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DOE OSTI2024

Making Plasticized Polymer Electrolytes Stable Against Sodium Metal for High‐Energy Solid‐State Sodium Batteries

Solid polymer electrolytes based on plastic crystals are promising for solid-state sodium metal (Na 0 ) batteries, yet their practicality has been hindered by the notorious Na 0 -electrolyte interface instability issue, the underlying cause of which remains poorly understood. Here, in this study, by leveraging a model plasticized polymer electrolyte based on conventional succinonitrile plastic crystals, we uncover its failure origin in Na 0 batteries is associated with the formation of a thick and non-uniform solid electrolyte interphase (SEI) and whiskery Na 0 nucleation/growth. Furthermore, we design a new additive-embedded plasticized polymer electrolyte to manipulate the Na 0 deposition and SEI formulation. For the first time, we demonstrate that introducing fluoroethylene carbonate (FEC) additive into the succinonitrile-plasticized polymer electrolyte can effectively protect Na 0 against interfacial corrosion by facilitating the growth of dome-like Na 0 with thin, amorphous, and fluorine-rich SEIs, thus enabling significantly improved performances of Na//Na symmetric cells (1,800 h at 0.5 mA cm −2 ) and Na//Na 3 V 2 (PO 4 ) 3 full cells (93.0 % capacity retention after 1,200 cycles at 1 C rate in coin cells and 93.1 % capacity retention after 250 cycles at C/3 in pouch cells at room temperature). Our work provides valuable insights into the interfacial failure of plasticized polymer electrolytes and offers a promising solution to resolving the interfacial instability issue.

25 ENERGY STORAGE↗

DOE OSTI2025

Hot Hydrogen Exposure of U x Zr 1-x C y Nuclear Fuel: The Effect of Additional Carbon

Nuclear thermal propulsion (NTP) using hydrogen as propellant in a solid-state fission reactor to reach temperatures of up to 3000K can achieve significantly higher specific impulse than chemical propulsion. A promising fuel that is again considered for NTP is U x Zr 1-x C y . To reduce the overall mass loss as well as the uranium fuel loss, a range of experiments using additional carbon in hot hydrogen (2600 K, 6 SLPM flow rate) were performed for up to 5-6 h. Both a CH 4 addition (0.1 and 0.2 vol%) in the hydrogen stream and the use of sacrificial graphite pieces upstream of the samples were tested, with sample compositions from 5 at% UC to 30 at% UC. The results showed a strong reduction of mass loss, up to a factor of 3, as well as a reduction of surface uranium losses in the presence of additional carbon in the atmosphere. Even with additional carbon in the atmosphere, material with 30 at% UC was not stable, but material with 20 at% UC was stable for up to 6h. The sample surfaces showed texturing after processing, possibly by grain growth on the surface. This led to a separation into grains with high uranium content close to the (100)-orientation, and with low uranium content in grains close to the (111)-orientation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2008

Aerosol and Cloud Microphysical Characteristics of Rifts and Gradients in Maritime Stratocumulus Clouds

A cloud rift is characterized as a large-scale, persistent area of broken, low reflectivity stratocumulus clouds usually surrounded by a solid deck of stratocumulus. A rift observed off the coast of Monterey Bay, California on 16 July 1999 was studied to compare the aerosol and cloud microphysical properties in the rift with those of the surrounding solid stratus deck. Variables measured from an instrumented aircraft included temperature, water vapor, and cloud liquid water. These measurements characterized the thermodynamic properties of the solid deck and rift areas. Microphysical measurements made included aerosol, cloud drop and drizzle drop concentrations and cloud condensation nuclei (CCN) concentrations. The microphysical characteristics in a solid stratus deck differ substantially from those of a broken, cellular rift where cloud droplet concentrations are a factor of 2 lower than those in the solid cloud. Further, CCN concentrations were found to be about 3 times greater in the solid cloud area compared with those in the rift and aerosol concentrations showed a similar difference as well. Although drizzle was observed near cloud top in parts of the solid stratus cloud, the largest drizzle rates were associated with the broken clouds within the rift area. In addition to marked differences in particle concentrations, evidence of a mesoscale circulation near the solid cloud rift boundary is presented. This mesoscale circulation provides a mechanism for maintaining a rift, but further study is required to understand the initiation of a rift and the conditions that may cause it to fill.

