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At least 559 records · Page 31
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Understanding (La,Sr)(Co,Fe)O$_{3-δ}$ Phase Instability within SOECs Using a Combined Experimental and Atomistic Modeling Approach

Understanding the onset of degradation in the air electrode within solid oxide electrolysis cells (SOECs), and the subsequent impact on cell performance, is a critical step in mitigating the performance losses and stability issues of SOECs. In an effort to identify early onset degradation phenomena, SOECs were characterized as fabricated and after testing potentiostatically at 1.3 V for 1000 h at 750 °C. SOEC air electrodes composed of a 1:1 composite of La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3–δ (6428-LSCF) and Gd 0.1 Ce 0.9 O 1.95 (GDC) were studied using synchrotron X-ray diffraction (XRD), scanning transmission electron microscopy coupled with energy dispersive X-ray spectroscopy (STEM-EDS), and X-ray absorption near-edge spectroscopy (XANES) to evaluate the changes in the air electrode structurally and chemically. These techniques show the migration of Sr species from the air electrode through pores in the GDC barrier layer, progressing to the electrolyte boundary, where it accumulates and reacts with (Zr 0.84 Y 0.16 )O 2–δ (YSZ) to form SrZrO 3 . Microscopy results are paired with atomistic simulations to better understand the relationship between the thermodynamic instability of 6428-LSCF and cell fabrication/testing conditions. First-principles calculations reveal that LSCF-6428 is not stable during cell manufacturing and testing conditions, which supports the experimental identification of secondary phases in both as-fabricated and tested cells. Together, these results demonstrate that the challenging environments encountered by SOECs during cell manufacturing and operation lead to instabilities of the target 6428-LSCF anode material and underscore the need for more durable, high-performing SOEC components.

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

Quantifying Graphite Solid-Electrolyte Interphase Chemistry and its Impact on Fast Charging

The solid-electrolyte interphase (SEI) enables the remarkable capacity retention of lithium-ion batteries, yet a comprehensive quantitative description of the SEI composition remains elusive. Using a combination of differential electrochemical mass spectrometry and mass spectrometry titration, we quantify graphite SEI components formed under electrolytes of varying salt concentrations. We find that, regardless of salt concentration, a conversion of initially deposited lithium ethylene dicarbonate to monocarbonates (likely lithium ethylene monocarbonate) and noncarbonate species occurs, and the extent of this conversion increases with electrolyte aging. Here, we additionally demonstrate that as the concentration increases (up to 2.0 M LiPF6), the SEI becomes progressively thinner with more LiF and less solid carbonates deposited. Finally, we reveal that less dead lithium formation and less solid carbonate deposition occur during prolonged fast charging for higher-concentration electrolytes. Because of the advantages imparted by a thinner SEI, the onset state of charge for lithium plating for the 2.0 M electrolyte is later than that predicted by a standard electrochemical model, underscoring the importance of explicit SEI effects in future electrochemical models.

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

Effects of fluorinated solvents on electrolyte solvation structures and electrode/electrolyte interphases for lithium metal batteries

Electrolyte is very critical to the performance of the high-voltage lithium (Li) metal battery (LMB), which is one of the most attractive candidates for the next generation high-density energy storage systems. Electrolyte formulation and structure determine the physical properties of the electrolytes and their interfacial chemistries on the electrode surfaces. Localized high-concentration electrolytes (LHCEs) outperform state-of-the-art carbonate electrolytes in many aspects in LMBs due to their unique solvation structure. Types of fluorinated co-solvents used in LHCEs are investigated here in searching for the most suitable diluent for high concentration electrolytes (HCEs). Non-solvating solvents (including fluorinated ethers, fluorinated borate and fluorinated orthoformate) added in HCEs enable the formation of LHCEs with high-concentration solvation structures. However, low solvating fluorinated carbonate will coordinate with Li+ ions and form a second solvation shell or a pseudo-LHCE which diminishes the benefits of LHCE. In addition, it is evident that the diluent has significant influence on the electrode/electrolyte interphases (EEIs) beyond retaining the high-concentration solvation structures. Diluent molecules surrounding the high-concentration clusters could accelerate or decelerate the anion decomposition through co-participation of diluent decomposition in the EEI formation. The varied interphase features lead to significantly different battery-performance. This study points out the importance of diluents and their synergetic effects with the conductive salt and the solvating solvent in designing LHCEs. These systematic comparisons and fundamental insights into LHCEs using different types of fluorinated solvents can guide further development of advanced electrolytes for high-voltage LMBs.

