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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Permeability of Single–Layer–Free–Standing Meshes at Varying Capillary Pressure via a Novel Method

The permeability of mesh wicks is important for various applications, including two–phase heat transfer. However, the understanding of the permeability of single–layer, free–standing mesh wicks, with liquid–gas interfaces on both sides, is limited. A novel and simpler method is presented to determine the permeability of a free–standing wick and apply it to a representative mesh. This method involves modifying the capillary pressure via elevation and simultaneously measuring the permeability to determine the permeability–capillary pressure relationship. When applied to a copper mesh with plain weave having undergone surface cleaning, the permeability is found to decrease as capillary pressure for deionized water increases. A dimensional analysis is presented to generalize this data for other mesh sizes with similar weaves and fluids. The behavior of mesh in application is modeled, based on the integration of Darcy's law with an analytic function fit to measured data, and parametric studies are conducted to investigate the superficial velocity of liquids through the mesh under varying driving pressures, transport lengths, and liquid viscosity, based on the obtained capillary pressure–permeability relationship. This study provides valuable insights into the transport properties of mesh wicks, with potential applications in fields such as electronics cooling, electrochemical devices, and fluid purification technologies.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Direct Recycling of Blended Cathode Materials by Froth Flotation

We report that direct Li-ion battery recycling involves separating cathode active materials in the solid phase while preserving their electrochemical performance. To reuse the recycled ones in new batteries, it is necessary to separate individual cathode components, which would typically occur prior to the rejuvenation and any compositional reformulation processes. Herein, a froth flotation process is developed to separate pristine lithium nickel-manganese-cobalt oxide (LiNi 0.333 Mn 0.333 Co 0.333 O 2 , NMC111) and lithium manganese oxide (LMO) materials. The flotation results show that with multiple stages of the separation processes, a satisfactory separation is achieved with 95% grade or above of NMC111 in the froth product and 95% grade of LMO in the tailing product. The electrochemistry results show that the flotation chemicals have negligible impact on the electrochemical performance of recycled active materials, whereas the NMC111 exhibits a minor capacity fade after being in contact with deionized water at 2% solid concentration. An improvement in both the rate and cycling performance is achieved at 10% solid concentration or higher. It is found that there is little compositional and structural change to the aqueous recycled NMC111 powders. An effective and low-cost separation method for direct recycling mixed cathode compositions is demonstrated.

25 ENERGY STORAGE↗
DOE OSTI2024

Geochemical assessment of mineral sequestration of carbon dioxide in the midcontinent rift

Abstract This study examines the potential of Midcontinent Rift rocks to facilitate long‐term CO 2 sequestration by providing the necessary Ca and Mg for carbonate mineralization. Surface samples were collected from the Oronto and Bayfield‐Jacobsville Groups around Lake Superior and used for petrography and X‐ray diffraction to determine their mineral composition. Also, X‐ray fluorescence was also used to assess their bulk chemical composition. The samples were then exposed to CO 2 and deionized water in Teflon‐lined vessels at 90°C, and the resulting leachate fluids were analyzed for the cation released during the testing. SEM microscopy was used to examine the samples for potential mineralization of carbonate minerals. The Oronto Group sediments consist primarily of feldspathic to feldspathic lithic arenites with a chlorite‐dominated matrix, and the primary porosity is blocked by calcite and hematite cement. The Bayfield–Jacobsville sequences are porous quartz arenites to feldspathic quartz arenites that do not contain significant accumulation of Ca‐, Mg‐, and Fe‐bearing minerals. The leachate fluids obtained from Oronto Group samples exhibit a maximum Ca release rate (5.2 × 10 −4 mole/cm 2 .day), indicating rapid calcite cement dissolution and increased porosity and permeability. SEM/EDS microanalysis revealed areas where pore‐filling calcite was preferentially dissolved. Longer‐term rock‐water reactions resulted in induced carbonate mineralization, as evidenced by calcite crystals observed in a sample reacted for 102 days. © 2024 Society of Chemical Industry and John Wiley & Sons, Ltd.

