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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
NASA NTRS1996

Structural relations between collagen and mineral in bone as determined by high voltage electron microscopic tomography

Aspects of the ultrastructural interaction between collagen and mineral crystals in embryonic chick bone have been examined by the novel technique of high voltage electron microscopic tomography to obtain three-dimensional information concerning extracellular calcification in this tissue. Newly mineralizing osteoid along periosteal surfaces of mid-diaphyseal regions from normal chick tibiae was embedded, cut into 0.25 microns thick sections, and documented at 1.0 MV in the Albany AEI-EM7 high voltage electron microscope. The areas of the tissue studied contained electron dense mineral crystals associated with collagen fibrils, some marked by crystals disposed along their cylindrically shaped lengths. Tomographic reconstructions of one site with two mineralizing fibrils were computed from a 5 degrees tilt series of micrographs over a +/- 60 degrees range. Reconstructions showed that the mineral crystals were platelets of irregular shape. Their sizes were variable, measured here up to 80 x 30 x 8 nm in length, width, and thickness, respectively. The longest crystal dimension, corresponding to the c-axis crystallographically, was generally parallel to the collagen fibril long axis. Individual crystals were oriented parallel to one another in each fibril examined. They were also parallel in the neighboring but apparently spatially separate fibrils. Crystals were periodically (approximately 67 nm repeat distance) arranged along the fibrils and their location appeared to correspond to collagen hole and overlap zones defined by geometrical imaging techniques. The crystals appeared to be continuously distributed along a fibril, their size and number increasing in a tapered fashion from a relatively narrow tip containing smaller and infrequent crystals to wider regions having more densely packed and larger crystals. Defined for the first time by direct visual 3D imaging, these data describe the size, shape, location, orientation, and development of early crystals in normal bone collagen. The results suggest that platelet-shaped crystals are arranged in channels or grooves which are formed by collagen hole zones in register and that crystal sizes may exceed the dimensions of hole zones. Such data agree with those from mineral-matrix interaction in normally calcifying avian tendon obtained by similar high voltage tomographic means, but in addition they indicate a possible gradual and continuous deposition of crystals in collagen of bone unlike tendon and imply that individual collagen fibrils in local regions of osteoid are organized such that they all may be aligned in a coherent manner.

NASA Discipline Number 40-40↗
NASA NTRS2014

Impact-Induced Chondrule Deformation and Aqueous Alteration of CM2 Murchison

Deformed chondrules in CM2 Murchison have been found to define a prominent foliation [1,2] and lineation [3] in 3D using X-ray computed tomography (XCT). It has been hypothesized that chondrules in foliated chondrites deform by "squeezing" into surrounding pore space [4,5], a process that also likely removes primary porosity [6]. However, shock stage classification based on olivine extinction in Murchison is consistently low (S1-S2) [4-5,7] implying that significant intracrystalline plastic deformation of olivine has not occurred. One objective of our study is therefore to determine the microstructural mechanisms and phases that are accommodating the impact stress and resulting in relative displacements within the chondrules. Another question regarding impact deformation in Murchison is whether it facilitated aqueous alteration as has been proposed for the CMs which generally show a positive correlation between degree of alteration and petrofabric strength [7,2]. As pointed out by [2], CM Murchison represents a unique counterpoint to this correlation: it has a strong petrofabric but a relatively low degree of aqueous alteration. However, Murchison may not represent an inconsistency to the proposed causal relationship between impact and alteration, if it can be established that the incipient aqueous alteration post-dated chondrule deformation. Methods: Two thin sections from Murchison sample USNM 5487 were cut approximately perpendicular to the foliation and parallel to lineation determined by XCT [1,3] and one section was additionally polished for EBSD. Using a combination of optical petrography, SEM, EDS, and EBSD several chondrules were characterized in detail to: determine phases, find microstructures indicative of strain, document the geometric relationships between grain-scale microstructures and the foliation and lineation direction, and look for textural relationships of alteration minerals (tochilinite and Mg-Fe serpentine) that indicate timing of their formation relative to deformation event(s). Preliminary Results: Deformed chondrules are dominated by forsterite and clinoenstatite with lesser amounts of Fe-Mg serpentine, sulfides, and low calcium pyroxene. Olivine grains are commonly fractured but generally show sharp optical extinction. The pyroxene, in contrast, is not only fractured but also often displays undulose extinction. In addition, the clinoenstatite is frequently twinned but it is unclear whether the twins are the result of mechanical deformation or inversion from protoenstatite [8]. EBSD work is currently ongoing to determine if areas of higher crystallographic strain can be imaged and mapped, and to determine the pyroxene twin orientations. In regards to alteration, we have found evidence for post-deformation formation of tochilinite and Mg-Fe serpentine indicating that aqueous alteration has indeed post-dated the deformation of the chondrules.

