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All sourcesNASA NTRSDOE OSTI
NASA NTRSDate not supplied

Natural Fiber Simulations and Analysis for Composites

As the U.S. government and the aviation industry strive to achieve net-zero carbon emissions by 2050, the Sustainable Manufacturing of Aircraft (SUMAC) project, supported by the Convergent Aeronautics Solutions (CAS) program of the National Aeronautics and Space Administration (NASA), aims to develop sustainably derived thermoplastic composites and manufacturing technologies for future aviation. A multidisciplinary team of experts drives this initiative through a collective effort. The team’s key focus areas are sustainably derived thermoplastic resins, natural fiber reinforcement, composite manufacturing, structural health monitoring, computational materials modeling, and systems analysis. This presentation will give an overview of the SUMAC project. Fiber-scale microscopy analysis characterized fiber cross sections finding that hemp and flax fibers are very deformable and non-circular (circularities of 0.2 were observed), and diameters range from submicron to 20 μm. Fiber shapes range from flattened, with aspect ratios Rlong/Rshort up to 5, to round, Rlong/Rshort =1. And Fiber core perimeters, which likely drives deformability, were calculated Pcore=7 μm. Explicit-fiber yarn simulations, parameterized from single-fiber measurements, resolved and identified slack as a cause for yarn strain-hardening tensile behavior. The bonded network model of PLA, PHA and PA11 resins captures tensile behavior, and can model an infused weave. Computational models of the weave unit cells matched the pattern (including plain, twill and triaxial braid), yarn ply (1to 2), and yarn twist from optical microscopy.

thermoplastic↗
NASA NTRSDate not supplied

Natural Fiber Simulations and Analysis for Composites

As the U.S. government and the aviation industry strive to achieve net-zero carbon emissions by 2050, the Sustainable Manufacturing of Aircraft (SUMAC) project, supported by the Convergent Aeronautics Solutions (CAS) program of the National Aeronautics and Space Administration (NASA), aims to develop sustainably derived thermoplastic composites and manufacturing technologies for future aviation. A multidisciplinary team of experts drives this initiative through a collective effort. The team’s key focus areas are sustainably derived thermoplastic resins, natural fiber reinforcement, composite manufacturing, structural health monitoring, computational materials modeling, and systems analysis. This presentation will give an overview of the SUMAC project. Fiber-scale microscopy analysis characterized fiber cross sections finding that hemp and flax fibers are very deformable and non-circular (circularities of 0.2 were observed), and diameters range from submicron to 20 μm. Fiber shapes range from flattened, with aspect ratios Rlong/Rshort up to 5, to round, Rlong/Rshort =1. And Fiber core perimeters, which likely drives deformability, were calculated Pcore=7 μm. Explicit-fiber yarn simulations, parameterized from single-fiber measurements, resolved and identified slack as a cause for yarn strain-hardening tensile behavior. The bonded network model of PLA, PHA and PA11 resins captures tensile behavior, and can model an infused weave. Computational models of the weave unit cells matched the pattern (including plain, twill and triaxial braid), yarn ply (1to 2), and yarn twist from optical microscopy.

thermoplastic↗
DOE OSTI2025

Ternary molecular switching in a single-crystal optical actuator with correlated crystal strain

A growing portfolio of single-crystal optical actuators is forging a new class of photonic materials that hold prospects for quantum technologies. Ruthenium-based complexes that exhibit this phenomenon via SO 2 -linkage photoisomerisation are of particular interest since they display multiple metastable states, once induced by green light; yet, complete photoconversion into each SO 2 -isomeric state is rarely achieved. We discover a new complex, trans-[Ru(SO 2 )(NH 3 ) 4 (4-bromopyridine)]tosylate 2 , that produces 100% photoconverted η 1 -OSO isomeric crystal structures at 90 K, which fully transition into η 2 -(OS)O photoisomers upon warming to 100 K, while the dark-state η 1 -SO 2 structure is wholly recovered by heating the crystal to room temperature. Crystal structures and optical-absorption profiles of each state are captured via in-situ light-induced single-crystal X-ray diffraction and optical-absorption spectroscopy. Results show that both photoisomeric species behave as optical switches, but with distinct optical properties. The photoisomerisation process causes thermally-reversible micro- and nanoscopic crystal strain, as characterised by optical microscopy and in-situ light-induced atomic-force microscopy.

