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At least 1,387 records · Page 77
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Biological Redox Cycling Of Iron In Nontronite And Its Potential Application In Nitrate Removal

Redox cycling of structural Fe in phyllosilicates provides a potential method to remediate nitrate contamination in natural environment. Past research has only studied chemical redox cycles or a single biologically mediated redox cycle of Fe in phyllosilicates. The objective of this research was to study three microbially driven redox cycles of Fe in one phyllosilicate, nontronite (NAu-2). During the reduction phase structural Fe(III) in NAu-2 served as electron acceptor, lactate as electron donor, AQDS as electron shuttle, and dissimilatory Fe(III)-reducing bacteria Shewanella putrefaciens CN32 as mediator in bicarbonate-buffered and PIPES-buffered media. During the oxidation phase, biogenic Fe(II) served an electron donor, nitrate as electron acceptor, and nitrate-dependent Fe(II)-oxidizing bacteria Pseudogulbenkiania sp. strain 2002 as mediator in the same media. For all three cycles, structural Fe in NAu-2 was able to reversibly undergo 3 redox cycles without significant reductive or oxidative dissolution. X-ray diffraction and scanning and transmission electron microscopy revealed that NAu-2 was the dominant residual mineral throughout the 3 redox cycles with some dissolution textures but no significant secondary mineralization. Mössbauer spectroscopy revealed that Fe(II) in bio-reduced samples likely occurred in two distinct environments, at edges and the interior of the NAu-2 structure. Nitrate was completely reduced to nitrogen gas under both buffer conditions and this extent and rate did not change with Fe redox cycles. Mössbauer spectroscopy further revealed that nitrate reduction was coupled to predominant/preferred oxidation of edge Fe(II). These results suggest that structural Fe in phyllosilicates may represent a renewable source to continuously remove nitrate in natural environments.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2016

A 2.5D Reactive Transport Model for Fracture Alteration Simulation

Understanding fracture alteration resulting from geochemical reactions is critical in predicting fluid migration in the subsurface and is relevant to multiple environmental challenges. Here in this paper, we present a novel 2.5D continuum reactive transport model that captures and predicts the spatial pattern of fracture aperture change and the development of an altered layer in the near-fracture region. The model considers permeability heterogeneity in the fracture plane and updates fracture apertures and flow fields based on local reactions. It tracks the reaction front of each mineral phase and calculates the thickness of the altered layer. Given this treatment, the model is able to account for the diffusion limitation on reaction rates associated with the altered layer. The model results are in good agreement with an experimental study in which a CO 2 -acidified brine was injected into a fracture in the Duperow Dolomite, causing dissolution of calcite and dolomite that result in the formation of a preferential flow channel and an altered layer. Finally, with an effective diffusion coefficient consistent with the experimentally observed porosity of the altered layer, the model captures the progressive decrease in the dissolution rate of the fast-reacting mineral in the altered layer.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2016

Replacement of Calcite (CaCO 3 ) by Cerussite (PbCO 3 )

The mobility of toxic elements, such as lead (Pb) can be attenuated by adsorption, incorporation, and precipitation on carbonate minerals in subsurface environments. Here in this paper, we report a study of the bulk transformation of single-crystal calcite (CaCO 3 ) into polycrystalline cerussite (PbCO 3 ) through reaction with acidic Pb-bearing solutions. This reaction began with the growth of a cerussite shell on top of calcite surfaces followed by the replacement of the remaining calcite core. The external shape of the original calcite was preserved by a balance between calcite dissolution and cerussite growth controlled by adjusting the Pb 2+ concentration and pH. The relation between the rounded calcite core and the surrounding lath-shaped cerussite aggregates was imaged by transmission X-ray microscopy, which revealed preferentially elongated cerussite crystals parallel to the surface and edge directions of calcite. The replacement reaction involved concurrent development ~100 nm wide pores parallel to calcite c-glide or (1$\overline{20}$) planes, which may have provided permeability for chemical exchange during the reaction. X-ray reflectivity measurements showed no clear epitaxial relation of cerussite to the calcite (104) surface. These results demonstrate Pb sequestration through mineral replacement reactions and the critical role of nanoporosity (3% by volume) on the solid phase transformation through a dissolution-recrystallization mechanism.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Sea Level Rise Induced Arsenic Release from Historically Contaminated Coastal Soils

