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DOE OSTI2020

Integrated Evaporator for Efficient Solar-Driven Interfacial Steam Generation

Solar-driven interfacial steam generation is a promising technique for clean water production as it can minimize thermal loss by localizing solar-to-heat conversion at the air/liquid interface. Here we report an integrated solar-evaporator by partially growing two-dimensional polypyrrole microsheets within a melamine foam through chemical vapor polymerization. These microsheets can induce multiple light reflections within the foam, enable omnidirectional light absorption, provide abundant surfaces to promote heat transfer, and achieve spatially-defined hydrophobicity to facilitate vapor escape. Meanwhile, the inherent hydrophilicity of the bottom part of the foam promotes spontaneous upward water transport and suppresses heat loss. The composite foam exhibits an excellent apparent evaporation rate of ~2 kg/(m 2 ·h) and solar-to-vapor efficiency of ~91%. Here, the combined advantages of large surface area, high efficiency, low cost, all weather application, excellent durability, and scalable manufacturing make our integrated design promising for fabricating large-scale solar steam generation systems that are suitable for practical clean water production.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Pyrolysis in Molten Salts Converts Plastics into a Mesoporous Electrocatalyst with a High Density of Atomic Fe–N–C Active Site

Upcycling plastic waste into value-added products is a promising strategy for both economic and environmental sustainability. However, achieving control over structure–property correlations during the upcycling process remains challenging. Here, in this study, we investigate the modulation of active site formation during pyrolytic conversion of plastics to carbon by composition-controlled molten salts. Using melamine formaldehyde (MF) foams as a precursor, we demonstrate that their pyrolysis in eutectic chloride molten salts with Fe 2+ , Na + , and K + ions directs the carbonization process toward the formation of mesoporous functional carbon enriched with atomically dispersed Fe–N–C sites, which are well-known for their catalytic activity in oxygen reduction reaction (ORR). Compared to pyrolysis in the FeCl 2 -only salt, the incorporation of alkali metal ions (Na + , K + ) in the eutectic mixture facilitates nitrogen retention in the carbon matrix and modulates iron speciation. This synergistic environment promotes a higher density and more uniform dispersion of Fe–N–C moieties within the carbon matrix. Consequently, the resulting catalyst exhibits a high surface area, hierarchical porosity, and improved electrochemical properties. When tested as an ORR catalyst, the Fe–N–C-enriched catalyst delivers a high half-wave potential (E 1/2 = 0.875 V vs RHE) with nearly exclusive 4e – pathway. These properties are comparable to those of commercial Pt/C catalysts, along with improved stability.

Fe−N−C active sites↗

DOE OSTI2025

Characterization of a mock up nuclear waste package using energy resolved MeV neutron analysis

Reliable radiographic methods for characterizing nuclear waste packages non-destructively (without the need to open containers) have the potential to significantly contribute to safe handling and future disposal options, particularly for legacy waste of unknown content. Due to required shielding of waste containers and the need to characterize materials consisting of light elements, X-ray methods are not suitable. Here, energy-resolved MeV neutron radiography is demonstrated as a first-of-its-kind application for non-destructive and remote examination of mock up nuclear waste packages from a safe position using time-of-flight techniques enabled by a novel event-mode imaging detector system. Energy-resolved neutron transmission spectra were measured spatially, permitting the detection of analogue materials to actual nuclear waste such as water, melamine, and ion exchange resin within a 2.54 cm wall thickness steel pipe. The results demonstrate the capability to locate the materials through this wall thickness by radiography and tomographic reconstruction, revealing detailed 3D distributions and structural anomalies. The method effectively detects residual water in ion exchange resin, highlighting its sensitivity to moisture content, a crucial parameter for nuclear waste characterization. Monte Carlo simulations are in agreement with the experimental findings, providing a pathway to simulate waste forms more difficult to tackle experimentally. This work paves the way to apply sub-nanosecond intense MeV neutron sources, such as laser-driven neutron sources under development, to nuclear waste characterization.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Structural transformation of dusty plasma crystal in dc discharge plasma by changing confinement ring bias