actuators↗
DOE OSTI2020

Atomic Force Microscopy-Based Force Spectroscopy and Multiparametric Imaging of Biomolecular and Cellular Systems

During the last three decades, a series of key technological improvements turned atomic force microscopy (AFM) into a nanoscopic laboratory to directly observe and chemically characterize molecular and cell biological systems under physiological conditions. In this work, we review key technological improvements that have established AFM as an analytical tool to observe and quantify native biological systems from the micro- to the nanoscale. Native biological systems include living tissues, cells, and cellular components such as single or complexed proteins, nucleic acids, lipids, or sugars. We showcase the procedures to customize nanoscopic chemical laboratories by functionalizing AFM tips and outline the advantages and limitations in applying different AFM modes to chemically image, sense, and manipulate biosystems at (sub)nanometer spatial and millisecond temporal resolution. We further discuss theoretical approaches to extract the kinetic and thermodynamic parameters of specific biomolecular interactions detected by AFM for single bonds and extend the discussion to multiple bonds. Finally, we highlight the potential of combining AFM with optical microscopy and spectroscopy to address the full complexity of biological systems and to tackle fundamental challenges in life sciences.

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

Nano-compositional imaging of the lanthanum silicide system at THz wavelengths

Terahertz scattering-type scanning near-field optical microscopy (THz-sSNOM) provides a noninvasive way to probe the low frequency conductivity of materials and to characterize material compositions at the nanoscale. However, the potential capability of atomic compositional analysis with THz nanoscopy remains largely unexplored. Here, we perform THz near-field imaging and spectroscopy on a model rare-earth alloy of lanthanum silicide (La–Si) which is known to exhibit diverse compositional and structural phases. We identify subwavelength spatial variations in conductivity that is manifested as alloy microstructures down to much less than 1 μ m in size and is remarkably distinct from the surface topography of the material. Signal contrasts from the near-field scattering responses enable mapping the local silicon/lanthanum content differences. These observations demonstrate that THz-sSNOM offers a new avenue to investigate the compositional heterogeneity of material phases and their related nanoscale electrical as well as optical properties.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

3D Reconstruction of a High-Energy Diffraction Microscopy Sample Using Multi-modal Serial Sectioning with High-Precision EBSD and Surface Profilometry

High-energy diffraction microscopy (HEDM) combined with in situ mechanical testing is a powerful nondestructive technique for tracking the evolving microstructure within polycrystalline materials during deformation. This technique relies on a sophisticated analysis of X-ray diffraction patterns to produce a three-dimensional reconstruction of grains and other microstructural features within the interrogated volume. However, it is known that HEDM can fail to identify certain microstructural features, particularly smaller grains or twinned regions. Characterization of the identical sample volume using high-resolution surface-specific techniques, particularly electron backscatter diffraction (EBSD), can not only provide additional microstructure information about the interrogated volume but also highlight opportunities for improvement of the HEDM reconstruction algorithms. In this study, a sample fabricated from undeformed “low solvus, high refractory” nickel-based superalloy was scanned using HEDM. The volume interrogated by HEDM was then carefully characterized using a combination of surface-specific techniques, including epi-illumination optical microscopy, zero-tilt secondary and backscattered electron imaging, scanning white light interferometry, and high-precision EBSD. Custom data fusion protocols were developed to integrate and align the microstructure maps captured by these surface-specific techniques and HEDM. The raw and processed data from HEDM and serial sectioning have been made available via the Materials Data Facility (MDF) at https://doi.org/10.18126/4y0p-v604 for further investigation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Probing subwavelength in-plane anisotropy with antenna-assisted infrared nano-spectroscopy

