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All sourcesNASA NTRSDOE OSTI
NASA NTRS1989

Luminescence and ESR studies of relationships between O(-)-centres and structural iron in natural and synthetically hydrated kaolinites

Luminescence, induced by dehydration and by wetting with hydrazine and unsymmetrically substituted hydrazine, and related ESR spectra have been observed from several kaolinites, synthetically hydrated kaolinites, and metahalloysites. The amine-wetting luminescence results suggest that intercalation, not a chemiluminescence reaction, is the luminescence trigger. Correlation between hydration-induced luminescence and g = 2 ESR signals associated with O(-)-centres in several natural halloysites, and concurrent diminution of the intensity of both these signal types as a function of aging in two 8.4 angstroms synthetically hydrated, kaolinites, confirm a previously-reported relationship between the luminescence induced by dehydration and in the presence of O(-)-centres (holes, i.e., electron vacancies) in the tetrahedral sheet. Furthermore, the ESR spectra of the 8.4 angstroms hydrate showed a concurrent change in the line shape of the g = 4 signal from a shape usually associated with structural Fe in an ordered kaolinite, to a simpler one typically observed in more disordered kaolinite, halloysite, and montmorillonite. Either structural Fe centres and the O(-)-centres interact, or both are subject to factors previously associated with degree of order. The results question the long-term stability of the 8.4 angstroms hydrate, although XRD does not indicate interlayer collapse over this period. Complex inter-relationships are shown between intercalation, stored energy, structural Fe, and the degree of hydration which may be reflected in catalytic as well as spectroscopic properties of the clays.

NASA Center ARC↗
NASA NTRS2005

Competitive Oxidation and Hydration During Aqueous Alteration of Asteroids

Introduction: Studies of chondrites show that incorporation of H2O ice during formation of asteroids followed by radioactive heating caused partial oxidation and hydration of primary reduced and anhydrous rocks. Oxidation of kamacite, phosphides, troilite and organic polymers occurred through consumption of water s oxygen and release of H2. Hydration caused formation of serpentine, saponite, chlorite, talc and hydrated salts. Since H2O was the major reactant in oxidation and hydration, these processes could have been competitive. Redox reactions in asteroids should have been closely connected to hydration (dehydration) during aqueous alteration and thermal metamorphism. For example, dehydration and reduction release H2O that can be consumed in oxidation and hydration, respectively. We model asteroidal processes in order to quantify the fate of H2O and water s oxygen in major redox and hydration/dehydration reactions. Model: Equilibrium compositions in the gas-solid-liquid

Zolotov, M. Y.↗
DOE OSTI2026

Oil in Alaska North Slope Gas Hydrate Reservoir: Micro-CT and Flow Simulation Insights into Permeability

Gas hydrate-bearing sands on the Alaska North Slope (ANS) host minor volumes of crude oil whose impact on formation permeability has never been quantified relative to a gas hydrate reservoir system. Here, we combine in situ pressure-core microcomputed-tomography (μ-CT), thermogravimetric analysis (TGA), gas-chromatography–mass-spectrometry (GC–MS), scanning-electron microscopy coupled with energy-dispersive spectroscopy (SEM-EDS), and Stokes-flow simulation to (i) quantify oil saturation, (ii) infer its source, and (iii) evaluate its influence on permeability after gas-hydrate dissociation. μ-CT and SEM-EDS imaging identify the host sediment as silty, with some grain-coating clay present. Eight representative 3003-voxel subvolumes extracted from a preserved pressure core (Core 15P-3c, from the B1 sand (unit B), HYDRATE 02 Geo Data Well (GDW), 886.96–887.29 m measured depth, MD) exhibit porosities of 0.34–0.37 and an average oil saturation of 0.09 ± 0.03, in comparison to an independent TGA-based estimate of 0.16. GC-MS fingerprints obtained from an adjacent depressurized core (Core 17P-1, 891.37–891.44 m MD), together with oil pore habit revealed by μ-CT, suggest that the oil is partly native but also includes contributions from mineral oil-based drilling fluid contamination. Further analysis of oil–porewater interactions and flushing tests confirms that native oil saturation in the analyzed samples ranges from 0.04 to 0.08 with an average of approximately 0.06, and the oil is highly immobile. Flow simulations demonstrate that the native oil saturation of ≈0.06 reduces permeability by approximately 50% due to both pore blockage and increased flow-path tortuosity. These findings reveal the potential presence of native oil within the ANS gas hydrate reservoir and suggest that future simulation models may need to account for its impact on permeability to improve long-term performance predictions of gas and water production.

