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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 397 records · Page 22
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

How do super concentrated electrolytes push the Li-ion batteries and supercapacitors beyond their thermodynamic and electrochemical limits?

Increasing the energy density of energy storage devices is currently the key target of many battery and supercapacitor research activities. For both types of devices, the electrochemical stability window (ESW) determines the effective energy density of the device. ESWs are defined by the effective oxidation and reduction potentials of the electrolyte, which are controlled by many various factors, including the HOMO/LUMO (highest/lowest unoccupied molecular orbital) energies of the electrolyte molecules, the nature of the electrode/electrolyte interphases, and other physicochemical properties. The concentration of the electrolyte would affect the HOMO/ LUMO levels thus also change the ESW. A higher concentration of salt induces specific arrangements among the anion, cation, and solvent molecules of an electrolyte, altering the bulk behavior of the electrolyte, resulting in drastic change in the electrode interfaces. These uniquely modified physicochemical properties extend the ESW in several different ways, including the enhancement in the kinetic stability of the electrodes, as well as the thermodynamic and Nernst shifts of the oxidation/reduction potentials of the electrolyte. For organic electrolytes, it is the reduced amount of free solvent molecules that plays the key role in such changes; whereas for aqueous electrolytes, it is the scarcity of free water molecules and the reduced water activity that control the key properties of the electrolyte. Here, we focus on elucidating the fundamental structural changes occurring within an electrolyte system with increasing salt concentrations. The underlying mechanisms which not only facilitates the extension of the ESW, but also enables higher rate capabilities and mitigates aluminum dissolution for batteries with organic electrolytes, are meticulously explained. Further, we thoroughly discuss the importance of high-voltage stability in aqueous battery systems by exploiting the changed properties observed with higher concentrations of salts. To finish, high-voltage supercapacitors enabled by superconcentrated electrolytes are also explored.

25 ENERGY STORAGE↗
DOE OSTI2019

Corrosion of carbon steel and the passivating properties of corrosion films formed under high-PT geothermal conditions

Corrosion is a major obstacle to a safe implementation of geotechnical applications. Here, using a novel approach that includes vertical scanning interferometry (VSI) and electrochemical impedance spectroscopy (EIS) we discuss time-dependent carbon steel corrosion and film formation at geothermally relevant temperatures (80-160 °C) in CO 2 -saturated mildly acidic Na—Cl brine. Iron dissolution kinetics follows a logarithmic rate at 80 and 160 °C and a linear rate at 120 °C. At 80 °C, high initial corrosion rates (first 24 h) generate H 2 at a minimum rate of 12 μmol h -1 cm -2 and lead to the formation of a continuous ~100 μm thick porous corrosion film. It exhibits a duplex structure with a crystalline outer FeCO 3 layer and an inner layer composed of a skeletal network of Fe 3 C impregnated with FeCO 3 . Being an electrical conductor we hypothesize the Fe 3 C to strongly enhance corrosion rates by providing additional cathodic sites. Pseudo-passivity due to an anodic film-forming reaction (presumably Fe-oxide) was observed at 120 and 160 °C, soon followed by the initiation of pitting at 120 °C. Steady-state corrosion rates at 160 °C are at least one order of magnitude lower than for 120 °C. Lastly, our experimental approach demonstrated potential for general applicability in studying corrosion-related phenomena.

36 MATERIALS SCIENCE↗
DOE OSTI2014

An Alternative Mechanism for Accelerated Carbon Sequestration in Concrete

The increased rate of carbon dioxide sequestration (carbonation) is desired in many primary and secondary life applications of concrete in order to make the life cycle of concrete structures more carbon neutral. Most carbonation rate studies have focused on concrete exposed to air under various conditions. An alternative mechanism for accelerated carbon sequestration in concrete was investigated in this research based on the pH change of waters in contact with pervious concrete which have been submerged in carbonate laden waters. The results indicate that the concrete exposed to high levels of carbonate species in water may carbonate faster than when exposed to ambient air, and that the rate is higher with higher concentrations. Validation of increased carbon dioxide sequestration was also performed via thermogravimetric analysis (TGA). It is theorized that the proposed alternative mechanism reduces a limiting rate effect of carbon dioxide dissolution in water in the micro pores of the concrete.