Cao, Xia↗
DOE OSTI2021

Stoichiometric irreversibility of aged garnet electrolytes

Solid-state lithium batteries (SSLBs) have been regarded as one of the next-generation energy storage systems. With the adoption of solid-state electrolytes (SSEs) and lithium metal anodes, SSLBs enable higher energy density and more reliable safety than the state-of-the-art lithium-ion batteries. Among potential SSEs, the cation-doped Li 7 La 3 Zr 2 O 12 (LLZO) is promising for its high ionic conductivity (~10 –3 S cm –2 ) at room temperature and high stability with Li metal anode. However, the storage of doped LLZO in the ambient condition suffers the aging effect, including the structural transition (i.e. low-temperature cubic form) and the stoichiometric changes (i.e. Li 2 CO 3 ). These changes are detrimental to LLZO ionic conductivity and interfacial stability in SSLBs. To this end, in this study we are motivated to investigate the structural and stoichiometric reversibility of aged LLZO during thermal treatment. With the help of an in-situ synchrotron-based high-energy X-ray diffraction technique, our experiments revealed that the LLZO powders became a low-temperature cubic phase when exposed to the ambient condition for an extended period of time. A high temperature cubic form can be restored after a thermal treatment of the aged LLZO powder, regardless of the type of dopant. However, the restoration of the stoichiometry remained a challenge, and the degree of the restoration showed a clear dependence on the dopant chemistry.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Tailoring Ion Transport in Li 3‐3y Ho 1+y Cl 6‐x Br x via Transition‐Metal Free Structural Planes and Charge Carrier Distribution

Abstract Localized atomistic disorder in halide‐based solid electrolytes (SEs) can be leveraged to boost Li + mobility. In this study, Li + transport in structurally modified Li 3 HoCl 6 , via Br − introduction and Li + deficiency, is explored. The optimized Li 3‐3 y Ho 1+ y Cl 6‐ x Br x achieves an ionic conductivity of 3.8 mS cm −1 at 25 °C, the highest reported for holmium halide materials. 6,7 Li nuclear magnetic resonance and relaxometry investigations unveil enhanced ion dynamics with bromination, attaining a Li + motional rate neighboring 116 MHz. X‐ray diffraction analyses reveal mixed‐anion‐induced phase transitions with disproportionate octahedral expansions and distortions, creating Ho‐free planes with favorable energetics for Li + migration. Bond valence site energy analysis highlights preferred Li + transport pathways, particularly in structural planes devoid of Ho 3+ blocking effects. Molecular dynamics simulations corroborate enhanced Li + diffusion with Br − introduction into Li 3 HoCl 6 . Li‐Ho electrostatic repulsions in the (001) plane presumably drive Li + diffusion into the Ho‐free (002) layer, enabling rapid intraplanar Li + motion and exchange between the 2d and 4h sites. Li 3‐3 y Ho 1+ y Cl 6‐ x Br x also demonstrates good battery cycling stability. These findings offer valuable insights into the intricate correlations between structure and ion transport and will help guide the design of high‐performance fast ion conductors for all‐solid‐state batteries.