Climate change-induced perturbations in the hydrologic regime are expected to impact biogeochemical processes, including contaminant mobility and cycling. Elevated levels of geogenic and anthropogenic arsenic are found along many coasts around the world, most notably in south and southeast Asia but also in the United States, particularly along the Mid-Atlantic coast. The mechanism by and the extent to which arsenic may be released in contaminated coastal soils due to sea level rise are unknown. Here we show a series of data from a coastal arsenic-contaminated soil exposed to sea and river waters in biogeochemical microcosm reactors across field-validated redox conditions. We find that reducing conditions lead to arsenic release from historically contaminated coastal soils through reductive dissolution of arsenic-bearing mineral oxides in both sea and river water inundations, with less arsenic release from seawater scenarios than river water due to inhibition of oxide dissolution. For the first time, we systematically display gradation of solid phase soil-arsenic speciation across defined redox windows from reducing to oxidizing conditions in natural waters by combining biogeochemical microcosm experiments and X-ray absorption spectroscopy. Here, our results demonstrate the threat of sea level rise stands to impact arsenic release from contaminated coastal soils by changing redox conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Incorporating Nanoscale Effects into a Continuum-Scale Reactive Transport Model for CO 2 -Deteriorated Cement

We present that wellbore cement deterioration is critical for wellbore integrity and the safety of CO 2 storage in geologic formations. Our previous experimental work highlighted the importance of the portlandite (CH)-depleted zone and the surface dissolution zone in the CO 2 -attacked cement. In this study, we simulated numerically the evolution of the CH-depleted zone and the dissolution of the cement surfaces utilizing a reduced-dimension (1D) reactive transport model. The approach shows that three nanoscale effects are important and had to be incorporated in a continuum-scale model to capture experimental observations: First, it was necessary to account for the fact that secondary CaCO 3 precipitation does not fill the pore space completely, with the result that acidic brine continues to diffuse through the carbonated zone to form a CH-depleted zone. Second, secondary precipitation in brine begins via nucleation kinetics, and this could not be described with previous models using growth kinetics alone. Third, our results suggest that the CaCO 3 precipitates in the confined pore space are more soluble than those formed in brine. Finally, this study provides a new platform for a reduced dimension model for CO 2 attack on cement that captures the important nanoscale mechanisms influencing macroscale phenomena in subsurface environments.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2015

Structure and Solution Speciation of U IV Linked Phosphomolybdate (Mo V ) Clusters

Crystals of [NaU(Mo 6 P 4 O 31 H 7 ) 2 ]·5Na·(H 2 O)$_n$ (NaUMo 6 ) have been synthesized by slow evaporation of an aqueous mixture containing uranyl nitrate, sodium molybdate, phosphoric acid, and sodium dithionate. Single crystal diffraction of NaUMo 6 reveals the assembly of {Mo 6 P 4 } clusters linked into one-dimensional chains with alternating Na + and U 4+ cations. To our knowledge, NaUMo 6 is a unique example of Mo 5+ based polyoxometalate associated with actinides. With the use of similar synthesis conditions but without uranium in the aqueous solution, [Na(Mo 6 P 4 O 31 H 10 ) 2 ]·5Na·(H 2 PO 4 )·(H 2 O)$_n$ (NaMo 6 ) is obtained. NaMo 6 is a sandwich type cluster which is built on the assemblage of two {Mo 6 P 4 } units linked by one sodium cation. Using small-angle X-ray scattering techniques and aqueous electrolyte based dissolution strategies, we can accurately observe chains of [UNa(Mo 6 P 4 O 31 H 7 ) 2 ]$_n$$^{5n}$, where $n = 7$ is the dominant soluble specie. Likewise, the dimeric form of [Na(Mo 6 P 4 O 31 H 10 ) 2 ] 5– dominates the aqueous solution, revealing the structural units observed in the crystal structure are also stable in solution, under appropriate dissolution conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Allotropic control: How certain fluorinated carbonate electrolytes protect aluminum current collectors by promoting the formation of insoluble coordination polymers