We report an experimental study of the structural transition of a stable complex plasma crystal to a solid-liquid phase coexistence by the controlled adjustment of the confinement potential, while keeping all other parameters constant. The experiments are carried out on a tabletop linear dusty plasma experimental device, which consists of a circular powered electrode and an extended grounded cathode plate. A stationary crystal of melamine formaldehyde particles is formed in a background of argon plasma inside a confining ring that is isolated from the cathode by a ceramic cover. The stable crystal structure breaks in the core region and transitions to a coexistent state by carefully changing the confining potential, thereby modifying the sheath structure. The transition is confirmed by evaluating the variation in different characteristic parameters such as the pair correlation function, local bond order parameter, and dust kinetic temperature as a function of confining bias potential. It is found that melting in the core is due to the onset of dust fluctuations in the layers beneath the topmost layer, which grow in amplitude as the confining bias potential is reduced below a threshold value. The present technique of changing confinement provides a unique feature to study structural transitions of plasma crystals without affecting the overall plasma parameters.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2026

Optimization of an Energy Tuning Assembly for High Explosives Detection

The Portable Isotopic Neutron Spectroscopy (PINS) system, employs neutron-induced gamma-ray spectroscopy and provides a nondestructive method for high explosives detection. In standard operation it uses Californium-252 as a neutron source. Operating PINS with a deuterium-tritium (DT) neutron generator has some advantages over Cf-252, including lifetime and ability to produce high-energy inelastic scattering gamma rays. However, current systems using DT neutron generators suffer from a high environmental background and reduced ability to induce neutron capture, reducing spectral quality and limiting nitrogen sensitivity. Here, this study presents the development of an energy-tuning assembly (ETA) designed to optimize the DT neutron energy spectrum to increase nitrogen reaction rates in a target, thereby improving high explosive detection capabilities. A metaheuristic optimization framework, MultiGNOWEE, coupled with MCNP, was employed to generate two ETA configurations: a single-objective ETA, which maximizes nitrogen capture reactions, and a multi-objective ETA, which balances neutron capture and inelastic scattering. Simulations demonstrated the optimized configurations achieved up to a 10-fold improvement in nitrogen capture rates compared to the bare configuration. Experimental validation was conducted using a DT neutron generator and a high-purity germanium (HPGe) detector. Two prototype ETAs were constructed and assessed on a melamine simulant. Measurements demonstrated improved nitrogen detection for both prototype ETA configurations when compared to the standard system.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2022

A scalable solid-state nanoporous network with atomic-level interaction design for carbon dioxide capture

Carbon capture and sequestration reduces carbon dioxide emissions and is critical in accomplishing carbon neutrality targets. Here, we demonstrate new sustainable, solid-state, polyamine-appended, cyanuric acid–stabilized melamine nanoporous networks (MNNs) via dynamic combinatorial chemistry (DCC) at the kilogram scale toward effective and high-capacity carbon dioxide capture. Polyamine-appended MNNs reaction mechanisms with carbon dioxide were elucidated with double-level DCC where two-dimensional heteronuclear chemical shift correlation nuclear magnetic resonance spectroscopy was performed to demonstrate the interatomic interactions. We distinguished ammonium carbamate pairs and a mix of ammonium carbamate and carbamic acid during carbon dioxide chemisorption. The coordination of polyamine and cyanuric acid modification endows MNNs with high adsorption capacity (1.82 millimoles per gram at 1 bar), fast adsorption time (less than 1 minute), low price, and extraordinary stability to cycling by flue gas. This work creates a general industrialization method toward carbon dioxide capture via DCC atomic-level design strategies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Materials Data on HgC6(N4Cl)3 by Materials Project