02 PETROLEUM↗
DOE OSTI2024

Surface Dynamics of Selective Hydration of Rutile TiO 2 : A Kinetic Monte Carlo Approach

The utility of atomic layer deposition (ALD) continues to expand beyond conformal thin-film fabrication to include area- or site-selective ALD. We previously identified a strategy for site-selective ALD (SS-ALD) via the evaluation of thermodynamically preferred hydration of rutile TiO 2 surfaces, as deduced from electronic structure calculations. Here, we report a novel kinetic Monte Carlo (KMC) model that allows for the investigation of surface dynamics and kinetics that improves our understanding of and intuition for the selective hydration strategy. Here we demonstrate the validity of the strategy with respect to step-edge defects for the lowest energy (110) facet as well as report results for the other common facets which agree with experimental STM observations. The results here indicate that the selective hydration strategy is feasible both thermodynamically (evaluated in our previous publication) and kinetically (from the KMC model). Because diffusion has a slower rate than others, we find that any proximity effects between terrace and defect sites are unlikely to affect the selective hydration strategy for rutile TiO 2 . The KMC model further provides relevant timescales for achieving selectivity experimentally and establishes the kinetic viability of the selective hydration approach to SS-ALD.

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

Combined Machine Learning and Molecular Dynamics Reveal Two States of Hydration of a Single Functional Group of Cationic Polymeric Brushes

The state of hydration of a macromolecular system regulates a plethora of different properties of such a system. In this article, we develop a novel machine learning (ML) approach, based on the unsupervised clustering algorithm, for probing the hydration behavior of the {N(CH 3 ) 3 } + functional group of the PMETAC [Poly(2-(methacryloyloxy)ethyl trimethylammonium chloride] polyelectrolyte (PE) brush system. The PE brushes and the brush-supported water molecules and counterions (chloride ions) are first described using all-atom molecular dynamics (MD) simulations. The simulation data is subsequently used in our ML framework to identify that (1) the {N(CH 3 ) 3 } + functional groups of the PMETAC brushes have two distinct hydration states with one state (state 1) being characterized by less structured water molecules and the other state (state 2) being characterized by more structured water molecules and (2) an enhancement in the brush grafting density leads to the progressive dissapparenace of state 2. An increase in the grafting density increases the number of chloride counterions in a given volume around the {N(CH 3 ) 3 } + functional group and increases the number of shared water molecules between the {N(CH 3 ) 3 } + and Cl - . The chloride counterions are associated with a hydration layer with much less structured water molecules. Therefore, with an increase in the grafting density, an increase in the percentage of shared water molecules leads to the prevalence of the hydration state [of the {N(CH 3 ) 3 } + moiety] with less structured water molecules. Finally, we explain how the present findings are commensurate with two key previous related results, namely a significantly large chloride ion mobility inside the PMETAC brush layer and the {N(CH 3 ) 3 } + -Cl - average distance remaining independent of the PMETAC brush grafting density. Furthermore, we anticipate that the combined ML-MD-simulation approach proposed in this study can be adapted to probe other soft matter systems to reveal new insights of the underlying mechanisms of emergent phenomenon.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Hydration-Controlled Proton Transport in Respiratory Complex I

Proton pumping by respiratory complex I is one essential element for generating the proton motive force that drives ATP synthesis in mitochondria. Although it is understood that electrons from NADH reduce ubiquinone at the peripheral arm and that four protons are transferred in the membrane domain, the mechanism by which this redox reaction initiates proton translocation remains unclear. A lateral pathway linking the quinone binding site to the membrane domain via ND1, ND3, and ND4L subunits has been proposed as a possible initial path of an excess proton. However, experimental structures indicate that the hydration connectivity between D66 ND3 and E34 ND4L is comparatively weaker than in neighboring segments, suggesting a potential regulatory point for proton transfer. Using multiscale reactive molecular dynamics (MS-RMD) and a water wire connectivity metric, we directly simulate proton transport through this region as coupled to the hydration by water molecules. Our results reveal that proton transfer is thermodynamically feasible when transient hydration aligns with the presence of an excess proton, revealing the strong coupling between hydration and proton transfer (PT) in this region of Complex I. These findings support a model where proton injection enhances local hydration, dynamically opening the pathway for proton transfer and regulating the onset of proton pumping in Complex I.

