗
NASA NTRS1990

Polysiloxanes derived from the controlled hydrolysis of tetraethoxysilane as precursors to silica for use in ceramic processing

Synthesis, properties, and potential applications in ceramic processing for two polysiloxane silica precursors derived from the controlled hydrolysis of tetraethoxysilane (TEOS) are presented. The higher molecular weight TEOS-A is a thick adhesive liquid of viscosity 8000 to 12,000 c.p. having a SiO2 char yield of about 55 percent. The lower molecular weight TEOS-B is a more fluid liquid of viscosity 150 to 200 c.p. having a SiO2 char yield of about 52 percent. The acid catalyzed hydrolysis of TEOS to hydrated silica gel goes through a series of polysiloxane intermediates. The rate of this transition increases with the quantity of water added to the TEOS; thus, for ease of polymer isolation, the amount of water added must be carefully determined so as to produce the desired polymer in a reasonable time. The water to TEOS mole ratio falls in the narrow range of 1.05 for TEOS-A and 0.99 for TEOS-B. Further polymerization or gelation is prevented by storing at -5 C in a freezer. Both polysiloxanes thermoset to a glassy solid at 115 C. The liquid polymers are organic in nature in that they are miscible with toluene and ethanol, slightly souble in heptane, but immiscible with water. For both polymers, results on viscosity versus time are given at several temperatures and water additions. Based on these results, some examples of practical utilization of the precursors for ceramic fabrication are given.

Philipp, Warren H.↗
DOE OSTI2026

Revealing multiscale competing processes in the solid-state synthesis of single-crystalline layered oxide positive electrodes

Solid-state synthesis involves a web of coupled chemical reactions and physical changes that unfold across multiple scales. Efforts to fine-tune its parameters have historically followed heuristic, trial-driven workflows that demand significant time and resources. In this study, we aimed to open this black box by employing multiscale in situ synchrotron imaging and diffraction. Using LiNi 0.5 Mn 0.3 Co 0.2 O 2 battery positive electrode material as a model system and Ba-based sintering aids, we reveal dopant segregation, intergranular mass transport, and porosity evolution as key drivers of single-crystalline particle formation. Notably, we uncovered a dynamic competition between particle-level grain coalescence and atomic-scale cation disordering, both of which are thermally activated yet have opposing impacts on battery performance. These findings highlight the coupled, multiscale nature of structure development and offer a mechanistic basis for optimizing the solid-state synthesis process. This framework provides a path toward more controlled, efficient, and scalable production of high-performance battery positive electrode materials.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Laser-enhanced synthesis and processing of diamond films from liquid hydrocarbons

We report synthesis of diamond films by pulsed laser irradiation on copper substrate immersed into liquid benzene. It is envisaged that carbon released from benzene at the liquid-solid interface is converted into diamond as a result of rapid quenching from a high temperature. The diamond crystallites were characterized using high resolution transmission electron microscopy imaging and electron diffraction techniques. Growth of thicker diamond films by subsequent chemical vapor deposition has been investigated by transmission and scanning electron microscopy techniques. Thin diamond film deposited during liquid phase provided seed for diamond growth during subsequent chemical vapor deposition.

Singh, Jogender↗
NASA NTRS1999

The Effects of Gravity on Combustion and Structure Formation During Synthesis of Advanced Materials

Combustion in a variety of heterogeneous systems, leading to the synthesis of advanced materials, is characterized by high temperatures (2000-3500 K) and heating rates (up to 10(exp 6) K/s) at and ahead of the reaction front. These high temperatures generate liquids and gases which are subject to gravity-driven flow. The removal of such gravitational effects is likely to provide increased control of the reaction front, with a consequent improvement in control of the microstructure of the synthesized products. Thus, microgravity experiments can lead to major advances in the understanding of fundamental aspects of combustion and structure formation under the extreme conditions of the combustion synthesis wave. In addition, the specific features of microgravity environment allow one to produce unique materials, which cannot be obtained under terrestrial conditions. The general goals of the current research are: 1) to improve the understanding of fundamental phenomena taking place during combustion of heterogeneous systems, 2) to use low-gravity experiments for insight into the physics and chemistry of materials synthesis processes, and 3) based on the obtained knowledge, to optimize processing conditions for synthesis of advanced materials with desired microstructures and properties. This research follows logically from the results of investigations we have conducted in the framework of our previous grant on gravity influence on combustion synthesis (CS) of gasless systems. Prior work, by others and by us, has clearly demonstrated that gravity plays an important role during combustion synthesis of materials. The immediate tasks for the future are to quantitatively identify the nature of observed effects, and to create accurate local kinetic models of the processes, which can lead to a control of the microstructure and properties of the synthesized materials. In summary, this is the value of the proposed research. Based on our prior work, we focus on the fundamental aspects of combustion and structure formation under the unique condition of microgravity.