Sharon, Tarah M.↗

DOE OSTI2025

FY24 Task 5: Leachate Disposition

Directly feeding sludge solids to the high-level waste (HLW) Waste Treatment Plant represents an alternative flowsheet seeking to initiate sludge processing as soon as possible. Key processing functions previously captured during baseline pretreatment operations include leaching and washing prior to solids concentration. These operations should be considered in the potential direct feed flowsheets to maximize waste feed loading, minimize HLW volume, and mitigate corrosion challenges associated with vitrification of high phosphate and fluoride concentrations. Additionally, single-shell tank (SST) retrievals and waste transfers to double-shell tanks (DSTs) in a direct feed flowsheet would likely also benefit from some level of leaching, washing, and solids concentration in order to reduce DST space and mission duration. These operations could occur in a new facility or potentially in available DSTs. If washing and leaching are utilized, an effective disposition pathway for the wash water and leachate solutions are needed. Three target species that benefit significantly from leaching and washing are phosphate, fluoride and aluminum. Phosphate (PO 4 3- ) and fluoride (F - ) can contribute substantially to the amount of carrier fluid needed for dissolution, and the resulting volume of liquid generated. Disposition of this retrieval solution should be evaluated in order to prevent crystallization of these anions throughout system processing. Since there is a high probability that any retrieval solutions will be at or near their PO 4 3- and F - solubility limits, evaporation or blending with a high Na supernate (>3.5 M) is not recommended for the wash water streams without a method to remove precipitants prior to solution disposal. Additionally, aluminum present in the southeast quadrant of the Hanford site represents roughly 60% of the waste solids in the initial processing tanks. These aluminum solids are in the form of gibbsite (Al(OH) 3 ) and can pose significant challenges for processing due to the fast-settling times and high solids loading associated with these materials. Easily remediated by caustic addition to the solids, these wash solutions could be processed through crystalline silicotitanate (CST) ion exchange columns to prepare the supernate solutions for disposition. The current target for feed conditions to the Low Activity Waste (LAW) melter are waste streams that contain nominally 5-6 M Na. Fractions within the tanks contain upwards of 0.2 M phosphate and fluoride in solution at 3.5 M Na. Concentrating these solutions above 5 M Na would result in an exceedance of the solubility limits, and potential for uncontrolled precipitation of the phosphate and fluoride crystal material. The resulting crystalline salt material is typically sodium fluoride phosphate, also referred to as natrophosphate (Na 7 FPO 4 ·19H 2 O). Salt phases are of importance in tank waste due to their chemical reactivity, which can result in precipitation, dissolution, or transformation, impacting any downstream processes (Bolling et al. 2020, Russell, Snow, and Peterson 2010). Salt generation and precipitation could pose challenges by causing system plugging and melter corrosion if left in the supernate stream, or limit sodium molarity of the supernate that would be accepted without incident in waste operations. To understand the impact of this salt generation, the crystallization of natrophosphate in multiple simulant feed matrices was studied to understand the implications of various tank waste supernate chemistries. Three matrices were examined: high PO 4 3- /low F - , low PO 4 3- /high F - , and an average matrix. Subsequent testing was performed with the average matrix with the inclusion of CsNO 3 , and a final run with the average matrix including CsNO 3 and a 137 Cs spike for tracer purposes.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Tunable and Robust Optical and Structural Properties of a Cooperative Squaraine-Dye Aggregate-DNA DX-DAE Tile System