Infrared nano-spectroscopy based on scattering-type scanning near-field optical microscopy (s-SNOM) is commonly employed to probe the vibrational fingerprints of materials at the nanometer length scale. However, due to the elongated and axisymmetric tip shank, s-SNOM is less sensitive to the in-plane sample anisotropy in general. In this article, we report an easy-to-implement method to probe the in-plane dielectric responses of materials with the assistance of a metallic disk micro-antenna. As a proof-of-concept demonstration, we investigate here the in-plane phonon responses of two prototypical samples, i.e. in (100) sapphire and x-cut lithium niobate (LiNbO 3 ). In particular, the sapphire in-plane vibrations between 350 cm–1 to 800 cm–1 that correspond to LO phonon modes along the crystal b- and c-axis are determined with a spatial resolution of < λ/10, without needing any fitting parameters. In LiNbO 3 , we identify the in-plane orientation of its optical axis via the phonon modes, demonstrating that our method can be applied without prior knowledge of the crystal orientation. Furthermore, our method can be elegantly adapted to retrieve the in-plane anisotropic response of a broad range of materials, i.e. subwavelength microcrystals, van-der-Waals materials, or topological insulators.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Infrared Chemical Nano-Imaging: Accessing Structure, Coupling, and Dynamics on Molecular Length Scales

This Perspective highlights recent advances in infrared vibrational chemical nano-imaging. In its implementations of scattering scanning near-field optical microscopy (s-SNOM) and photothermal-induced resonance (PTIR), IR nanospectroscopy provides few-nanometer spatial resolution for the investigation of polymer, biomaterial, and related soft-matter surfaces and nanostructures. Broad-band IR s-SNOM with coherent laser and synchrotron sources allows for chemical recognition with small-ensemble sensitivity and the potential for sensitivity reaching the single-molecule limit. Probing selected vibrational marker resonances, it gives access to nanoscale chemical imaging of composition, domain morphologies, order/disorder, molecular orientation, or crystallographic phases. Local intra- and intermolecular coupling can be measured through frequency shifts of a vibrational marker in heterogeneous environments and associated inhomogeneities in vibrational dephasing. In combination with ultrafast spectroscopy, the vibrational coherent evolution of homogeneous sub-ensembles coupled to their environment can be observed. Outstanding challenges are discussed in terms of extensions to coherent and multidimensional spectroscopies, implementation in liquid and in situ environments, general sample limitations, and engineering s-SNOM scanning probes to better control the nano-localized optical excitation and to increase sensitivity.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2018

Ultrafine Mineral Associations in Superhigh-Organic-Sulfur Kentucky Coals

Two high-organic-sulfur Kentucky coals, the eastern Kentucky River Gem coal and the western Kentucky Davis coal, are examined by scanning electron microscopy, (SEM) and transmission electron microscopy (TEM), both including elemental analysis by energy-dispersive spectroscopy (EDS). From the SEM-EDS analysis, it is observed that the western Kentucky coal had areas with Pb and Cd in addition to the expected Fe and S and the eastern Kentucky coal had individual Fe-S-rich areas with La and Ni and with Si, Al, Cr, Ni, and Ti. TEM and selected area electron diffraction (SAED) analyses demonstrate that anglesite with a rim of Pb-bearing amorphous Fe-oxide occurs in the western Kentucky coal. Melanterite, an Fe-sulfate, with minor Al, Si, and K EDS peaks, suggests that clay minerals may be in close association with the sulfate, is also detected in the coal. A polycrystalline metal in the eastern Kentucky sample with a composition similar to stainless steel is adjacent to an Al-rich shard. Euhedral pyrite grains surrounded by kaolinite and gibbsite are detected. Overall, it is noted that element associations should not be assumed to be organic just because minerals cannot be seen with optical microscopy or with standard bulk analytical techniques, such as X-ray diffraction (XRD).

organic sulfur, kentucky coals, geoscience, SEM↗
NASA NTRS1998

Experiment 1: Orbital Processing of High-Quality Zn-Alloyed CdTe Compound Semiconductors