Varma, A.↗
NASA NTRS2003

Traceability Through Automatic Program Generation

Program synthesis is a technique for automatically deriving programs from specifications of their behavior. One of the arguments made in favour of program synthesis is that it allows one to trace from the specification to the program. One way in which traceability information can be derived is to augment the program synthesis system so that manipulations and calculations it carries out during the synthesis process are annotated with information on what the manipulations and calculations were and why they were made. This information is then accumulated throughout the synthesis process, at the end of which, every artifact produced by the synthesis is annotated with a complete history relating it to every other artifact (including the source specification) which influenced its construction. This approach requires modification of the entire synthesis system - which is labor-intensive and hard to do without influencing its behavior. In this paper, we introduce a novel, lightweight technique for deriving traceability from a program specification to the corresponding synthesized code. Once a program has been successfully synthesized from a specification, small changes are systematically made to the specification and the effects on the synthesized program observed. We have partially automated the technique and applied it in an experiment to one of our program synthesis systems, AUTOFILTER, and to the GNU C compiler, GCC. The results are promising: 1. Manual inspection of the results indicates that most of the connections derived from the source (a specification in the case of AUTOFILTER, C source code in the case of GCC) to its generated target (C source code in the case of AUTOFILTER, assembly language code in the case of GCC) are correct. 2. Around half of the lines in the target can be traced to at least one line of the source. 3. Small changes in the source often induce only small changes in the target.

Richardson, Julian↗
DOE OSTI2025

Fuel Salt Synthesis for the Molten Chloride Reactor Experiment: Scale-up, Operations, and Production Update

Over the previous 5 years, Idaho National Laboratory (INL) has been working with Southern Co. and TerraPower on the Advanced Reactor Demonstration Program (ARDP) funded Molten Chloride Reactor Experiment (MCRE) project. As part of this effort, INL has developed a fuel synthesis process to produce the NaCl-UCl3 fuel salt that MCRE will need for operation. Dr. Phillips will present on process development and scale-up testing and results, as well as provide an update on the current status of fuel production for MCRE. To date, the fuel synthesis process has been demonstrated at full scale using depleted uranium, and the equipment necessary for production of the fuel for MCRE has been installed in the Fuel Manufacturing Facility (FMF) at the INL’s Materials and Fuels Complex (MFC). The NaCl-UCl3 produced to-date has been shown to be of 99.99% purity or greater, and be within tolerance for all relevant parameters. Overall process efficiency in terms of uranium utilization has been demonstrated to be above 90%. The synthesis operation has also been shortened to allow for completion of the reaction within a single 10 hour working shift. Consequently, the process developed is expected to be capable of meeting all project objectives for efficiency, purity, scale, and scheduling. Production of NaCl-UCl3 fuel salt for MCRE is projected to begin during the Summer of 2025.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1987

Processing of laser formed SiC powder

Processing research was undertaken to demonstrate that superior SiC characteristics could be achieved through the use of ideal constituent powders and careful post-synthesis processing steps. Initial research developed the means to produce approximately 1000 A uniform diameter, nonagglomerated, spherical, high purity SiC powders. Accomplishing this goal required major revision of the particle formation and growth model from one based on classical nucleation and growth to one based on collision and coalescence of Si particles followed by their carburization. Dispersions based on pure organic solvents as well as steric stabilization were investigated. Test parts were made by the colloidal pressing technique; both liquid filtration and consolidation (rearrangement) stages were modeled. Green densities corresponding to a random close packed structure were achieved. After drying, parts were densified at temperatures ranging from 1800 to 2100 C. This research program accomplished all of its major objectives. Superior microstructures and properties were attained by using powders having ideal characteristics and special post-synthesis processing procedures.

Haggerty, J. S.↗
NASA NTRS1990

Application of advanced multidisciplinary analysis and optimization methods to vehicle design synthesis

Advanced multidisciplinary analysis and optimization methods, namely system sensitivity analysis and non-hierarchical system decomposition, are applied to reduce the cost and improve the visibility of an automated vehicle design synthesis process. This process is inherently complex due to the large number of functional disciplines and associated interdisciplinary couplings. Recent developments in system sensitivity analysis as applied to complex non-hierarchic multidisciplinary design optimization problems enable the decomposition of these complex interactions into sub-processes that can be evaluated in parallel. The application of these techniques results in significant cost, accuracy, and visibility benefits for the entire design synthesis process.

Consoli, Robert David↗