Molecular excitons, which are excitations delocalized over multiple dyes in a wavelike manner, are of interest for a wide range of applications, including quantum information science. Numerous studies have templated a variety of synthetic dyes via a DNA scaffold to induce dye aggregation to create molecular excitons upon photoexcitation. Dye aggregate optical properties are critically dependent on relative dye geometry and local environment; therefore, an understanding of dye-dye and DNA-dye interactions is critical for advancing toward more complex DNA-dye systems. The extensively studied DNA Holliday junction (HJ) and less-studied double-crossover (DX) tile motif are fundamental test beds for designing complex and ultimately modular DNA-dye architectures. Here, we report the first study of single-linked squaraine dye aggregation and exciton delocalization on a larger and more stable (compared with the HJ) DX tile motif. We first highlight a few DNA-dye constructs that support single dyes and aggregates with distinct optical properties that are both tunable—through sample design, buffer conditions, and heat treatment—and robust to environment changes, including transfer to solid phase. Next, we assess several experimental and design considerations that demonstrate directed dye-driven assembly of a novel double-tile DNA configuration. Our results demonstrate that single-linked squaraine dyes templated to DX tiles provide a viable research path to design and evaluate dye aggregate networks that support exciton delocalization. We include herein the first report of exciton delocalization in the solid phase in a DNA-dye construct. Additionally, our findings indicate that dye aggregation impacts the assembly of the DNA-dye construct, and, in some cases, thereby cooperates with the DNA to determine a final robust system configuration. Finally, we show that a controlled annealing schedule can be employed to promote the homogeneous assembly of DNA-dye constructs. The findings in this study contribute to the understanding of DNA-dye systems and the relevant factors involved in their directed assembly to achieve specific constructs with desirable properties.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Development of an advanced spacecraft water and waste materials processing system

An Integrated Waste Management-Water System (WM-WS) which uses radioisotopes for thermal energy is described and results of its trial in a 4-man, 180 day simulated space mission are presented. It collects urine, feces, trash, and wash water in zero gravity, processes the wastes to a common evaporator, distills and catalytically purifies the water, and separates and incinerates the solid residues using little oxygen and no chemical additives or expendable filters. Technical details on all subsystems are given along with performance specifications. Data on recovered water and heat loss obtained in test trials are presented. The closed loop incinerator and other projects underway to increase system efficiency and capacity are discussed.

Murray, R. W.↗

NASA NTRS1980

A contribution to the knowledge of HMX decomposition and application of results

The decomposition of cyclotramethylenetetranitramine (HMX) in the solid and liquid phase was studied by isothermal and nonisothermal heating at atmospheric pressure. Decomposition rates of solid HMX changed with sample size and gaseous environment. Kinetic parameters were obtained from weight loss measurements in the temperature range 229 C - 269 C. These tests also yielded highly porous solid residues. Qualitative aspects of solid and liquid phase decomposition of HMX with additives were also investigated in isothermal and nonisothermal tests.

Kraeutle, K. J.↗

NASA NTRS1982

Polyimides: Tribological properties and their use as lubricants

Friction, wear, and wear mechanisms of several different polyimide films, solid bodies, composites, and bonded solid lubricant films are compared and discussed. In addition, the effect of such parameters as temperatures, type of atmosphere, contact stress, and specimen configuration are investigated. A friction and wear transition occurs in some polyimides at elevated temperatures and this transition is related to molecular relaxations that occur in polyimides. Friction and wear data from an accelerated test (pin-on-disk) are compared to similar data from an end use test device (plain spherical bearing), and to other polymers investigated in a similar geometry.

Fusaro, R. L.↗

NASA NTRS1984

Polyimides - Tribological properties and their use as lubricants

Fusaro, R. L.↗

NASA NTRS1986

Analysis of boron carbides' electronic structure

The electronic properties of boron-rich icosahedral clusters were studied as a means of understanding the electronic structure of the icosahedral borides such as boron carbide. A lower bound was estimated on bipolaron formation energies in B12 and B11C icosahedra, and the associated distortions. While the magnitude of the distortion associated with bipolaron formation is similar in both cases, the calculated formation energies differ greatly, formation being much more favorable on B11C icosahedra. The stable positions of a divalent atom relative to an icosahedral borane was also investigated, with the result that a stable energy minimum was found when the atom is at the center of the borane, internal to the B12 cage. If incorporation of dopant atoms into B12 cages in icosahedral boride solids is feasible, novel materials might result. In addition, the normal modes of a B12H12 cluster, of the C2B10 cage in para-carborane, and of a B12 icosahedron of reduced (D sub 3d) symmetry, such as is found in the icosahedral borides, were calculated. The nature of these vibrational modes will be important in determining, for instance, the character of the electron-lattice coupling in the borides, and in analyzing the lattice contribution to the thermal conductivity.