Zinc-alloyed cadmium telluride (Zn:CdTe) crystals were grown in unit gravity and in microgravity for comparative analysis. Two crystals were grown on USML-1/STS-50 in 1992, and two additional crystals were grown on USML-2/STS-73 in 1995. The Crystal Growth Furnace (CGF) in the seeded Bridgman-Stockbarger crystal growth geometry was utilized on both missions. Crystals grown on USML-1/STS-50 were found to have solidified with partial wall contact due to the near-absence of the hydrostatic pressure in microgravity, a residual g-vector that was not axial, and the nonwetting sample/ampoule wetting conditions. Crystals grown on USML-2/STS-73 included: a sample/ampoule identical to the USML-1/STS-73 sample/ampoule, with the addition of a restraining spring to simulate hydrostatic pressure internally, and a tapered ampoule which accomplished 2.2 cm of crystal growth without wall contact. Infrared transmission of all ground and flight samples was found to be 63-66 percent, very close to the theoretical 66 percent, suggesting good stoichiometric control. Infrared microscopy confirmed that the primary precipitates were Te and their size (1-10 microns) and density suggested that the flight- and ground-base samples experienced similar thermal histories. Longitudinal macrosegregation, calculated using scaling analysis, was predicted to be low. Nearly diffusion controlled growth was achieved even in unit gravity and macrosegregation data could be fit with a diffusion controlled model. Radial segregation was monitored and was found to vary with fraction solidified, particularly through the shoulder region, where the sample cross section was varying significantly. It was also disturbed in the flight samples in regions where asymmetric wall contact was noted. In regions where a steady state was established, the radial segregation was invariant within our experimental measurement error. Flight samples were found to be much higher in structural perfection than samples processed in unit gravity under identical growth conditions. In regions where solidification had occurred without wall contact, the free surfaces evidenced virtually no twinning, although twins appeared in the flight samples in regions of wall contact and were pervasive in the ground samples. These results were confirmed using optical microscopy and synchrotron x-ray white beam topography. Full-width half-maximum rocking curve widths (FWHM), recorded in arc-seconds, were significantly reduced from 20 a-s (1 g) to 9 a-s (micro-g) for the best regions of the crystals. The 9 a-s (FWHM) rocking curve value in the unconfined flight samples equals the best value reported terrestrially for this material. The ground samples exhibited a fully developed (111)[110] dislocation mosaic structure, whereas dislocations within the flight samples were discrete and no mosaic structure was evident. The defect density was quantitatively reduced from 75,000 (1 g) to 800 (micro-g) +/-50 percent. Dislocation etch pit density results were confirmed using transmission synchrotron white beam and monochromated beam topography. The low defect density is thought to have resulted from the near absence of hydrostatic pressure, which allowed the molten boule to solidify with little or no wall contact. This minimized the transfer of hoop stresses during solidification and post-solidification processing.

Larson, D. J., Jr.↗
DOE OSTI2012

Influence of helium dilution of silane on microstructure and opto-electrical properties of hydrogenated nanocrystalline silicon (nc-Si:H) thin films deposited by HW-CVD

Highlights: ► nc-Si:H films synthesized using HW-CVD method from silane and helium gas mixture without hydrogen. ► Volume fraction of crystallites and its size in the films decreases with increase in He dilution of SiH{sub 4}. ► Increase in Urbach energy and defect density with increase in He dilution of SiH{sub 4}. ► Increasing He dilution, hydrogen bonding in the films shifts from Si-H{sub 2} and (Si-H{sub 2}){sub n} complexes to Si-H. ► Hydrogen content films were found to be <2.2 at.% but the bandgap remains as high as 2.0 eV or even more. -- Abstract: We report influence of helium dilution of silane in hot wire chemical vapor deposition for hydrogenated nano-crystalline silicon films. Structural properties of these films have been investigated by using Raman spectroscopy, low angle x-ray diffraction, Fourier transform infra-red spectroscopy and non-contact atomic force microscopy. Optical characterization has been performed by UV–visible spectroscopy. It has been observed that in contrast to conventional plasma enhanced chemical vapor deposition, the addition of helium with silane in hot wire chemical vapor deposition has an adverse effect on the crystallinity and the material properties. Hydrogen content in the films was found <2.2 at.% whereas the bandgap remain as high as 2 eV or more. Increase in Urbach energy and defect density also suggests the deterioration effect of helium on material properties. The possible reasons for the deterioration of crystallinity and the material properties have been discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Mechanical Properties and Microstructural Evolution of Yb-Modified Al-20%Si Alloy