Chemistry↗
DOE OSTI2025

Developing Lanthanide-Nitrate Cluster Chemistry toward Rare Earth Separations

Nitrate-decorated hexamers with a [Ln 6 (μ 6 -O)(μ 3 –OH) 8 ] 8+ core have been reported for nearly every lanthanide ion and are used as precursors for the assembly of functional metal–organic frameworks. Yet, few studies have examined the correlation between the solution and solid-state species, and the formation of mixed-metal clusters. Toward this end, a series of homo- and heterometal lanthanide nitrate hexamers was prepared via pH adjustment of aqueous lanthanide nitrate solutions. Examination of the homometallic europium solutions using Small Angle X-ray Scattering and nESI-MS showed that lower order complexes dominate lanthanide speciation in nitrate media. Yet, powder X-ray diffraction data of the precipitated phase confirmed the formation of [Ln 6 (μ 6 -O)(μ 3 -OH) 8 (NO 3 ) 6 (H 2 O) 12 ]·2(NO 3 )·n(H 2 O), Ln 6 , for Ln = Eu and Tb. For heterometal systems, analysis of the solid-state product by ICP–MS showed the selective incorporation of the heavier rare earths into Ln 6 . Selectivity was quantified by calculating an average separation factor, which is defined as the ratio of recovery factors of both metals. Further examination of the luminescence behavior of mixed metal [Tb 6–x Eu x (μ 6 -O)(μ 3 -OH) 8 (NO 3 ) 6 (H 2 O) 12 ]·2(NO 3 )·n(H 2 O), with x = 1.1–3.6, showed that the relative intensities of the peaks at 489 nm (terbium, 5 D 4 → 7 F 6 ) and 690 nm (europium, 5 D 0 → 7 F 4 ) trend with the percent incorporation of europium and terbium into the cluster.

anions↗
DOE OSTI2025

Time-resolved electrical potential pump – X-ray photoelectron spectroscopy probe developments for investigating dynamic processes occurring at electrochemical interfaces

Electrode–electrolyte interfaces are of critical importance in several fields, including renewable energy, corrosion, and environmental chemistry. However, investigating these interfaces under operational conditions poses considerable challenges due to the limitations of the instrumentation employed. While recent advancements in in situ and operando techniques have enhanced our comprehension of the steady-state properties of solid-liquid interfaces, the dynamic behaviors of these systems remain inadequately explored. This study introduces a time-resolved X-ray photoelectron spectroscopy (XPS) technique designed to capture transient reaction intermediates and charging dynamics at electrified interfaces. The presented proof-of-principle study demonstrates that electrochemical processes, represented by an equivalent electrical circuit (EEC) model, can be probed and understood using square wave voltage pulses of a potentiostat synchronized to the modified data acquisition of an XPS setup. This method offers a valuable alternative to traditional pump–probe techniques, facilitating the investigation of a broader range of electrochemical systems. A dedicated software package for analyzing time- and energy-resolved XPS with a focus on extracting parameters of the EEC is geared towards benchmarking different EECs in future real-world electrochemical experiments.

Electrochemistry↗
DOE OSTI2023

CHGNet as a pretrained universal neural network potential for charge-informed atomistic modelling

Large-scale simulations with complex electron interactions remain one of the greatest challenges for atomistic modelling. Although classical force fields often fail to describe the coupling between electronic states and ionic rearrangements, the more accurate ab initio molecular dynamics suffers from computational complexity that prevents long-time and large-scale simulations, which are essential to study technologically relevant phenomena. Here we present the Crystal Hamiltonian Graph Neural Network (CHGNet), a graph neural network-based machine-learning interatomic potential (MLIP) that models the universal potential energy surface. CHGNet is pretrained on the energies, forces, stresses and magnetic moments from the Materials Project Trajectory Dataset, which consists of over 10 years of density functional theory calculations of more than 1.5 million inorganic structures. The explicit inclusion of magnetic moments enables CHGNet to learn and accurately represent the orbital occupancy of electrons, enhancing its capability to describe both atomic and electronic degrees of freedom. We demonstrate several applications of CHGNet in solid-state materials, including charge-informed molecular dynamics in Li x MnO 2 , the finite temperature phase diagram for Li x FePO 4 and Li diffusion in garnet conductors. We highlight the significance of charge information for capturing appropriate chemistry and provide insights into ionic systems with additional electronic degrees of freedom that cannot be observed by previous MLIPs.

