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DOE OSTI2024

Machine learning-driven descriptions of protein dynamics at solid-liquid interfaces

This chapter has described how ML has enabled quantitative analysis of HS-AFM data to discover the physical phenomena governing protein dynamics and ordering at solid-liquid interfaces. The research detailed in this chapter modeled the rotation models of protein nanorods, the discovery of which would otherwise not be possible. By tracking the trajectories of individual protein rods from frame to frame, it was possible to model Brownian type motion and behaviors and Levy-flight dynamics that had not previously been shown. We also described the application of the Python package AtomAI, which has been developed specifically to analyze and extract physical phenomena, providing exemplar code for training an ensemble of deep neural networks to produce the semantic segmentation of AFM data and functions for encoding and decoding local environments. We last described a combinatorial approach to analyze very noisy data with a densely covered substrate where the emergence of order for the protein liquid crystals could be elucidated. By combining the methods from Case 1 and 2, it was possible to obtain the center of mass and angle for each rod in the images and track the assembly of the rods over time into a 2D liquid crystal array on the surface of mica.

protein dynamics, solid-liquid interfaces, atomic ↗

DOE OSTI2018

Emergence of Kondo Resonance in Graphene Intercalated with Cerium

The interaction between a magnetic impurity, such as cerium (Ce) atom, and surrounding electrons has been one of the core problems in understanding many-body interaction in solid and its relation to magnetism. Kondo effect, the formation of a new resonant ground state with quenched magnetic moment, provides a general framework to describe many-body interaction in the presence of magnetic impurity. In this Letter, a combined study of angle-resolved photoemission (ARPES) and dynamic mean-field theory (DMFT) on Ce-intercalated graphene shows that Ce-induced localized states near Fermi energy, E F , hybridized with the graphene π-band, exhibit gradual increase in spectral weight upon decreasing temperature. The observed temperature dependence follows the expectations from the Kondo picture in the weak coupling limit. These results provide a novel insight how Kondo physics emerges in the sea of two-dimensional Dirac electrons.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Processing Effects on the Self-Assembly of Brush Block Polymer Photonic Crystals

Here,the self-assembly of poly(dimethylsiloxane)-b-poly(trimethylene carbonate) (PDMS-b-PTMC) bottlebrush block polymers was investigated under different processing conditions. Small-angle X-ray scattering (SAXS) and UV/Visible spectroscopy provided insight into the self-assembly and structure in response to heating and applied pressure. In the absence of applied pressure (i.e., before annealing), the PDMS-b-PTMC bottlebrush block polymers are white solids and adopt small, randomly oriented lamellar grains. Heating the materials to 140 °C in the absence of applied pressure appears to “lock in” the isotropic, short-range-ordered state, preventing the formation of the long-range-ordered lamellar structure responsible for photonic properties. Applying modest anisotropic pressure (3 psi) between parallel plates at ambient temperature orients the short-range lamellar grains; however, applied pressure alone does not produce long-range order. Only when the bottlebrush block polymers were heated (>100 °C) under modest pressure (3 psi) were long-range-ordered photonic crystals formed. Analysis of the SAXS data motivated analogies to liquid crystals and revealed the potential self-assembly pathway. These results provide insight into the structure and self-assembly of bottlebrush block polymers with low glass transition temperature side chains in response to different processing conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

An overview of selected current approaches to the characterization of aqueous inorganic clusters

This Perspective article highlights some of the traditional and non-traditional analytical tools that are currently used to characterize aqueous inorganic nanoscale clusters and polyoxometalate ions. The techniques discussed in this article include nuclear magnetic resonance spectroscopy (NMR), small angle X-ray scattering (SAXS), dynamic and phase analysis light scattering (DLS and PALS), Raman spectroscopy, and quantum mechanical computations (QMC). For each method we briefly describe how it functions and illustrate how these techniques are used to study cluster species in the solid state and in solution through several representative case studies. In addition to highlighting the utility of these techniques, we also discuss limitations of each approach and measures that can be applied to circumvent such limits as it pertains to aqueous inorganic cluster characterization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1977

The photometric functions of Phobos and Deimos. II - Surface photometry of Deimos