Chemical structure↗
DOE OSTI2025

Coupled THM modeling of bentonite heating and hydration in tank tests with a new temperature-dependent water retention model

This study presents a coupled thermo-hydro-mechanical (THM) model for simulating the heating and hydration behavior of bentonite, a buffer material in deep geological repositories (DGRs). The model incorporates a new temperature-dependent soil water retention curve which captures the thermal-induced shift in water retention behavior. It also distinguishes between liquid and gas permeability, modeling intrinsic gas permeability as a function of accessible porosity to improve vapor transport and desaturation predictions. The model was validated against two large-scale tank tests, demonstrating good agreement with measured temperature, relative humidity, and water inflow data. It revealed a complex porosity evolution driven by thermal expansion, vapor movement, vapor condensation, and hydration-induced swelling during heating and hydration processes. The simulation results also suggest that the permeability of the hydration layer plays a critical role in controlling water intake. Clogging of this layer can significantly reduce the volume of water inflow during the hydration phase. Furthermore, while the model effectively captures key THM behavior, further development of the mechanical constitutive law is required to account for possible thermo-elasto-plastic volume changes and microstructural effects. Overall, the model provides a robust tool for evaluating the evolution of bentonite-based barrier material in DGRs.

Guo, Guanlong [Lawrence Berkeley National Laborato↗
DOE OSTI2024

Influence of Water Sorption on Ionic Conductivity in Polyether Electrolytes at Low Hydration

Ion-containing polymers are subject to a wide range of hydration conditions across electrochemical and water treatment applications. Significant work on dry polymer electrolytes for batteries and highly swollen membranes for water purification has informed our understanding of ion transport under extreme conditions. However, knowledge of intermediate conditions (i.e., low hydration) is essential to emerging applications (e.g., electrolyzers, fuel cells, and lithium extraction). Ion transport under low levels of hydration is distinct from the extreme conditions typically investigated, and the relevant physics cannot be extrapolated from existing knowledge, stifling materials design. In this study, we conducted ion transport measurements in LiTFSI-doped polyethers that were systematically hydrated from dry conditions. A semiautomated apparatus that performs parallel measurements of water uptake and ionic conductivity in thin-film polymers under controlled humidity was developed. For the materials and swelling range considered in this study (i.e., <0.07 g water/g dry polymer electrolyte), ionic conductivity depends nonlinearly on water uptake, with the initial sorbed water weakly affecting conductivity. With additional increases in swelling, more significant increases in conductivity were observed. Remarkably, changes in conductivity induced by water sorption were correlated with the number of water molecules per lithium ion, with the normalized molar conductivity of different samples effectively collapsing onto one another until this unit of hydration exceeded the solvation number of lithium ions under aqueous conditions. Furthermore, these results provide important knowledge regarding the effects of trace water contamination on conductivity measurements in polymer electrolytes and demonstrate that the lithium-ion solvation number marks a key transition point regarding the influence of water on ion transport in ion-containing polymers.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Influence of Seawater Salts on Magnesium Oxide Hydration: Implications for Carbonation

The effects of individual component salts on MgO hydration and subsequent carbonation have not been systematically investigated despite the increase in utilization of seawater and other brines in the production of MgO-containing next-generation cements, fire retardants, and sorbents for CO2. Here, we present a study of MgO hydration in the presence of individual saltwater cations at a range of concentrations, as well as binary mixtures at seawater concentrations, and subsequent carbonation. We observed that the presence of the cations increased MgO dissolution rates and that the subsequent carbonation extent of the hydrated material remained constant or even increased. Since the presence of these salts during hydration does not show negative effects on subsequent carbonation in our experimental study, the application of seawater and other brines containing high concentrations of these salts to hydrate MgO in industrial processes is likely feasible.