36 MATERIALS SCIENCE↗
NASA NTRS2006

Following the Water: the Evolution of Ice-forming Regions in the Early Solar Nebula

The abundances of water-vapor and water-ice during the first ten million years of the protoplanetary solar nebula are simulated using a new condensation/sublimation model. This study builds on a "snow line" model reported in ApJ 627 L153 (2005); it uses a simple phenomenological model where water vapor molecules evolve from solar atomic abundance and eventually condenses to ice at colder points in the nebula once the water-vapor partial pressure exceeds a value determined by the phase diagram for water. The synthesis of water vapor from elementary species is modeled with a chemical network consisting of about 400 species and 4000 reactions. The evolution of the icy zone (and its relative abundance of solid ice) is traced from a limited region in the early hotter disk to its final state at the time when the gas is expelled and a planetary system begins to form. Possible effects of this dynamic motion on disk chemistry and organic molecule formation are also described.

Davis, Sanford S.↗
DOE OSTI2021

Computation-guided discovery of coating materials to stabilize the interface between lithium garnet solid electrolyte and high-energy cathodes for all-solid-state lithium batteries

All-solid-state batteries with a lithium metal anode, enabled by lithium garnet solid electrolytes such as Li 7 La 3 Zr 2 O 12 (LLZO), are a promising next-generation energy-storage technology. The further development of all-solid-state battery requires the integration of high-energy cathodes such as LiNi 1-x-y Mn x Co y O 2 (NMC) with the garnet solid electrolyte with stable and low-resistance interfaces, which requires a coating layer to stabilize the interface during high-temperature sintering and electrochemical cycling. In order to guide the future development of interfacial coatings, we perform high-throughput thermodynamic analyses based on first-principles computation to investigate the stability of LLZO garnet and high-energy NMC cathodes with a wide range of materials chemistries. Here our study reveals the factors governing the materials stability with LLZO garnet and NMC cathodes, and identifies the mechanisms of good coating layers stable with LLZO and NMC. In addition to classifying known coating layers, our study provides detailed guiding charts and multiple new materials systems as promising coatings for stabilizing LLZO—NMC interfaces to enable high-energy-density garnet-based all-solid-state batteries. Our demonstrated computation scheme and high-throughput analyses are generally applicable to investigate and screen coating materials for stabilizing interfaces in energy-related applications.

25 ENERGY STORAGE↗
DOE OSTI2024

Actinium chelation and crystallization in a macromolecular scaffold

Abstract Targeted alpha therapy (TAT) pairs the specificity of antigen targeting with the lethality of alpha particles to eradicate cancerous cells. Actinium-225 [ 225 Ac; t 1/2 = 9.920(3) days] is an alpha-emitting radioisotope driving the next generation of TAT radiopharmaceuticals. Despite promising clinical results, a fundamental understanding of Ac coordination chemistry lags behind the rest of the Periodic Table due to its limited availability, lack of stable isotopes, and inadequate systems poised to probe the chemical behavior of this radionuclide. In this work, we demonstrate a platform that combines an 8-coordinate synthetic ligand and a mammalian protein to characterize the solution and solid-state behavior of the longest-lived Ac isotope, 227 Ac [t 1/2 = 21.772(3) years]. We expect these results to direct renewed efforts for 225 Ac-TAT development, aid in understanding Ac coordination behavior relative to other +3 lanthanides and actinides, and more broadly inform this element’s position on the Periodic Table.

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

ThO 2 and Th 1– x U x O 2 Nanoscale Materials and Thin Films for Nuclear Science Applications