Carbonation↗
DOE OSTI2019

Temperature-Dependent Solubility of Solid Electrolyte Interphase on Silicon Electrodes

The lithium-ion batteries powering mass market electric vehicles must be capable of operating in a wide temperature range. Temperature variation has the possibility to greatly affect the stability of the solid electrolyte interphase (SEI) responsible for mitigating capacity fade due to electrolyte decomposition in the lithium-ion battery. Here, we explore the solubility of the SEI on the silicon (Si) electrode, an alternative anode material to the conventional graphite electrode, at temperatures ranging from -10 to 50 °C. Through use of an electrochemical protocol with a high cathodic cutoff voltage, we measure the evolution of the SEI independently of competing Si mechanical stress. We correlate the electrochemical data with three-dimensional resistivity versus depth profiling as well as atomic force microscopy to show that SEI dissolution occurs at significantly faster rates at higher temperatures.

25 ENERGY STORAGE↗
DOE OSTI2016

Chlorite, Biotite, Illite, Muscovite, and Feldspar Dissolution Kinetics at Variable pH and Temperatures up to 280 C

Summary Sheet silicates and clays are ubiquitous in geothermal environments. Their dissolution is of interest because this process contributes to scaling reactions along fluid pathways and alteration of fracture surfaces, which could affect reservoir permeability. In order to better predict the geochemical impacts on long-term performance of engineered geothermal systems, we have measured chlorite, biotite, illite, and muscovite dissolution and developed generalized kinetic rate laws that are applicable over an expanded range of solution pH and temperature for each mineral. This report summarizes the rate equations for layered silicates where data were lacking for geothermal systems.

15 GEOTHERMAL ENERGY↗
DOE OSTI2015

Empirical kinetics and their role in elucidating the utility of transition-state theory to mineral–water reactions. A comment upon, ''Evidence and Potential Implications of Exponential Tails to Concentration Versus Time Plots for the Batch Dissolution of Calcite'' by V. W. Truesdale

Transition-state theory (TST) is a successful theory for understanding many different types of reactions, but its application to mineral-water systems has not been successful, especially as the system approaches saturation with respect to a rate-limiting phase. A number of investigators have proposed alternate frameworks for using the kinetic rate data to construct models of dissolution, including Truesdale (Aquat Geochem, 2015; this issue). This alternate approach has been resisted, in spite of self-evident discrepancies between TST expectations and the data. The failure of TST under certain circumstances is a result of the presence of metastable intermediaries or reaction layers that form on the surface of reacting solids, and these phenomena are not anticipated by the current theory. Furthermore, alternate approaches, such as the shrinking object model advocated by Truesdale, represent a potentially important avenue for advancing the science of dissolution kinetics.

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

Real-Time Atomic-Scale Structural Analysis Resolves the Amorphous to Crystalline CaCO 3 Mechanism Controversy

Amorphous calcium carbonate (ACC) occurs as a precursor to geological and biogenic calcium carbonate (CaCO 3 ), yet its transformation pathways and reaction mechanisms remain inconsistent and controversial. In this study, we investigated the transformation of ACC to calcite under both solution and dry conditions, in the presence and absence of impurity ions, utilizing operando time-resolved synchrotron X-ray diffraction (TRXRD) and reactive transport modeling. Results demonstrate that TRXRD techniques allow us to differentiate dissolution-reprecipitation versus solid-state transformation mechanisms for amorphous to crystalline phase transitions. Specifically, we observe that in environments with abundant water, ACC transforms to calcite through a dissolution-reprecipitation mechanism. This features an activation energy of 63 ± 2 kJ/mol and unit cell volume contraction during calcite crystal growth. Conversely, under water-limited conditions, ACC to calcite transformation proceeds via a solid-state transformation mechanism, with an activation energy of 210 ± 2 kJ/mol, three times greater than the dissolution-reprecipitation route, and a unit cell expansion during crystalline calcite growth. Further, to illustrate the magnitude of these effects, the rates of calcite growth were similar during dissolution-reprecipitation at 3 °C [0.00207(35) s –1 ] and solid-state transformation at 280 °C [0.00134(11) s –1 ]. Moreover, the incorporation of an impurity, strontium, significantly retards the rate of calcite growth while expanding its unit cell but whose incorporation is history dependent. Reactive transport modeling of the dissolution–precipitation kinetics suggests that ACC must be dissolving as compact aggregates. These various transformation mechanisms drive diverse geological and biological carbonate formations, impacting their use as paleoenvironmental markers and functional materials synthesis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Phase instabilities in austenitic steels during particle bombardment at high and low dose rates