Here, there is a strong incentive for increasing the operation voltage of Li-ion cells above 4.5 V in order to increase the density of stored energy. Aluminum is an inexpensive, lightweight metal that is commonly used as a positive electrode current collector in these cells. Imide LiX salts, such as lithium bis(trifluoromethylsulfonyl)imide (X = TFSI), and lithium bis(fluorosulfonyl)imide (X = FSI), are chemically stable on the energized lithiated transition metal oxide electrodes, but their presence in the electrolyte causes rapid anodic dissolution and pitting of Al current collectors at potentials exceeding 4.0 V versus Li/Li + . For LiBF 4 and LiPF 6 , the release of HF near the energized surfaces passivates the exposed Al metal, inhibiting this pitting corrosion, but it also causes the gradual degradation of the cathode active material, negating this important advantage. Here we report that in certain electrolytes containing fluorinated carbonate solvents and LiX salts, the threshold voltage for safe operation of Al current collectors can be increased to 5.5 V versus Li/Li + . Interestingly, the most efficient solvent also facilitates the formation of an insoluble gel when AlX 3 is introduced into this solvent. We suggest that this solvent promotes the aggregation of coordination polymers of AlX 3 at the exposed Al surface that isolate this surface from the electrolyte, thereby preventing further Al dissolution and corrosion. Other examples of Al collector protection may also involve this mechanism. Our study suggests that such “allotropic control” could be a way of widening the operation window of Li-ion cells without electrode deterioration, Al current collector corrosion, and electrolyte breakdown.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Chemical stability of Lithium 2-trifluoromethyl-4,5-dicyanoimidazolide, an electrolyte salt for Li-ion cells

Lithium hexafluorophosphate (LiPF 6 ) is ubiquitous in commercial lithium-ion batteries, but it is hydrolytically unstable and corrosive on electrode surfaces. Using a more stable salt would confer multiple benefits for high-voltage operation, but many such electrolyte systems facilitate anodic dissolution and pitting corrosion of aluminum current collectors that negate their advantages. Lithium 2-trifluoromethyl-4,5-dicyanoimidazolide (LiTDI) is a new salt that was designed specifically for high-voltage cells. In this study we demonstrate that in carbonate electrolytes, LiTDI prevents anodic dissolution of Al current collectors, which places it into a select group of corrosion inhibitors. However, we also demonstrate that LiTDI becomes reduced on lithiated graphite, undergoing sequential defluorination and yielding a thick and resistive solid-electrolyte interphase (SEI), which increases impedance and lowers electrode capacity. The mechanistic causes for this behavior are examined using computational chemistry methods in the light of recent spectroscopic studies. Here, we demonstrate that LiTDI reduction can be prevented by certain electrolyte additives, which include fluoroethylene carbonate, vinylene carbonate and lithium bis(oxalato)borate. This beneficial action is due to preferential reduction of these additives over LiTDI at a higher potential vs. Li/Li + , so the resulting SEI can prevent the direct reduction of LiTDI at lower potentials on the graphite electrode.

25 ENERGY STORAGE↗
DOE OSTI2019

Electrodissolution Inhibition of Gold Nanorods with Oxoanions

Metal nanoparticles experience varied chemical environments that can cause corrosion and dissolution in electronics, electrocatalysis, and sensing applications. Understanding oxidative dissolution is important for plasmonic nanoparticles because their optical properties strongly depend on size and shape. Here, we demonstrate that the addition of low relative concentrations of oxoanions to aqueous halide electrolyte solutions improves the morphological stability of plasmonic gold nanorods at anodic electrochemical potentials that otherwise induce complete oxidative electrodissolution. Single particle hyperspectral dark-field imaging and correlated scanning electron microscopy show that oxoanions alter the electrodissolution onset potential, electrodissolution pathway, and nanoparticle reaction heterogeneity, as compared to chloride-only electrolyte solutions. We identify five mechanistic contributors to the corrosion inhibition capabilities of oxoanions in the presence of chloride ions, with the aim of expanding the range of electrochemical sensing and catalysis applications for plasmonic metal nanoparticles. Of the contributors investigated, the pH, adsorption potential, and ionicity of the oxoanion are found to be the most influential factors, supporting the superior corrosion inhibition observed with bicarbonate and phosphate.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Real-Time Monitoring of Cation Dissolution/Deintercalation Kinetics from Transition-Metal Oxides in Organic Environments

