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DOE OSTI2022

NaCo 2 (SeO 3 ) 2 (OH): competing magnetic ground states of a new sawtooth structure with 3d 7 Co 2+ ions

While certain magnetic sublattices have long been known theoretically to give rise to emergent physics via competing magnetic interactions and quantum effects, finding such configurations in real materials is often deeply challenging. Here we report the synthesis and characterization of a new such material, NaCo 2 (SeO 3 ) 2 (OH) which crystallizes with a highly frustrated sublattice of sawtooth Co 2+ chains. Single crystals of NaCo 2 (SeO 3 ) 2 (OH) were synthesized using a low-temperature hydrothermal method. X-ray single crystal structure analysis reveals that the material crystallizes in orthorhombic space group of Pnma (no. 62). Its crystal structure exhibits one-dimensional chains of corner-sharing isosceles triangles that are made of two crystallographically distinct 3d 7 Co 2+ sites (Co(1) and Co(2)). The chains run along the b-axis and are interconnected via [SeO 3 ] groups to form a three-dimensional structure mediating super-exchange interactions. The temperature dependent magnetization data show a ferromagnetic-like (FM) transition at 11 K (T 1 ) followed by an antiferromagnetic (AFM) transition at about 6 K (T 2 ). Neutron-powder diffraction measurements reveal that at T 1 = 11 K only the Co(2) site orders magnetically, forming ferromagnetic zigzag chains along the b-axis. Below T 2 = 6 K, both Co(1) and Co(2) sites order in a nearly orthogonal configuration, with Co(1) moments lying inside the plane of the sawtooth chain while Co(2) moments cant out of the plane. The canting of the magnetic moments leads to a net ferromagnetic component along b-axis, parallel to the chain direction. The ordered moments are fully compensated in the ac-plane. Inelastic neutron scattering measurements reveal crystal field excitations that are consistent with the presence of a spin–orbital entangled pseudo-spin state J eff = 1/2 for the Co 2+ ions. Low-energy spin-wave excitations are observed below the second magnetic transition. The analysis of powder excitation spectrum suggests complex exchange interactions that go beyond a Heisenberg Hamiltonian model with nearest neighbor couplings. Our results demonstrate the richness of the magnetic properties of sawtooth-type structures and encourage the study of similar structures with different oxyanion groups.

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

Single atoms and small clusters of atoms may accompany Au and Pd dendrimer-encapsulated nanoparticles

Here we report the presence of small clusters of atoms (<1 nm) (SCs) and single atoms (SAs) in solutions containing 1–2 nm dendrimer-encapsulated nanoparticles (DENs). Au and Pd DENs were imaged using aberration-corrected scanning transmission electron microscopy (ac-STEM), and energy dispersive spectroscopy (EDS) was used to identify and quantify the SAs/SCs. Two main findings have emerged from this work. First, the presence or absence of SAs/SCs depends on both the terminal functional group of the dendrimer (–NH 2 or –OH) and the elemental composition of the DENs (Au or Pd). Second, dialysis can be used to remove the majority of SAs/SCs in cases where a high density of SAs/SCs are present. The foregoing conclusions provide insights into the mechanisms for Au and Pd DEN synthesis and stability. Ultimately, these results demonstrate the need for careful characterization of systems containing nanoparticles to ensure that SAs/SCs, which may be below the detection limit of most analytical methods, are taken into consideration (especially for catalysis experiments).

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2022

Customized metallodielectric colloids and their behavior in dielectrophoretic fields

A synthetic strategy for fabricating colloidal particles with spatially segregated amine-functionalized lobes enables regioselective coating with gold to afford metallodielectric particles with a variety of shapes and lobe sizes. This approach can produce either dissymmetric dumbbell-shaped two-lobed Au-TPM particles (Au-T) or dissymmetric or symmetric three-lobed particles with gold coating on one (Au-T-T and T-Au-T) or two lobes (Au-T-Au). Dielectrophoretic (DEP) forces exerted by an AC field confined between two opposing electrodes generate aggregates ranging from 1D chains to 2D close-packed lattices, depending on the particle shape and lobe arrangement. Furthermore, the aggregate structures reflect the lowest energy configurations resulting from the induced dipole moments created in particle lobes within the confined electric field.