This study investigates the dynamics and mechanisms of solution combustion synthesis (SCS) for the preparation of nanoscale ThO 2 and Th 1–x U x O 2 materials, utilizing metal nitrates (Th(NO 3 ) 4 and UO 2 (NO 3 ) 2 ) and acetylacetone (C 5 H 8 O 2 ) as reactants dissolved in a 2-methoxyethanol (C 3 H 8 O 2 ) solvent. By combining thermodynamic calculations, dynamic time–temperature profile measurements with differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), this research reveals how variations in acetylacetone concentration and uranium content influence the structural parameters of the synthesized oxides. The time–temperature measurements show that the heating rate and maximum combustion temperatures are sensitive to acetylacetone concentration. DSC-TGA results indicate shifts in exothermic peak temperatures as the uranium content changes. The complexation between thorium and acetylacetone emerges as a critical factor, impacting combustion parameters and the structural characteristics of the final products. The uniform distribution of Th and U in the Th 1–x U x O 2 solid solution and the formation of nanoscale particles with strained crystallites are considered essential for the low-temperature densification of these materials for nuclear fuel pellet applications. Additionally, high-quality ThO 2 and Th 1–x U x O 2 thin (100–150 nm) films are successfully synthesized via electrospray deposition of combustible solutions followed by a brief period of heat treatment. Furthermore, these films exhibit excellent structural and morphological uniformity, making them ideal candidates for nuclear measurements, irradiation damage studies, and investigations into the physical properties of both pure and mixed oxides.

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

Carbon Dioxide Capture Chemistry of Amino Acid Functionalized Metal-Organic Frameworks in Humid Flue Gas

Here, metal-organic framework-808 has been functionalized with 11 amino acids (AA) to produce a series of MOF-808-AA structures. The adsorption of CO 2 under flue gas conditions revealed that glycine- and DL-lysine-functionalized MOF-808 (MOF-808-Gly and -DL-Lys) have the highest uptake capacities. Enhanced CO 2 capture performance in the presence of water was observed and studied using single-component sorption isotherms, CO 2 /H 2 O binary isotherm, and dynamic breakthrough measurements. The key to the favorable performance was uncovered by deciphering the mechanism of CO 2 capture in the pores and attributed to the formation of bicarbonate as evidenced by 13 C and 15 N solid-state nuclear magnetic resonance spectroscopy studies. Based on these results, we examined the performance of MOF-808-Gly in simulated coal flue gas conditions and found that it is possible to capture and release CO 2 by vacuum swing adsorption. MOF-808-Gly was cycled at least 80 times with full retention of performance. This study significantly advances our understanding of CO 2 chemistry in MOFs by revealing how strongly bound amine moieties to the MOF backbone create the chemistry and environment within the pores, leading to the binding and release of CO 2 under mild conditions without application of heat.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2022

Structure of diopside, enstatite, and magnesium aluminosilicate glasses: A joint approach using neutron and x-ray diffraction and solid-state NMR

Neutron diffraction with magnesium isotope substitution, high energy x-ray diffraction, and 29 Si, 27 Al, and 25 Mg solid-state nuclear magnetic resonance (NMR) spectroscopy were used to measure the structure of glassy diopside (CaMgSi 2 O 6 ), enstatite (MgSiO 3 ), and four (MgO) x (Al 2 O 3 ) y (SiO 2 ) 1–x–y glasses, with x = 0.375 or 0.25 along the 50 mol. % silica tie-line (1 – x – y = 0.5) or with x = 0.3 or 0.2 along the 60 mol. % silica tie-line (1 – x – y = 0.6). The bound coherent neutron scattering length of the isotope 25 Mg was remeasured, and the value of 3.720(12) fm was obtained from a Rietveld refinement of the powder diffraction patterns measured for crystalline 25 MgO. The diffraction results for the glasses show a broad asymmetric distribution of Mg–O nearest-neighbors with a coordination number of 4.40(4) and 4.46(4) for the diopside and enstatite glasses, respectively. As magnesia is replaced by alumina along a tie-line with 50 or 60 mol. % silica, the Mg–O coordination number increases with the weighted bond distance as less Mg 2+ ions adopt a network-modifying role and more of these ions adopt a predominantly charge-compensating role. 25 Mg magic angle spinning (MAS) NMR results could not resolve the different coordination environments of Mg 2+ under the employed field strength (14.1 T) and spinning rate (20 kHz). The results emphasize the power of neutron diffraction with isotope substitution to provide unambiguous site-specific information on the coordination environment of magnesium in disordered materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Synthesis and Characterization of Tris(oxazolinyl)borato Copper(II) and Copper(I) Complexes