Hanna, R. D.↗
NASA NTRS1987

The localization and crystallographic dependence of Si suboxide species at the SiO2/Si interface

X-ray photoemission spectroscopy has been used to examine the localization and crystallographic dependence of Si(+), Si(2+), and Si(3+) suboxide states at the SiO2/Si interface for (100)and (111)-oriented substrates with gate oxide quality thermal oxides. The Si(+) and Si(2+) states are localized within 6-10 A of the interface while the Si(3+) state extends about 30 A into the bulk SiO2. The distribution of Si(+) and Si(2+) states shows a strong crystallographic dependence with Si(2+) dominating on (100) substrates and Si(+) dominating on (111) substrates. This crystallographic dependence is anticipated from consideration of ideal unreconstructed (100) and (111) Si surfaces, suggesting that (1) the Si(+) and Si(2+) states are localized immediately within the first monolayer at the interface and (2) the first few monolayers of substrate Si atoms are not significantly displaced from the bulk. The total number of suboxide states observed at the SiO2/Si interface corresponds to 94 and 83 percent of a monolayer for these (100) and (111) substrates, respectively.

Grunthaner, P. J.↗
DOE OSTI2020

Probing the Consequences of Cubic Particle Shape and Applied Field on Colloidal Crystal Engineering with DNA

Abstract In a magnetic field, cubic Fe 3 O 4 nanoparticles exhibit assembly behavior that is a consequence of a competition between magnetic dipole–dipole and ligand interactions. In most cases, the interactions between short hydrophobic ligands dominate and dictate assembly outcome. To better tune the face‐to‐face interactions, cubic Fe 3 O 4 nanoparticles were functionalized with DNA. Their assembly behaviors were investigated both with and without an applied magnetic field. Upon application of a field, the tilted orientation of cubes, enabled by the flexible DNA ligand shell, led to an unexpected crystallographic alignment of the entire superlattice, as opposed to just the individual particles, along the field direction as revealed by small and wide‐angle X‐ray scattering. This observation is dependent upon DNA length and sequence and cube dimensions. Taken together, these studies show how combining physical and chemical control can expand the possibilities of crystal engineering with DNA.

Urbach, Zachary J.↗
DOE OSTI2020

Probing the Consequences of Cubic Particle Shape and Applied Field on Colloidal Crystal Engineering with DNA

In a magnetic field, cubic Fe 3 O 4 nanoparticles exhibit assembly behavior that is a consequence of a competition between magnetic dipole-dipole and ligand interactions. In most cases, the interactions between short hydrophobic ligands dominate and dictate assembly outcome. To better tune the face-to-face interactions, cubic Fe3O4 nanoparticles were functionalized with DNA. Their assembly behaviors were investigated both with and without an applied magnetic field. Upon application of a field, the tilted orientation of cubes, enabled by the flexible DNA ligand shell, led to an unexpected crystallographic alignment of the entire superlattice, as opposed to just the individual particles, along the field direction as revealed by small and wide-angle X-ray scattering. This observation is dependent upon DNA length and sequence and cube dimensions. Taken together, these studies show how combining physical and chemical control can expand the possibilities of crystal engineering with DNA.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Automated TEM Reveals Intercrystalline Correlations of Conjugated Polymers

Transmission electron microscopy (TEM) continues to transform polymer science by revealing key aspects of chain packing, phase separation and nanoscale structure. The development of instrumentation and data analyses tools is driving the field forward and enabling new experiments. Here, we use automated high-resolution TEM (HRTEM) and image processing to identify the structure of a conjugated polymer used in organic electronics. Analysis of more than 600 HRTEM images reveals lattice parameters and orientation correlations between crystals, including the preferred alignment of neighboring crystals along the same crystallographic direction that is likely the result of liquid crystalline order.

Fair, Ryan A. [Pennsylvania State University, Univ↗
DOE OSTI2023

Texture measurements on quartz single crystals to validate coordinate systems for neutron time-of-flight texture analysis

In crystallographic texture analysis, ensuring that sample directions are preserved from experiment to the resulting orientation distribution is crucial to obtain physical meaning from diffraction data. This work details a procedure to ensure instrument and sample coordinates are consistent when analyzing diffraction data with a Rietveld refinement using the texture analysis software MAUD . A quartz crystal is measured on the HIPPO diffractometer at Los Alamos National Laboratory for this purpose. The methods described here can be applied to any diffraction instrument measuring orientation distributions in polycrystalline materials.