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

Ionic Peltier effect in Li-ion electrolytes

The coupled transport of charge and heat provide fundamental insights into the microscopic thermodynamics and kinetics of materials. We describe a sensitive ac differential resistance bridge that enables measurements of the temperature difference on two sides of a coin cell with a resolution of better than 10 μK. We use this temperature difference metrology to determine the ionic Peltier coefficients of symmetric Li-ion electrochemical cells as a function of Li salt concentration, solvent composition, electrode material, and temperature. The Peltier coefficients Π are negative, i.e., heat flows in the direction opposite to the drift of Li ions in the applied electric field, large, –Π > 30 kJ mol –1 , and increase with increasing temperature at T > 300 K. The Peltier coefficient is approximately constant on time scales that span the characteristic time for mass diffusion across the thickness of the electrolyte, suggesting that heat of transport plays a minor role in comparison to the changes in partial molar entropy of Li at the interface between the electrode and electrolyte. Here, our work demonstrates a new platform for studying the non-equilibrium thermodynamics of electrochemical cells and provides a window into the transport properties of electrochemical materials through measurements of temperature differences and heat currents that complement traditional measurements of voltages and charge currents.

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

Luminescent and magnetic [TbEu] 2D metal–organic frameworks

Here, we present the synthesis, through a simple, microwave-assisted method, of lanthanoid-based 2D metal–organic frameworks (MOFs) of general formula [Ln x Ln' 1–x (MeCOO)(PhCOO) 2 ], including homonuclear compounds (x = 1), Ln$=$Eu, Tb, and heterometallic compounds, [TbEu]. The crystalline material is formed by neutral nanosheets held together by van der Waals interactions, which can be easily exfoliated by sonication. Photoluminescent emission in the visible range was observed for all of the synthesized 2D MOF compounds via excitation of the ligand, showing benzoates are efficient antenna ligands. Efficient energy transfer from Tb → Eu was observed in the heterometallic [TbEu] compounds, which could potentially perform as luminescent thermometers. Inks containing nanosheets of 2D MOFs exfoliated in solution were prepared, and luminescent prints of Tb and Eu 2D MOFs on paper were made to show the possible application for anticounterfeiting. Frequency-dependent ac susceptibility results show the occurrence of slow magnetic relaxation in [TbEu] compounds through direct relaxation mechanisms, affected by bottleneck effect. A slowing down of the relaxation time is observed as the Eu/Tb ratio increases.

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

Tungsten-dioxo single-site heterogeneous catalyst on carbon: synthesis, structure, and catalysis

This study investigates the application of a novel third-row metal, tungsten, to carbon-supported single-site metal-oxo heterogeneous catalysis. Tungsten is a green and earth-abundant metal, but an unexplored candidate in this role. The carbon (AC = activated carbon)-supported tungsten dioxo complex, AC/WO 2 was prepared via grafting of (DME)WO 2 Cl 2 (DME = 1,2-dimethoxyethane) onto high-surface-area activated carbon. AC/WO 2 was fully characterized by ICP-OES, XPS, EXAFS, XANES, SMART-EM, and DFT. W 4d 7/2 XPS and W L III -Edge XANES assign the oxidation state as W(VI), while EXAFS reveals two W=O double and two W–O single bonds at distances of 1.73 and 1.92 Å, respectively. These data align well with DFT computational results, supporting the structure as Carbon(–μ-O–) 2 M(=O) 2 . SMART-EM verifies that single W(VI) catalytic sites are bonded in an out-of-plane manner. The catalytic performance of air- and water-stable AC/WO 2 is compared to that of AC/MoO 2 . AC/WO 2 is more active and selective than the molybdenum analog in mediating alcohol dehydration of various substrates, and is recyclable. Notably, AC/WO 2 is an effective and recyclable catalyst for primary aliphatic alcohol dehydration and forms no dehydrogenation side products in contrast to AC/MoO 2 . However, AC/WO 2 is less effective in epoxidation and PET depolymerization. Overall, this work demonstrates the potential of carbon-supported third row metals for future studies.

