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All sources NASA NTRS DOE OSTI

DOE OSTI2024

Tailoring Solvation Solvent in Localized High-Concentration Electrolytes for Lithium||Sulfurized Polyacrylonitrile

Sulfurized polyacrylonitrile (SPAN) is a promising cathode material for lithium-sulfur (Li-S) batteries due to its significantly reduced polysulfide (PS) dissolution compared to the elemental S cathode. Although conventional carbonate-based electrolytes is stable with SPAN electrodes, it is less stable with Li metal anode (LMA). Recently, localized high-concentration electrolytes (LHCEs) have been developed to improve the stability of LMA. Here, we report a new strategy to further improve the performance of LI||SPAN batteries by replacing the conventional solvating solvent 1,2-dimethoxyethane (DME) in the LHCE with a new solvating solvent, 1,2-diethoxyethane (DEE), the new LHCEs exhibits less reactivity against Li 2 S 2 , alleviates PS dissolution, forms a better cathode-electrolyte interphase layer on the SPAN, and enhances structure reversibility even at elevated temperature (ET, 45°C). With the same salt and diluent as in other LHCEs, the LHCE with DEE leads to better performance in Li||SPAN batteries (with 82.9% capacity retention after 300 cycles at ET), preservation of SPAN cathode structure, and suppression of the volume change of LMA. The similar strategy on tailoring the solvating solvents in LHCEs can also be used in other rechargeable batteries to improve their performances.

1,2-diethoxyethane↗

DOE OSTI2023

High–performance water electrolyzer with minimum platinum group metal usage: Iron nitride–iridium oxide core–shell nanostructures for stable and efficient oxygen evolution reaction

Not Available

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1985

Advanced research and technology programs for advanced high-pressure oxygen-hydrogen rocket propulsion

A research and technology program for advanced high pressure, oxygen-hydrogen rocket propulsion technology is presently being pursued by the National Aeronautics and Space Administration (NASA) to establish the basic discipline technologies, develop the analytical tools, and establish the data base necessary for an orderly evolution of the staged combustion reusable rocket engine. The need for the program is based on the premise that the USA will depend on the Shuttle and its derivative versions as its principal Earth-to-orbit transportation system for the next 20 to 30 yr. The program is focused in three principal areas of enhancement: (1) life extension, (2) performance, and (3) operations and diagnosis. Within the technological disciplines the efforts include: rotordynamics, structural dynamics, fluid and gas dynamics, materials fatigue/fracture/life, turbomachinery fluid mechanics, ignition/combustion processes, manufacturing/producibility/nondestructive evaluation methods and materials development/evaluation. An overview of the Advanced High Pressure Oxygen-Hydrogen Rocket Propulsion Technology Program Structure and Working Groups objectives are presented with highlights of several significant achievements.

Marsik, S. J.↗

NASA NTRS1985

Advanced research and technology program for advanced high pressure oxygen-hydrogen rocket propulsion

Marsik, S. J.↗

DOE OSTI2024

Analytical Tools to Assess Polymer Biodegradation: A Critical Review and Recommendations

Many petroleum-derived plastic materials are highly recalcitrant and persistent in the environment, posing significant threats to human and ecological receptors due to their accumulation in ecosystems. In recent years, research efforts have focused on advancing biological methods for polymer degradation. Enzymatic depolymerization has emerged as particularly relevant for biobased plastic recycling, potentially scalable for industrial use. Biodegradation involves adsorption to the plastic solid surface, followed by an interfacial reaction, resulting in cleavage of bonds of polymer chains exposed on the surface. Here, widely varying substrate-specific kinetics are observed, with the polymer’s properties possessing a significant impact on the rate of this interfacial catalysis. Thus, there is a critical need for sensitive and accurate characterization of the material surface during and after interfacial depolymerization to fully understand the reaction mechanisms. Here, we provide a critical review of a range of techniques used in the analysis of material surfaces to characterize the chemical, topological, and morphological features relevant to the study of enzymatic biocatalysis, including microscopy techniques, spectroscopic techniques (e.g., X-ray diffraction analysis, Fourier transform infrared attenuated total reflectance spectroscopy, and mass spectrometry detection of analytes associated with degradation). Techniques for evaluation of surface energy and topology in their relevancy for sensitive detection of biological surface modifications are also discussed. In addition, this paper provides an overview of the strengths of these techniques and compares their performance in both sensitivity and throughput, including emerging techniques, which can be useful, particularly for the rapid analysis of the surface properties of polymeric materials in high-throughput screening of candidate biocatalysts. This research serves as a starting point in selecting and applying appropriate methodologies that provide direct evidence to the ongoing biotic degradation of polymeric materials.