Energy & Fuels↗
DOE OSTI2024

The Critical Influence of Spin–Dry Technique on the Surface Passivation Quality of Crystalline Silicon Solar Cell Structures

This study examines the effects of spin-dry (SD) and N 2 blow-dry (ND) techniques on the quality and surface passivation performance of silicon oxide grown in ozone-dissolved deionized water. The SD method achieves greater oxide thickness uniformity, averaging 1.39 nm ± 4.17% across 49 points, compared to 1.68 nm ± 21.67% for the ND wafers. However, persistently poor passivation of ozonated oxide-grown wafers following the SD process is exhibited, with carrier lifetime, τ eff < 0.3 ms and saturation current density, J 0 (per side) ranging from 26 to 45 fA cm 2 . These findings are analyzed in the context of the fundamental phenomena involved in the drying processes of both techniques. Following this, an optimized spin-drying process is developed, resulting in improved τ eff and J 0 values of 1.4 ms and 5.6 fA cm –2 , respectively. Scanning electron microscopy further confirms that the oxide films dried with the enhanced SD technique are free of pinholes.

14 SOLAR ENERGY↗
DOE OSTI2022

Effect of PVD-coated chromium on the subcooled flow boiling performance of nuclear reactor cladding materials

Here we elucidate the separate effect of a thin Cr coating deposited by physical vapor deposition (PVD) on the subcooled flow boiling performance of zircaloy-4. First, we run flow boiling experiments on prototypical zircaloy-4 surfaces mimicking the scratch pattern and surface roughness of nuclear reactor claddings. Then, we PVD-coat a 0.3 µm thick chromium layer on the same exact surface and repeat the same flow boiling investigations. All experiments are run using deionized water at atmospheric pressure, flowing on a 1 × 3 cm 2 rectangular cross section channel at a rate of 1000 kg/m 2 /s and a subcooling of 10 K. We measure the average temperature of the boiling surface at increasing surface heat fluxes, covering a wide range of heat transfer regimes, from single-phase forced convection to the boiling crisis. We also record high-speed videos of the boiling process, which we postprocess to measure bubble nucleation site density, growth time, departure diameter and frequency. The surface analysis reveals that, while the chromium coating does not seem change the surface roughness and morphology, it improves surface wettability. However, it decreases the critical heat flux. The chromium coating causes an increase of nucleation temperature, bubble departure diameter and growth time, and a reduction of the nucleation site density. The concurrence of these observations indicates that a size reduction of the nucleation sites, conformally covered by the chromium coating, may be the cause of the boiling performance deterioration. We confirm this hypothesis repeating the same analysis on a FeCrAl sample prepared and tested using the same protocol as the zircaloy-4 sample, but with a different initial surface texture.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2022

Origins of wear-induced tungsten corrosion defects in semiconductor manufacturing during tungsten chemical mechanical polishing

During chemical mechanical polishing (CMP) process optimization, a unique corrosion defect was identified in the tungsten (W) contact plugs, which were investigated to develop practical solutions to improve CMP mass productivity. The corrosion defect occurred in the absence of external incident energy and was observed to occur only at the W plugs connected to the P + /n-well close to the wafer edge. To examine the root cause of the corrosion, a series of experiments was carried out at each W CMP step, using in-line defect inspection. Additional experiments were conducted using on-line inductively coupled plasma mass spectrometry (ICP-MS) to understand pH- and potential-dependent electrochemical dissolution behaviors of W. Experimentally, W corrosion was confirmed to be exacerbated if the surface oxide of the W plugs is removed by the deionized water (DIW) rinsing step under wafer pressurization, then exposed to DIW and alkaline cleaning solution. Although the DIW rinsing step is commonly performed to clean polishing pads right after the main polishing, a small amount of applied pressure (0.5 psi) without slurry supply can lead to corrosion defects. Finally, this wear-induced corrosion of the W plugs can be prevented by removing the applied pressure during the post DIW rinsing step of W CMP.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Mechanical Characterization of Low Modulus Polymer-Modified Calcium-Silicate-Hydrate (C-S-H) Binder