Howard, Iris A.↗

NASA NTRS1990

Phillips CO-oxidation catalyts for long-lived CO2 lasers: Activity and initial characterization studies

Four different catalysts have been developed specifically for use in sealed carbon dioxide lasers. The catalysts have been designed to be low dusting, stable to shock and vibration, have high activity at low temperatures and have long active lifetimes. Measured global CO oxidation rates range from 1.4 to 2.2 cc CO converted per minute per gram of catalyst at ambient temperature. The catalysts also retain substantial activity at temperatures as low as -35 C. The Phillips laser catalysts are prepared in a variety of different shapes to meet the different pressure drop and gas flow profiles present in the many different styles of lasers. Each catalyst has been tested in sealed TEA lasers and has been shown to substantially increase the sealed life of the laser. Activity measurements made on the precious metal catalysts which were prepared with and without activity promoters showed that the promoter materials increase catalyst CO oxidation activity at least an order of magnitude at ambient temperature. Initial studies using H2 and CO chemisorption, X ray diffraction (XRD) and X ray photoelectron spectroscopy (XPS) have shown that the activity promoters do not significantly affect the precious metal crystallite size or the electronic structure around the precious metal. In addition, the formation or lack of formation of solid solutions between the precious metal and promoters has also been shown not to affect the activity of the promoted catalyst.

Kolts, J. H.↗

NASA NTRS1989

Vector representation of tourmaline compositions

The vector method for representing mineral compositions of amphibole and mica groups is applied to the tourmaline group. Consideration is given to the methods for drawing the relevant vector diagrams, relating the exchange vectors to one another, and contouring the diagrams for constant values of Na, Ca, Li, Fe, Mg, Al, Si, and OH. The method is used to depict a wide range of possible tourmaline end-member compositions and solid solutions, starting from a single point. In addition to vector depictions of multicomponent natural tourmalines, vectors are presented for simpler systems such as (Na,Al)-tourmalines, alkali-free tourmalines, and elbaites.

Burt, Donald M.↗

NASA NTRS1995

Aerodynamic sound of flow past an airfoil

The long term objective of this project is to develop a computational method for predicting the noise of turbulence-airfoil interactions, particularly at the trailing edge. We seek to obtain the energy-containing features of the turbulent boundary layers and the near-wake using Navier-Stokes Simulation (LES or DNS), and then to calculate the far-field acoustic characteristics by means of acoustic analogy theories, using the simulation data as acoustic source functions. Two distinct types of noise can be emitted from airfoil trailing edges. The first, a tonal or narrowband sound caused by vortex shedding, is normally associated with blunt trailing edges, high angles of attack, or laminar flow airfoils. The second source is of broadband nature arising from the aeroacoustic scattering of turbulent eddies by the trailing edge. Due to its importance to airframe noise, rotor and propeller noise, etc., trailing edge noise has been the subject of extensive theoretical (e.g. Crighton & Leppington 1971; Howe 1978) as well as experimental investigations (e.g. Brooks & Hodgson 1981; Blake & Gershfeld 1988). A number of challenges exist concerning acoustic analogy based noise computations. These include the elimination of spurious sound caused by vortices crossing permeable computational boundaries in the wake, the treatment of noncompact source regions, and the accurate description of wave reflection by the solid surface and scattering near the edge. In addition, accurate turbulence statistics in the flow field are required for the evaluation of acoustic source functions. Major efforts to date have been focused on the first two challenges. To this end, a paradigm problem of laminar vortex shedding, generated by a two dimensional, uniform stream past a NACA0012 airfoil, is used to address the relevant numerical issues. Under the low Mach number approximation, the near-field flow quantities are obtained by solving the incompressible Navier-Stokes equations numerically at chord Reynolds number of 104. The far-field noise is computed using Curle's extension to the Lighthill analogy (Curle 1955). An effective method for separating the physical noise source from spurious boundary contributions is developed. This allows an accurate evaluation of the Reynolds stress volume quadrupoles, in addition to the more readily computable surface dipoles due to the unsteady lift and drag. The effect of noncompact source distribution on the far-field sound is assessed using an efficient integration scheme for the Curle integral, with full account of retarded-time variations. The numerical results confirm in quantitative terms that the far-field sound is dominated by the surface pressure dipoles at low Mach number. The techniques developed are applicable to a wide range of flows, including jets and mixing layers, where the Reynolds stress quadrupoles play a prominent or even dominant role in the overall sound generation.

