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DOE OSTI2023

Hierarchical Self-Assembly of Carbon Dots into High-Aspect-Ratio Nanowires

Here, we report a spontaneous and hierarchical self-assembly mechanism of carbon dots prepared from citric acid and urea into nanowire structures with large aspect ratios (>50). Scattering-type scanning near-field optical microscopy (s-SNOM) with broadly tunable mid-IR excitation was used to interrogate details of the self-assembly process by generating nanoscopic chemical maps of local wire morphology and composition. s-SNOM images capture the evolution of wire formation and the complex interplay between different chemical constituents directing assembly over the nano- to microscopic length scales. We propose that residual citrate promotes tautomerization of melamine surface functionalities to produce supramolecular shape synthons comprised of melamine-cyanurate adducts capable of forming long-range and highly directional hydrogen-bonding networks. This intrinsic, heterogeneity-driven self-assembly mechanism reflects synergistic combinations of high chemical specificity and long-range cooperativity that may be harnessed to reproducibly fabricate functional structures on arbitrary surfaces.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2017

Shape Effect Undermined by Surface Reconstruction: Ethanol Dehydrogenation over Shape-Controlled SrTiO 3 Nanocrystals

For this research, to gain an in-depth understanding of the surface properties relevant for catalysis using ternary oxides, we report the acid–base pair reactivity of shape-controlled SrTiO 3 (STO) nanocrystals for the dehydrogenation of ethanol. Cubes, truncated cubes, dodecahedra, and etched cubes of STO with varying ratios of (001) and (110) crystal facets were synthesized using a hydrothermal method. Low-energy ion scattering (LEIS) analysis revealed that the (001) surface on cubes of STO is enriched with SrO due to surface reconstruction, resulting in a high ratio of strong base sites. Chemical treatment with dilute nitric acid to form etched cubes of STO resulted in a surface enriched with Ti cations and strong acidity. Furthermore, the strength and distribution of surface acidic sites increase with the ratio of (110) facet from cubes to truncated cubes to dodecahedra for STO. Kinetic, isotopic, and spectroscopy methods show that the dehydrogenation of ethanol proceeds through the facile dissociation of the alcohol group, followed by the cleavage of the C α –H bond, which is the rate-determining step. Co-feeding of various probe molecules during catalysis, such as NH 3 , 2,6-di-tert-butylpyridine, CO 2 , and SO 2 , reveals that a pair of Lewis acid site and basic surface oxygen atom is involved in the dehydrogenation reaction. The surface density of acid–base site pairs was measured using acetic acid as a probe molecule, allowing initial acetaldehyde formation turnover rates to be obtained. Comparison among various catalysts reveals no simple correlation between ethanol turnover rate and the percentage of either surface facet ((001) or (110)) of the STO nanocrystals. Instead, the reaction rate is found to increase with the strength of acid sites but reversely with the strength of base sites. The acid–base property is directly related to the surface composition as a result from different surface reconstruction behaviors of the shaped STO nanocrystals. Lastly, the finding in this work underscores the importance of characterizing the top surface compositions and sites properties when assessing the catalytic performance of shape-controlled complex oxides such as perovskites.

(001) facet↗

DOE OSTI2021

Product Characteristics and Synergy Study on Supercritical Methanol Liquefaction of Lignocellulosic Biomass and Plastic

Bio-oil originating from lignocellulosic biomass (LCB) is a potential next-generation fuel because of its abundant, renewable, and sustainable resources compared to other types. However, these bio-oils are typically of low quality compared to petroleum-derived oils due to their low calorific value, high acidity, and oxygen content. This work intends to provide a feasible method for producing hydrocarbon-rich oils by supercritical methanol (scMeOH) coliquefaction of LCB and plastic waste. Both rice straw (RS) and linear low-density polyethylene (LLDPE) are coliquefied under 300 °C for 60 min in scMeOH at various RS/LLDPE mass ratios of 2:1, 1:1, and 1:2. Positive effects were found in terms of oil yield and fuel quality, such as higher hydrocarbons content and calorific value. The oil yield increased from 26.72 to 30.07 wt % with LLDPE addition of 67%. Around 79.15–92.24% of the oil was hydrocarbons, phenols, ketones, and diverse functional group compounds. The complex compounds led to various degrees of the synergetic effect on oil chemical compositions. Among various RS/LLDPE ratios in this work, RS/LLDPE of 1:2 was supposed to be an optimal ratio for hydrocarbon-rich fuel production because it presented the highest oil yield of 30.07 wt % and quality-high oil with 71.42% hydrocarbons. In addition, scMeOH coliquefaction of LCB and plastic waste shows a synergetic effect on the improvement of carbon and hydrogen contents in solid products. These results indicate that scMeOH coliquefaction of LCB with plastic is a feasible and promising means to improve fuel quality and also to realize the thermal recycling of plastic wastes.