Calcium-silicate-hydrate (C-S-H) represents a key microstructural phase that governs the mechanical properties of concrete at a large scale. Defects in the C-S-H phase are also responsible for the poor ductility and low tensile strength of concrete. Manipulating the microstructure of C-S-H can lead to new cementitious materials with improved structural performance. This paper presents an experimental investigation aiming to characterize a new synthetic polymer-modified synthetic calcium-silicate-hydrate (C-S-H)/styrene-butadiene rubber (SBR) binder. The new C-S-H/SBR binder is produced by calcining calcium carbonate and mixing this with fumed silica (SiO 2 ), deionized water and SBR. Mechanical, physical, chemical and microstructural characterization was conducted to measure the properties of new hardened C-S-H binder. Results from the experimental investigation demonstrate the ability to engineer a new C-S-H binder with low elastic modulus and improved toughness and bond strength by controlling the SBR content and method of C-S-H synthesis. The new binder suggests the possible development of a new family of low-modulus silica-polymer binders that might fit many engineering applications such as cementing oil and gas wells.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Dual-Functional Thermocapacitive Heat Pump with Electrochemical Supercapacitors for Building Thermal Management and Energy Storage

Efficient heating and cooling technologies can help reduce the energy consumption and carbon emissions of buildings. This work explores the use of supercapacitive cells in a multifunctional, liquid-regenerated thermocapacitive heat pump that can provide electrical energy storage in addition to heating and cooling. A proof-of-concept prototype based on eight commercial supercapacitors and using deionized water as a liquid regenerator demonstrated cooling and energy storage capabilities. A peak cooling coefficient of performance (COPc) of 0.27 was achieved at a temperature drop of 0.24 K. The highest measured electrical energy storage density of the cells was 5.93 J cm-3, and the highest cooling power delivered relative to the volume of the cells was 0.58 mW cm-3. This work demonstrates the use of electrochemical energy storage devices in multifunctional equipment for thermal management in buildings.

25 ENERGY STORAGE↗
DOE OSTI2021

On the influence of test speed and environment in the fatigue life of small diameter nitinol and stainless steel wire

Here, to better understand the complex interplay of speed and environment on metals commonly used in implants, rotary bend fatigue tests were conducted on stainless steel and nitinol wires. A range of alternating strains was tested to create ε-N curves at two speeds (physiologic and accelerated) and in three environments (deionized water at body temperature, phosphate buffered saline at body temperature, and laboratory air at ambient room temperature). Results indicate that speed and environment can affect the observed fatigue life in nuanced ways. An electropotential monitoring technique was demonstrated to characterize fatigue crack growth which may be useful in future investigations.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Immobilization of cesium and iodine into Cs 3 Bi 2 I 9 perovskite-silica composites and core-shell waste forms with high waste loadings and chemical durability

Cs$_3$Bi$_2$I$_9$, a defect perovskite derivative, is a potential host phase to immobilize iodine and cesium with high waste loadings. In this work, two strategies were explored to form Cs$_3$Bi$_2$I$_9$-silica composites and a core-shell structure in order to improve chemical durability of waste form materials meanwhile maintaining high waste loadings. Cs$_3$Bi$_2$I$_9$ loadings as high as 70 wt.% were incorporated into a silica matrix to form silica-ceramic composites, and 20 wt.% Cs$_3$Bi$_2$I$_9$ was encapsulated into silica to form a core–shell structure by low temperature spark plasma sintering. Chemical durability of the composite and core-shell waste forms was evaluated by semi-dynamic leaching experiments, and Cs and I were incongruently released from waste form matrices. A BiOI alteration layer formed, acting as a passivation layer to reduce the release of radionuclides. The long-term iodine release rate was low (30 mg m$^{-2}$ day$^{-1}$) for the 70 wt.%Cs$_3$Bi$_2$I$_9$–silica composite leached in deionized water at 90 °C, which can be further reduced to 5 × 10$^{-3}$ mg m$^{-2}$ day$^{-1}$ for the 20 wt.% core-shell structure. This work highlights a robust way to immobilize the highly mobile radionuclides with high waste loadings through encapsulation into durable matrices and a surface passivating mechanism that can greatly reduce the elemental transport from waste form materials and significantly enhance their chemical durability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Design of non-fluorinated proton exchange membranes from Poly(Terphenyl fluorenyl isatin) with fluorene-linked sulfonate groups and microblock structures