HgC3(N2Cl)3(CN2)3 crystallizes in the monoclinic P2_1 space group. The structure is zero-dimensional and consists of two melamine(1+) molecules and two HgC3(N2Cl)3 clusters. In each HgC3(N2Cl)3 cluster, Hg1+ is bonded in a 4-coordinate geometry to one N+1.83- and three Cl1- atoms. The Hg–N bond length is 3.06 Å. There are a spread of Hg–Cl bond distances ranging from 2.37–2.47 Å. There are three inequivalent C4+ sites. In the first C4+ site, C4+ is bonded in a trigonal planar geometry to three N+1.83- atoms. All C–N bond lengths are 1.36 Å. In the second C4+ site, C4+ is bonded in a trigonal planar geometry to three N+1.83- atoms. There is one shorter (1.35 Å) and two longer (1.36 Å) C–N bond length. In the third C4+ site, C4+ is bonded in a trigonal planar geometry to three N+1.83- atoms. All C–N bond lengths are 1.36 Å. There are six inequivalent N+1.83- sites. In the first N+1.83- site, N+1.83- is bonded in a single-bond geometry to one C4+ atom. In the second N+1.83- site, N+1.83- is bonded in a distorted bent 120 degrees geometry to one Hg1+ and two C4+ atoms. In the third N+1.83- site, N+1.83- is bonded in a bent 120 degrees geometry to two C4+ atoms. In the fourth N+1.83- site, N+1.83- is bonded in a single-bond geometry to one C4+ atom. In the fifth N+1.83- site, N+1.83- is bonded in a bent 120 degrees geometry to two C4+ atoms. In the sixth N+1.83- site, N+1.83- is bonded in a single-bond geometry to one C4+ atom. There are three inequivalent Cl1- sites. In the first Cl1- site, Cl1- is bonded in a single-bond geometry to one Hg1+ atom. In the second Cl1- site, Cl1- is bonded in a single-bond geometry to one Hg1+ atom. In the third Cl1- site, Cl1- is bonded in a single-bond geometry to one Hg1+ atom.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Structural transformation of dusty plasma crystal in dc discharge plasma by changing confinement ring bias

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2022

High-Fidelity Mock Development for the Insensitive High Explosive TATB

Due to the violent reaction potential of high explosives, in tests where a reaction is not desired, it can be safe and convenient to use an inert mock that can mimic relevant properties of the associated explosive. Use of mock materials is well-established in explosives work, but most existing mocks are generally meant to mimic only one or two properties of a given explosive, potentially failing to match the explosive in other critical ways. Recently, there has been interest in developing robust thermomechanical mocks for many common explosives. Here, eleven materials are systematically chosen and investigated as potential thermomechanical mocks for TATB, the explosive component of PBX 9502. DSC, nanoindentation, and compression testing are used to narrow down to most appropriate mocks and identify their advantages and limitations. Hardness and elastic modulus are reported for the first time for the molecular crystals iodoanthranilic acid, hexamine, melamine, and trithiolane dioxide, and the crystal structure is reported for the first time for the molecular crystals iodoanthranilic acid and iodosalicylic acid.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Ru Single Atoms on One-Dimensional CF@g-C 3 N 4 Hierarchy as Highly Stable Catalysts for Aqueous Levulinic Acid Hydrogenation

Herein, we report a stable catalyst with Ru single atoms anchored on a one-dimensional carbon fiber@graphitic carbon nitride hierarchy, by assembling wet wipes composed of fiber-derived carbon fiber (CF), melamine-derived graphitic carbon nitride (g-C3N4) and RuCl3 before NaBH4 reduction. The atomically dispersed Ru species (3.0 wt%) are tightly attached via N-coordination provided by exterior g-C3N4 nanosheets, and further stabilized by the interior mesoporous CF. The obtained CF@g-C3N4–Ru SAs catalyst can be cycled six times without notable leaching of Ru or loss of GVL yield in the acidic media. This catalyst is more stable than Ru nanoparticles supported on CF@g-C3N4, as well as Ru single atoms anchored on CF and g-C3N4, and proves to be one of the most efficient metal catalysts for aqueous LA hydrogenation to γ-valerolactone (GVL). The isolated Ru atoms by strong N-coordination, and their enhanced electron/mass transfer afforded by the one-dimensional hierarchy, can be responsible for the excellent durability of CF@g-C3N4–Ru SAs under harsh reaction conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1972

Origin of organic matter in early solar system. VI - Catalytic synthesis of nitriles, nitrogen bases and porphyrin-like pigments.