Disruption of phase stability by energetic particle bombardment is a major challenge in designing advanced radiation-tolerant alloys and ion beam processing of nanocomposites. Particularly, ballistic dissolution susceptibility of different solute nanocluster species in alloys is poorly understood. Here, low dose rate neutron irradiations were conducted on a Fe-Cr-Ni based austenitic steel in the BOR-60 reactor (9.4 × 10 -7 dpa/s, 318 °C) followed by accelerated dose rate ion irradiations at multiple temperatures ( 10 -3 dpa/s, 380 – 420 °C). Using atom probe tomography, the stability of radiation-enhanced Cu-rich and radiation-induced Ni-Si-Mn-rich nanoclusters was evaluated. During neutron irradiation, Cu-rich clusters nucleated with their core concentrations progressively increasing with dose, while Ni-Si-Mn-rich clusters formed and evolved into G-phase precipitates. Ion irradiations dramatically altered the nanoclusters. Cu-rich clusters were ballistically dissolved, but Ni-Si-Mn-rich clusters remained stable and coarsened with dose at 400 and 420 °C, highlighting that different nanocluster species in a single microstructure can have innately distinct ballistic dissolution susceptibilities. Solute-specific recoil rates were incorporated into the Heinig precipitate stability model, which shows that in addition to radiation-enhanced diffusion, recovery from ballistic dissolution depends on solute concentration gradient near cluster interfaces. Finally, the combined experimental-modeling study quantified the critical temperatures and damage rates where ballistic dissolution dominates for each cluster species.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Nanoporous Fe 2 O 3 and Soluble Fe(II) Intermediates Accelerate the Electrodeposition of Fe in NaOH(aq)

Electrochemical conversion of iron oxide to iron metal can enable low-cost batteries for long duration energy storage and zero-emissions ironmaking for steel. Iron oxides, such as hematite, can be electrochemically reduced to metallic iron in concentrated alkaline electrolytes at modest temperatures, but the relative influences of solid-state and dissolved intermediates at practical reaction rates remains unclear. Here, in this study, we prepare a homologous set of well-defined hematite particles to measure how the nanoscale morphology of oxides controls both their reactivity and apparent reduction mechanism in concentrated hydroxide. Correlated electron microscopy and rotating-ring-disk-electrode measurements revealed that nanoporous hematite and solid intermediates formed iron via a dissolution-redeposition pathway. In contrast, dense hematite particles directly formed iron metal via reactive fracture. While previous studies on iron electrowinning have primarily emphasized the role of particle diameter at the micron scale, these results demonstrate the importance of the dissolution-redeposition pathway to support rapid reaction rates and suggest that nanoscale porosity controls iron oxide reactivity at temperatures <100 °C. Therefore, iron-oxide-to-metal electrolyzers and fast-charging iron-air batteries supported by curtailed electricity can increase the rate of metal formation by accelerating fracture and dissolution in reactant oxides.