Colachis, Matthew↗

DOE OSTI2020

Ambient Ion Trapping and Separations for High Throughput Structurally Selective Material Deposition

While ion mobility coupled to mass spectrometry (IMS/MS) has been increasingly adapted to biological analysis, the structural and molecular specificity offered by IMS/MS has untapped potential for creating novel materials (for energy, catalysis, biomolecular switches etc.) with rationally tailored properties by precisely controlling the chemical structure and composition of these materials. While electrochemical and catalytic properties of the bulk material are understood by mass-selective ion-soft-landing, different structures of one molecule can exhibit distinct properties from the bulk. Many biological phenomenon occur at interfaces and are highly structurally specific. IMS/MS offers means to separate molecules in a sample (which is first ionized and released to gas phase from the condensed phase) based on mass and structure. Species thus separated can potentially be deposited onto surfaces with molecular and structural specificity, to perform fundamental investigations for understanding critical interfacial phenomenon. Key performance metrics for IMS/MS analysis are resolution of separations and sensitivity. Recently developed Structures for Lossless Ion Manipulations (SLIM)4 enabled unprecedented resolution in IMS separations. In addition, high sensitivity was enabled in SLIM due to lossless confinement of ions using radio frequency fields. Thus, SLIM enabled extremely long path length separations (up to 0.1 km thus far) providing efficient separation of molecular ions never before achieved (e.g. isotopologues, D&L amino acids). While SLIM has unprecedented analytical separations power/utility, the use of SLIM platform for depositing mobility and mass selected molecular ions has two specific technological challenges: (a) Pulsed nature of IMS separations and their low duty cycle and (b) the need for a low vacuum of ~4 torr for lossless ion confinement. These limitations lead to long deposition times due to loss of ions generated from the sample. Enabling ion confinement at atmospheric pressure will be path-breaking contribution to the fundamental understanding of ion manipulations and separations and will also enable novel science currently precluded due to the inability of the present technologies to confine ions under ambient conditions. Traditionally used radio frequency fields are ineffective in confining ions at high pressures due to ion/neutral collisions. To address these, we propose to (a) develop methods for confining and manipulating ions for lossless IMS separations at atmospheric pressure enabling high sensitivity and throughput and (b) use the high specificity of IMS/MS and high throughput from ambient ion confinement to perform mobility and mass selective ion deposition at atmospheric pressure. Our goal is to enable the study of the fundamental properties of energy/catalysis materials and biomolecules. This project paves the way for high-throughput, mass and structure selective material deposition for highly specific surface creation/functionalization (discussed in Section 2 of the report). Further, the developments reported continue to push the boundaries of this process to ambient conditions (discussed in Section 3 of the report). We conclude with a list of specific intellectual property and publications which have been the outcome of this funded project.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Early Progress Toward the Feasibility of the Centrifugal Nuclear Thermal Rocket

The Centrifugal Nuclear Thermal Rocket (CNTR) is a Nuclear Thermal Propulsion (NTP) concept designed to heat propellant directly by the reactor fuel. The primary difference between the CNTR concept and traditional NTP systems is that rather than using traditional solid fuel elements, the CNTR uses liquid fuel with the liquid contained in rotating cylinders by centrifugal force. If the concept can be successfully realized, the CNTR would have a high specific impulse (~1800 seconds) at high thrust, which may enable (i) viable near-term human Mars exploration by reducing round-trip times to 420 days and (ii) direct injection orbits for scientific missions to the Solar System outer planets and potentially Kuiper Belt objects. The CNTR could also use storable propellants such as ammonia, methane, or hydrazine at an Isp of ~900 seconds, enabling long-term in-space storage of a dormant system. Significant engineering challenges must be addressed to establish the technical viability of the CNTR. Research is presently underway to determine resolutions for these engineering challenges. In particular, research has begun on the analytical modeling and simulation of the two-phase heat transfer between the liquid metallic uranium fuel and the gaseous propellant. A paper was presented at the 2021 IAC which described these challenges and the study plan to address them. This paper describes the analytical and experimental progress to date toward resolving these challenges and establishing the engineering feasibility of the CNTR technology

High Performance Nuclear Thermal Propulsion NTP SN↗

DOE OSTI2022

Role of nanocellulose in tailoring electroanalytical performance of hybrid nanocellulose/multiwalled carbon nanotube electrodes