36 MATERIALS SCIENCE↗
NASA NTRS2000

Crystallography of Alumina-YAG-Eutectic

Multiple descriptions of the alumina-YAG eutectic crystallography appear in the ceramic literature. The orientation between two phases in a eutectic system has direct impact on residual stress, morphology, microstructural stability, and high temperature mechanical properties. A study to demonstrate that the different crystallographic relationships can be correlated with different growth constraints was undertaken. Fibers produced by Laser-Heated Float Zone (LHFZ) and Edge-defined Film-fed Growth (EFG) were examined. A map of the orientation relationship between Al2O3 and Y3Al5O12 and their relationship to the fiber growth axis as a function of pull rate are presented. Regions in which a single orientation predominates are identified.

Farmer, Serene C.↗
DOE OSTI2021

Strong Magnetocrystalline Anisotropy Arising from Metal–Ligand Covalency in a Metal–Organic Candidate for 2D Magnetic Order

Layered metal–organic frameworks are promising candidates for new two-dimensional magnets, as their synthetic programmability of these materials can provide a route to diverse structural and electronic properties. However, such framework materials typically lack the heavy elements that engender magnetocrystalline anisotropy in the monolayer ferromagnets reported to date. Alternative sources of magnetic anisotropy are therefore needed in these materials. Here, we report the synthesis of single crystals of the framework material (NMe 4 ) 2 [Fe 2 L 3 ] (H 2 L = 3,6-dichloro-2,5-dihydroxybenzoquinone) and evaluate the angular dependence of its magnetic properties. Oriented-crystal magnetization measurements reveal strong uniaxial anisotropy, where the easy axis is aligned with the crystallographic c axis. While the spin carriers of this structure are isotropic $S = ^5/_2$ Fe III metal centers and $S = ^1/_2$ organic linkers, the anisotropy energy of the framework material is comparable to that of reported 2D ferromagnets. Density functional theory calculations indicate that the observed magnetocrystalline anisotropy arises from ligand-to-metal charge transfer that enhances the magnetic anisotropy of the otherwise isotropic Fe centers, suggesting that metal–ligand covalency can be utilized as a general additive for the development of 2D magnets. These results in this study show the possibility for (NMe 4 ) 2 [Fe 2 L 3 ] to retain magnetic order down to the 2D monolayer limit. In addition, the combination of large magnetic anisotropy and semiconducting character in (NMe 4 ) 2 [Fe 2 L 3 ] highlights its potential as a new 2D magnetic semiconductor.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Epitaxial registry and transport properties in V4O7 thin films

We report the growth of V4O7 thin films deposited simultaneously on amorphous SiO2 and crystalline c-cut Al2O3 substrates. x-ray diffraction shows that films grown on SiO2 are polycrystalline with no preferred orientation, while films grown on Al2O3 exhibit a well-defined out-of-plane orientation and an in-plane registry consistent with epitaxial growth. Transmission electron microscopy confirms the crystallographic relationship between the V4O7 film and the Al2O3 substrate. Atomic force microscopy indicates substantially lower surface roughness for films grown on Al2O3 (~6 nm) compared to those grown on SiO2 (~22 nm), and Raman spectroscopy confirms stabilization of the same V4O7 phase on both substrates. Electrical transport measurements reveal a metal–insulator transition near 244 K for both substrates, with thermal hysteresis not exceeding ~1 K. Although the transition temperature remains essentially unchanged, films grown on Al2O3 exhibit higher conductivity over the entire temperature range, exceeding that of films grown on SiO2 by approximately two orders of magnitude at 100 K and by a factor of five at 300 K. These results indicate that the conductivity differences are consistent with variations in microstructural connectivity associated with crystallographic order.

36 MATERIALS SCIENCE↗
NASA NTRS1982

The effect of grooves in amorphous substrates on the orientation of metal deposits. I - Carbon substrates

The graphoepitaxial alignment of vapor-deposited discrete metal crystallites is investigated in the nucleation and growth stages and during annealing by in situ UHV/TEM techniques. Various stages of nucleation, growth and coalescence of vapor deposits of Au, Ag, Pb, Sn, and Bi on amorphous, topographically structured C substrates are analyzed by advanced dark-field techniques to detect preferred local orientations. It is found that the topography-induced orientation of metal crystallites depends strongly on their mobility and their respective tendency to develop pronounced crystallographic shapes. Lowering of the average surface free energies and increasing the crystallographic surface energy anisotropies cause generally improved graphoepitaxial alignments.