02 PETROLEUM↗
DOE OSTI2025

Thermodynamically leveraged solventless aerobic deconstruction of polyethylene-terephthalate plastics over a single-site molybdenum-dioxo catalyst

Here, we describe the solventless catalytic deconstruction of polyethylene-terephthalate (PET) under an aerobic atmosphere, mediated by an earth-abundant, low-cost activated carbon (AC)-supported single-site molybdenum-dioxo catalyst (AC/MoO 2 ). Catalytic amounts of AC/MoO 2 selectively convert waste PET into its monomer, terephthalic acid (TPA), within 4 h at 265 °C with yields as high as 94% under 1 atm air. Pure crystalline TPA product sublimes from the reaction hot zone, crystallizing on the reactor cold zone, thus avoiding the need for separation and purification steps. This process does not employ any hazardous/toxic reducing agents or solvents, and the catalyst can be recycled multiple times without loss of activity, rendering this process highly atom-efficient. According to computational and experimental mechanistic studies, the AC/MoO 2 catalyst mediates a thermoneutral metal-catalyzed β-scission step, followed by an exothermic step that converts the vinyl benzoate intermediate to TPA and acetaldehyde using trace amounts of moisture in the air. The formation of gaseous acetaldehyde makes the isolation of TPA from the reaction mixture facile and industrially favorable, especially since solvents are unnecessary. The present methodology is also extended to the deconstruction of other frequently used polyester plastics, polybutylene terephthalate (PBT), polyethylene naphthalate (PEN), and polyethylene furanoate (PEF), and operates equally well with post-consumer waste products. Notably, this process is also compatible with plastic mixtures of polyesters with polyolefins, polyamides, and polycarbonates, leading to the selective conversion of each polyester to the corresponding monomer, leaving the residual polymer unchanged and polyester-free.

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

HunStat2 – a simple and low-cost potentiostat with electrochemical impedance spectroscopy capability

We have developed a low-cost (30 USD), simple do-it-yourself (DIY) potentiostat with cyclic voltammetry (CV), open circuit potential (OCP) and electrochemical impedance spectroscopy (EIS) capability. The HunStat2 potentiostat is based on Analog Devices' AD5941 Analog Front End chip, which significantly simplifies the construction of potentiostats for both direct and alternating current (DC and AC, respectively) techniques. Interested readers are provided with circuit diagrams and a bill of materials to build the potentiostat on their own. In addition, control software is also provided free of charge. The software enables acquisition and visualization of data. In summary, HunStat2 introduces a simple and low-cost DIY potentiostat recommended for both analytical and educational purposes.

Vamos, Istvan [Lajos Petrik Vocational Chemistry S↗
DOE OSTI2025

Advanced spectroscopic studies of (PPh 4 ) 2 [Co(N 3 ) 4 ], a field-induced single-ion magnet

The high-spin Co II complex (PPh 4 ) 2 [Co(N 3 ) 4 ] (Co-N 3 )has been investigated using advanced spectroscopic techniques [far-IR magneto-spectroscopy (FIRMS), high-frequency and high-field EPR (HFEPR), and inelastic neutron scattering (INS)] to study its zero-field-splitting (ZFS), giving spin-Hamiltonian (SH) parameters. The analysis of multi-frequency HFEPR reveals the easy-axis anisotropy with a D value of −10.39(5) cm −1 and a rhombic ratio (E/D) of 0.21(1). The magnetic properties have also been probed by direct-current (DC) magnetometry, suggesting minor differences in anisotropy from the previously reported polymorph (Co-N 3 ′). Ligand-field theory (LFT) analysis indicates that the structures of Co-N 3 and Co-N 3 ′ are closer to D 2d symmetry than other symmetries considered. Alternate-current (AC) susceptibility reveals slow magnetic relaxation under an applied field, indicating that Co-N 3 is a field-induced single-ion magnet (SIM). Here, while both Co-N 3 and Co-N 3 ′ were studied by DC magnetometry, one unusual aspect of the current work on Co-N 3 is that advanced spectroscopies HFEPR, FIRMS, and INS were used to directly observe transitions between ZFS split states, giving accurate SH parameters.