Wang, Meng↗

NASA NTRS2003

Wireless Temperature-Monitoring System

A relatively inexpensive instrumentation system that includes units that are connected to thermocouples and that are parts of a radio-communication network has been developed to enable monitoring of temperatures at multiple locations. Because there is no need to string wires or cables for communication, the system is well suited for monitoring temperatures at remote locations and for applications in which frequent changes of monitored or monitoring locations are needed. The system can also be adapted to monitoring of slowly varying physical quantities, other than temperature, that can be transduced by solid-state electronic sensors. The system comprises any number of transmitting units and a single receiving unit (see figure). Each transmitting unit includes connections for as many as four external thermocouples, a signal-conditioning module, a control module, and a radio-communication module. The signal- conditioning module acts as an interface between the thermocouples and the rest of the transmitting unit and includes a built-in solid ambient-temperature sensor that is in addition to the external thermocouples. The control module is a "system-on-chip" embedded processor that includes analog-to-digital converters, serial and parallel data ports, and an interface for local connection to an analog meter that is used during installation to verify correct operation. The radio-communication module contains a commercial spread-spectrum transceiver that operates in the 900-MHz industrial, scientific, and medical (ISM) frequency band. This transceiver transmits data to the receiving unit at a rate of 19,200 baud. The receiving unit includes a transceiver like that of a transmitting unit, plus a control module that contains a system-on-chip processor that includes serial data port for output to a computer that runs monitoring and/or control software, a parallel data port for output to a printer, and a seven-segment light-emitting-diode display.

Solano, Wanda↗

NASA NTRS2007

Chemochromic Hydrogen Sensors

As fossil fuel supplies decline, hydrogen is quickly becoming an increasingly important fuel source. Currently hydrogen is the prime fuel of today's space vehicles (e.g., Space Shuttle) and featured as a fuel for some prototype vehicles such as the BMW seven series model. Hydrogen is a colorless, odorless gas with a 4% lower explosive limit which makes leak detection a priority. In an effort to support the use of hydrogen, a chemochromic (color changing) sensor was developed that is robust, simple to use, and does not require active operation. It can be made into a thin tape which can be conveniently used for leak detection at flanges, valves, or outlets. Chemochromic sensors can be either reversible or irreversible; however, irreversible chemochromic sensors will be analyzed in this report. The irreversible sensor is useful during hazardous operations when personnel cannot be present. To actively monitor leaks, testing of the irreversible sensor against environmental effects was completed and results indicated this material is suitable for outdoor use in the harsh beachside environment of Kennedy Space Center. The experiments in this report will give additional results to the environmental testing by adding solid rocket booster residue as a variable. The primary motivation for these experiments is to prepare the sensors for the launch pad environment at the Kennedy Space Center. In an effort to simulate the atmosphere at the pads before and after launch, the chemochromic sensors are exposed to solid rocket residue under various conditions.

