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DOE OSTI2026

Silyl Hot-Injection Versus Thiocyanate Heat-Up Synthesis of Chalcohalides: Pushing the Size and Composition Envelope

Chalcohalide semiconductors are rapidly gaining traction as stable, biocompatible materials for energy conversion applications. While the solid-state synthesis of bulk chalcohalides is relatively well-developed, the colloidal chemistry of these materials is still in its early stages. Colloidal semiconductors are often advantageous in device fabrication due to the cost effectiveness of solution processing. Thus, we aim to increase the utility of chalcohalides in device fabrication by establishing solution phase chemistry of promising compositions. We show that silyl hot-injection is a versatile and effective method of making colloidal PnChI (Pn = Sb, Bi; Ch = S, Se) and Sn 2 PnS 2 I 3 (Pn = Sb, Bi) chalcohalides of tunable sizes and compositions. Furthermore, we demonstrate the preparation of mixed-pnictide chalcohalides through direct hot-injection and/or postsynthetic cation exchange, the latter being one of the few reported instances in chalcohalides. Additionally, we use the thiocyanate heat-up approach in combination with density functional theory to study halide mixing in quaternary tin chalcohalides. By pushing the limits of each synthetic technique, we have designed more soluble chalcohalides with tunable compositions while also gaining a better understanding of the efficacy of each procedure in respect to thin film and subsequent device fabrication. In addition to size and composition tuning, silyl hot-injection can help facilitate the future development and wide-scale application of chalcohalide-based devices by expanding the selection of solution-processable chalcohalides.

halogens↗

DOE OSTI2022

Leveraging Nitrogen Linkages in the Formation of a Porous Thorium–Organic Nanotube Suitable for Iodine Capture

We report the synthesis, characterization, and iodine capture application of a novel thorium–organic nanotube, TSN-626, [Th 6 O 4 (OH) 4 (C 6 H 4 NO 2 ) 7 (CHO 2 ) 5 (H 2 O) 3 ]·3H 2 O. The classification as a metal–organic nanotube (MONT) distinguishes it as a rare and reduced dimensionality subset of metal–organic frameworks (MOFs); the structure is additionally hallmarked by low node connectivity. TSN-626 is composed of hexameric thorium secondary building units and mixed O/N-donor isonicotinate ligands that demonstrate selective ditopicity, yielding both terminating and bridging moieties. Because hard Lewis acid tetravalent metals have a propensity to bind with electron donors of rival hardness (e.g., carboxylate groups), such Th–N coordination in a MOF is uncommon. However, the formation of key structural Th–N bonds in TSN-626 cap some of the square antiprismatic metal centers, a position usually occupied by terminal water ligands. TSN-626 was characterized by using complementary analytical and computational techniques: X-ray diffraction, vibrational spectroscopy, N 2 physisorption isotherms, and density functional theory. TSN-626 satisfies design aspects for the chemisorption of iodine. The synergy between accessibility through pores, vacancies at the metal–oxo nodes, and pendent N-donor sites allowed a saturated iodine loading of 955 mg g –1 by vapor methods. Furthermore, the crystallization of TSN-626 diversifies actinide–MOF linker selection to include soft electron donors, and these Th–N linkages can be leveraged for the investigation of metal-to-ligand bonding and unconventional topological expressions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Rapid Mineral Precipitation During Shear Fracturing of Carbonate-Rich Shales

Target subsurface reservoirs for emerging low-carbon energy technologies and geologic carbon sequestration typically have low permeability and thus rely heavily on fluid transport through natural and induced fracture networks. Sustainable development of these systems requires deeper understanding of how geochemically mediated deformation impacts fracture microstructure and permeability evolution, particularly with respect to geochemical reactions between pore fluids and the host rock. Here, a series of triaxial direct shear experiments was designed to evaluate how fractures generated at subsurface conditions respond to penetration of reactive fluids with a focus on the role of mineral precipitation. Calcite-rich shale cores were directly sheared under 3.5 MPa confining pressure using BaCl 2 -rich solutions as a working fluid. Experiments were conducted within an X-ray computed tomography (xCT) scanner to capture 4-D evolution of fracture geometry and precipitate growth. Three shear tests evidenced nonuniform precipitation of barium carbonates (BaCO 3 ) along through-going fractures, where the extent of precipitation increased with increasing calcite content. Precipitates were strongly localized within fracture networks due to mineral, geochemical, and structural heterogeneities and generally concentrated in smaller apertures where rock:water ratios were highest. The combination of elevated fluid saturation and reactive surface area created in freshly activated fractures drove near-immediate mineral precipitation that led to an 80% permeability reduction and significant flow obstruction in the most reactive core. While most previous studies have focused on mixing-induced precipitation, this work demonstrates that fluid–rock interactions can trigger precipitation-induced permeability alterations that can initiate or mitigate risks associated with subsurface energy systems.

