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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 OSTI2024

Angle-Resolved Polarized Raman Study of Layered Cr 2 Se 3

The polarization-resolved Raman spectra of two-dimensional Cr 2 Se 3 synthesized via chemical vapor deposition (CVD) and chemical vapor transport (CVT) techniques were investigated in detail. The samples were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDS). A distinct polarization dependence was observed in the Raman intensity of all the Cr-Cr, Cr-Se, and Se-Se modes in both samples. The observed angle-dependent Raman intensities of each peak could be related to the crystal structure-specific Raman tensor. XRD results of the bulk Cr 2 Se 3 sample synthesized via CVT confirm its trigonal crystal structure, and the Raman peaks can be fitted using the Raman tensors for the A g and E g modes for both the parallel and crossed polarizations. However, for the Cr 2 Se 3 samples directly grown on Si/SiO 2 substrates by CVD, it was necessary to assume the triclinic crystal structure in order to explain the polarized Raman dependence of all the peaks in both parallel and crossed polarization directions. Furthermore, this is the first experimental result suggesting the existence of triclinic Cr 2 Se 3 crystal structure, which has been theoretically predicted in the Materials Project database.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Measurement of the effective leptonic weak mixing angle

Using pp collision data at $\sqrt{s}$ = 13 TeV, recorded by the LHCb experiment between 2016 and 2018 and corresponding to an integrated luminosity of 5.4 fb −1 , the forward-backward asymmetry in the pp → Z/γ* → μ + μ − process is measured. The measurement is carried out in ten intervals of the difference between the muon pseudorapidities, within a fiducial region covering dimuon masses between 66 and 116 GeV, muon pseudorapidities between 2.0 and 4.5 and muon transverse momenta above 20 GeV. These forward-backward asymmetries are compared with predictions, at next-to-leading order in the strong and electroweak couplings. The measured effective leptonic weak mixing angle is ${\sin}^2{\theta}_{\textrm{eff}}^{\ell }=0.23147\pm 0.00044\pm 0.00005\pm 0.00023,$ where the first uncertainty is statistical, the second arises from systematic uncertainties associated with the asymmetry measurement, and the third arises from uncertainties in the fit model used to extract ${\sin}^2{\theta}_{\textrm{eff}}^{\ell }$ from the asymmetry measurement. This result is based on an arithmetic average of results using the CT18, MSHT20, and NNPDF31 parameterisations of the proton internal structure, and is consistent with previous measurements and with predictions from the global electroweak fit.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2025

Direct observation of strain-enhanced hydrogen segregation and failure at high-angle grain boundaries in nickel

Understanding the mechanisms underlying hydrogen embrittlement remains difficult, even in single-element metals. Both microstructure and stress state influence hydrogen distribution in metals and alloys, which impacts deformation and failure. Here, in this work, we use in-situ Kelvin probe force microscopy (KPFM) to monitor the hydrogen distribution in pure nickel over time at 1.1 % and 3.5 % strain. The sample strained to 3.5 % results in preferential hydrogen segregation to high-angle grain boundaries whereas the sample strained to 1.1 % does not exhibit preferential hydrogen segregation. Optical digital image correlation (DIC) shows that hydrogen charging results in both localized and reduced strains during tensile testing of a notched sample. Later stages of deformation and failure (e.g. microcracking) are studied by using in-situ transmission X-ray microscopy (TXM). TXM reveals nanoscale structural changes to a propagating crack in a hydrogen environment. Localized void growth and secondary cracking occur at grain boundaries near the primary crack front. Correlative electron backscattering diffraction (EBSD) is used to relate the cracking at grain boundaries to the hydrogen segregation observed in KPFM. These findings are unified in a proposed hydrogen embrittlement mechanism that describes the interaction of hydrogen with grain boundaries, and the role of grain boundaries in hydrogen embrittlement.

Grain boundary fracture↗

DOE OSTI2025

Information theory optimization of signals from small-angle scattering measurements