09 BIOMASS FUELS↗

DOE OSTI2018

Structural Characterization of Loblolly Pine Derived Biochar by X-ray Diffraction and Electron Energy Loss Spectroscopy

Biochar from lignocellulosic biomass is emerging as a sustainable material with versatile applications, but its detailed properties are poorly understood because of its structural complexity. We propose a biochar structural development model based on experimental results including composition analysis, surface area and pore analysis, X-ray diffraction analysis, electron microscopy imaging, and electron energy loss spectroscopy. Loblolly pine derived biochars were produced at different carbonization temperatures between 300 to 1000 °C. Fixed carbon, sp 2 content, and number of graphene layers increased with increased carbonization temperature. Alternating average C–C bond length, interlayer spacing distance, and layer coherence length were observed. Bulk plasmon excitation energy was correlated to the average C–C bond length, and it serves as a good indicator of the carbon structure development when compared to the perfect graphitic carbon structure. On the basis of the experimental results, four different structural development phases are identified, which provide a comprehensive understanding of biochar nanocarbon crystallite development. Unlike previous biochar structure models, which proposed radially growing polyaromatic carbon crystallite, we propose a lengthwise growing polyaromatic carbon crystallite model. Furthermore, this experiment-based biochar model should be helpful when determining the structure of unknown biomass-derived carbon materials and disordered pyrolytic carbon materials.

Biomass carbonization↗

DOE OSTI2020

Polysaccharide niche partitioning of distinct Polaribacter clades during North Sea spring algal blooms

Massive releases of organic substrates during marine algal blooms trigger growth of many clades of heterotrophic bacteria. Algal polysaccharides represent the most diverse and structurally complex class of these substrates, yet their role in shaping the microbial community composition is poorly understood. We investigated, whether polysaccharide utilization capabilities contribute to niche differentiation of Polaribacter spp. (class Flavobacteriia; known to include relevant polysaccharidedegraders) that were abundant during 2009–2012 spring algal blooms in the southern North Sea. We identified six distinct Polaribacter clades using phylogenetic and phylogenomic analyses, quantified their abundances via fluorescence in situ hybridization, compared metagenome-assembled genomes, and assessed in situ gene expression using metaproteomics. Four clades with distinct polysaccharide niches were dominating. Polaribacter 2-a comprised typical first responders featuring small genomes with limited polysaccharide utilization capacities. Polaribacter 3-a were abundant only in 2010 and possessed a distinct sulfated α-glucoronomannan degradation potential. Polaribacter 3-b responded late in blooms and had the capacity to utilize sulfated xylan. Polaribacter 1-a featured high numbers of glycan degradation genes and were particularly abundant following Chattonella algae blooms. These results support the hypothesis that sympatric Polaribacter clades occupy distinct glycan niches during North Sea spring algal blooms.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

Hetero-Orbital Two-Component Fractional Quantum Hall States in Bilayer Graphene

A two-dimensional electron system exposed to a strong magnetic field produces a plethora of strongly interacting fractional quantum Hall (FQH) states, the complex topological orders of which are revealed through exotic emergent particles, such as composite fermions, and fractionally charged Abelian and non-Abelian anyons. Much insight has been gained by the study of multicomponent FQH states, where spin and pseudospin indices of the electron contribute additional correlation. Traditional multicomponent FQH states develop in situations where the components share the same orbital states and the resulting interactions are pseudospin independent; this homo-orbital nature is also crucial to their theoretical understanding. Here, we study “hetero-orbital” two-component FQH states, in which the orbital index is part of the pseudospin, rendering the multicomponent interactions strongly SU(2) anisotropic in the pseudospin space. Such states, obtained in bilayer graphene at the isospin transition between 𝑁 = 0 and 𝑁 = 1 electron Landau levels, are markedly different from previous homo-orbital two-component FQH states. In particular, we observe strikingly different behaviors for the parallel-vortex and reverse-vortex attachment composite fermion states, and an anomalously strong two-component 2/5 state over a wide range of magnetic field before it abruptly disappears at a high field. Our findings, combined with detailed theoretical calculations, reveal the surprising robustness of the hetero-orbital FQH effects, significantly enriching our understanding of FQH physics in this novel regime.