In the study, the mechanical properties and microstructural evolution of hypereutectic Al-20%Si-xYb alloys (x = 0, 0.1, 0.3, 0.5 and 0.7 wt.%) were studied. The as-prepared samples were characterized by scanning electron microscopy, optical microscope, x-ray diffraction (XRD) and electron probe microanalysis. The characterization results showed with the addition amount of Yb increasing to 0.5%, the eutectic Si structure was gradually modified from coarse needle-like/platelet-like structure into fine coral-like fibrous structure and the primary Si phases were gradually converted from coarse platelet-like/star-like/polygonal shape into fine blocky shape. In particular, according to the results of WDS and XRD analyses, the Yb-rich intermetallic phase in the Al-20%Si alloy is Al{sub 3}Yb. Tensile test was carried out to study the mechanical properties of Al-20%Si-x%Yb alloys, and results showed that the elongation and ultimate tensile strength increased by 73.6% and 64.5%, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Quantitative Reflectance Spectra of Solid Powders as a Function of Particle Size

We have recently developed vetted methods for obtaining quantitative infrared directional-hemispherical reflectance spectra using a commercial integrating sphere. In this paper, the effects of particle size on the spectral properties are analyzed for several samples such as ammonium sulfate, calcium carbonate, and sodium sulfate as well as one organic compound, lactose. We prepared multiple size fractions for each sample and confirmed the mean sizes using optical microscopy. Most species displayed a wide range of spectral behavior depending on the mean particle size. General trends of reflectance vs. particle size are observed such as increased albedo for smaller particles: for most wavelengths, the reflectivity drops with increased size, sometimes displaying a factor of 4 or more drop in reflectivity along with a loss of spectral contrast. In the longwave infrared, several species with symmetric anions or cations exhibited reststrahlen features whose amplitude was nearly invariant with particle size, at least for intermediate- and large-sized sample fractions; that is, > ~150 microns. Trends of other types of bands (Christiansen minima, transparency features) are also investigated as well as quantitative analysis of the observed relationship between reflectance vs. particle diameter.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Liquidus temperature in the spinel primary phase field: A comparison between optical and crystal fraction methods

Liquidus temperature (TL) was measured for simulated high-level waste borosilicate glasses covering a Hanford composition region, using an optical method and a crystal-fraction extrapolation method with X-ray diffraction data from isothermal heat treatments. The 38 glasses encompassed a one-component-at-a-time variation of a 16-component matrix. The TL values ranged from 1006°C to 1603°C. First-order polynomial models were fitted to data to obtain coefficients in terms of the effect of 1 mass% component addition on the TL: TL-increasing oxides Cr2O3 (264°C), “Others” (minor components, 163°C), oxides of noble metals (137°C), NiO (91°C), Al2O3 and Fe2O3 (~19–21°C); TL-decreasing oxides K2O (-26°C), Na2O (-41°C), and Li2O (-68°C); oxides of little effect MnO, P2O5, ZrO2, F, Bi2O3, SiO2, B2O3, and CaO (9 to -12°C). Also presented are temperatures (T1%) at which glasses contain 1 vol% of spinel as these values are considered relevant to the Hanford Tank Waste Treatment and Immobilization Plant. The measured and estimated values are compared and contrasted and the effect of TL and T1% on glass formulation is discussed.

crystal fraction↗
DOE OSTI2017

On the Evolution From Micrometer-Scale Inhomogeneity to Global Overheated Structure During the Intense Joule Heating of a z-Pinch Rod