Mariner 9 television pictures of Deimos are used to study the uniformity of a certain photometric scattering parameter over the surface of the satellite. It is shown that the photometric data considered satisfy the reciprocity principle and that the Hapke-Irvine scattering law is adequate for describing the surface. Phase functions for Deimos are obtained from scans along the photometric equator, and the photometric behavior of the brightest and darkest areas on the satellite's disk is examined. The results indicate that the surface of Deimos is covered uniformly by a dark and texturally complex material whose photometric behavior is well-represented by the Hapke-Irvine law, that the intrinsic phase coefficient of this material is about 0.017 mag/deg over the phase-angle range from 20 to 80 deg, and that slightly brighter material is present near some craters. Since enhanced brightening was not observed at the specular point of the photometric equator in any of the pictures studied, it is concluded that large exposures of solid rock are absent from the Mars-facing side of Deimos.

Noland, M.↗

NASA NTRS1979

Measurement in multiphase reacting flows

A survey is presented of diagnostic techniques and measurements made in multiphase reacting flows. The special problems encountered by the presence of liquid droplets, soot and solid particles in high temperature chemically reacting turbulent environments are outlined. The principal measurement techniques that have been tested in spray flames are spark photography, laser anemometry, thermocouples and suction probes. Spark photography provides measurement of drop size, drop size distribution, drop velocity, and angle of flight. Photographs are analysed automatically by image analysers. Photographic techniques are reliable, inexpensive and proved. Laser anemometers have been developed for simultaneous measurement of velocity and size of individual particles in sprays under conditions of vaporization and combustion. Particle/gas velocity differentials, particle Reynolds numbers, local drag coefficients and direct measurement of vaporization rates can be made by laser anemometry. Gas temperature in sprays is determined by direct in situ measurement of time constants immediately prior to measurement with compensation and signal analysis by micro-processors. Gas concentration is measured by suction probes and gas phase chromatography. Measurements of particle size, particle velocity, gas temperature, and gas concentration made in airblast and pressure atomised liquid spray flames are presented.

Chigier, N. A.↗

NASA NTRS1980

Inlet flow distortion in turbomachinery. I - Comparison of theory and experiment in a transonic fan stage. II - A parameter study

In the present paper, a semi-actuator-disk theory is reviewed that was developed previously for the distorted inflow to a single-stage axial-flow compressor. Flow distortion occurs far upstream; it may be a distortion in stagnation temperature, stagnation pressure, or both. Losses, quasi-steady deviation angles, and reference incidence correlations are included in the analysis, and both subsonic and transonic relative Mach numbers are considered. The theory is compared with measurements made in a transonic fan stage, and a parameter study is carried out to determine the influence of solidity on the attenuation of distortions in stagnation pressure and stagnation temperature.

Seidel, B. S.↗

NASA NTRS1988

Application of Navier-Stokes analysis to stall flutter

A solution procedure was developed to investigate the two-dimensional, one- or two-dimensional flutter characteristics of arbitrary airfoils. This procedure requires a simultaneous integration in time of the solid and fluid equations of motion. The fluid equations of motion are the unsteady compressible Navier-Stokes equations, solved in a body-fitted moving coordinate system using an approximate factorization scheme. The solid equations of motion are integrated in time using an Euler implicit scheme. Flutter is said to occur if small disturbances imposed on the airfoil attitude lead to divergent oscillatory motions at subsequent times. The flutter characteristics of airfoils in subsonic speed at high angles of attack and airfoils in high subsonic and transonic speeds at low angles of attack are investigated. The stall flutter characteristics are also predicted using the same procedure.

Wu, J. C.↗

NASA NTRS1990

Integrated Electro-optical Laser-Beam Scanners

Scanners using solid-state devices compact, consume little power, and have no moving parts. Integrated electro-optical laser scanner, in conjunction with external lens, points outgoing beam of light in any number of different directions, depending on number of upper electrodes. Offers beam-deflection angles larger than those of acousto-optic scanners. Proposed for such diverse applications as nonimpact laser printing, color imaging, ranging, barcode reading, and robotic vision.

Boord, Warren T.↗

NASA NTRS1956

Flight Investigation of the Performance of a Two-stage Solid-propellant Nike-deacon (DAN) Meteorological Sounding Rocket

A flight investigation of two Nike-Deacon (DAN) two-stage solid-propellant rocket vehicles indicated satisfactory performance may be expected from the DAN meteorological sounding rocket. Peak altitudes of 356,000 and 350,000 feet, respectively, were recorded for the two flight tests when both vehicles were launched from sea level at an elevation angle of 75 degrees. Performance calculations based on flight-test results show that altitudes between 358,000 feet and 487,000 feet may be attained with payloads varying between 60 pounds and 10 pounds.