The future of high-voltage rechargeable batteries is closely tied to the fundamental understanding of the processes that lead to the potential-dependent degradation of electrode materials and organic electrolytes. To date, however, there have been no methods able to provide quantitative, in situ and in real time information about the electrode dissolution kinetics and concomitant electrolyte decomposition during charge/discharge. We describe the development of such a method, which is of both fundamental and technological significance. Our novel approach enables simultaneous and independent measurements of transition-metal cation dissolution rates from different oxide hosts (Co 3+/4+ or Cr 3+/4+ ), deintercalation kinetics of working cations (Mg 2+ ), and the relative rate of electrolyte decomposition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Evidence for Carbonate Surface Complexation during Forsterite Carbonation in Wet Supercritical Carbon Dioxide

Continental flood basalts are attractive formations for geologic sequestration of carbon dioxide because of their reactive divalent-cation containing silicates, such as forsterite (Mg2SiO4), suitable for long-term trapping of CO2 mineralized as metal carbonates. The goal of this study was to investigate at a molecular level the carbonation products formed during the reaction of forsterite with supercritical CO2 (scCO2) as a function of the concentration of H2O adsorbed to the forsterite surface. Experiments were performed at 50 °C and 90 bar using an in situ IR titration capability, and post-reaction samples were examined by ex situ techniques, including SEM, XPS, FIB-TEM, TGA-MS, and MAS-NMR. Carbonation products and reaction extents varied greatly with adsorbed H2O. We show for the first time evidence of Mg-carbonate surface complexation under wet scCO2 conditions. Carbonate is found to be coordinated to Mg at the forsterite surface in a predominately bidentate fashion at adsorbed H2O concentrations below 27 µmol/m2. Above this concentration and up to 76 µmol/m2, monodentate coordinated complexes become dominant. Beyond a threshold adsorbed H2O concentration of 76 µmol/m2, crystalline carbonates continuously precipitate as magnesite, and the particles that form are hundreds of times larger than the estimated thicknesses of the adsorbed water films of about 7 to 15 Å. At an applied level, these results suggest that mineral carbonation in scCO2 dominated fluids near the wellbore and adjacent to caprocks will be insignificant and limited to surface complexation, unless adsorbed H2O concentrations are high enough to promote crystalline carbonate formation. At a fundamental level, the surface complexes and their dependence on adsorbed H2O concentration give insights regarding forsterite dissolution processes and magnesite nucleation and growth.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2026

Tuning the Solvation and Solubility Properties of Molecularly Heterogeneous Nonionic Deep Eutectic Solvents via Interface Organization

Common separation techniques, such as liquid− liquid extraction, are usually used for extractions and purifications due to their industrial scalability and affordability. However, these well-established practices are hindered by low selectivity and challenges in recovering solutes and solvents. Deep eutectic solvents (DES), a fairly new type of solvent, have the potential to overcome these issues. DESs are binary mixtures whose physical properties can be tuned by selecting the appropriate precursors to facilitate and/or enhance processes such as extraction. A promising DES for selective separations is formed when lauric acid (LA) is mixed with N-methylacetamide (NMA). This LA-NMA DES has a heterogeneous microscopic structure that can solvate compounds with completely different polarities. This study explores how forming an organized structure on the mesoscale affects the solubility of nonpolar solutes in nonionic DESs. To this end, the molecular and mesoscale structures and their effect on the solubility and solvation properties are evaluated for the LA-NMA DES and two new DESs with slight chemical variations in their precursors. It is observed that the organization of the nonpolar DES domains and, consequently, of their interfaces directly relates to the solubility of nonpolar compounds. Specifically, correctly selecting the DES precursors that form organized nonpolar domains leads to an organized interface in which the nonpolar solutes are solvated, thereby increasing the solubility. Additionally, enhanced dissolution power was observed in a completely different DES with mesoscale order in its molecular structure and composed of menthol and lauric acid. The latter result further validates the proposed tunability of the DES dissolution power through organized interfaces, extending it beyond a specific DES family and opening the possibility of new extraction-tailored designer solvents.