TEM↗
DOE OSTI2015

Spontaneous Water Oxidation at Hematite (α-Fe2O3) Crystal Faces

Hematite (α-Fe2O3) persists as a promising candidate for photoelectrochemical water splitting but a slow oxygen evolution reaction (OER) at its surfaces remains a limitation. Here we extend a series of studies that examine pH-dependent surface potentials and electron transfer properties of effectively perfect low-index crystal faces of hematite in contact with simple electrolyte. Zero resistance amperometry was performed in a two electrode configuration to quantify spontaneous dark current between hematite crystal face pairs (001)/(012), (001)/(113), and (012)/(113) at pH 3. Exponentially decaying currents initially of up to 200 nA were reported between faces over four minute experiments. Fourth order ZRA kinetics indicated rate limitation by the OER for current that flows between (001)/(012) and (001)/(113) face pairs, with the (012) and (113) faces serving as the anodes when paired with (001). The cathodic partner reaction is reductive dissolution of the (001) face, converting surface Fe3+ to solubilized aqueous Fe2+, at a rate maintained by the OER at the anode. In contrast, OER rate limitation does not manifest for the (012)/(113) pair. The uniqueness of the (001) face is established in terms of a faster intrinsic ability to accept the protons required for the reductive dissolution reaction. OER rate limitation inversely may thus arise from sluggish kinetics of hematite surfaces to dispense with the protons that accompany the four-electron OER. The results are explained in terms of semi-quantitative energy band diagrams. The finding may be useful as a consideration for tailoring the design of polycrystalline hematite photoanodes that present multiple terminations to the interface with electrolyte.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2014

AFS-2 FLOWSHEET MODIFICATIONS TO ADDRESS THE INGROWTH OF PU(VI) DURING METAL DISSOLUTION

In support of the Alternate Feed Stock Two (AFS-2) PuO{sub 2} production campaign, Savannah River National Laboratory (SRNL) conducted a series of experiments concluding that dissolving Pu metal at 95°C using a 6–10 M HNO{sub 3} solution containing 0.05–0.2 M KF and 0–2 g/L B could reduce the oxidation of Pu(IV) to Pu(VI) as compared to dissolving Pu metal under the same conditions but at or near the boiling temperature. This flowsheet was demonstrated by conducting Pu metal dissolutions at 95°C to ensure that PuO{sub 2} solids were not formed during the dissolution. These dissolution parameters can be used for dissolving both Aqueous Polishing (AP) and MOX Process (MP) specification materials. Preceding the studies reported herein, two batches of Pu metal were dissolved in the H-Canyon 6.1D dissolver to prepare feed solution for the AFS-2 PuO{sub 2} production campaign. While in storage, UV-visible spectra obtained from an at-line spectrophotometer indicated the presence of Pu(VI). Analysis of the solutions also showed the presence of Fe, Ni, and Cr. Oxidation of Pu(IV) produced during metal dissolution to Pu(VI) is a concern for anion exchange purification. Anion exchange requires Pu in the +4 oxidation state for formation of the anionic plutonium(IV) hexanitrato complex which absorbs onto the resin. The presence of Pu(VI) in the anion feed solution would require a valence adjustment step to prevent losses. In addition, the presence of Cr(VI) would result in absorption of chromate ion onto the resin and could limit the purification of Pu from Cr which may challenge the purity specification of the final PuO{sub 2} product. Initial experiments were performed to quantify the rate of oxidation of Pu(IV) to Pu(VI) (presumed to be facilitated by Cr(VI)) as functions of the HNO{sub 3} concentration and temperature in simulated dissolution solutions containing Cr, Fe, and Ni. In these simulated Pu dissolutions studies, lowering the temperature from near boiling to 95 °C reduced the oxidation rate of Pu(IV) to Pu(VI). For 8.1 M HNO{sub 3} simulated dissolution solutions, at near boiling conditions >35% Pu(VI) was present in 50 h while at 95 °C <10% Pu(VI) was present at 50 h. At near boiling temperatures, eliminating the presence of Cr and varying the HNO{sub 3} concentration in the range of 7–8.5 M had little effect on the rate of conversion of Pu(IV) to Pu(VI). HNO{sub 3} oxidation of Pu(IV) to Pu(VI) in a pure solution has been reported previously. Based on simulated dissolution experiments, this study concluded that dissolving Pu metal at 95°C using a 6 to 10 M HNO{sub 3} solution 0.05–0.2 M KF and 0–2 g/L B could reduce the rate of oxidation of Pu(IV) to Pu(VI) as compared to near boiling conditions. To demonstrate this flowsheet, two small-scale experiments were performed dissolving Pu metal up to 6.75 g/L. No Pu-containing residues were observed in the solutions after cooling. Using Pu metal dissolution rates measured during the experiments and a correlation developed by Holcomb, the time required to completely dissolve a batch of Pu metal in an H-Canyon dissolver using this flowsheet was estimated to require nearly 5 days (120 h). This value is reasonably consistent with an estimate based on the Batch 2 and 3 dissolution times in the 6.1D dissolver and Pu metal dissolution rates measured in this study and by Rudisill et al. Data from the present and previous studies show that the Pu metal dissolution rate decreases by a factor of approximately two when the temperature decreased from boiling (112 to 116°C) to 95°C. Therefore, the time required to dissolve a batch of Pu metal in an H-Canyon dissolver at 95°C would likely double (from 36 to 54 h) and require 72 to 108 h depending on the surface area of the Pu metal. Based on the experimental studies, a Pu metal dissolution flowsheet utilizing 6–10 M HNO{sub 3} containing 0.05–0.2 M KF (with 0–2 g/L B) at 95°C is recommended to reduce the oxidation of Pu(IV) to Pu(VI) as compared to near boiling conditions. The time required to completely dissolve a batch of Pu metal will increase, however, by approximately a factor of two as compared to initial dissolutions at near boiling (assuming the KF concentration is maintained at nominally 0.1 M). By lowering the temperature to 95°C under otherwise the same operating parameters as previous dissolutions, the Pu(VI) concentration should not exceed 15% after a 120 h heating cycle. Increasing the HNO{sub 3} concentration and lowering Pu concentration are expected to further limit the amount of Pu(VI) formed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Impact of Zr Content on Radionuclide Release Rates in Metal Waste Forms