MISSILES, SPECIFIC TYPES↗

NASA NTRS1994

Diagenetic Microcrystalline Opal Varieties from the Monterey Formation, CA: HRTEM Study of Structures and Phase Transformation Mechanisms

Microcrystalline opal varieties form as intermediary precipitates during the diagenetic transformation of biogenically precipitated non-crystalline opal (opal-A) to microquartz. With regard to the Monterey Formation of California, X-ray powder diffraction studies have shown that a decrease in the primary d-spacing of opal-CT toward that of cristobalite occurs with increasing diagenesis. The initial timing of opal-CT/quartz formation and the value of the primary opal-CT d-spacing, are influenced by the sediment. lithology. Transmission electron microscopy methods (CTEM/HRTEM) were used to investigate the structure of the diagenetic phases and establish transformation mechanisms between the varieties of microcrystalline opals in charts and porcelanites from the Monterey Formation. HRTEM images revealed that the most common fibrous varieties of microcrystalline opals contain varying amounts of structural disorder. Finite lamellar units of cristobalite-and tridymite-type. layer sequences were found to be randomly stacked in a direction perpendicular to the fiber axis. Disordered and ordered fibers were found to have coprecipitated within the same radial fiber bundles that formed within the matrix of the Most siliceous samples. HRTEM images, which reveal that the fibers within radial and lepispheric fiber bundles branch non-crystallographically, support an earlier proposal that microspheres in chert grow via a spherulitic growth mechanism. A less common variety of opal-CT was found to be characterized by non-parallel (low-angle) stacking sequences that often contain twinned lamellae. Tabular-shaped crystals of orthorhombic tridymite (PO-2) were also identified in the porcelanite samples. A shift in the primary d-spacing of opal-CT has been interpreted as an indication of solid-state ordering g toward a predominantly cristobalite structure, (opal-C). Domains of opal-C were identified as topotactically-oriented overgrowths on discrete Sections of opal-CT fibers and as lamellar domains within relict opal-CT fibers. These findings indicate that the type of transformation mechanism depends upon the primary structural characteristics of the authigenic opaline. varieties that are in turn influenced by the sediment lithology.

Cady, Sherry L.↗

DOE OSTI2013

Dual-Remote Raman Technology for In-Situ Identification of Tank Waste

A new Raman spectroscopic system for in-situ identification of the composition of the solid nuclear tank waste is being developed by collaborative effort between Pacific Northwest National Laboratory (PNNL) and EIC, Inc. The recent advancements in the Raman technology allow probing the chemical composition of the tank waste without sample collection. In the newly tested configuration, the Raman probe is installed on the top of the tank riser and sends the incident laser beam to the bottom of the tank, 10 – 70 feet away. The returning light containing chemical information is collected by the Raman probe and transmits it via fiber optic cable to the spectrometer located outside the tank farm area. This dual remote technology significantly expands currently limited options for the safe rapid in-situ identification of the solid tank waste needed for the retrieval decisions. The developed Raman system was extensively tested for acceptability prior tank farm deployment. This testing included calibration of the system with the respect of the distance between the Raman probe and the sample, incident laser beam angle, and presence of the optical interferences. The Raman system was successfully deployed to C-111 tank at the US DOE Hanford site. As the result of this deployment, the composition of the hardpan at the bottom of C-111 tank was identified. Further development of the dual-remote Raman technology will provide a significant safety enhancement eliminating the potential of personnel radiation exposure associated with the grab sample collection and expands options of the rapid and cost-effective in-situ chemical analysis of the tank waste.