Small-angle X-ray scattering (SAXS) of particles in solution informs on the conformational states and assemblies of biological macromolecules (bioSAXS) outside of cryo- and solid-state conditions. In bioSAXS, the SAXS measurement under dilute conditions is resolution limited, and through an inverse Fourier transform, the measured SAXS intensities directly relate to the physical space occupied by the particles via the P (r)-distribution. Yet, this inverse transform of SAXS data has been historically cast as an ill-posed, ill-conditioned problem requiring an indirect approach. Here, we show that through the applications of matrix and information theories, the inverse transform of SAXS intensity data is a well-conditioned problem. The so-called ill-conditioning of the inverse problem is directly related to the Shannon number. By exploiting the oversampling enabled by modern detectors, a direct inverse Fourier transform of the SAXS data is possible, provided the recovered information does not exceed the Shannon number. The Shannon limit corresponds to the maximum number of significant singular values that can be recovered in a SAXS experiment, suggesting this relationship is a fundamental property of band-limited inverse integral transform problems. This correspondence reduces the complexity of the inverse problem to the Shannon limit and maximum dimension. We propose a hybrid scoring function using an information theory framework that assesses both the quality of the model-data fit as well as the quality of the recovered P (r)-distribution. The hybrid score utilizes the Akaike information criteria and Durbin-Watson statistic that considers parameter-model complexity, i.e., degrees of freedom, and the randomness of the model-data residuals. The described tests and findings extend the boundaries for bioSAXS by completing the information theory formalism initiated by Peter B. Moore to enable a quantitative measure of resolution in SAXS, robustly determine maximum dimension, and more precisely define the best parameter model appropriately representing the observed scattering data.

Rambo, Robert P. [Science and Technology Facilitie↗

DOE OSTI2025

The structure of high-Mg alkali-bearing aluminosilicate glasses investigated in situ at ambient and high pressure by multi-angle energy dispersive X-ray diffraction and infrared microspectroscopy

The structural properties of synthetic high-Mg alkali-bearing aluminosilicate glasses analogues of natural picritic-to-komatiitic magmas were investigated in situ by multiangle energy dispersive X-ray diffraction at 2.1 GPa and ambient pressure and by Fourier Transform infrared spectroscopy up to 5.4 GPa in a cycle of compression and decompression experiments. Our results show that the intermediate range ordering of the glass structure at 2.1 GPa is 3.14 Å, increasing to 3.19 Å when decompressed. The local structure shows T-O lengths of 1.66 Å (2.1 GPa) and 1.65 Å (ambient pressure), T-T distances of 3.19 Å at high pressure, which lengthen to 3.21 Å at ambient pressure, causing the T-O-T angle of 147° determined at 2.1 GPa to widen to 154° upon decompression. The deconvoluted infrared spectra result in the presence of Q 1 , Q 2 , Q 3 populations in the aluminosilicate spectral region, whose proportions remain relatively unchanged up to 5.4 GPa. The structural response of the investigated glasses to cold-compression does not involve changes in polymerization, but rather a shrinking and compaction of the structure as evidenced by the Qn species shifting to higher wavenumbers as a function of pressure. The structural properties determined from X-ray diffraction for this glass composition are discussed together with those of glasses emerging from previous studies to highlight a compositional dependence mainly dictated by the amount of SiO 2 and Al 2 O 3 .

glass structure↗

DOE OSTI2024

Structural characterization of high-protein system through ultra-small and small-angle X-ray scattering

High-protein systems exhibit a hierarchical structure consisting of interconnected multiscale length assemblies. Recent investigations are directed toward identifying these structural units under various processing and environmental conditions to establish structure–function correlations. Ultra-small and small-angle X-ray scattering (USAXS/SAXS) has become a crucial tool for characterizing the structures of proteins and their clusters/aggregates, ranging from nanometers to micrometers, with minimal disruption to their original state. Here, this review first describes the facilities and principles of X-ray scattering, followed by discussions on the analysis of scattering data, including the interpretation of fitting models. It then delves into the main applications of USAXS/SAXS in plant and dairy protein-rich systems. Future strategies to enhance the utilization of scattering techniques for elucidating the structure of high-protein systems are also included.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2025

Unravelling the origins of shale nanoporosity using small-angle neutron scattering (SANS)

Hydrocarbon production from tight rocks is constrained by slow diffusion within the shale matrix, limited by small pore sizes and low permeability. The nanopore proportion and size distribution significantly influence matrix permeability, a key property for optimizing hydrocarbon recovery and supporting hydrogen production while minimizing environmental impacts. Small-angle neutron scattering (SANS) has been an important tool for exploring the characteristics and structure of shale nanopores. This study used SANS to analyze nanoporosity and pore size distribution (<100 nm) in tight rocks with varying compositions to determine the influence of rock heterogeneity on SANS measurements. Results showed that nanoporosity correlates with clay content, with the highest clay-rich shale (52.48 wt% clay) exhibiting 8.8 % nanoporosity. SANS also revealed more nanopores than traditional nitrogen adsorption measurements, affirming its ability to reflect bulk mineralogy and upholding the relevance of experimental findings using this technique to optimize field operational approaches.