Proton exchange membranes (PEMs) are essential components in energy storage and conversion devices, such as fuel cells and electrolyzers. Here, in this study, we developed a series of non-fluorinated PEMs from poly(terphenyl fluorenyl isatin) with fluorene-pendent disulfonate groups. These polymers feature a microblock structure composed of hydrophobic blocks, hydrophilic blocks, and alternating blocks, arising from the differences in reactivity, concentration, and solubility between the hydrophobic p-terphenyl and hydrophilic disulfonated fluorene monomers. As a result, the sulfonic acid groups are unevenly distributed along the polymer chains, forming densely charged regions (IEC = 3.52 meq/g) with large ion clusters and lightly charged regions (IEC = 2.16 meq/g) with small ion clusters. This microstructure, combined with the degree of sulfonation, significantly influences the overall properties of the membranes, including robust mechanical strength (47.1–63.2 MPa), high thermal stability (up to 270 °C), low swelling ratio (18–25% at 80 °C), and high proton conductivity (136–169 mS/cm in deionized water at 80 °C). The PFLSH60 membrane demonstrated comparable fuel cell performance to Nafion 212. Its hydrogen crossover current density was more than two times lower (0.86 mA/cm 2 for PFLSH60 compared to 1.83 mA/cm 2 for Nafion 212) under testing conditions of 80 °C and 100% RH. This significantly reduced crossover improves fuel utilization in fuel cell stacks. This work offers valuable insights into the design of robust, high-performance PEMs by systematically analyzing the relationships between membrane structure, properties, and performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Spectroscopic features of dissolved iodine in pristine and gamma-irradiated nitric acid solutions

While iodine speciation is important for a wide range of nuclear activities, understanding the mechanisms of the transformations of iodine between chemical forms and the sensitivity of these transitions to solution conditions and exposure to radiation remains an active area of research. This work curates spectroscopic data from several experimental techniques and establishes their sensitivity and limitations in detecting changes in iodine speciation in both neutral and acidic regimes. The techniques include Raman spectroscopy, Fourier Transform Infrared (FTIR) spectroscopy, 127 I NMR spectroscopy, and ultraviolet-visible (UV-Vis) spectroscopy. Analysis of these data indicates that these commonly accessible spectroscopies often have dynamic ranges of measurable concentrations that do not always overlap between all techniques. The experimental techniques are disparately sensitive to iodide (I - ), molecular iodine (I 2 ), iodate (IO 3 - ), and periodate (IO 4 - ) species. Raman, FTIR, and NMR spectra were subsequentially analyzed using two-dimensional correlation analyses to generate high-resolution autocorrelation spectra. Here, the use of these spectroscopies is then extended to tracking acidification-induced and gamma irradiation-induced transformations of dissolved sodium iodate in deionized water and concentrated nitric acid. Both dissolution into nitric acid and irradiation with a gamma source are demonstrated to perturb the iodine speciation promoting their assembly into molecular iodine (I 2 ) and/or triiodide (I 3 - ). While I 2 and I 3 - species are undetectable with FTIR spectroscopy and 127 I NMR spectroscopy, the species can be detected with UV-Vis spectroscopy, and in some instances, I 3 - can be detected with Raman spectroscopy in the low wavenumber region. Ultimately, the results of this work provide a path to designing optimal combinations of techniques to detect forms of iodine across a wide range of concentrations and conditions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2022

Zinc speciation and desorption kinetics in a mining waste impacted tropical soil amended with phosphate