Evans, Barbara [ORNL] (ORCID:0000000225742567)↗
DOE OSTI2024

Selective ion transport through hydrated micropores in polymer membranes

Abstract Ion-conducting polymer membranes are essential in many separation processes and electrochemical devices, including electrodialysis 1 , redox flow batteries 2 , fuel cells 3 and electrolysers 4,5 . Controlling ion transport and selectivity in these membranes largely hinges on the manipulation of pore size. Although membrane pore structures can be designed in the dry state 6 , they are redefined upon hydration owing to swelling in electrolyte solutions. Strategies to control pore hydration and a deeper understanding of pore structure evolution are vital for accurate pore size tuning. Here we report polymer membranes containing pendant groups of varying hydrophobicity, strategically positioned near charged groups to regulate their hydration capacity and pore swelling. Modulation of the hydrated micropore size (less than two nanometres) enables direct control over water and ion transport across broad length scales, as quantified by spectroscopic and computational methods. Ion selectivity improves in hydration-restrained pores created by more hydrophobic pendant groups. These highly interconnected ion transport channels, with tuned pore gate sizes, show higher ionic conductivity and orders-of-magnitude lower permeation rates of redox-active species compared with conventional membranes, enabling stable cycling of energy-dense aqueous organic redox flow batteries. This pore size tailoring approach provides a promising avenue to membranes with precisely controlled ionic and molecular transport functions.

Science & Technology - Other Topics↗
DOE OSTI2024

Pore occupancy of gas hydrate

Methane hydrate deposits are one of the largest fractions of hydrocarbons in the Earth's crust. They are found mainly in ocean sediments, and the configuration of the deposits—at the largest (kilometer) and smallest (micrometer) scales—determines how and when gaseous methane is released. Here, in this work, using thermodynamic arguments, we show how the confined spaces of the sediment allow methane hydrate to coexist with both water and gas to create a three-phase region. We find that the hydrate pore occupancy changes depending on the depth of the three-phase region, due to changes in methane density of the gas phase. We estimate the thickness of three-phase regions (hydrate, gas, and water) within ocean sediments. We further show how this directly predicts how the presence of hydrate affects the flow properties of gaseous methane and water through porous media.

flows in porous media↗
NASA NTRS2001

Initiation of Martian Outflow Channels: Related to the Dissociation of Gas Hydrate?

We propose that the disruption of subpermafrost aquifers on Mars by the thermal- or pressure-induced dissociation of methane hydrate may have been a frequent trigger for initiating outflow channel activity. This possibility is raised by recent work that suggests that significant amounts of methane and gas hydrate may have been produced within and beneath the planet's cryosphere. On Earth, the build-up of overpressured water and gas by the decomposition of hydrate deposits has been implicated in the formation of large blowout features on the ocean floor. These features display a remarkable resemblance (in both morphology and scale) to the chaotic terrain found at the source of many Martian channels. The destabilization of hydrate can generate pressures sufficient to disrupt aquifers confined by up to 5 kilometers of frozen ground, while smaller discharges may result from the water produced by the decomposition of near-surface hydrate alone.

Max, Michael D.↗
NASA NTRS1998

Chloral hydrate alters the organization of the ciliary basal apparatus and cell organelles in sea urchin embryos

The mitotic inhibitor, chloral hydrate, induces ciliary loss in the early embryo phase of Lytechinus pictus. It causes a breakdown of cilia at the junction of the cilium and the basal body known as the basal plate. This leaves the plasma membrane temporarily unsealed. The basal apparatus accessory structures, consisting of the basal body, basal foot, basal foot cap, striated side arm, and striated rootlet, are either misaligned or disintegrated by treatment with chloral hydrate. Furthermore, microtubules which are associated with the basal apparatus are disassembled. Mitochondria accumulate at the base of cilia - underneath the plasma membrane - and show alterations in their structural organization. The accumulation of mitochondria is observed in 40% of all electron micrograph sections while 60% show the areas mostly devoid of mitochondria. The microvilli surrounding a cilium and striated rootlet remain intact in the presence of chloral hydrate. These results suggest that deciliation in early sea urchin embryos by chloral hydrate is caused by combined effects on the ciliary membrane and on microtubules in the cilia. Furthermore, it is suggested that chloral hydrate can serve as a tool to explore the cytoskeletal mechanisms that are involved in cilia motility in the developing sea urchin embryo.