Extraction↗
DOE OSTI2019

Electrochemical Degradation of Pt–Ni Nanocatalysts: An Identical Location Aberration-Corrected Scanning Transmission Electron Microscopy Study

The evolution of Pt–Ni nanoparticles supported on amorphous carbon is investigated before and after electrochemical potential cycling (0.6-1.1 V), using aberration-corrected scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDS). During voltage cycling and due to the dissolution of nanoparticles, single ions/atoms and ionic/atomic clusters emerge and diffuse across the carbon support toward larger nanoparticles, where they redeposit. We observe that the preferred locations for the dissolution are the steps and corners of the nanoparticles. On the other hand, the redeposition process happens often on {111} type planes. In addition, contrary to the conventional view, where larger particles grow isotropically from smaller ones, this research work shows that anisotropic growth of smaller particles occurs during potential cycling. The reason for this behavior seems to be related to the fact that smaller particles with thicker Pt-rich shells trigger the nucleation and deposition of Pt.

catalysts↗
DOE OSTI2025

Assessing the Long-Term Stability of Anion Exchange Membranes for Electrochemical CO 2 Reduction

Materials and cell components used in CO 2 electrolysis have largely been adapted from technologies initially developed for water electrolysis and fuel cells. However, electrochemical CO 2 reduction introduces distinct material challenges due to the unique chemical environment in this process. Here, in this study, we conducted ex-situ 1000 h stability tests on commonly used anion exchange membranes, exposing them exclusively to electrolytes and organic molecules used or produced during CO 2 electrolysis, at concentrations relevant to and compatible with postseparation processes. Notably, 15% w/w n-propanol and 5 M acetic acid caused complete dissolution or partial disintegration of the membranes unless cross-linking was present and remained stable throughout the test. When the membranes stayed physically intact, most of them exhibited excellent chemical stability in alkaline medium containing alcohols or formic acid, which was confirmed by vibrational spectroscopy and ion exchange capacity measurements. However, exposure to alcohol-and acid-containing solutions led to a substantial increase in swelling and water uptake, with potential implications for mechanical stability, ion/product crossover, and compression management of adjacent components. The potential effects of CO 2 electroreduction products on membrane stability, their subsequent impact on electrolyzer performance, and mitigation strategies are discussed.

CO2RR↗
DOE OSTI2018

Strain-Driven Mn-Reorganization in Overlithiated Li x Mn 2 O 4 Epitaxial Thin-Film Electrodes

Here, lithium manganate Li x Mn 2 O 4 (LMO) is a lithium ion cathode that suffers from the widely observed but poorly understood phenomenon of capacity loss due to Mn dissolution during electrochemical cycling. Here, operando X-ray reflectivity (low- and high-angle) is used to study the structure and morphology of epitaxial LMO (111) thin film cathodes undergoing lithium insertion and extraction to understand the inter-relationships between biaxial strain and Mn-dissolution. The initially strain-relieved LiMn 2 O 4 films generate in-plane tensile and compressive strains for delithiated (x < 1) and overlithiated (x > 1) charge states, respectively. The results reveal reversible Li insertion into LMO with no measurable Mn-loss for 0 < x < 1, as expected. In contrast, deeper discharge (x > 1) reveals Mn loss from LMO along with dramatic changes in the intensity of the (111) Bragg peak that cannot be explained by Li stoichiometry. These results reveal a partially reversible site reorganization of Mn ions ithin the LMO film that is not seen in bulk reactions and indicates a transition in Mn-layer toichiometry from 3:1 to 2:2 in alternating cation planes. Density functional theory calculations confirm that compressive strains (at x = 2) stabilize LMO structures with 2:2 Mn site distributions, therefore providing new insights into the role of lattice strain in the stability of LMO.