03 NATURAL GAS↗

DOE OSTI2025

Interplay between hydrogen, temperature, and character angle on dissociated dislocation energies in Fe–Ni–Cr austenitic stainless steels

Dislocation energy has an important role in the mechanical performance of structural metals. While dislocation energies cannot be fully obtained from continuum theories due to the contribution of the dislocation core, they have been calculated via atomistic simulations in elemental metals. However, constraints on the local atomic environments have prevented the use of such approaches in systems that incorporate alloying or interstitial solutes. In this work, we develop robust molecular dynamics methods to resolve these issues through a geometric construction of dislocation dipoles and the calculation of time-averaged energies. Furthermore, we apply these methods to calculate dislocation energies (including core energies) in an Fe 70 Ni 11 Cr 19 austenitic steel at a variety of character angles, hydrogen concentrations, temperatures, and dipole spacings. The resulting highly converged energies show an excellent agreement with continuum expressions. Overall, hydrogen concentrations up to 1.0 % do not have a significant effect on the elastic parameters and dislocation energy. The methods and insights derived in this work have the potential to facilitate the calculation of dislocation energies in a wide range of systems, and to guide our understanding of hydrogen embrittlement.

Alloyed systems↗

DOE OSTI2025

Protecting air/moisture-sensitive samples using perdeuterated paraffin wax for solid-state NMR experiments under magic-angle spinning

Solid-state nuclear magnetic resonance (SSNMR) spectroscopy is a powerful technique for materials characterization, yet its application to air- and moisture-sensitive materials is often hindered by the difficulty in maintaining an inert environment during magic-angle spinning (MAS). This is particularly true for fast-MAS rotors that do not generally provide tight seals. Herein, we present a generalizable approach employing perdeuterated paraffin waxes—n-icosane-d42 and c-dodecane-d24—as protective embedding media to analyze sensitive organometallic catalysts using SSNMR. We demonstrate that these waxes significantly slow oxidative degradation under MAS conditions. Weak background 1 H and 13 C NMR signals from the waxes are effectively suppressed using double-quantum filtration and cross-polarization techniques. In conclusion, these findings offer a robust method for expanding the scope of SSNMR to air-sensitive systems, with implications for the structural study of reactive materials and catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Wetting mechanism and alteration of nano-sized shale pores: Insights from contrast variation small angle neutron scattering

Wettability of tight shale is crucial for fluid flow and mass transport process in energy geosciences. However, understanding the interfacial chemistry and wetting mechanisms at sub-nano-pore scales remains a formidable challenge. Here, in this study, the Contrast Variation technique of Small Angle Neutron Scattering (CV-SANS) is employed to investigate shale’s interfacial chemistry using reagents that possess a range of different polarities, including water, n-decane, toluene, and dimethyl methanamide. Through five different experimental strategies, we have demonstrated a successful modification of shale wettability, ranging from enhancement, weakening, to reversal. Delving into the mechanisms, we illustrated the crucial role of pre-existing liquid films in these changes, where the uniquely co-existing polar and non-polar functional groups in dimethyl methanamide acted as a conduit for interfacial chemistry adjustments. Furthermore, a solvent immersion led to matrix dilation as well as liberation of residual oil-occupied pores, resulting in altered pore size distributions, with hydrogen bonding playing a significant role in the polar groups. Interestingly, despite shale exhibiting a stronger affinity for oil over water, hydrophilic solvents induced more substantial dilation than lipophilic ones. Collectively, this work elucidates the dynamic change of interfacial chemistry via the configuration of polarity using chemical reagents, and the CV-SANS technique underscores its invaluable utilities in decoding the interfacial wettability traits in nanopore space of shale.

58 GEOSCIENCES↗

DOE OSTI2025

Portable Distortion Free Large Solid Angle Coverage Detector

Neutron single crystal diffractometers require large solid angle coverage for optimum performance. This can be achieved by tiling flat detectors in a cylindrical or spherical geometry, but results in large gaps in detector coverage and parallax distortion. The detector edges exhibit degraded resolution, distortion, and gamma rejection. Since the detector edge regions are a significant fraction of the detector active area, they must be removed from the experimental data set, requiring extra beam time to collect enough analysis data. A spherical detector with a continuous surface would effectively address this issue while eliminating most boundary ‘dead’ areas. Here we report on the development of a novel hemispherical shaped neutron detector using seamlessly tiled readout modules to form the desired shape. The heart of the detector is a specially developed curved neutron scintillator coupled to high resolution silicon photomultiplier (SiPM) Anger cameras via custom made fiber optic tapers (FOTs). The detector has been assembled and initial tests have been conducted at the High Flux Isotope Reactor (HFIR) beamlines at Oak Ridge National Laboratory (ORNL). Here, in this work, we describe details of the scintillator design, fabrication and characterization, evaluation of individual detector modules, the details of the detector design implementation, and evaluation of the assembled detector at ORNL beamlines.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2026