Non-NASA Center↗
NASA NTRS2008

Phyllosilicate and Hydrated Sulfate Deposits in Meridiani

Several phyllosilicate and hydrated sulfate deposits in Meridiani have been mapped in detail with high resolution MRO CRISM [1] data. Previous studies have documented extensive exposures of outcrop in Meridiani (fig 1), or etched terrain (ET), that has been interpreted to be sedimentary in origin [e.g., 2,3]. These deposits have been mapped at a regional scale with OMEGA data and show enhanced hydration (1.9 m absorption) in several areas [4]. However, hydrated sulfate detections were restricted to valley exposures in northern Meridiani ET [5]. New high resolution CRISM images show that hydrated sulfates are present in several spatially isolated exposures throughout the ET (fig 1). The hydrated sulfate deposits in the valley are vertically heterogeneous with layers of mono and polyhydrated sulfates and are morphologically distinct from other areas of the ET. We are currently mapping the detailed spatial distribution of sulfates and searching for distinct geochemical horizons that may be traced back to differential ground water recharge and/or evaporative loss rates. The high resolution CRISM data has allowed us to map out several phyllosilicate deposits within the fluvially dissected Noachian cratered terrain (DCT) to the south and west of the hematite-bearing plains (Ph) and ET (fig 1). In Miyamoto crater, phyllosilicates are located within ~30km of the edge of Ph, which is presumably underlain by acid sulfate deposits similar to those explored by Opportunity. The deposits within this crater may record the transition from fluvial conditions which produced and/or preserved phyllosilicates deposits to a progressively acid sulfate dominated groundwater system in which large accumulations of sulfate-rich evaporites were deposited .

Wiseman, S. M.↗
NASA NTRS2011

Improved Design and Fabrication of Hydrated-Salt Pills

A high-performance design, and fabrication and growth processes to implement the design, have been devised for encapsulating a hydrated salt in a container that both protects the salt and provides thermal conductance between the salt and the environment surrounding the container. The unitary salt/container structure is known in the art as a salt pill. In the original application of the present design and processes, the salt is, more specifically, a hydrated paramagnetic salt, for use as a refrigerant in a very-low-temperature adiabatic demagnetization refrigerator (ADR). The design and process can also be applied, with modifications, to other hydrated salts. Hydrated paramagnetic salts have long been used in ADRs because they have the desired magnetic properties at low temperatures. They also have some properties, disadvantageous for ADRs, that dictate the kind of enclosures in which they must be housed: Being hydrated, they lose water if exposed to less than 100-percent relative humidity. Because any dehydration compromises their magnetic properties, salts used in ADRs must be sealed in hermetic containers. Because they have relatively poor thermal conductivities in the temperature range of interest (<0.1 K), integral thermal buses are needed as means of efficiently transferring heat to and from the salts during refrigeration cycles. A thermal bus is typically made from a high-thermal-conductivity met al (such as copper or gold), and the salt is configured to make intimate thermal contact with the metal. Commonly in current practice (and in the present design), the thermal bus includes a matrix of wires or rods, and the salt is grown onto this matrix. The density and spacing of the conductors depend on the heat fluxes that must be accommodated during operation.