Reference alloy waste forms (RAW) underwent hybrid corrosion/immersion testing to parameterize the ANL analytical oxidative-dissolution model to enable the calculation of fractional release rates. The waste forms tested at SRNL were variations of the RAW-3 formulation that uses HT9 as the main alloy component, and are meant to enable evaluation of the impact of Zr:U ratio on the release rates of actinides and Tc-99. The test solutions were air saturated alkaline and acidic brines, representing potential repositories with those conditions. The testing approach consisted of 4 major steps; 1) bare surface corrosion measurements, 2) hybrid potentiostatic hold/exposure measurements, 3) measurement of radionuclide concentrations and relations to anodic current from potentiostatic holds, and 4) identification of corroding phases using SEM/EDS of electrodes.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

Atomistic thermodynamics and kinetics of dicalcium silicate dissolution

Low-temperature cement manufacturing has garnered academic and industrial attention for its low environmental footprints. However, the sluggish hydration kinetics of the resultant cement affects their early-age strength development. This motivates fundamental studies to unravel the mechanistic picture of the dissolution process and discover science-informed pathways to accelerate hydration. Standard atomistic simulations seldomly exceed a microsecond making them impractical to study slow dissolution processes. We are using rare event sampling techniques, we provide the mechanistic picture of Ca 2+ ion dissolution from a kink site on the dicalcium silicate surface. The Ca 2+ ion dissolution is comprised of two sequential stages: breaking restraints from the kink sites to form a ledge adatom and detaching from the ledge/terrace adatom sites into the solution. The first and second stages feature free energy barriers of ~63 kJ/mol and ~ 29 kJ/mol respectively, making the first stage the rate-limiting step of the entire Ca 2+ dissolution kinetics. Using the reactive flux method, the rate and equilibrium constants for each reaction step are calculated, which yield the Ca 2+ ion activity of ~1.03 × 10 -5 . The diffusion calculations indicate that the surface effects lower the self-diffusion coefficient of Ca 2+ ions at the solid-water interface.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Chlorite dissolution kinetics at pH 3–10 and temperature to 275°C

Sheet silicates and clays are ubiquitous in geothermal environments. Their dissolution is of interest because this process contributes to scaling reactions along fluid pathways and alteration of fracture surfaces which could affect reservoir permeability. Here, in order to better predict the geochemical impacts on long-term performance of engineered geothermal systems, we have measured chlorite dissolution and developed a generalized kinetic rate law applicable over an expanded range of solution pH and temperature. Chlorite, (Mg,Al,Fe) 12 (Si,Al) 8 O 20 (OH) 16 , commonly occurs in many geothermal host rocks as either a primary mineral or alteration product.