Mining is an important component of the Brazilian economy. However, it may also contribute to environmental problems such as the pollution of soils with zinc and other potentially toxic metals. Our objective was to evaluate changes in the chemical speciation and mobility of Zn in a soil amended with phosphate. Soil samples were collected from a deactivated mining area in the state of Minas Gerais, Brazil, and amended with NH 4 H 2 PO 4 saturated with deionized water to 70 % of maximum water retention and incubated at 25 ± 2 °C in open containers for 60 days. The soil was chemically and mineralogically characterized, and sequential extraction, desorption kinetics, and speciation were carried out using synchrotron bulk-sample and micro–X-ray Absorption Near-Edge Structure (XANES/μ-XANES) spectroscopy at the Zn K-edge, and X-ray fluorescence microprobe analysis (μ-XRF). The combination of μ-XRF and μ-XANES techniques made it possible to identify Zn hotspots in the main species formed after phosphate remediation. The best fit combination for bulk XANES and μ-XANES was observed in Zn-montmorillonite, Zn-kerolite, Zn-ferrihydrite, and gahnite. In the course of phosphate treatment, gahnite, Zn layered double hydroxides (Zn-LDH), Zn3(PO4), and ZnO were identified by bulk XANES, while Zn-ferrihydrite, Zn-montmorillonite, and scholzite were identified by μ-XANES. Zinc in the phosphate-amended soil had the strongest partial correlations (r' > 0.05) with Ni, Co, Fe, Cr, Mn, Si, P, Cd, Pb, and Cd, while the unamended soil showed the strongest correlation with Cu, Pb, Fe, and Si. The application of NH 4 H 2 PO 4 altered Zn speciation and favored an increase in Zn desorption. Here, the most available Zn contents after phosphate amendment were correlated with the release of exchangeable Zn fractions, associated with carbonate and organic matter.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Inhibition of Reaction Layer Formation on MgO(100) by Doping with Trace Amounts of Iron

Despite extensive research on MgO’s reactivity in the presence of CO 2 under various conditions, little is known about whether impurities incorporated into the solid, such as iron, enhance or impede hydroxylation and carbonation reactions. The purity of the MgO required for the successful implementation of MgO looping as a direct air capture technology affects the deployment costs. With this motivation, we tested how incorporated iron impacts MgO (100) reactivity and passivation layer formation under ambient conditions by using atomic force microscopy, electron microscopy, and synchrotron-based X-ray scattering. Based on electron microprobe analysis, our MgO samples were 0.5 wt % iron, and Mössbauer spectroscopy results indicated that 70% of the iron is present as Fe(II). We find that even these low levels of iron dopants impeded both the hydroxylation at various relative humidities (10%, 33%, 75%, and >95%) and carbonation in CO 2 (33%, 75%, and >95%) on the (100) surface. Crystalline reaction products were formed. Reaction layers on the sample were easily removed by exposing the sample to deionized water for 2 min. Overall, our findings demonstrate that the presence of iron dopants slows the reaction rate of MgO, indicating that MgO without incorporated iron is preferable for mineral looping applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

An Interfacial Engineering Approach toward Operation of a Porous Solid Electrolyte CO 2 Electrolyzer

Waste CO 2 can be repurposed as a carbon feedstock for synthesizing valuable chemicals via CO 2 electrolysis. Porous solid electrolyte (PSE) CO 2 electrolysis has been demonstrated as an economically viable method to produce high purity products. This work applies an interfacial engineering approach to determine key factors to improve performance in PSE CO 2 electrolyzers. We standardize the assembly by binding the ionic resin into an ionomer wafer and utilize Computational Fluid Dynamics (CFD) to design gaskets for uniform fluid flow. Here, we employ the distribution of relaxation times (DRT) method to determine that anionic-conducting interfaces are the primary contributor to energy losses. To address this, we demonstrate that enhancing the contact between the cathode and the anion exchange membrane (AEM) and the AEM-ionic resin interface allows for low overpotential in deionized water operation.

09 BIOMASS FUELS↗
DOE OSTI2025

Two-Dimensional Tantalum Carbo-Selenide for Hydrogen Evolution

Herein, we report the synthesis of two-dimensional Ta 2 Se 2 C (2D-Ta 2 Se 2 C) nanosheets using electrochemical lithiation in multilayer Ta 2 Se 2 C followed by sonication in deionized water. Multilayer Ta 2 Se 2 C was obtained via solid-state synthesis of Fe x Ta 2 Se 2 C followed by chemical etching of Fe. 2D-Ta 2 Se 2 C exhibited promising electrocatalytic activity for the hydrogen evolution reaction from water compared to multilayer Ta 2 Se 2 C and 2D-TaSe 2 . 2D-Ta 2 Se 2 C showed an overpotential at 10 mA·cm -2 (η 10 ) of 264 mV, a Tafel slope of 91 mV·dec -1 , and an electrochemically active surface area of 17.61 m ECSA 2 ·g catalyst -1 . The high performance could be attributed to the large surface area of single sheets which hence maximizes the number of exposed catalytic sites and increased density of vacancies, observed with transmission electron microscopy, during synthesis and processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