Hand, Adam T. [Univ. of Tennessee, Knoxville, TN (↗
DOE OSTI2026

A new layered kagome strip structure Na 2 Co 3 (AsO 4 ) 2 (OH) 2 : static and dynamic magnetic properties

One-dimensional kagome strip chains share much of the same frustrated structural motif as two-dimensional kagome antiferromagnets, making them valuable for deepening our understanding of kagome lattice magnetism. In this paper, we report the hydrothermal synthesis and detailed structural and property characterization of Na 2 Co 3 (AsO 4 ) 2 (OH) 2 , a striped kagome system. The crystal structure was characterized using single crystal X-ray diffraction which reveals that Na 2 Co 3 (AsO 4 ) 2 (OH) 2 crystallizes in monoclinic crystal system C2/m. The structure features a one-dimensional kagome strip lattice built from Co 2+ ions and undergoes an antiferromagnetic transition at T N = 14 K. The magnetic ground state at zero field was characterized using neutron powder diffraction. Below the magnetic transition, Na 2 Co 3 (AsO 4 ) 2 (OH) 2 orders into an antiferromagnetic structure with a k-vector (0.5, 0.5, 0.5). In the proposed model, the Co1 moment is predominantly confined to the ac-plane while the Co2 moment is primarily aligned along the b-axis. Two flat bands were observed in the inelastic neutron spectra below the magnetic transition, 5 and 10 meV. Inelastic neutron spectra were modeled with a Heisenberg Hamiltonian including three nearest-neighbor exchange interactions (J 1 , J 2 , J 3 ) and strong single-ion anisotropy to stabilize the observed magnetic structure. Our study highlights the complexity of Co 2+ -based kagome strip magnetic lattice compound Na 2 Co 3 (AsO 4 ) 2 (OH) 2 which provides an excellent platform to broaden our understanding of the frustrated kagome magnetic lattice space.

Liurukara, Duminda S. [Oak Ridge National Laborato↗
DOE OSTI2026

Revealing short- and long-range Li-ion diffusion in Li 2 MnO 3 from finite-temperature dynamical mean field theory

Li 2 MnO 3 is a key component of Li-excess layered cathodes of the form (1 − x), LiMO 2 + x, Li 2 MnO 3 (M = Mn, Ni, Co, …), yet its role in setting Li-ion transport limitations remains under debate. Here, in this study, we combine DFT+U, finite-temperature DFT+DMFT with a continuous-time quantum Monte Carlo impurity solver, and nudged-elastic-band (NEB) calculations to study Li + migration in paramagnetic Li 2 MnO 3 in the presence of a single Li vacancy. Evaluating DMFT total energies along the DFT+U NEB geometries reveals that dynamical correlations strongly renormalize the lowest-barrier processes, reducing the activation energies to E a = 0.18 eV for the shortest-range hop and E a = 0.50 eV for the next-lowest (transport-controlling) step. The 0.18 eV barrier quantitatively reproduces the short-range activation energy from µ+SR, while the 0.50 eV barrier is consistent with the long-range transport scale extracted from ac-impedance measurements. This single-vacancy, paramagnetic DMFT description thus provides a unified interpretation of local and macroscopic probes without invoking clustered vacancy configurations or strong extrinsic disorder, consistent with nearly stoichiometric Li 2 MnO 3 powders. More broadly, our results highlight finite-temperature dynamical correlations as an essential ingredient for predicting ionic migration energetics in correlated oxide electrodes.

Lee, Alex Taekyung [University of Illinois, Chicag↗
DOE OSTI2024

Adaptive Narrowband Damping for Improving Harmonic Stability of Modular Multilevel Converter

Harmonic instability events between modular multilevel converter (MMC) and ac systems have been widely reported in recent years. To damp harmonic resonance, this paper proposes an adaptive narrowband damping control that automatically programs, adds, and adjusts the damping around the oscillation frequency when an oscillation is detected. First, the paper presents a low-pass filter design for MMC control loops that pushes all negative damping of the MMC impedance down to the medium-frequency range (< ~ 1000 Hz). Then, an adaptive damping control that uses online oscillation detection is proposed, which can automatically configure the narrowband damper to provide positive damping to the MMC around the detected oscillation frequency. In contrast to existing narrowband damping methods, the proposed adaptive narrowband damper dynamically adjusts the damping gain and the width of the damping range based on continuous monitoring of system resonance conditions (e.g., adjust damping gain to zero when the system resonance disappears). Electromagnetic transient simulation results validate the efficacy of the proposed method in two typical MMC-based power systems.