15 GEOTHERMAL ENERGY↗
DOE OSTI2018

Ignition and self-propagating reactions in Al/Pt multilayers of varied design

The different rate-limiting processes underlying ignition and self-propagating reactions in Al/Pt multilayers are examined through experiments and analytical modeling. Freestanding, ~1.6 μm-thick Al/Pt multilayers of varied stoichiometries and nanometer-scale layer thicknesses ignite at temperatures below the melting point of both reactants (and eutectics) demonstrating that initiation occurs via solid-state mixing. Equimolar multilayers exhibit the lowest ignition temperatures when comparing structures having a specific bilayer thickness. An activation energy of 76.6 kJ/mol at. associated with solid state mass transport is determined from the model analysis of ignition. High speed videography shows that equimolar Al/Pt multilayers undergo the most rapid self-sustained reactions with wavefront speeds as large as 73 m/s. Al- and Pt-rich multilayers react at reduced rates (as low as 0.3 m/s), consistent with reduced heat of reaction and lower adiabatic temperatures. An analytical model that accounts for key thermodynamic properties, preliminary mixing along interfaces, thermal transport, and mass diffusion is used to predict the wavefront speed dependencies on bilayer thickness. Finally, good fits to experimental data provide estimates for activation energy (51 kJ/mol at.) associated with mass transport subject to high heating rates and thermal diffusion coefficient of premixed interfacial volumes (2.8 × 10 -6 m 2 /s). Pt dissolution into molten Al is identified as a rate-limiting step underlying high temperature propagating reactions in Al/Pt multilayers.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Capping layer growth rate and the optical and structural properties of GaAsSbN-capped InAs/GaAs quantum dots

Changing the growth rate during the heteroepitaxial capping of InAs/GaAs quantum dots (QDs) with a 5 nm-thick GaAsSbN capping layer (CL) strongly modifies the QD structural and optical properties. A size and shape transition from taller pyramids to flatter lens-shaped QDs is observed when the CL growth rate is decreased from 1.5 to 0.5 ML/s. This indicates that the QD dissolution processes taking place during capping can be controlled to some extent by the GaAsSbN CL growth rate, with high growth rates allowing a complete preservation of the QDs. However, the dissolution processes are shown to have a leveling effect on the QD height, giving rise to a narrower size distribution for lower growth rates. Contrary to what could be expected, these effects are opposite to the strong blue-shift and improvement of the photoluminescence (PL) observed for higher growth rates. Nevertheless, the PL results can be understood in terms of the strong impact of the growth rate on the Sb and N incorporation into the CL, which results in lower Sb and N contents at higher growth rates. Besides the QD-CL band offsets and QD strain, the different CL composition alters the band alignment of the system, which can be transformed to type-II at low growth rates. These results show the key role of the alloyed CL growth parameters on the resulting QD properties and demonstrate an intricate correlation between the PL spectra and the sample morphology in complex QD-CL structures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2012

Accurate rates of the complex mechanisms for growth and dissolu-tion of minerals using a combination of rare event theories

Mineral growth and dissolution are often treated as occurring via a single, reversible process that governs the rate of reaction. We show that multiple, distinct intermediate states can occur during both growth and dissolution. Specifically, we have used metadynamics, a method to efficiently explore the free energy landscape of a system, coupled to umbrella sampling and reactive flux calculations, to examine the mechanism and rates of attachment and detachment of a barium ion onto a stepped, barite (BaSO4) surface. The activation energies calculated for the rate limiting reactions, which are different for attachment and detachment, precisely match those measured experimentally during both growth and dissolution. These results can potentially explain anomalous, non-steady state mineral reaction rates observed experimentally, and will enable the design of more efficient growth inhibitors and facilitate an understanding of the effect of impurities.

74 ATOMIC AND MOLECULAR PHYSICS↗