Bilayer graphene↗

DOE OSTI2019

Intrinsic anisotropy versus effective pinning anisotropy in YBa 2 Cu 3 O 7 thin films and nanocomposites

The intrinsic and effective anisotropies, both in the liquid and solid vortex regimes, of YBa 2 Cu 3 O 7 (YBCO) pristine and nanocomposite thin films have been investigated in this paper. Angular resistivity measurements under varying fields and temperatures were performed to characterize the intrinsic vs effective anisotropy of samples in the regime of long-range vortex displacements. The effective anisotropy γ eff was determined from the scaling of the irreversibility line, applying the Blatter approach developed for uniaxial anisotropic superconductors. Resistive measurements in flux flow were utilized, in addition to H c2 measurements in ultrahigh-fields, to determine the intrinsic anisotropy mass γ , enabling the study of a large number of samples with varied nanoparticle compositions. In order to access the intrinsic anisotropy in the vortex solid phase, complex impedance measurements at high microwave frequencies were performed, allowing us to access the flux-flow intrinsic anisotropy in the regime of very short vortex oscillations within the pinning potential wells. Results show that while the effective anisotropy γ eff decays as the nanoparticles-induced nanostrain in the YBCO films increases, the intrinsic anisotropy γ (determined both in dc and at microwave frequency) remains unaltered.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2024

Leveraging Additive Manufacturing to Fabricate High Temperature Alloys With Co-Designed Mechanical Properties and Environmental Resistance

A paradigm shift in the traditional sequential design approaches is critically essential to create application-specific hierarchical and multifunctional materials with superior long-term performance for next-generation energy technologies involving extreme environments. In the current work, we aim to leverage the flexibility and geometric/compositional complexity offered by additive manufacturing to demonstrate this new approach by codesigning a compositionally graded Ni-based alloy for molten salts\sCO 2 heat exchangers to enable mitigation of environmental degradation of surfaces exposed to molten halide salts, while simultaneously suppressing the consequent deterioration in mechanical stability. Further, thermokinetic modeling describing the underlying physics of thermally- and environmentally induced spatiotemporal compositional and microstructural evolution will be employed to predict the parameter space of material deposition processes and precisely identify the required composition gradient. Preliminary corrosion and mechanical testing of the dual material demonstrated the potential of the material to replace existing solid solution strengthened materials for this application.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Autonomous discovery of emergent morphologies in directed self-assembly of block copolymer blends

The directed self-assembly (DSA) of block copolymers (BCPs) is a powerful approach to fabricate complex nanostructure arrays, but finding morphologies that emerge with changes in polymer architecture, composition, or assembly constraints remains daunting because of the increased dimensionality of the DSA design space. Here, we demonstrate machine-guided discovery of emergent morphologies from a cylinder/lamellae BCP blend directed by a chemical grating template, conducted without direct human intervention on a synchrotron x-ray scattering beamline. This approach maps the morphology-template phase space in a fraction of the time required by manual characterization and highlights regions deserving more detailed investigation. These studies reveal localized, template-directed partitioning of coexisting lamella- and cylinder-like subdomains at the template period length scale, manifesting as previously unknown morphologies such as aligned alternating subdomains, bilayers, or a “ladder” morphology. This work underscores the pivotal role that autonomous characterization can play in advancing the paradigm of DSA.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Considering the Lives of Microbes in Microbial Communities

ABSTRACT Over the last decades, sequencing technologies have transformed our ability to investigate the composition and functional capacity of microbial communities. Yet, critical questions remain about these complex systems that cannot be addressed by the bulk, community-averaged data typically provided by sequencing methods. In this Perspective, I propose that future advances in microbiome research will emerge from considering “the lives of microbes”: we need to create methods to explicitly interrogate how microbes exist and interact in native-setting-like microenvironments. This approach includes developing approaches that expose the phenotypic heterogeneity of microbes; exploring the effects of coculture cues on cellular differentiation and metabolite production; and designing visualization systems that capture features of native microbial environments while permitting the nondestructive observation of microbial interactions over space and time with single-cell resolution.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2023