The reaction of To M Tl (To M =tris(4,4-dimethyl-2-oxazolinyl)phenylborate) and CuBr 2 in benzene at 60 °C provides To M CuBr (1) as an entry-point into tris(oxazolinyl)phenylborato copper chemistry. In this work, To M CuO t Bu (2) and To M CuOAc (3) are prepared by the reactions of To M CuBr with KO t Bu and NaOAc, respectively. To M CuO t Bu is transformed into (To M CuOH) 2 (4) through hydrolysis. NMR, FT-IR, and EPR spectroscopies are used to determine the electronic and structural properties of these copper(II) compounds, and the solid-state structures were characterized by X-ray crystallography. Reduction of copper is observed upon treatment of To M CuO t Bu with phenylsilane in an attempt to synthesize monomeric copper(II) hydride. To M Cu (5) and To M 2 Cu (6) were independently synthesized and characterized for comparison.

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

Li 3– x Zr x (Ho/Lu) 1– x Cl 6 Solid Electrolytes Enable Ultrahigh-Loading Solid-State Batteries with a Prelithiated Si Anode

We report two new families of lithium metal chloride solid electrolytes Li 3–x Zr x (M) 1–x Cl 6 (0 ≤ x ≤ 0.8; M = Ho or Lu) with ionic conductivities of up to 1.8 mS cm –1 and a low activation energy of 0.34 eV. Structural elucidation via high-resolution neutron diffraction determines the Li ion distribution in trigonal Li 3 HoCl 6 , orthorhombic-I Li 3 LuCl 6 , and orthorhombic-II Li 2.4 Zr 0.6 (Ho/Lu) 0.4 Cl 6 . The last compound exhibits well-connected Li-ion pathways and abundant Li-ion carriers/vacancies to promote diffusion. All-solid-state batteries with Li 2.6 Zr 0.4 (Ho/Lu) 0.6 Cl 6 solid electrolytes and NCM85 cathodes exhibit stable cycling up to 4.6 V vs Li + /Li, which is even preserved up to 4.8 V. Stable cathode interphases are formed for both electrolytes upon cycling to 4.3, 4.6, and 4.8 V cutoff potentials, as identified by a ToF-SIMS analysis. Solid-state cells with a prelithiated Li 0.7 Si anode exhibit a significantly increased initial coulombic efficiency of 94.5% compared to Si and a high areal capacity of up to 16.3 mAh·cm –2 .

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

First Principles Modeling of Cluster-Based Solid Electrolytes (Final Technical Report)

Given the trend of global warming and the urgent need to transition from fossil fuels to green energy, lithium-ion batteries continue to be an integral part of our lives. Design, development, and understanding of novel solid-state electrolyte materials play the key role for achieving next-generation all-solid-state batteries with high energy and great safety. The current modeling schemes to develop advanced solid electrolytes are focusing on materials in which the building blocks are individual atoms. Our theoretical approach is a paradigm shift in solid-state electrolyte design. Instead of atoms, we focus on clusters as the building blocks and model these solid electrolytes and their interfaces with electrodes, especially Li-metal anode, for their successful implementation in solid-state batteries. The advantage of using the cluster ions to replace elemental ions is that the size, composition, and shape of the former can be tailored to achieve higher ionic conductivity at room temperature, electrochemical stability, and charge transfer across solid-solid interfaces than conventional materials. Specifically, the project includes: (1) Developing cluster-based solid electrolytes, where the halogen components are replaced by cluster ions that mimic the chemistry of halogens but are characterized by additional degrees of freedom, including the size, shape, composition, and motional dynamics under excitation. (2) Providing a fundamental understanding of the ion conduction mechanism in the developed cluster-based solid electrolytes; (3) Modeling the interfacial properties (i.e., structural, chemical, and transport properties) between the cluster-based solid electrolytes and electrodes at the atomic level. For the cluster-based solid electrolytes incompatible with the Li-metal anode or cathode materials, potential candidates for interfacial coatings are identified and studied. (4) Providing a theoretical framework towards optimizing critical parameters of the solid-state electrolytes that guides experimentalists to attain desired cathode-electrode interface for cluster-based solid-state electrolytes.

25 ENERGY STORAGE↗