Abstract Nanocellulose has emerged as a promising green dispersant for carbon nanotubes (CNTs), and there is an increasing trend in developing nanocellulose/CNT hybrid materials for electrochemical detection of various small molecules. However, there have been very few comprehensive studies investigating the role of nanocellulosic material properties upon the electroanalytical performance of the resultant hybrid electrodes. In this work, we demonstrate the influence of both nanocellulose functionalization and geometry, utilizing sulfated cellulose nanocrystals, sulfated cellulose nanofibers, and TEMPO-oxidized cellulose nanofibers. Transmission electron microscopy tomography enables direct visualization of the effect of nanocellulosic materials on the hybrid architectures. High resolution X-ray absorption spectroscopy verifies that the chemical nature of CNTs in the different hybrids is unmodified. Electroanalytical performances of the different nanocellulose/CNT hybrid electrodes are critically evaluated using physiologically relevant biomolecules with different charge such as, dopamine (cationic), paracetamol (neutral), and uric acid (anionic). The hybrid electrode containing fibrillar nanocellulose geometry with a high degree of sulfate group functionalization provides the highest electroanalytical sensitivity and strongest enrichment towards all studied analytes. These results clearly demonstrate for the first time, the extent of tailorability upon the electroanalytical response of nanocellulose/CNT hybrid electrodes towards different biomolecules, offered simply by the choice of nanocellulosic materials.

Durairaj, Vasuki↗

DOE OSTI2021

Mass transport in nanoarray monolithic catalysts: An experimental-theory study

Reducing the mass transfer resistance globally of a catalyst is a key to enhancing the catalytic reaction kinetics and fully utilizing the catalyst activity. Despite the success in tailoring the external mass transfer in the widely studied washcoat monoliths, the internal mass transfer resistance is difficult to be reduced due to the requirement of increasing macroporosity while maintaining high specific surface area and mechanical stability. Therefore, nanostructured array-based monolithic catalysts (nanoarray catalysts) have been developed in the past decade as a promising class of structured catalysts that may complement or substitute washcoat catalysts. This work fundamentally elucidates the enhanced mass transport properties of the nanoarray monolithic catalysts by a combination of experimental measurements and theoretical modeling. Using a low-dimensional model, the relative contributions of resistances were quantified in terms of chemical kinetics, internal and external mass transfers based on a probe model of C2H4 oxidation over the TiO2 supported Pt-based monolithic catalysts. The nanoarray catalysts displayed a lower internal mass transfer resistance than the washcoat counterparts as a result of the high macroporosity and small thickness of nanoarray layers. Finally, the nanoarray configuration provides a new pathway towards designing high-performance monolithic reactors and catalysts with low internal diffusion limitations for various gas phase reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Confined Ni-In intermetallic alloy nanocatalyst with excellent coking resistance for methane dry reforming

Carbon dioxide and methane are two main greenhouse gases which are contributed to serious global warming. Fortunately, dry reforming of methane (DRM), a very important reaction developed decades ago, can convert these two major greenhouse gases into value-added syngas or hydrogen. The main problem retarding its industrialization is the seriously coking formation upon the nickel-based catalysts. Herein, a series of confined indium-nickel (In-Ni) intermetallic alloy nanocatalysts (In x Ni@SiO 2 ) have been prepared and displayed superior coking resistance for DRM reaction. The sample containing 0.5 wt.% of In loading (In 0.5 Ni@SiO 2 ) shows the best balance of carbon deposition resistance and DRM reactivity even after 430 h long term stability test. The boosted carbon resistance can be ascribed to the confinement of core–shell structure and to the transfer of electrons from Indium to Nickel in In-Ni intermetallic alloys due to the smaller electronegativity of In. Additionally, both the silica shell and the increase of electron cloud density on metallic Ni can weaken the ability of Ni to activate C–H bond and decrease the deep cracking process of methane. The reaction over the confined InNi intermetallic alloy nanocatalyst was conformed to the Langmuir-Hinshelwood (L-H) mechanism revealed by in situ diffuse reflectance infrared Fourier transform spectroscopy (in-situ DRIFTS). This work provides a guidance to design high performance coking resistance catalysts for methane dry reforming to efficiently utilize these two main greenhouse gases.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Addressing the Challenge of Electrochemical Ionomer Oxidation in Future Anion Exchange Membrane Water Electrolyzers