Shirron, Peter J.↗
NASA NTRSDate not supplied

Coordinated analyses of hydrated Kuiper Belt dust

We report on coordinated mineralogical, chemical, and isotopic analyses of hydrated carbon-rich interplanetary dust particles (IDPs). We focus on hydrated IDPs that contain high solar flare track densities consistent with an origin in outer Solar System bodies such as Edgeworth-Kuiper belt objects (EKBOs) [1]. We are searching for evidence of the heavy water reservoir predicted by self-shielding models [2]. The IDPs were embedded in sulfur and microtome thin sections were obtained for Fourier-transform infrared (FTIR), transmission electron microscopy (TEM), and nanoSIMS analyses. The IDPs were only partly microtomed and the remainder was extracted from the sulfur and pressed into In or Au for high precision O isotopic analyses. The hydrated IDPs in this study are compact low-porosity objects with a mineralogy dominated by fine-grained saponite and lesser serpentine, Fe-Ni sulfides, Mg-Fe carbonates, rare crystaline silicates, and abundant organic matter. The C in the IDPs is abundant (typically >4X CI) and occurs as isolated nanoglobules and finely disseminated within the phyllosilicate matrix of the IDPs. TEM analyses of the nanoglobules show O-rich, S-depleted rims with higher carbonyl functionality than their cores. FTIR spectra show strong aliphatic C-H stretches consistent with the presence of short-chain aliphatic hydrocarbons in these IDPs. The oxygen isotopic compositions measured in 6 IDPs all plot within error of the CCAM line [3]. For several of the IDPs we were able to obtain multiple analyses. The ∆^(17)O values range from -23‰ up to +3.4‰ with most analyses clustering above the terrestrial fractionation line. The O isotopic compositions and the high C contents of these IDPs are distinct from known hydrated carbonaceous chondrites. The track-rich hydrated IDPs record parent body aqueous alteration effects through interactions with 16O-poor H2O on a EKBO parent body. The aqueous alteration activity likely resulted from the heat generated by collisional processes among EKBOs given that these objects are believed to have accreted late after the decay of 26Al [4].

Lindsay P. Keller↗
NASA NTRS2022

Simulated Lunar Surface Hydration Measurements using Multispectral Lidar at 3 µm

Accurately measuring the variability of spectroscopic signatures of hydration (H2O + OH) on the illuminated lunar surface at 3 µm as a function of latitude, lunar time of day, and composition is crucial to determining the generation and destruction mechanisms of OH species and understanding the global water cycle. A prime complication in analysis of the spectroscopic feature is the accurate removal of thermal emission, which can modify or even eliminate the hydration feature depending on the data processing methods used and assumptions made. An orbital multispectral lidar, with laser illumination at key diagnostic wavelengths, would provide uniform, zero-phase geometry, complete latitude and time of day coverage from a circular polar orbit, and is agnostic to the thermal state of the surface. We have performed measurement simulations of a four-wavelength multispectral lidar using spectral mixtures of hydrated mid-ocean ridge basalt (MORB) glasses and lunar regolith endmembers to assess the lidar performance in measuring hydration signatures on the lunar surface. Our results show a feasible system with wavelengths at 1.5 µm, 2.65 µm, 2.8 µm, and 3.1 µm can measure lunar hydration with a precision of 52 ppm (1σ) or better. These results, combined with the uniform measurement capabilities of multispectral lidar make it a valuable spectroscopic technique for elucidating mechanisms of OH/H2O generation, migration, and destruction.

D. R. Cremons↗
DOE OSTI2025

The Effects of Morphology and Hydration on Anion Transport in Self-Assembled Nanoporous Membranes

Ordered nanoporous polymer membranes offer opportunities for systematically probing the mechanisms of ion transport under confinement and for realizing useful materials for electrochemical devices. Here, we examine the impact of morphology and ion hydration on the transport of hydroxide and bromide anions in nanostructured polymer membranes with 1 nm scale pores. We use aqueous lyotropic self-assembly of an amphiphilic monomer, with a polymerizable surfactant to create direct hexagonal (H I ) and gyroid mesophases. UV-induced cross-linking leads to the formation of nanoporous polymers with water continuous channels. The membranes are mechanically robust and chemically durable, resisting degradation during extended exposure to 1 M NaOH solutions. We use a combination of electrochemical impedance spectroscopy, pulsed-field gradient NMR spectroscopy, and molecular simulations to elucidate anion and water transport. The as-prepared hexagonal systems display higher conductivity and lower activation energies for both anions relative to the gyroid system. When compared at equivalent hydration, however, gyroid and hexagonal membranes show similar activation energies, with nearly identical conductivities at ambient temperatures. Both ionic conductivity and water diffusivity increase with increasing hydration. Here, the water uptake as a function of relative humidity for the hexagonal and gyroid mesophases ultimately dictates the water diffusion and magnitude of the ionic conductivity, with the hexagonal system showing overall higher capacity for hydration and thus faster ion transport. The durability of these materials under aggressive alkaline conditions and their relatively high hydroxide ion conductivity suggest that these nanostructured polymers could be of interest as membranes for alkaline fuel cells.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