The effectiveness of D 2 pellet and gas injection in reducing intra-ELM tungsten erosion and heat flux in the DIII-D small angle slot divertor

Edge localized modes (ELMs) in H-mode plasmas can melt and erode plasma-facing components (PFCs) and lead to impurities in the core, reducing confinement. This study analyzes the use of D 2 pellet and gas injection for ELM mitigation on the DIII-D tokamak during the 2022 Small Angle Slot V-shaped Tungsten (W) (SAS-VW) divertor campaign, reducing W erosion and heat flux during ELMs. D α (656 nm) and WI (400.9 nm) filterscopes and Langmuir probes provide photon emission and electron density/temperature to estimate W atom erosion using the S/XB method, while surface eroding thermocouples measured ELM peak heat flux at the outer strike point (OSP). Thomson Scattering measurements of pedestal T e and n e provided input to predict W divertor erosion and heat flux during ELMs via the Free-Streaming plus Recycling Model (FSRM). While a greater D 2 mass injection rate decreased the ELM peak heat flux, the impact on W erosion was not monotonic. The average ‘large’ intra-ELM W erosion was lower for plasma shots with D 2 mass injection compared to the plasma shots without any D 2 mass injection in the SAS-VW divertor. However, plasma shots did not see significant changes in ‘large’ intra-ELM W divertor erosion as the D 2 mass injection rate increased. On average, the FSRM overestimated SAS-VW experimental intra-ELM W erosion by a factor of 6.9, but the overestimation is reduced to a factor of 3.6 with the implication of C deposition effects. Generally, experimentally measured and predicted quantities were worse for plasma shots with a lower D 2 mass injection rate and corresponding higher plasma carbon (C) impurity percentage (f C ). The discrepancies are postulated to be due to C/W material mixing, for which a simple analytic mixed-material model is presented. These results highlight the importance of incorporating and improving the robustness of a mixed-material layer model in the analysis of PFC erosion on present and future tokamak devices.

Carbon (C)↗

DOE OSTI2025

In situ probing of structure and deagglomeration of SnO 2 colloids via small-angle X-ray scattering

Transforming dry nanopowders into stable colloidal dispersions remains challenging due to the cohesive forces between the nanoparticles (NPs) which promote agglomeration. Effective dispersion and deagglomeration of these agglomerates is a critical process in the formulation and preparation of nanoparticle-based functional materials via the colloidal route. Understanding the deagglomeration dynamics provides information to improve microstructural quality in various applications by enabling engineering of agglomerate size, structure and morphology. However, the deagglomeration process dynamics with respect to the evolution of the fractal agglomerate structures, particularly for very small NPs, is still poorly understood and requires further investigation. This study employs in situ small-angle X-ray scattering (SAXS) to investigate the sonication-induced deagglomeration of SnO 2 NPs. Electrostatically stabilized SnO 2 colloids with varying primary particle size (6–21 nm) are investigated in a specifically designed in situ cell using synchrotron-based SAXS to study the influence of sonication time and intensity on the nanoscaled agglomerates. Complete structural analysis via SAXS reveals a direct correlation between changes in agglomerate size and structure, size-dependent deagglomeration behavior and a dependence on the overall energy introduced during sonication into the dispersion regardless of the actual power as well as ultrasonic process parameters in case of SnO 2 NPs. The results suggest that control of the dispersion process during ultrasonic deagglomeration results in tailoring agglomerates with respect to size and structure.

Deagglomeration↗

DOE OSTI2024

Importance of viewing angle: Hotspot effect improves the ability of satellites to track terrestrial photosynthesis

The product of near-infrared reflectance of vegetation and photosynthetic active radiation (NIRvP) is a new tool for monitoring gross primary productivity (GPP) dynamics in terrestrial ecosystems, due to the discovered linear correlation between NIRvP and GPP. While remote sensing-based NIRvP is considerably influenced by sensor geometry, such geometry impacts on the NIRvP-GPP relationship remain underexplored. In this study, we calculate NIRvP using observations from the Deep Space Climate Observatory (DSCOVR) that provide unique hotspot observation geometry in which the sensor viewing angle coincides with the sun direction. We evaluated the linear correlation between NIRvP and GPP in both the common nadir direction and the special hotspot direction. The results indicate that NIRvP in the hotspot direction significantly outperforms that in the nadir direction for tracking GPP variations across different ecosystems from diurnal to daily scales. This conclusion is further supported by data from the MODerate resolution Imaging Spectroradiometer (MODIS) and simulations using the Soil Canopy Observation Photosynthesis Energy (SCOPE) model. Finally, our research highlights the value of using the unconventional hotspot-based sun-tracking satellite observations for a more accurate characterization of GPP dynamics in terrestrial ecosystems.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2026