Hydrogen production through anion-exchange membrane water electrolyzers (AEMWEs) offers cost advantages over proton-exchange membrane counterparts, mainly due to the good oxygen evolution reaction (OER) activity of platinum-group-metal-free catalysts in alkaline environments. However, the electrochemical oxidation of ionomers at the OER catalyst interface can decrease the local electrode pH, which limits AEMWE performance. Various strategies at the single-cell-level have been explored to address this issue. Here, this work reviews the current understanding of electrochemical ionomer oxidation and strategies to mitigate it, providing our perspective on each approach. Our analysis highlights the competitive adsorption strategy as particularly promising for mitigating ionomer oxidation. This Perspective also outlines future directions for advancing high-performance alkaline AEMWEs and other energy devices using hydrocarbon ionomers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Direct ladderization of cyclooctatetraene-containing, processable conjugated ladder polymers from annulated bis-zirconacyclopentadienes

Conjugated ladder polymers (CLPs) are difficult yet captivating synthetic targets due to their fully unsaturated fused backbones. Inherent challenges associated with their synthesis often lead to low yields, structural defects, and insoluble products. Here a new method to form CLPs is demonstrated, utilizing a high-yielding dimerization of annulated zirconacyclopentadienes to form cyclooctatetraene (COT) monomer units. The resulting COT-containing polymers form rapidly in a single ladderization step from the bis-zirconacyclopentadiene precursors and display M n up to 29.7 kg mol -1 . The polymers represent rare examples of CLPs with negatively curved rings, resulting in the observation of unusual properties. The rigid tub-shaped COT units embedded in the backbone imbue the polymers with microporosity, exhibiting BET surface areas up to 555 m 2 g -1 . Additionally, the remarkable solubility of these CLPs in organic solvents enables the fabrication of thin films showcasing high dielectric performance with a discharged energy density as high as 6.54 J cm -3 at 650 MV m -1 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1972

Hydrogen-oxygen catalytic ignition and thruster investigation. Volume 1: Catalytic ignition and low pressure thruster evaluations

An experimental and analytical program was conducted to evaluate catalytic igniter operational limits, igniter scaling criteria, and delivered performance of cooled, flightweight gaseous hydrogen-oxygen reaction control thrusters. Specific goals were to: (1) establish operating life and environmental effects for both Shell 405-ABSG and Engelhard MFSA catalysts, (2) provide generalized igniter design guidelines for high response without flashback, and (3) to determine overall performance of thrusters at chamber pressures of 15 and 300 psia (103 and 2068 kN/sq m) and thrust levels of 30 and 1500 lbf, respectively. The experimental results have demonstrated the feasibility of reliable, high response catalytic ignition and the effectiveness of ducted chamber cooling for a high performance flightweight thruster. This volume presents the results of the catalytic igniter and low pressure thruster evaluations are presented.

Johnson, R. J.↗

NASA NTRS1973

Investigation of flow fields within large scale hypersonic inlet models

Analytical and experimental investigations were conducted to determine the internal flow characteristics in model passages representative of hypersonic inlets for use at Mach numbers to about 12. The passages were large enough to permit measurements to be made in both the core flow and boundary layers. The analytical techniques for designing the internal contours and predicting the internal flow-field development accounted for coupling between the boundary layers and inviscid flow fields by means of a displacement-thickness correction. Three large-scale inlet models, each having a different internal compression ratio, were designed to provide high internal performance with an approximately uniform static-pressure distribution at the throat station. The models were tested in the Ames 3.5-Foot Hypersonic Wind Tunnel at a nominal free-stream Mach number of 7.4 and a unit free-stream Reynolds number of 8.86 X one million per meter.

Gnos, A. V.↗

NASA NTRS1980

An assessment of the readiness of ablative materials for preflight application to the shuttle orbiter

The shuttle orbiter relies primarily on a reusable surface insulation (RSI) thermal protection system (TPS). The RSI is very efficient in its thermal performance; however, the RSI tile system has shown poor mechanical integrity. The state-of-the-art of the ablative TPS is reviewed, and an assessment made of the ablator's readiness for use on the shuttle orbiter. Unresolved technical issues with regard to the ablative TPS are identified. Short time, highly focused analytical and experimental programs were initiated to: (1) identify candidate ablation materials; (2) assess the data base for these materials; (3) evaluate the need and kind of waterproof coating; (4) calculate thermal and other stresses in an ablator tile; (5) identify an acceptable ablator/RSI tile joint filler; and (6) assess the sensitivity of the ablator to sequential heat pulses. Results from some of these programs are discussed.