58 GEOSCIENCES↗

DOE OSTI2023

Revisiting Interior Water Mass Responses to Surface Forcing Changes and the Subsequent Effects on Overturning in the Southern Ocean

Abstract Two coupled climate models, differing primarily in horizontal resolution and treatment of mesoscale eddies, were used to assess the impact of perturbations in wind stress and Antarctic ice sheet (AIS) melting on the Southern Ocean meridional overturning circulation (SO MOC), which plays an important role in global climate regulation. The largest impact is found in the SO MOC lower limb, associated with the formation of Antarctic Bottom Water (AABW), which in both models is enhanced by wind and weakened by AIS meltwater perturbations. Even though both models under the AIS melting perturbation show similar AABW transport reductions of 4–5 Sv (50%–60%), the volume deflation of AABW south of 30°S is four times greater in the higher resolution simulation (−20 vs. −5 Sv). Water mass transformation (WMT) analysis reveals that surface‐forced dense water formation on the Antarctic shelf is absent in the higher resolution and reduced by half in the lower resolution model in response to the increased AIS melting. However, the decline of the AABW volume (and its inter‐model difference) far exceeds the surface‐forced WMT changes alone, which indicates that the divergent model responses arise from interactions between changes in surface forcing and interior mixing processes. This model divergence demonstrates an important source of uncertainty in climate modeling, and indicates that accurate shelf processes together with scenarios accounting for AIS melting are necessary for robust projections of the deep ocean's response to anthropogenic forcing.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Compositional and structural control in LLZO solid electrolytes

Garnet-based solid-state electrolytes (SSEs) represent a promising class of materials for next-generation batteries with improved safety and performance. However, lack of control over the composition and crystal structure of the well-known Li 7 La 3 Zr 2 O 12 (LLZO) garnet material has led to poor reproducibility with a wide range of ionic conductivities reported in the literature. In this study, the role of precursor homogeneity in controlling the compositional and structural evolution of Al-doped LLZO is explored. A novel solution-based synthesis approach is employed to demonstrate enhanced atomic-scale mixing of the starting materials in comparison to conventional solid-state preparation methods. Through this technique, it is shown that the stability and formation temperature of the highly conductive cubic phase is directly impacted by the spatial distribution of the doping element and reactant species in the precursor mixture. Precursor homogeneity was also an important factor in mitigating the formation of unwanted secondary impurities. These findings can be used to guide the synthesis of SSEs with reproducible material characteristics and enhanced electrolytic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Development and investigation of efficient resonance ionization mass spectrometry schemes of gadolinium

Resonance ionization mass spectrometry of gadolinium can be used for nuclear forensics and to further the understanding of stellar nucleosynthesis but has been used only a handful of times due to the high laser power required and interference from non-resonant ionization of molecules of other elements. Herein we present the development of two novel resonance ionization spectroscopy schemes for gadolinium that provide improvements in isotopic fractionation and ionization efficiency, respectively, opening new applications for gadolinium analysis. The schemes are demonstrated and compared in a mixed sample of gadolinium and neodymium.

and nuclear chemistry↗

DOE OSTI2024

Efficient laser-driven proton acceleration from a petawatt contrast-enhanced second harmonic mixed-glass laser system