Wiggins, Bryan C.↗

DOE OSTI2026

Multinuclear Solid-State NMR and NMR Crystallography of Solid Forms of Creatine and Creatinine

Creatine is a performance-enhancing supplement with two widely available commercial solid forms, namely, creatine monohydrate (creatine·H 2 O) and creatine HCl, the latter of which does not have a reported crystal structure. Moreover, commercial formulations of creatine may contain creatinine, an undesired impurity phase resulting from the self-cyclization of creatine during manufacturing. Therefore, reliable methods for characterizing the different solid forms of creatine and detecting the presence of creatinine are essential. Herein, we address these challenges using 13 C, 15 N, and 35 Cl solid-state NMR (SSNMR) spectroscopy to obtain distinct spectral fingerprints for creatine·H 2 O and creatine HCl, along with creatinine and creatinine HCl. The acquisition of these SSNMR spectra offers a robust approach for both the rapid characterization of each solid form and the detection of the impurity phases. Additionally, quadrupolar NMR crystallography-guided crystal structure prediction (QNMRX-CSP) was applied for the de novo crystal structure determination of creatine HCl, which was validated by the subsequently determined single-crystal X-ray diffraction (SCXRD) structure. Finally, to investigate the relationship between NMR parameters and structural features, 13 C and 15 N chemical shifts and 35 Cl electric field gradient (EFG) tensors were computed from geometry-optimized structures of the four solid forms by using dispersion-corrected DFT-D2* methods. Finally, this integrative approach offers a powerful framework for advancing the structural understanding and quality control of creatine-based supplements and next-generation formulations, as well as a wide range of other solid pharmaceuticals and nutraceuticals.

NMR↗

DOE OSTI2026

Electrode Modification by Laser Ablation to Overcome Mechanical and Scalability Limitations of Solid-State Prealkylation of Electrode Architectures

In this work, laser ablation of Si electrode surfaces is utilized to provide localized strain relief during the Solid State Prealkylation of Electrode Architectures (SPEAR) process, in addition to volumetric expansion relief in the form of free volume channels across the electrode. A hexagonal mesh patterning was employed via laser ablation, where the hexagonal diameter (pitch) was varied from 250 to 1000 µm. It was demonstrated that these channels serve as expansion voids, accommodating the increase in electrode thickness observed during SPEAR and preventing cracking at the electrode surface. Optical microscopy and Raman mapping confirm that Li diffusion is the rate-limiting solid-state process, requiring a 24 h rest period to achieve homogeneous LixSi alloying through the electrode bulk. Electrochemical evaluations in full cells show that a 1000 μm pitch pattern yields a high initial discharge capacity of 2485 mA h g–1 and 86.4% capacity retention after 80 cycles, whereas smaller pitches (<500 μm) result in lithium plating at 4.1 V in full cells paired with NMC 811 due to excessive current collector exposure from the ablation process. XPS analysis reveals that the laser treatment modifies the electrode surface by increasing the Si–O and C–O species, changing the SEI composition observed via an increase in fluorophosphates upon cycling.

Musgrove, Amanda [ORNL] (ORCID:0009000220910389)↗

NASA NTRS1972

Multimaterial lamination as a means of retarding penetration and spallation failures in plates

Experimental data are presented which show that hypervelocity impact spallation and penetration failures of a single solid aluminum plate and of a solid aluminum plate spaced a distance behind a Whipple meteor bumper may be retarded by replacing the solid aluminum plate with a laminated plate. Four sets of experiments were conducted. The first set of experiments was conducted with projectile mass and velocity held constant and with polycarbonate cylinders impacted into single plates of different construction. The second set of experiments was done with single plates of various construction and aluminum spherical projectiles of similar mass but different velocities. These two experiments showed that a laminated plate of aluminum and polycarbonate or aluminum and methyl methacrylate could prevent spallation and penetration failures with a lower areal density than either an all-aluminum laminated plate or a solid aluminum plate. The aluminum laminated plate was in turn superior to the solid aluminum plate in resisting spallation and penetration failures. In addition, through an example of 6061-T6 aluminum and methyl methacrylate, it is shown that a laminated structure ballistically superior to its parent materials may be built. The last two sets of experiments were conducted using bumper-protected main walls of solid aluminum and of laminated aluminum and polycarbonate. Again, under hypervelocity impact conditions, the laminated main walls were superior to the solid aluminum main walls in retarding spallation and penetration failures.

Dibattista, J. D.↗