Interrogating the role of the milk microbiome in mastitis in the multi-omics era

There is growing interest in a functional understanding of milk-associated microbiota as there is ample evidence that host-associated microbial communities play an active role in host health and phenotype. Mastitis, characterized by painful inflammation of the mammary gland, is prevalent among lactating humans and agricultural animals and is associated with significant clinical and economic consequences. The etiology of mastitis is complex and polymicrobial and correlative studies have indicated alterations in milk microbial community composition. Recent evidence is beginning to suggest that a causal relationship may exist between the milk microbiota and host phenotype in mastitis. Multi-omic approaches can be leveraged to gain a mechanistic, molecular level understanding of how the milk microbiome might modulate host physiology, thereby informing strategies to prevent and ameliorate mastitis. In this paper, we review existing studies that have utilized omics approaches to investigate the role of the milk microbiome in mastitis. We also summarize the strengths and challenges associated with the different omics techniques including metagenomics, metatranscriptomics, metaproteomics, metabolomics and lipidomics and provide perspective on the integration of multiple omics technologies for a better functional understanding of the milk microbiome.

metabolomics↗

DOE OSTI2024

N-Doped Graphene (N-G)/MOF(ZIF-8)-Based/Derived Materials for Electrochemical Energy Applications: Synthesis, Characteristics, and Functionality

In recent years, graphene-type materials originating from metal–organic frameworks (MOFs) or integrated with MOFs have exhibited notable performances across various applications. However, a comprehensive understanding of these complex materials and their functionalities remains obscure. While some studies have reviewed graphene/MOF composites from different perspectives, due to their structural–functional intricacies, it is crucial to conduct more in-depth reviews focusing on specific sets of graphene/MOF composites designed for particular applications. In this review, we thoroughly investigate the syntheses, characteristics, and performances of N-G/MOF(ZIF-8)-based/derived materials employed in electrochemical energy conversion and storage systems. Special attention is given to realizing their fundamental functionalities. The discussions are divided into three segments based on the application of N-G/ZIF-8-based/derived materials as electrode materials for batteries, electrodes for electrochemical capacitors, and electrocatalysts. As electrodes for batteries, N-G/MOF(ZIF-8) materials can mitigate issues like an electrode volume expansion for Li-ion batteries and the ‘shuttle effect’ for Li-S batteries. As electrodes for electrochemical capacitors, these materials can considerably improve the ion transfer rate and electronic conductivity, thereby enhancing the specific capacitance while maintaining the structural stability. Also, it was observed that these materials could occasionally outperform standard platinum-based catalysts for the electrochemical oxygen reduction reaction (ORR). The reported electrochemical performances and structural parameters of these materials were carefully tabulated in uniform units and scales. Through a critical analysis of the present synthesis trends, characteristics, and functionalities of these materials, specific aspects were identified that required further exploration to fully utilize their inherent capabilities.

Electrochemistry↗

DOE OSTI2019

Chlorine-36/beryllium-10 burial dating of alluvial fan sediments associated with the Mission Creek strand of the San Andreas Fault system, California, USA

We utilize cosmogenic-nuclide burial dating using the 36 Cl -in-K-feldspar / /10 Be -in-quartz pair in fluvially transported granitoid clasts to determine the age of alluvial sediment displaced by the Mission Creek strand of the San Andreas Fault in southern California. Due to the half-lives of 36 Cl and /10 Be are more different than those of the commonly used 26 Al$^{/10}$Be pair, 36 Cl /10 Be burial dating should be applicable to sediments in the range ca. 0.2–0.5 Ma, which is too young to be accurately dated with the 26 Al$^{/10}$Be pair, and should be more precise for Middle and Late Pleistocene sediments in general. However, using the 36 Cl$^{/10}$Be pair is more complex because the 36 Cl$^{/10}$Be production ratio varies with the chemical composition of each sample. We use 36 Cl$^{/10}$Be measurements in samples of granodiorite exposed at the surface at present to validate calculations of the 36 Cl$^{/10}$Be production ratio in this lithology, and then we apply this information to determine the burial age of alluvial clasts of the same lithology. This particular field area presents the additional obstacle to burial dating (which is not specific to the 36 Cl$^{/10}$Be pair, but would apply to any) that most buried alluvial clasts are derived from extremely rapidly eroding parts of the San Bernardino Mountains and have correspondingly extremely low nuclide concentrations, the majority of which most likely derive from nucleogenic (for 36 Cl ) and post-burial production. Even though this precludes accurate burial dating of many clasts, data from surface and subsurface samples with higher nuclide concentrations, originating from lower-erosion-rate source areas, show that the age of upper Cabezon Formation alluvium is 260 ka. This is consistent with stratigraphic age constraints as well as independent estimates of long-term fault slip rates, and it highlights the potential usefulness of the 36 Cl$^{/10}$Be pair for dating Upper and Middle Pleistocene clastic sediments.