Efficient laser-driven plasma acceleration of ion beams requires precision control of the target–plasma profile, which is crucial to optimize the laser energy transfer. Along the laser propagation direction, this can be achieved by tailoring the temporal structure of the laser pulse. We show for the first time that frequency-doubling of a short pulse (hundreds-femtosecond range) petawatt-class mixed-glass laser system, which results in temporal intensity contrast enhancement, enables surface and volumetric laser–energy coupling, and the acceleration of proton beams from few-nanometer-thick foil targets. Experimentally, maximum ion energies and laser-to-proton energy conversion efficiencies were found to be both maximized at optimum laser and target conditions manifested when the normalized target density nearly equalizes the normalized laser vector potential, which is in agreement with theory and simulations. These signatures are recognized as a unique indication of the interaction between ultra-intense laser pulses with high temporal intensity contrast and ultra-thin nanometer-scale targets. Transverse modulations of accelerated proton beams in the form of bubble- and ring-like structures measured in the thinnest targets provide additional evidence of volumetric laser-driven particle acceleration regimes and transitional features in ultra-thin foil targets specific to laser–plasma interactions characterized by a high temporal intensity contrast. These results open avenues in the generation of high contrast laser pulses from short-pulse-femtosecond petawatt mixed-glass laser systems and demonstrate the feasibility of this technique for applications requiring high laser intensity contrast with high efficiency.

Physics↗

DOE OSTI2024

Heat transfer and transport property contrast effects on the compressible Rayleigh-Taylor instability

In extreme environments, the Rayleigh-Taylor instability (RTI) may occur under large variations in density and temperature and with fluid transport properties strongly dependent on temperature. Direct numerical simulations of the 3D fully compressible RTI are conducted, examining the idealized configuration of a hotter, less dense fluid pushing against a colder, denser fluid. Various temperature ratios and transport property configurations are explored to examine how heat conduction, large variations in transport properties, and sudden changes in transport properties can affect the evolution of the mixing layer. Nonuniform fluid expansion and contraction induced by heat transfer can significantly affect local density differences and overall instability growth, causing profile asymmetries about the initial interface for flow and mixing statistics. The departures from classical self-similar development of the instability along with misalignment between regions of mixing and regions of most intense turbulent activity caused by both heat transfer and transport property contrasts are examined. After sudden changes in fluid transport properties, which may occur as a result of rapid heating (e.g., in inertial confinement fusion), the flow quickly responds and begins to relax towards quasi-self-similar late-time evolution. For many dynamical quantities such as vorticity and dissipation, this late-time evolution resembles that of the configuration that already started with the final transport property magnitudes, suggesting that these quantities depend only on the transport properties and not on past flow history, provided that the density field distributions for the flows remain similar. On the other hand, the mixing evolution after the transport property change is unique, implying that both property magnitudes and previous history are impactful on the mixing. In conclusion, these simulations demonstrate how various temperature-related effects are extremely important to consider in compressible RTI flows with large temperature variations.

42 ENGINEERING↗

DOE OSTI2021

Microwave Sensing of Yeast Cell Species and Viability

We report the development of a simple interferometer-based microwave sensing system for multiple frequency characterization and differentiation of in-flow yeast cells. The interferometer uses a simple microstrip line, integrated with a microfluidic channel, for single-cell measurement. An algorithm was developed and verified with high-frequency structure simulator (HFSS) for complex permittivity, ε*( f ) = ε'( f ) - jε"(f), extraction from measured scattering parameters. The sensing system and the algorithm were evaluated by measuring polystyrene particles of different diameters and at different interferometer operating frequencies. Viable and nonviable Saccharomyces cerevisiae and Saccharomyces pastorianus cells were measured at those frequencies. The results showed frequency-dependent permittivity values for each species of yeast and viability as well as frequency-dependent permittivity differences between different yeast types. The differences at some frequency points are significant and enable the differentiation of cells in mixed suspension, which is also demonstrated with a prediction model developed in this work.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2026

Polyolefin blends with co-continuous architectures enabled by dynamic covalent crosslinking

Blending polymers produces brittle materials due to macrophase separation and poor interfacial adhesion, which is exemplified by mixtures of polyolefins. This presents a formidable challenge for the mechanical recycling of mixed plastic waste. Here, we demonstrate that dynamic covalent crosslinking of immiscible polyolefin blends creates macrophase separated co-continuous architectures, yet they display excellent mechanical properties, which challenges the conventional wisdom regarding morphology-property relationships in polymer blend compatibilization. We find that the position and orientation of dynamic crosslinks and their influence on crystallinity are key to understanding the structure-morphology-property relationships. In particular, high-resolution microscopy imaging reveals alignment of crystallite planes with strong orientational preference, particularly at polymer-polymer interfaces, which contribute to material performance. We further demonstrate that changes in crosslinker density and valency allow the properties of binary and ternary polyolefin blends to be tuned in a modular fashion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Angle-resolved polarized Raman spectroscopy study of phosphorene nanoribbons