A variety of nitrogen compounds have been synthesized by a static Fischer-Tropsch type reaction from CO, D2 and ND3, with Ni-Fe and Al2O3 catalysts. In this reaction, the gas is heated to 500-700 C for about 0.5 hr, and then cycled through lower temperatures (100-400 C) for 1-14 days. Products were analyzed by mass spectrometry in conjunction with gas chromatography and other chromatographic techniques. Compounds produced include alkyl cyanides, pyrroles, porphyrin-like compounds, guanidines, hydantoin, uracil and its derivatives, thymine, adenine, guanine, xanthine, melamine, as well as alkanes, alkenes and aromatic hydrocarbons. Such reactions may have been involved in the production of interstellar molecules, organic compounds in meteorites, and prebiotic organic matter on planets.

Hayatsu, R.↗

NASA NTRS1972

The development of an inert simulant for HNS/teflon explosive

The report describes the development and evaluation of an inert simulant for the thermally stable, heat-resistant plastic-bonded explosive HNS/Teflon. The simulant is made by dry blending vinylidene fluoride, melamine and Teflon which when compared has a pressed density and thermal properties corresponding closely to the explosive. In addition, the machinability and handling characteristics of the simulant are similar to the explosive.

Elban, W. L.↗

NASA NTRS1975

Purines and triazines in the Murchison meteorite

Two samples of the Murchinson C2 chondrite were analyzed for organic nitrogen compounds, using mass spectrometry in combination with paper and thin-layer chromatography. Under mild extraction conditions (water or formic acid), only alphatic amines and some alkylpyridines were seen. Drastic extraction conditions (hot 3-6 M HCL) a variety of nitrogen compounds appeared, including adenine (15 ppm), guanine (5ppm), melamine (20 ppm), cyanuric acid (20 to 30 ppm), guanylurea (30 to 45 ppm), and urea (25 ppm). It appears that these compounds are present mainly in macromolecular material. Failure of other investigators to identify these compounds in carboneceous chondrites is attributed to inadequate extraction conditions (water and formic acid rather than HCl).

Hayatsu, R.↗

NASA NTRS1976

Recent advances in the development of composites based on the NCNS resins

The NCNS resins, a new class of addition polymerized polyaromatic melamines, have undergone further development in the past year. Pilot plant quantities of resin NCNS-12M have been made available for evaluation. High solids laminating varnishes were prepared in alcohol/ethyl acetate and alcohol/chlorinated solvent mixtures. The prepregs had sufficient room temperature stability after three month storage to retain good processing characteristics and good bonded mechanical properties. Laminates were fabricated by vacuum bag-autoclave processing and by 5 minute press molding cycles. These laminates had low flame spread and low smoke emitting properties and retained good elevated temperature properties upon long-term oxidative aging. Humidity aging studies were carried out for 30 days at 95% R.H., 120 F. on NCNS/graphite fiber laminates. Initial results indicate that the NCNS resins, particularly those prepared from polymethylene polyphenylamines, are resistant to environmental degradation of elevated temperature mechanical strength.