Anton, R.↗
NASA NTRS1986

Anisotropic constitutive model for nickel base single crystal alloys: Development and finite element implementation

A tool for the mechanical analysis of nickel base single crystal superalloys, specifically Rene N4, used in gas turbine engine components is developed. This is achieved by a rate dependent anisotropic constitutive model implemented in a nonlinear three dimensional finite element code. The constitutive model is developed from metallurigical concepts utilizing a crystallographic approach. A non Schmid's law formulation is used to model the tension/compression asymmetry and orientation dependence in octahedral slip. Schmid's law is a good approximation to the inelastic response of the material in cube slip. The constitutive equations model the tensile behavior, creep response, and strain rate sensitivity of these alloys. Methods for deriving the material constants from standard tests are presented. The finite element implementation utilizes an initial strain method and twenty noded isoparametric solid elements. The ability to model piecewise linear load histories is included in the finite element code. The constitutive equations are accurately and economically integrated using a second order Adams-Moulton predictor-corrector method with a dynamic time incrementing procedure. Computed results from the finite element code are compared with experimental data for tensile, creep and cyclic tests at 760 deg C. The strain rate sensitivity and stress relaxation capabilities of the model are evaluated.

Dame, L. T.↗
NASA NTRS1985

Constitutive modeling of superalloy single crystals with verification testing

The goal is the development of constitutive equations to describe the elevated temperature stress-strain behavior of single crystal turbine blade alloys. The program includes both the development of a suitable model and verification of the model through elevated temperature-torsion testing. A constitutive model is derived from postulated constitutive behavior on individual crystallographic slip systems. The behavior of the entire single crystal is then arrived at by summing up the slip on all the operative crystallographic slip systems. This type of formulation has a number of important advantages, including the prediction orientation dependence and the ability to directly represent the constitutive behavior in terms which metallurgists use in describing the micromechanisms. Here, the model is briefly described, followed by the experimental set-up and some experimental findings to date.

Jordan, Eric↗
NASA NTRS1985

Orientation and temperature dependence of some mechanical properties of the single-crystal nickel-base superalloy Rene N4. 3: Tension-compression anisotropy

Single crystal superalloy specimens with various crystallographic directions along their axes were tested in compression at room temperature, 650, 760, 870, and 980 deg C. These results are compared with the tensile behavior studied previously. The alloy, Rene N4, was developed for gas turbine engine blades and has the nominal composition 3.7 Al, 4.2 Ti, 4 Ta, 0.5 Nb, 6 W, 1.5 Mo 9 Cr. 7.5 Co, balance Ni, in weight percent. Slip trace analysis showed that primary cube slip occurred even at room temperature for the 111 specimens. With increasing test temperature more orientations exhibited primary cube slip, until at 870 deg C only the 100 and 011 specimens exhibited normal octahedral slip. The yield strength for octahedral slip was numerically analysed using a model proposed by Lall, Chin, and Pope to explain deviations from Schmid's Law in the yielding behavior of a single phase Gamma prime alloy, Ni3(Al, Nb). The Schmid's Law deviations in Rene N4 were found to be largely due to a tension-compression anisotropy. A second effect, which increases trength for orientations away from 001, was found to be small in Rene N4. Analysis of recently published data on the single crystal superalloy PWA 1480 yielded the same result.

Miner, R. V.↗
DOE OSTI2022

Three-dimensional mapping of mineral in intact shark centra with energy dispersive x-ray diffraction

The centra of shark vertebrae consist of cartilage mineralized by a bioapatite similar to bone's carbonated hy-droxyapatite, and, without a repair mechanism analogous to remodeling in bone, these structures still survive millions of cycles of high-strain loading. The main structures of the centrum are an hourglass-shaped double cone and the intermedialia which supports the cones. Little is known about the nanostructure of shark centra, spe-cifically the relationship between bioapatite and cartilage fibers, and this study uses energy dispersive diffraction (EDD) with polychromatic synchrotron x-radiation to study the spatial organization of the mineral phase and its crystallographic texture. The unique energy-sensitive detector array at beamline 6-BM-B, the Advanced Photon Source, enables EDD to quantify the texture within each sampling volume with one exposure while constructing 3D maps via specimen translation across the sampling volume. Herein this study maps a centrum from two shark orders, a carcharhiniform and a lamniform, with different intermedialia structures. In the blue shark (Prionace glauca, Carcharhiniformes), the bioapatite's c-axes are oriented laterally within the centrum's cone walls but axially within the wide wedges of the intermedialia; the former is interpreted to resist lateral deformation, the latter to support axial loads. In the shortfin mako (Isurus oxyrinchus, Lamniformes), there is some tendency for c-axis variation with position, but the situation is unclear because one dimension of the sampling volume is consid-erably larger than the thickness and spacing of the intermedialia's radially-oriented lamellae. Because elastic modulus in collagen plus bioapatite mineralized tissues varies significantly with both volume fraction of bio-apatite and crystallographic texture, the present 3D EDD-derived maps should inform future 3D numerical models of shark centra under applied load.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Analysis of dislocation configurations in SiC crystals through X-ray topography aided by ray tracing simulations