We present a systematic angle-resolved polarized Raman spectroscopy (ARPRS) study of black phosphorus (BP) nanostructures formed via electrochemical sodium- and lithium-ion intercalation. Sodium intercalation leads to bundles of densely packed, highly uniform phosphorene nanoribbons (PNRs) separated by parallel amorphous channels, whereas lithium intercalation results in shorter, irregular nanoribbon-like segments with lower aspect ratios. In both cases, six additional Raman peaks (P1–P6) appear alongside the three primary Raman-active modes of BP (A$^{1}_{g}$, B 2g , and A$^{2}_{g}$). These peaks are attributed to the amorphous regions, as confirmed by their isotropic angular dependence in ARPRS measurements. The three BP modes show pronounced angular variations that differ significantly between the two intercalated samples. In sodium-intercalated BP, A$^{1}_{g}$ and A$^{2}_{g}$ modes retain a dumbbell-like angular dependence under parallel polarization with enhanced anisotropy and reduced symmetry under crossed polarization. At the same time, the B 2g mode transitions from four-lobed (cloverleaf) polar plot to a butterfly-like one. In contrast, lithium-intercalated BP exhibits weaker anisotropy and less distinct angular polar plots for all three modes. These differences reflect the sensitivity of phonon behavior to underlying nanostructure morphology. The vibrational frequencies density of states (FDOS) calculations attribute the B 2g mode transformation to phonon band folding and mode mixing in PNRs. This study demonstrates the power of ARPRS in probing phonon-structure relationships and highlights the influence of edge geometry and quantum confinement on phonon dispersion in PNRs.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2022

Mind-the-gap - Part III: Doppler velocity measurements from space

Convective motions and hydrometeors microphysical properties are highly sought-after parameters for evaluating atmospheric numerical models. With most of the Earth's surface covered by water, space-borne Doppler radars are ideal for acquiring such measurements at a global scale. While these systems have proven to be useful tools for retrieving cloud microphysical and dynamical properties from the ground, their adequacy, and specific requirements for spaceborne operation still need to be evaluated. Comprehensive forward simulations enable us to assess the advantages and drawbacks of six different Doppler radar architectures currently planned or under consideration by space agencies for the study of cloud dynamics. Radar performance is examined against state-of-the-art numerical model simulations of well-characterized shallow and deep, continental, and oceanic convective cases. Mean Doppler velocity (MDV) measurements collected at multiple frequencies (13, 35 and 94 GHz) provide complementary information in deep convective cloud systems. The high penetration capability of the 13-GHz radar enables to obtain a complete, albeit horizontally under-sampled, view of deep convective storms. The smaller instantaneous field of view (IFOV) of the 35-GHz radar captures more precise information about the location and size of convective updrafts above 5-8 km height of most systems which was determined is the portion of storms where the mass flux peak is typically located. Finally, the lower mean Doppler velocity uncertainty of displaced phase center antenna (DPCA) radars makes them an ideal system for studying microphysics in shallow convection and frontal systems, as well as ice and mixed-phase clouds. It is demonstrated that a 94-GHz DCPA system can achieve retrieval errors as low as 0.05-0.15 mm for raindrop volume-weighted mean diameter and 25% for rime fraction (for a -10 dBZ echo).

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Validated CFD Model for Multimode Gasoline Compression Ignition Engine

A validated CFD model for the multimode combustion engine developed under the DOE funded project DE-EE0008478 (Co-optimized Mixed-Mode Engine and Fuel Demonstrator for Improved Fuel Economy while Meeting Emissions Requirements). It incorporates advanced physics-based fuel surrogate models for thermophysical properties and reaction kinetics. The combustion modes include spark ignition (SI), low temperature combustion (LTC), and compression ignition (CI). The real fuel model was validated for RON60, RON70, RON80, RON90, and two biofuel blends. The validation cases can be found in https://doi.org/10.2172/1887341.