Kray, R. J.↗

NASA NTRS1978

Characterization of flammability properties of some thermoplastic and thermoset resins

The thermochemical and flammability properties of some thermally stable polymers considered for use in aircraft interiors are described. The properties studied include: (1) thermomechanical properties such as glass transition and melt temperature; (2) dynamic thermogravimetric analysis in anaerobic environment; (3) flammability properties such as oxygen index, flame spread, and smoke evolution; and (4) selected physical properties. The thermoplastic polymers evaluated included polyphenylene sulfide, polyaryl sulfone, 9,9-bis(4-hydroxyphenyl)-fluorene polycarbonate-poly(dimethylsiloxane) and polyether sulfone. The thermoset polymers evaluated included epoxy, bismaleimide, a modified phenolic and polyaromatic melamine resin. These resins were primarily used in the fabrication of glass reinforced prepregs for the construction of experimental panels. Test results and relative rankings of some of the flammability parameters are presented and the relationship of the molecular structure, char yield, and flammability properties of these polymers are discussed.

Kourtides, D. A.↗

NASA NTRS1979

Thermochemical characterization of some thermally stable thermoplastic and thermoset polymers

The thermochemical and flammability properties of some thermally stable polymers considered for use in aircraft interiors are described. The properties studied include: (1) thermomechanical properties such as glass transition and melt temperature; (2) dynamic thermogravimetric analysis in anaerobic environment; (3) flammability properties such as oxygen index, flame spread, and smoke evolution; and (4) selected physical properties. The thermoplastic polymers evaluated include polyphenylene sulfide, polyaryl sulfone, 9,9-bis(4-hydroxyphenyl)-fluorene polycarbonate-poly(dimethylsiloxane) and polyether sulfone. The thermoset polymers evaluated include epoxy, bismaleimide, a modified phenolic, and polyaromatic melamine resin. These resins were primarily used in the fabrication of glass-reinforced prepregs for the construction of experimental panels. Test results and relative rankings of some of the flammability parameters are presented, and the relationship of the molecular structure, char yield, and flammability properties of these polymers are discussed.

Kourtides, D. A.↗

NASA NTRS1981

Development of new addition-type composite resins

The most promising of a number of new addition type polyimides and polyaromatic melamine (NCNS) resins for use in high performance composite materials. Three different cure temperature ranges were of interest: 530-560 K (500-550 F), 475-530 K (400-500 F), and 450 K (350 F). Examined were a wide variety of polyimide precursors terminated with 5 norbornene groups and addition polymerized at 560 K similar to PMR-15 and LARC-160 polyimides. In addition, a number of lower curing cinnamal end capped polyimides and a bismaleimide were investigated but were not found promising. A group of NCNS resins were investigated and some were found to be superior to current epoxy resins in moisture resistance, oxidative aging and flame and smoke properties.

Kray, R. J.↗

NASA NTRS2003

Quantification Of Fire Signatures For Practical Spacecraft Materials

The overall objective of this project is to measure the fire signatures of typical spacecraft materials in 1-g and determine how these signatures may be altered in a microgravity environment. During this project, we will also develop a test technique to obtain representative low-gravity signatures. The specific tasks that will be accomplished to achieve these objectives are to: (1) measure the time history of various fire signatures of typical spacecraft materials in 1-g at varying heating rates, temperatures, convective velocities, and oxygen concentrations, (2) conduct tests in the Zero-Gravity Facility at NASA John H. Glenn Research Center to investigate the manner that a microgravity environment alters the fire signature,(3) compare 0-g and 1-g time histories and determine if 0-g data exhibits the same dependence on the test parameters as experienced in 1-g (4) develop a 1-g test technique by which 0-g fire signatures can be measured. The proposed study seeks to investigate the differences in the identities and relative concentrations of the volatiles produced by pyrolyzing and/or smoldering materials between normal gravity and microgravity environments. Test materials will be representative of typical spacecraft materials and, where possible, will be tested in appropriate geometries. Wire insulation materials of Teflon, polyimide, silicone, and PVC will be evaluated using either cylindrical samples or actual wire insulation. Other materials such as polyurethane, polyimide, melamine, and silicone-based foams will be tested using cylindrical samples, in addition to fabric materials, such as Nomex. Electrical components, such as resistors, capacitors, circuit board will also be tested.

VanderWal, Randy L.↗