in-situ Hanford tank, Raman measurement↗

DOE OSTI2013

Dual-Remote Raman Technology for In-Situ Identification of Tank Waste - 13549

A new Raman spectroscopic system for in-situ identification of the composition of solid nuclear tank waste is being developed by collaborative effort between Pacific Northwest National Laboratory (PNNL) and EIC Laboratories, Inc. The recent advancements in Raman technology allow probing the chemical composition of the tank waste without sample collection. In the newly tested configuration, the Raman probe is installed on the top of the tank riser and sends the incident laser beam to the bottom of the tank, 10 - 70 feet away. The returning light containing chemical information is collected by the Raman probe and is transmitted via fiber optic cable to the spectrometer located outside the tank farm area. This dual remote technology significantly expands currently limited options for the safe rapid in-situ identification of the solid tank waste needed for the retrieval decisions. The developed Raman system was extensively tested for acceptability prior to tank farm deployment. This testing included calibration of the system with respect of the distance between the Raman probe and the sample, incident laser beam angle, and presence of the optical interferences. The Raman system was successfully deployed on Tank C-111 at the US DOE Hanford site. As the result of this deployment, the composition of the hardpan at the bottom of C-111 tank was identified. Further development of the dual-remote Raman technology will provide a significant safety enhancement eliminating the potential of personnel radiation exposure associated with the grab sample collection and expands options of the rapid and cost-effective in-situ chemical analysis of the tank waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Characterization of MoS 2 films via simultaneous grazing incidence X-ray diffraction and grazing incidence X-ray fluorescence (GIXRD/GIXRF)

Physical vapor deposited (PVD) molybdenum disulfide (nominal composition MoS 2 ) is employed as a thin film solid lubricant for extreme environments where liquid lubricants are not viable. The tribological properties of MoS 2 are highly dependent on morphological attributes such as film thickness, orientation, crystallinity, film density, and stoichiometry. These structural characteristics are controlled by tuning the PVD process parameters, yet undesirable alterations in the structure often occur due to process variations between deposition runs. Nondestructive film diagnostics can enable improved yield and serve as a means of tuning a deposition process, thus enabling quality control and materials exploration. Grazing incidence X-ray diffraction (GIXRD) for MoS 2 film characterization provides valuable information about film density and grain orientation (texture). However, the determination of film stoichiometry can only be indirectly inferred via GIXRD. The combination of density and microstructure via GIXRD with chemical composition via grazing incidence X-ray fluorescence (GIXRF) enables the isolation and decoupling of film density, composition, and microstructure and their ultimate impact on film layer thickness, thereby improving coating thickness predictions via X-ray fluorescence. We have augmented an existing GIXRD instrument with an additional X-ray detector for the simultaneous measurement of energy-dispersive X-ray fluorescence spectra during the GIXRD analysis. This combined GIXRD/GIXRF analysis has proven synergetic for correlating chemical composition to the structural aspects of MoS 2 films provided by GIXRD. We present the usefulness of the combined diagnostic technique via exemplar MoS 2 film samples and provide a discussion regarding data extraction techniques of grazing angle series measurements.

MoS2↗

DOE OSTI2023

Fundamental studies of thermal and electrical transport in microporous metal-organic frameworks

In this work, we established porous metal-organic frameworks (MOFs) as designer conductors of electrons and ions relevant to fundamental research and technological applications. MOFs are porous, crystalline materials composed of organic linkers and inorganic nodes. While most MOFs are insulating with respect to ionic and electronic charge carriers, a number of exceptions have been reported in recent years. Electrically conductive MOFs are highly attractive for applications including electrical energy storage, chemiresistive sensing, and optoelectronics because of their high surface areas and tunable chemical properties. Ion-conducting MOFs are desirable for the synthetically tunable size, shape, and polarity of their pore environments, allowing for the tailored development of solid state electrolytes for metal-ion batteries. We developed systematic strategies for the design of MOFs that conduct ions and electrons. For each objective, we leveraged the versatile chemistry of these materials to obtain frameworks with targeted properties towards electronic or ionic charge carriers. We studied the factors that govern electrical transport in MOFs in order to gain fundamental knowledge of this emerging class of materials. We took several approaches to tackle this problem from multiple angles. Namely, we synthesized and characterized new frameworks, investigated post-synthetic modifications to enhance conductivity, and correlated theory and experiment to uncover new mechanistic findings. These results, which put forth new design principles for conductive MOFs, move the field toward one of the DOE Basic Energy Sciences Grand Challenges: to “design and perfect atom- and energy-efficient synthesis of revolutionary new forms of matter with tailored properties.” In addition to investigating the movement of electrons in MOFs, we also studied the movement of other charged species in MOFs, such as protons, lithium, and magnesium. Proton-conducting frameworks could be appealing materials for solid state electrolytes in fuel cells. In addition, they contain crystallographically defined proton-conducting channels, in contrast with state-of-the-art polymer membranes such as Nafion, which are amorphous. Controlling pore size and polarity in MOFs can thus shed light on proton and other ion transport mechanisms, ultimately enabling the design of more advanced electrolyte materials and potentially novel electrical energy storage materials.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Evaluation of polarization rotation in the scattering responses from individual semiconducting oxide nanorods