02 PETROLEUM↗

DOE OSTI2023

Ignition Delay Test with Spray & Combustion Vessel

Ignition delay test results of different fuels (RON60, RON70, RON80, RON90, and biofuel blends) under different engine operating conditions with a multi-hole injector. These results were used to better understand the spray and combustion characteristics and validate the CFD real fuel model (https://doi.org/10.5281/zenodo.8432075). This work was part of the DOE funded project (DE-EE0008478; Co-optimized Mixed-Mode Engine and Fuel Demonstrator for Improved Fuel Economy while Meeting Emissions Requirements; https://doi.org/10.2172/1887341).

02 PETROLEUM↗

NASA NTRS1975

Mixed isoparametric elements for Saint-Venant torsion

Mixed isoparametric elements are presented for the Saint-Venant torsion problem of laminated and anisotropic bars. Both triangular and quadrilateral elements are considered. The 'generalized' element stiffness matrix is obtained by using a modified form of the Hellinger-Reissner mixed variational principle. Group-theoretic techniques are used in conjunction with computerized symbolic integration to obtain analytic expressions for the stiffness coefficients. The accuracy of the mixed isoparametric elements developed is demonstrated by means of numerical examples, and their advantages over commonly used stress and displacement elements are discussed.

Noor, A. K.↗

NASA NTRS1977

Mixed isoparametric finite element models of laminated composite shells

Mixed shear-flexible isoparametric elements are presented for the stress and free vibration analysis of laminated composite shallow shells. Both triangular and quadrilateral elements are considered. The 'generalized' element stiffness, consistent mass, and consistent load coefficients are obtained by using a modified form of the Hellinger-Reissner mixed variational principle. Group-theoretic techniques are used in conjunction with computerized symbolic integration to obtain analytic expressions for the stiffness, mass and load coefficients. A procedure is outlined for efficiently handling the resulting system of algebraic equations. The accuracy of the mixed isoparametric elements developed is demonstrated by means of numerical examples, and their advantages over commonly used displacement elements are discussed.

Noor, A. K.↗

NASA NTRS1992

Differential correction technique for removing common errors in gas filter radiometer measurements

The Measurement of Air Pollution from Satellites (MAPS) gas filter radiometer experiment was designed to measure CO mixing ratios in the earth's atmosphere. MAPS also measures N2O to provide a reference channel for the atmospheric emitting temperature and to detect the presence of clouds. In this paper we formulate equations to correct the radiometric signals based on the spatial and temporal uniformity of the N2O mixing ratio in the atmosphere. Results of an error study demonstrate that these equations reduce the error in inferred CO mixing ratios. Subsequent application of the technique to the MAPS 1984 data set decreases the error in the frequency distribution of mixing ratios and increases the number of usable data points.

Wallio, H. A.↗

NASA NTRS1995

Model studies of the beam-filling error for rain-rate retrieval with microwave radiometers

Low-frequency (less than 20 GHz) single-channel microwave retrievals of rain rate encounter the problem of beam-filling error. This error stems from the fact that the relationship between microwave brightness temperature and rain rate is nonlinear, coupled with the fact that the field of view is large or comparable to important scales of variability of the rain field. This means that one may not simply insert the area average of the brightness temperature into the formula for rain rate without incurring both bias and random error. The statistical heterogeneity of the rain-rate field in the footprint of the instrument is key to determining the nature of these errors. This paper makes use of a series of random rain-rate fields to study the size of the bias and random error associated with beam filling. A number of examples are analyzed in detail: the binomially distributed field, the gamma, the Gaussian, the mixed gamma, the lognormal, and the mixed lognormal ('mixed' here means there is a finite probability of no rain rate at a point of space-time). Of particular interest are the applicability of a simple error formula due to Chiu and collaborators and a formula that might hold in the large field of view limit. It is found that the simple formula holds for Gaussian rain-rate fields but begins to fail for highly skewed fields such as the mixed lognormal. While not conclusively demonstrated here, it is suggested that the notionof climatologically adjusting the retrievals to remove the beam-filling bias is a reasonable proposition.

Ha, Eunho↗