Ultrafast optical microscopy of metal z-pinch rods pulsed with megaampere current is contributing new data and critical insight into what provides the fundamental seed for the magneto-Rayleigh-Taylor (MRT) instability. A two-frame near infrared/visible intensified-charge-coupled device gated imager with 2-ns temporal resolution and 3-μm spatial resolution captured emissions from the nonuniformly Joule heated surfaces of ultrasmooth aluminum (Al) rods. Nonuniform surface emissions are consistently first observed from discrete, 10-μm scale, subelectronvolt spots. Aluminum 6061 alloy, with micrometer-scale nonmetallic resistive inclusions, forms several times more spots than 99.999% pure Al 5N; 5-10 ns later, azimuthally stretched elliptical spots and distinct strata (40-100 μm wide by 10 μm tall) are observed on Al 6061, but not on Al 5N. In such overheat strata, aligned parallel to the magnetic field, we find that they are highly effective seeds for MRT instability growth. Our data give credence to the hypothesis that early nonuniform Joule heating, such as the electrothermal instability, may provide the dominant seed for MRT.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2021

Liquid Crystal Films as Active Substrates for Nanoparticle Control

Organizing nanoparticles in a controlled way allows us to monitor their optical properties. It is particularly interesting to organize them on top of liquid crystal films to take advantage, in a second step, of the easy actuation of liquid crystals with external parameters such as temperature, electric fields, and so forth. We show that despite their fluidity, nematic and smectic films allow the formation of well-ordered hexagonal domains of gold spherical nanoparticles (AuNPs) at their surface, but we also show that both nematic films and AuNP domains impact each other. Using optical microscopy, atomic force microscopy (AFM), scanning electron microscopy (SEM), and spectrophotometry, we compare nematic, polymer-stabilized nematic, and smectic films with AuNP domains made of NPs of diameter 6 nm. On the liquid crystal films, depressions are revealed below the AuNP domains, whereas the AuNP domains appear well-organized but with a hexagonal period shortened with respect to AuNP monolayers formed on hard substrates. We interpret these features by the anchoring tilt imposed by the AuNP domains on the liquid crystal molecules. The smectic-A layers characteristic of the nematic surface transform into smecticC layers, which induce the formation of depression. Here, the energy penalty associated with the local smectic-A/smectic-C transition induces the shortening of the AuNP domain period in order to decrease the AuNP domain surface. The observed large depth of the polymer-stabilized nematic depressions below AuNP domains may be explained either by an increased size of the polymer-stabilized smectic layers close to the surface or by an increased number of polymer-stabilized smectic liquid crystal smectic layers close to the surface with respect to pure nematic films.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Lanthanum and neodymium solubility in simplified SiO{sub 2}-B{sub 2}O{sub 3}-Na{sub 2}O-Al{sub 2}O{sub 3}-CaO high level waste glass

Lanthanum and neodymium incorporation in simplified high level waste glasses has been investigated for SiO{sub 2}B{sub 2}O{sub 3}Na{sub 2}OAl{sub 2}O{sub 3}CaO compositions quenched from 1200 degrees C, for varying La /(La + Nd) (atomic) and increasing rare-earth oxides contents. In this system and beyond the solubility limit, rare-earths (RE) elements are reported to form apatite phases with the general formula Ca{sub 2}RE{sub 8}(SiO{sub 4}){sub 6}O{sub 2}. In the current study, speciation of these trivalent RE{sup 3+} cations in both amorphous network and crystal phases was determined from X-ray diffraction, scanning electron microscopy, optical absorption at 10 K, Raman spectroscopy, and electron probe microanalysis. It appeared that RE{sub 2}O{sub 3} solubility was higher for La -rich formulations than for Nd -rich ones and that an increase in the RE oxide content reduces the connectivity of the network building units through formation of non-bridging oxygens at the expense of the oxygen bridges. This depolymerization of the glass network did not affect neodymium environment which consisted in silicate tetrahedra. The composition of the apatite crystals was found to be affected by the La /(La + Nd) of the parent glass and deviation from the ideal composition (Ca{sub 2}RE{sub 8}(SiO{sub 4}){sub 6}O{sub 2}) occurred in the neodymium end of the system. It thus appears that both RE{sub 2}O{sub 3} solubility and crystal composition are strongly dependent on the type and crystal chemistry of the RE elements. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