We investigate the interaction of visible light with the solid matters of semiconducting oxide nanorods (NRs) of zinc oxide (ZnO), indium tin oxide (ITO), and zinc tin oxide (ZTO) at the single nanomaterial level. We subsequently identify an intriguing, material-dependent phenomenon of optical rotation in the electric field oscillation direction of the scattered light by systematically controlling the wavelength and polarization direction of the incident light, the NR tilt angle, and the analyzer angle. This polarization rotation effect in the scattered light is repeatedly observed from the chemically pure and highly crystalline ZnO NRs, but absent on the chemically doped NR variants of ITO and ZTO under all measurement circumstances. We further elucidate that the phenomenon of polarization rotation detected from single ZnO NRs is affected by the NR tilt angle, while the phenomenon itself occurs irrespective of the wavelength and incident polarization direction of the visible light. Combined with the widespread optical and optoelectronic use of the semiconducting oxide nanomaterials, these efforts may provide much warranted fundamental bases to tailor material-specific, single nanomaterial-driven, optically modulating functionalities which, in turn, can be beneficial for the realization of high-performance integrated photonic circuits and miniaturized bio-optical sensing devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2019

Direct Visualization of Independent Ta Centers Supported on Two-Dimensional TiO 2 Nanosheets

Highly dispersed, supported oxides are ubiquitous solid catalysts but can be challenging to characterize with atomic precision. Here, it is shown that crystalline anatase TiO 2 nanosheets (~5 nm thick) are ideal supports for imaging highly dispersed active sites. Ta cations were deposited by several routes, and high-resolution high angle annular dark-field scanning transmission electron microscopy was used to determine the location of Ta with respect to the TiO 2 lattice and quantify Ta–Ta distances. In the best case, it is shown that >80% of Ta atoms are isolated from one another, whereas other techniques are blind to this critical catalytic property or give only qualitative estimates. TiO 2 nanosheets may prove to be a useful platform for other types of catalysis studies.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2024

Insights into controlling bacterial cellulose nanofiber film properties through balancing thermodynamic interactions and colloidal dynamics

In recent years, nanocellulose has emerged as a sustainable and environmentally friendly alternative to traditional petroleum-derived structural polymers. Sourced either from plants, algae, or bacteria, nanocellulose can be processed into colloid, gel, film and fiber forms. However, the required fundamental understanding of process parameters that govern the morphology and structure–property relationships of nanocellulose systems, from colloidal suspensions to bulk materials, has not been developed and generalized for all forms of cellulose. This further hinders the more widespread adoption of this biopolymer in applications. Our study investigates the dispersion of cellulose nanofibers (CNFs) produced by a bacterial–yeast co-culture, in solvents, highlighting the role of thermodynamic interactions in influencing their colloidal behavior. By adjusting Hansen solubility parameters, we controlled the thermodynamic relationship between CNFs and solvents across various concentrations, studying the dilute to semi-dilute regimes. Rheological measurements revealed that the threshold at which a concentration-based regime transition occurs is distinctly solvent-dependent. Complementing rheological analysis with small angle X-ray scattering and zeta potential measurements, our findings reveal that enhancing CNF–solvent interactions increases excluded volume in the dilute regime, emphasizing the importance of the balance between fiber–fiber and fiber–solvent interactions. Moreover, we investigated the transition from colloidal to solid state by creating films from dispersions with varying interaction parameters in semi-dilute regimes. Through mechanical testing and scanning electron microscopy imaging of the fracture surfaces, we highlight the significance of electrokinetic effects in such transitions, as dispersions with higher electrokinetic stabilization gave rise to stronger and tougher films despite having less favorable thermodynamic interaction parameters. Finally, our work provides insights into the thermodynamic and electrokinetic interplay that governs bacterial CNF dispersion, offering a foundation for future application and a deeper understanding of nanocellulose's colloidal and structure-property relationships.

59 BASIC BIOLOGICAL SCIENCES↗