Machine learning surrogates for ion energy–angle distributions in thermal and RF plasma sheaths

Ion energy–angle distributions (IEADs) at material surfaces are a critical input for plasma–material interaction (PMI) studies in fusion devices, yet they are computationally expensive to obtain using particle-in-cell (PIC) simulations. In this work, we develop a machine learning surrogate based on a deep deconvolutional neural network (DDeCNN) trained on large databases generated with the hPIC2 code. The surrogate is capable of reconstructing IEADs from sheath parameters for both thermal and radio-frequency (RF) plasmas, including cases with multiple ion species. Across thousands of test cases, the model achieves high accuracy, with over 97 % of predictions classified as good or average based on standard error metrics (MAE, MSE, L2). Even in the more challenging RF and multi-species regimes, the surrogate reliably captures the multi-peak structure of PIC results. Once trained, the surrogate produces IEADs in milliseconds on a common workstation, yielding speedups of six to seven orders of magnitude compared with running a full PIC simulation. This computational gain enables dense parameter scans and direct coupling of IEAD predictions with PMI and erosion models on whole-device scales in fusion-relevant conditions.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Structural Properties of [N1888][TFSI] Ionic Liquid: A Small Angle Neutron Scattering and Polarizable Molecular Dynamics Study

In this study, we investigate the quaternary ammonium-based ionic liquid (QAIL), methyltrioctylammonium bis(trifluoromethylsulfonyl)imide, [N 1888 ][TFSI], utilizing small angle neutron scattering (SANS) measurements and polarizable molecular dynamics (MD) simulations to characterize the shortand long-range liquid structure. Scattering structure factors show signatures of three length scales in reciprocal space indicative of alternating polarity (k ~ 0.44 Å –1 ), charge (k ~ 0.75 Å –1 ), and neighboring or adjacent (k ~ 1.46 Å –1 ) domains. Excellent agreement between simulation and experimental scattering structure factors validates various simulation analyses that provide detailed atomistic characterization of the different length scale correlations. The first solvation shell structure is illustrated by obtaining radial, angular, dihedral, and combined distribution functions, where two dominant spatial motifs, N + ···N – and N + ···O – , compete for optimal packing around the polar head of the [N 1888 ] + cation. Intermediate and long-range structures are governed by the balance between local electroneutrality and octyl chain networking, respectively. By computing the charge-correlation structure factor, S ZZ , and the spatial extent of the octyl chain network using graph theory, the bulk-phase structure of [N 1888 ][TFSI] is characterized in terms of electrostatic screening and apolar domain formation length scales.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Nanostructuring and Underscreening of Bisalt Electrolytes with Dual-Anion Effects: Insights from Small-Angle Scattering Prepeak Analysis

Using small-angle neutron scattering, we studied the nanostructure of a prototypical D(H)-bonded network electrolyte, alkaline sodium aluminate bisalt, at concentrations up to solute volume fraction of ~0.5. Analysis of the structure factor prepeak at 0.1 < Q < 1.0 Å-1 showed that its evolution is associated with nanoscopic species distribution in water-anion network., with differences in characteristic distance d between OD- and Al(OD)4- anions related to their distinct sizes and interactions. When the solute volume fraction approached 0.5, a common/maximum value of ~4.5 Å was found for the correlation length ? that characterizes the electrostatic force in concentrated electrolyte solution before precipitation occurred. This implies that the solutions’ morphology and behavior at high concentrations may be governed by geometric factors, rather than the chemistry of the specific anion. Furthermore, the scaling of ? with concentration yielded an exponent of 1.25(1), suggesting that ? is limited to a few Å. By combining the current observations of structural heterogeneity at the nanoscale, with dynamic heterogeneity at the microscopic scale from our previous quasi-elastic neutron scattering study, we have established a structural origin of local “caging” and restricted structural relaxation processes. These local solvent-solute interactions not only control dynamics heterogeneity in concentrated electrolytes but also are responsible for crystallization processes in industrial setting, such as aluminum production and radioactive waste treatment.

Wang, Hsiu-Wen↗