Silicon carbide as a wide bandgap semiconductor is of great research interest for its widespread deployment in a range of electronic and optoelectronic devices, particularly in power electronics. However, defects in silicon carbide crystals are still major concerns that is hampering the development of high-performance devices. X-ray topography, particularly using the synchrotron beam has been instrumental in characterizing and analyzing defect configurations in silicon carbide crystals to optimize crystal growth as well as understand the effect of defects on device performance. Here, in recent years, the use of ray-tracing simulation technique based on the orientation contrast mechanism to simulate contrast of defects observed on actual X-ray topographs has proven to be an effective approach to investigate the nature of crystallographic defects in various semiconductors. This review discusses the principle of ray-tracing simulation and its application and modifications to incorporate the effects of surface relaxation and photoelectric absorption to better simulate different dislocations observed in 4H–SiC as well as 6H–SiC crystals of various orientations. The adaptation to weak beam topography and plane wave topography is also discussed. The application of ray-tracing simulation in dislocation characterization of silicon carbide of different polytypes is systematically reviewed including different types of dislocations observed in both off-axis wafers and axial-sliced samples through synchrotron X-ray topography under various beam conditions, recording geometries and reflections. The result of ray-tracing simulation is further utilized in other studies including the investigation of effective penetration depth of all types of dislocations lying on the basal plane on grazing-incidence X-ray topography.

Engineering↗
DOE OSTI2021

Understanding the Reactions Between Fe and Se Binary Diffusion Couples

Spurred by recent discoveries of high-temperature superconductivity in Fe-Se based materials, the magnetic, electronic, and catalytic properties of iron-chalcogenides have drawn significant attention. Furthermore, much remains to be understood about the sequence of phase formation in these systems. In this work, we shed light on this issue by preparing a series of binary Fe-Se ultrathin diffusion couples via designed thin film precursors and investigating their structural evolution as a function of composition and annealing temperature. Two previously unreported Fe-Se phases crystallized during the deposition process on a nominally room-temperature Si substrate in the 27-33% and 37-47% Fe (atomic percent) composition regimes. Both phases completely decompose after annealing to 200°C in a nitrogen glovebox. At higher temperatures, the sequence of phase formation is governed by Se loss in the annealing process, consistent with what would be expected from the phase diagram. Films rich in Fe (53-59% Fe) crystalized during deposition as β-FeSe (P4/nmm) with preferred c-axis orientation to the amorphous SiO 2 substrate surface, providing a means to non-epitaxial self-assembly of crystallographically aligned, iron-rich β-FeSe for future research. Our findings suggest the crystallization of binary Fe-Se compounds at room temperature via near diffusionless transformations should be a significant consideration in future attempts to prepare metastable ternary and higher order compounds containing Fe and Se.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Mesocrystal growth through oriented sliding and attachment of nanoplates

Oriented attachment is a critical, yet poorly understood, crystal growth pathway based on the self-assembly of nanocrystals. During oriented attachment, solvent-separated particles align and coalesce through forces that enable precise rotation and translation. While prior studies emphasized intragap forces driving crystallographic alignment, the forces enabling uniform stacking and superlattice formation remain unclear. Here, we demonstrate how macroscopic gibbsite mesocrystals emerge from nanoplates guided into staggered positions by directional sliding. Electron microscopy and X-ray scattering reveal the monoclinic superlattice structure, based on nanoplate stacking with a uniform ≈50° stagger along the gibbsite [010] direction. In situ liquid-cell TEM captures preferential sliding along the gibbsite [010] direction, decelerating with increasing particle overlap. Molecular dynamics simulations reveal that this staggered arrangement corresponds to a global free-energy minimum, rather than full alignment. The simulations also confirm that sliding along the [010] direction is energetically favored and provide insight into the role of interfacial water in achieving long-range ordered assemblies. These insights highlight the energy landscape’s role in oriented attachment, with implications for material synthesis and hierarchical structures in nature.

36 MATERIALS SCIENCE↗