58 GEOSCIENCES↗

NASA NTRS1970

Nuclear alkylated pyridine aldehyde polymers and conductive compositions thereof

A thermally stable, relatively conductive polymer was disclosed. The polymer was synthesized by condensing in the presence of catalyst a 2, 4, or 6 nuclear alklylated 2, 3, or 4 pyridine aldehyde or quaternary derivatives thereof to form a polymer. The pyridine groups were liked by olefinic groups between 2-4, 2-6, 2-3, 3-4, 3-6 or 4-6 positions. Conductive compositions were prepared by dissolving the quaternary polymer and an organic charge transfer complexing agent such as TCNQ in a mutual solvent such as methanol.

Rembaum, A.↗

NASA NTRS1985

Study of the physical properties of crystalline rocks in the southeast Voronezh anteclise

The physical properties of rocks, in the crystalline mass of the Voronezh anteclise, were studied. The study of the physical properties of rocks is important for the improvement of geophysical methods for mapping crystalline rocks in the foundation and exploration of different geological objects which are associated with the crystalline foundation, covered by the sedimentary mantle. It is found that: (1) rocks in the crystalline foundation are very different in physical properties; (2) the physical properties are closely related to their substance composition and genesis; (3) petrographic properties give clues of rock afficiation to certain complexes; and (4) physical and magnetic properties should be examined by petrography, chemical and X-ray analysis.

Dmitriyevskiy, V. S.↗

NASA NTRS1984

Current research on shear buckling and thermal loads with PASCO - Panel analysis and sizing code

The stiffened composite structural panel analysis and sizing code designated 'PASCO' encompasses both the generality required for the exploitation of composite materials' design flexibility and an accurate buckling analysis for the detection of complex buckling modes. PASCO can accordingly design for buckling, frequency, material strength, and panel stiffness requirements. Attention is given to an additional thermal loading design capability. Design studies illustrate the importance of the multiple load condition capability when thermal loads are present.

Stroud, W. J.↗

NASA NTRS1985

Computational structural mechanics: A new activity at the NASA Langley Research Center

Complex structures considered for the late 1980's and early 1990's include composite primary aircraft structures and the space station. These structures are much more difficult to analyze than today's structures and necessitate a major upgrade in computerized structural analysis technology. A major research activity in computational structural mechanics (CSM) was initiated. The objective of the CSM activity is develop advanced structural analysis technology that will exploit modern and emerging computers such as computers with vector and/or parallel processing capabilities. The three main research activities underway in CSM include: (1) structural analysis methods development; (2) a software testbed for evaluating the methods; and (3) numerical techniques for parallel processing computers. The motivation and objectives of the CSM activity are presented and CSM activity is described. The current CSM research thrusts, and near and long term CSM research thrusts are outlined.

Knight, N. F., Jr.↗

NASA NTRS1988

AGT (Advanced Gas Turbine) technology project

An overall summary documentation is provided for the Advanced Gas Turbine Technology Project conducted by the Allison Gas Turbine Division of General Motors. This advanced, high risk work was initiated in October 1979 under charter from the U.S. Congress to promote an engine for transportation that would provide an alternate to reciprocating spark ignition (SI) engines for the U.S. automotive industry and simultaneously establish the feasibility of advanced ceramic materials for hot section components to be used in an automotive gas turbine. As this program evolved, dictates of available funding, Government charter, and technical developments caused program emphases to focus on the development and demonstration of the ceramic turbine hot section and away from the development of engine and powertrain technologies and subsequent vehicular demonstrations. Program technical performance concluded in June 1987. The AGT 100 program successfully achieved project objectives with significant technology advances. Specific AGT 100 program achievements are: (1) Ceramic component feasibility for use in gas turbine engines has been demonstrated; (2) A new, 100 hp engine was designed, fabricated, and tested for 572 hour at operating temperatures to 2200 F, uncooled; (3) Statistical design methodology has been applied and correlated to experimental data acquired from over 5500 hour of rig and engine testing; (4) Ceramic component processing capability has progressed from a rudimentary level able to fabricate simple parts to a sophisticated level able to provide complex geometries such as rotors and scrolls; (5) Required improvements for monolithic and composite ceramic gas turbine components to meet automotive reliability, performance, and cost goals have been identified; (6) The combustor design demonstrated lower emissions than 1986 Federal Standards on methanol, JP-5, and diesel fuel. Thus, the potential for meeting emission standards and multifuel capability has been initiated; (7) Small turbine engine aerodynamic and mechanical design capability has been initiated; and (8) An infrastructure of manpower, facilities, materials, and fabrication capabilities has been established which is available for continued development of ceramic component technology in gas turbine and other heat engines.

Source record↗