active damping↗
DOE OSTI2021

The LSBmax algorithm for boosting resilience of electric grids post (N‐2) contingencies

Abstract A computationally improved algorithm is presented to find the best transmission switching (TS) candidate for boosting resilience of electricity grids subject to ( N ‐2) contingencies. Here, resilience is computed as the reduction in load shed after the above‐mentioned ( N‐ ) contingencies. TS is a planned line outage, and past research shows that changing the transmission system's topology changes the power flow and removes post contingency violations. Finding the best TS candidate in a computationally suitable time for effectively boosting resilience is a challenge. The best TS candidate is found using a novel heuristic method by decreasing the search space based on proximity to the bus with the maximum load shedding (LSB). The LSB algorithm is faster than existing algorithms in the literature; and, it is compatible with both the AC and DC optimal power flow formulations. To validate the authors' claims of speedup and accuracy, two metrics are used to analyze the results from the IEEE 39‐bus and 118‐bus systems. Finally, the inherent parallelism of the LSB algorithm is leveraged on a high‐performance computing platform and applied to the large‐scale Polish 2383‐bus test system to validate scalability in both size and speedup in computation time.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2020

TDCOSMO - IV. Hierarchical time-delay cosmography – joint inference of the Hubble constant and galaxy density profiles

The H0LiCOW collaboration inferred via strong gravitational lensing time delays a Hubble constant value of H0 = 73.3−1.8+1.7 km s−1 Mpc−1, describing deflector mass density profiles by either a power-law or stars (constant mass-to-light ratio) plus standard dark matter halos. The mass-sheet transform (MST) that leaves the lensing observables unchanged is considered the dominant source of residual uncertainty in H0. We quantify any potential effect of the MST with a flexible family of mass models, which directly encodes it, and they are hence maximally degenerate with H0. Our calculation is based on a new hierarchical Bayesian approach in which the MST is only constrained by stellar kinematics. The approach is validated on mock lenses, which are generated from hydrodynamic simulations. We first applied the inference to the TDCOSMO sample of seven lenses, six of which are from H0LiCOW, and measured H0 = 74.5−6.1+5.6 km s−1 Mpc−1. Secondly, in order to further constrain the deflector mass density profiles, we added imaging and spectroscopy for a set of 33 strong gravitational lenses from the Sloan Lens ACS (SLACS) sample. For nine of the 33 SLAC lenses, we used resolved kinematics to constrain the stellar anisotropy. From the joint hierarchical analysis of the TDCOSMO+SLACS sample, we measured H0 = 67.4−3.2+4.1 km s−1 Mpc−1. This measurement assumes that the TDCOSMO and SLACS galaxies are drawn from the same parent population. The blind H0LiCOW, TDCOSMO-only and TDCOSMO+SLACS analyses are in mutual statistical agreement. The TDCOSMO+SLACS analysis prefers marginally shallower mass profiles than H0LiCOW or TDCOSMO-only. Without relying on the form of the mass density profile used by H0LiCOW, we achieve a ∼5% measurement of H0. While our new hierarchical analysis does not statistically invalidate the mass profile assumptions by H0LiCOW – and thus the H0 measurement relying on them – it demonstrates the importance of understanding the mass density profile of elliptical galaxies. The uncertainties on H0 derived in this paper can be reduced by physical or observational priors on the form of the mass profile, or by additional data.Key words: gravitational lensing: strong / galaxies: general / galaxies: kinematics and dynamics / distance scale / cosmological parameters / cosmology: observations⋆ The full analysis is available at https://github.com/TDCOSMO/hierarchy_analysis_2020_public.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2025