Tompkins, S. S.↗

NASA NTRS1989

Apollo Lightcraft Project

The ultimate goal for this NASA/USRA-sponsored Apollo Lightcraft Project is to develop a revolutionary manned launch vehicle technology which can potentially reduce payload transport costs by a factor of 1000 below the Space Shuttle Orbiter. The Rensselaer design team proposes to utilize advanced, highly energetic, beamed-energy sources (laser, microwave) and innovative combined-cycle (airbreathing/rocket) engines to accomplish this goal. The research effort focuses on the concept of a 100 MW-class, laser-boosted Lightcraft Technology Demonstrator (LTD) drone. The preliminary conceptual design of this 1.4 meter diameter microspacecraft involved an analytical performance analysis of the transatmospheric engine in its two modes of operation (including an assessment of propellant and tankage requirements), and a detailed design of internal structure and external aeroshell configuration. The central theme of this advanced propulsion research was to pick a known excellent working fluid (i.e., air or LN sub 2), and then to design a combined-cycle engine concept around it. Also, a structural vibration analysis was performed on the annular shroud pulsejet engine. Finally, the sensor satellite mission was examined to identify the requisite subsystem hardware: e.g., electrical power supply, optics and sensors, communications and attitude control systems.

Myrabo, Leik N.↗

NASA NTRS1994

Unsteady aerodynamic analyses for turbomachinery aeroelastic predictions

Applications for unsteady aerodynamics analysis in this report are: (1) aeroelastic: blade flutter and forced vibration; (2) aeroacoustic: noise generation; (3) vibration and noise control; and (4) effects of unsteadiness on performance. This requires that the numerical simulations and analytical modeling be accurate and efficient and contain realistic operating conditions and arbitrary modes of unsteady excitation. The assumptions of this application contend that: (1) turbulence and transition can be modeled with the Reynolds averaged and using Navier-Stokes equations; (2) 'attached' flow with high Reynolds number will require thin-layer Navier-Stokes equations, or inviscid/viscid interaction analyses; (3) small-amplitude unsteady excitations will need nonlinear steady and linearized unsteady analyses; and (4) Re to infinity will concern inviscid flow. Several computer programs (LINFLO, CLT, UNSVIS, AND SFLOW-IVI) are utilized for these analyses. Results and computerized grid examples are shown. This report was given during NASA LeRC Workshop on Forced Response in Turbomachinery in August of 1993.

Verdon, Joseph M.↗

NASA NTRS2017

Milli-Watt Radioisotope Power to Enable Small, Long-Term Robotic “Probe” Space Exploration

Milli-watt Radioisotope Power Systems (RPS) based on Radioisotope Heater Units (RHUs) could be an ideal power source for certain spacecraft that cannot use solar power due to large distances from the sun, or other environmental constraints, and where they enable or significantly enhance the ability of a mission to meet its scientific or operational goals. Various modular, compact RHU-based thermoelectric (TE) generator concepts developed or derived from current NASA Small Business Innovation Research (SBIR) projects satisfying this need have been investigated. These modular, compact and low mass power systems could support small, highly-mobile robotic exploration packages, and could be incorporated into different robotic package concepts, spacecraft or satellites. Current modular RPS design concepts with 40mW, 80mW and 120mW power levels use RHUs and Bi2Te3 TE converters. Skutterudites materials could be used in the future if new higher thermal energy output and higher temperature miniature heat sources were developed, for example, using technologies currently in the General Purpose Heat Source (GPHS) used in higher electric power output RTGs. Small (a.k.a., “mice-like”) robotic packages could effectively utilize these RHU-driven power levels to accommodate crawling, climbing, monitoring, taking measurements, and communicating during long-term planetary missions aimed at gathering environmental and geologic data (i.e., over multiple decades). Waste heat from the cold side of the TE converter could also be directed toward the electronics and / or energy storage (e.g. batteries) to keep them within design temperature ranges. In addition to power generation and electronics / battery heating, the RHU / TE configuration could be designed to survive an external 500°C bake out procedure for critical spacecraft sterilization, environmental certification and planetary protection. Analytical studies have been performed to optimize various design configurations for power, mass, volume and robotic mobility. Specific power (mW/kg) and volumetric specific power (mW/cm3) characteristics of various design configurations will be presented and key conceptual design tradeoffs will be discussed. Hot- and cold-side thermal interfaces required to meet power and mass goals and associated design sensitivities will also be discussed. RHU / TE systems must overcome critical design challenges to survive high-g loadings in some robotic applications and we will examine the mass impacts required to satisfy various dynamic loading environments up to 10,000 g’s. Power can be generated for a minimum of 30 years or more using plutonium-238 dioxide heat sources (given that Pu-238 has an 87.7 year half-life) with some reduction in power as the heat source naturally degrades.

Bahrami, Poyan↗