25 ENERGY STORAGE↗
DOE OSTI2018

Structure and Solution Dynamics of Lithium Methyl Carbonate as a Protective Layer For Lithium Metal

Herein, Lithium methyl carbonate (LMC) is synthesized in a single step and investigated as a coating material for Li protection. The LMC layer can be formed in situ during Li plating on Cu foil. The chemical and crystal structure of the ~1 μm thick coating is confirmed, which remains intact during lithium cycling. SEM also confirms the dissolution of the LMC layer after being transferred into the commercial LiPF 6 -carbonate electrolyte. Presaturating the electrolyte with LMC powder prevents the dissolution of the LMC coating layer, which improves the Li plating/stripping Coulombic efficiency from 90.5% (bare Cu in commercial electrolyte) to 96.1% at 0.5 mA cm –2 and 1 mAh cm –2 .

25 ENERGY STORAGE↗
DOE OSTI2022

Failure Modes of Platinized pn+-GaInP Photocathodes for Solar-Driven H2 Evolution

The long-term stability for the hydrogen-evolution reaction (HER) of homojunction pn+-Ga0.52In0.48P photocathodes (band gap = 1.8 eV) with an electrodeposited Pt catalyst (pn+-GaInP/Pt) has been systematically evaluated in both acidic and alkaline electrolytes. Electrode dissolution during chronoamperometry was correlated with changes over time in the current density-potential (J-E) behavior to reveal the underlying failure mechanism. Pristine pn+-GaInP/Pt photocathodes yielded an open-circuit photopotential (Eoc) as positive as >1.0 V vs the potential of the reversible hydrogen electrode (RHE) and a light-limited current density (Jph) of >12 mA cm-2 (1-sun illumination). However, Eoc and Jph gradually degraded at either pH 0 or pH 14. The performance degradation was attributed to three different failure modes: (1) gradual thinning of the n+-emitter layer due to GaInP dissolution in acid; (2) active corrosion of the underlying GaAs substrate at positive potentials causing delamination of the upper GaInP epilayers; and (3) direct GaAs/electrolyte contact compromising the operational stability of the device. This work reveals the importance of both substrate stability and structural integrity of integrated photoelectrodes toward stable solar fuel generation.

CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSICS,S↗
DOE OSTI2023

Tuning Bulk Redox and Altering Interfacial Reactivity in Highly Fluorinated Cation-Disordered Rocksalt Cathodes

Lithium-excess, cation-disordered rocksalt (DRX) materials have been subject to intense scrutiny and development in recent years as potential cathode materials for Li-ion batteries. Despite their compositional flexibility and high initial capacity, they suffer from poorly understood parasitic degradation reactions at the cathode-electrolyte interface. These interfacial degradation reactions deteriorate both the DRX material and electrolyte, ultimately leading to capacity fade and voltage hysteresis during cycling. In this work, differential electrochemical mass spectrometry (DEMS) and titration mass spectrometry are combined to quantify the extent of bulk redox and surface degradation reactions for a set of Mn 2+/4+ -based DRX oxyfluorides during initial cycling with a high-voltage charging cutoff (4.8 V vs Li/Li + ). Increasing the fluorine content from 7.5 to 33.75% is shown to diminish oxygen redox and suppresses high-voltage O 2 evolution from the DRX surface. Additionally, electrolyte degradation processes resulting in the formation of both gaseous species and electrolyte-soluble protic species are observed. Subsequently, DEMS is paired with a fluoride-scavenging additive to demonstrate that increasing fluorine content leads to increased dissolution of fluorine from the DRX material into the electrolyte. Finally, a suite of ex situ spectroscopy techniques (X-ray photoelectron spectroscopy, inductively coupled plasma optical emission spectroscopy, and solid-state nuclear magnetic resonance spectroscopy) are employed to study the change in DRX composition during charging, revealing the dissolution of manganese and fluorine from the DRX material at high voltages. Here this work provides insight into the degradation processes occurring at the DRX-electrolyte interface and points toward potential routes of interfacial stabilization.

25 ENERGY STORAGE↗