TDCOSMO 2025: Cosmological constraints from strong lensing time delays

We present cosmological constraints from eight strongly lensed quasars (hereafter, the TDCOSMO-2025 sample). Building on previous work, our analysis incorporated new deflector stellar velocity dispersions measured from spectra obtained with the James Webb Space Telescope (JWST), the Keck Telescopes, and the Very Large Telescope (VLT), utilizing improved methods. We used integrated JWST stellar kinematics for five lenses, VLT-MUSE for 2, and resolved kinematics from Keck and JWST for RX J1131−1231. We also considered two samples of non-time-delay lenses: 11 from the Sloan Lens ACS (SLACS) sample with Keck-KCWI resolved kinematics; and four from the Strong Lenses in the Legacy Survey (SL2S) sample. We improved our analysis of line-of-sight effects, the surface brightness profile of the lens galaxies, and orbital anisotropy, and corrected for projection effects in the dynamics. Our uncertainties are maximally conservative by accounting for the mass-sheet degeneracy in the deflectors’ mass density profiles. The analysis was blinded to prevent experimenter bias. Our primary result is based on the TDCOSMO-2025 sample, in combination with Ωm constraints from the Pantheon+ Type Ia supernovae (SN) dataset. In the flat Λ cold dark matter (CDM), we find H0 = 71.6+3.9−3.3 km s−1 Mpc−1. The SLACS and SL2S samples are in excellent agreement with the TDCOSMO-2025 sample, improving the precision on H0 in flat ΛCDM to 4.6%. Using the Dark Energy Survey SN Year-5 dataset (DES-SN5YR) or DESI-DR2 baryonic acoustic oscillations (BAO) likelihoods instead of Pantheon+ yields very similar results. We also present constraints in the open ΛCDM, wCDM, w0waCDM, and wϕCDM cosmologies. The TDCOSMO H0 inference is robust and consistent across all presented cosmological models, and our cosmological constraints in them agree with those from the BAO and SN.Key words: cosmological parameters / cosmology: observations / dark energy / distance scale⋆⋆ Brinson Fellow.⋆⋆⋆ NHFP Einstein Fellow.

Birrer, Simon [SUNY, Stony Brook] (ORCID:000000033↗
DOE OSTI2024

Unveiling Structural Heterogeneity and Imbalance of Gold Decahedral Nanoparticles using Four-dimensional Scanning Transmission Electron Microscopy

Multi-twinned structures have been observed in technologically important crystal systems, for example diamond cubic and face-centered cubic (FCC) lattices, that include materials such as diamond, silicon, a wide range of noble metals, and their nanoscale counterparts. Beyond atomic building blocks, the special arrangements also occur in the self-assembly of nanoparticles (NP) and μm-sized colloidal particles and occupy parts of their phase diagrams. Spanning a wide range of length scales, the universality of the structures arises when the systems attempt to achieve multitwinned structures by overcoming geometric misfits during minimizing surface energies with entirely {111} or close-packing facets. While it is fundamental to understand how strain is sustained upon twinned structures and symmetry breaking, the knowledge will be paramount in practical aspects such as guiding and controlling the thin film growth, anisotropic NP growth, and self-assembly of NPs. Au decahedral (Dh) NP, as the most prevalent multi-twinned model system, fits five tetrahedral motifs into a circle by sharing an axis resulting in a geometric misfit angle of 7.35°, or a disclination with power of -7.35°. Postulating how Au FCC lattice adopts the misfit, theoretical models have been developed to address the underlying lattice symmetry and inhomogeneous strain distribution separately. Yet, experimental reports regarding the former have been limited due to the relatively large X-ray beam sizes that do not fit the sizes of NPs. On the other hand, though the latter has been widely adapted in the thermodynamics of small (<10 nm) multi-twinned nanoparticles, previous literature has shown that, at edge length of 17 nm, the theory’s is invalidated by shear strain that is observed in a defect-free Au Dh NP by high-resolution transmission electron microscopy (HR-TEM) imaging. Though the advancement of aberrationcorrected scanning transmission electron microscopy (AC-STEM) imaging and ab initio calculation techniques brings new opportunities, along with challenges in complicated image analysis and limitation in particle size (usually below 10 nm), the gap between nanoscale and mesoscale has never been extended to gain insight from atomic system with straightforward interaction potentials.

4D-STEM↗