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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 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

In Situ 4D‐STEM Imaging of the Orientation of Lamellar Clusters in Polymer Crystallization

In semi‐crystalline polymeric materials, the initial stages of nucleation and the growth path of crystalline domains can determine the final performance. Here, in this work, we used four‐dimensional scanning transmission electron microscopy (4D‐STEM) imaging to analyze the changes in lamellar orientation in high‐density polyethylene (HDPE) during heating and cooling. This method allowed us to quantitatively detect the formation of lamellae clusters with different in‐plane orientations, which are not visible with traditional methods. Our analysis provided detailed insights into the orientation and size changes of crystalline domains. Additionally, this technique enabled direct observation of lattice structures in hierarchical lamellae and the growth of crystals, confirming the local variability in lamellar orientation. This innovative approach significantly improves our understanding of polymer crystallization, linking changes in morphology and lattice structures at different length scales.

4D-STEM↗
DOE OSTI2020

Preferred Void Orientation in Uniaxially Pressed PBX 9502

Ultra- and small-angle neutron scattering techniques were used to study the morphology of voids in directions parallel and perpendicular to the compaction plane of a uniaxially pressed cylinder of PBX 9502. Two-dimensional scattering patterns from samples cut parallel to the compaction plane had circular equal-intensity contours, implying that along this view the voids are circular or randomly oriented. Identical measurements of samples cut perpendicular to the compaction plane produced elliptical equal-intensity contours, indicating preferred orientation of voids. Analysis of the two dimensional scattering patterns confirmed that the voids are non-spherical with an average aspect ratio of 1.20, flattened so that the larger dimensions of the voids lie within the compaction plane. Model analysis of the combined ultra- and small-angle neutron scattering curves revealed that the PBX 9502 porosity is interconnected, in the form of aggregates comprised of non-spherical, primary voids. The volume dimension was found to be the same in both directions, indicating that the aggregate is randomly oriented throughout the sample, and that it is the primary voids that are preferentially oriented. Furthermore, void interfaces with the surrounding matrix were found to be rough or polydisperse, with a common roughness dimension or polydispersity in all directions.

42 ENGINEERING↗
DOE OSTI2025

V‐Groove Si Nanopatterning for the Direct Epitaxy of Orientation‐Patterned III–V Nonlinear Optical Crystals

Orientation‐patterned (OP) III–V semiconductors—used as quasi‐phase‐matched crystals for nonlinear optics applications—are typically epitaxially grown on expensive III–V substrates using a complex process requiring three separate epitaxy steps. In this work, a method is demonstrated for growing orientation‐patterned III–V crystals on Si substrates through V‐groove nanopatterning and a single epitaxial growth. V‐groove Si allows for suppression of random antiphase domain formation that is typical of III–V growth on (001)‐oriented Si through the use of (111)‐faceted trenches patterned on (001)‐oriented Si substrates. By alternating the directions of the V‐groove trenches between [110] and [10], antiphase boundaries can be selectively induced at the boundaries between the two directions of trenches due to the difference in symmetry between the III–V material and Si. This approach allows for a greatly simplified process for growing OP‐III‐Vs and more broadly is a new, robust approach for precisely patterning antiphase boundaries of arbitrary shape and length scales down to 50 nm.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2025

Methodologies and strategies for detecting fiber orientation in polymeric fiber-reinforced composites

In this review paper different methods and techniques for representing fiber orientation in advanced polymer matrix composites are presented. A description of the effect of fiber orientation on processing, fabrication and mechanical properties of a composite material is presented. The paper discusses the mathematical modeling and modeling techniques for fiber structure representation in polymeric composites, with an emphasis on fiber orientation in a composite part. The paper is divided into two sections; namely—destructive techniques and non-destructive techniques. The capabilities and limitations of each technique with respect to fiber orientation detection and measurements are discussed.

composites↗
DOE OSTI2019

Build Orientation Effects on Texture and Mechanical Properties of Selective Laser Melting Inconel 718

The production of components via selective laser melting (SLM) metal additive manufacturing results in microstructures unique to the process that are highly dependent on laser processing parameters and orientation of part geometry relative to the build direction. This study investigates the variation in tensile properties of SLM Inconel 718 at varying angles with respect to build direction. ASTM E8 tensile specimens were built in XY, Z, and B+45 from Z orientations to near-net shape, HIP and heat treated, and tensile tested at room temperature. Orientation dependence of mechanical properties was observed; Z samples had the lowest strength and highest elongation, while XY samples had the highest strength and lowest elongation. Optical, SEM, and EBSD analysis were conducted to probe for microstructure variation that could be the cause of the difference in mechanical properties. Analysis of pole figures and grain maps suggests a preferred grain texture and twinning orientation that aligns with the build direction, which may contribute to the anisotropic enhancement in ductility.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Subgroup analysis of efficacy and safety of orantinib in combination with TACE in Japanese HCC patients in a randomized phase III trial (ORIENTAL)

A randomized, phase III trial of orantinib in combination with transcatheter arterial chemoembolization (TACE) did not prolong overall survival (OS) over placebo (ORIENTAL study). A subgroup analysis was conducted to evaluate the efficacy and safety of orantinib in Japanese patients enrolled in the ORIENTAL study. The data of Japanese patients from this study were analyzed. The overall survival (OS), time to progression (TTP), and time to TACE failure (TTTF) were compared between orantinib and placebo arms using stratified log-rank test. Since TTTF in patients with Barcelona Clinic Liver Cancer stage B (BCLC-B) showed favor outcome in this study, the OS and TTTF according to BCLC staging system were also analyzed. The subgroup analysis consisted of 219 and 213 patients in the orantinib and placebo arms. Median OS was 32.5 vs 33.0 months (p = 0.906), median TTP was 4.7 vs 3.1 months (p = 0.011), and median TTTF was 25.3 vs 18.2 months (p = 0.160) in the orantinib and placebo groups, respectively. Patients with BCLC-B in the orantinib and placebo groups showed a median OS of 33.7 and 30.1 months, respectively (p = 0.260), while the corresponding median TTTF were 25.3 and 14.0 months (p = 0.125). The Japanese population safety profile was similar to all over population in the ORIENTAL study. No significant differences were observed in the OS and TTTF though the TTP was significantly improved in the orantinib arm. The OS and TTTF showed a tendency to be prolonged following orantinib treatment of Japanese HCC patients with BCLC-B in the ORIENTAL study.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2018

Orientation dependent spall strength of tantalum single crystals

We report that it is generally recognized that single crystals exhibit orientation-dependent elastic and plastic responses. However, it is less known how the dynamic tensile, or spall, strength depends on crystalline orientation, especially for BCC materials. It has been previously shown that the dynamic tensile strength of FCC materials is highly dependent on their plastic response under compression, with a direct correlation between plastic deformation and spall strength. In BCC materials like Ta, where the primary deformation mechanism at high strain rates is a combination of slip and twinning, the quantitative dependence of spall strength on these deformation mechanisms is less understood. To fill this gap in our knowledge, a series of non-equilibrium molecular dynamics simulations are completed for six tantalum single crystal orientations: <001>, <011>, <111>, <013>, <112>, <149>, to explore the role of directional anisotropy on ductile spallation. Our results show that due to the role of non-Schmid and release effects in BCC Ta, the evolution of plasticity follows a complex trajectory through shock compression, release, and tension. Orientations that contain residual twinning deformation have a reduced spall strength proportional to the amount of twinning present. Lastly, twins and their intersections function as regions of increased stress localization within the system due to compatibility requirements and their interactions with dislocations.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Effects of heat treatment and build orientation on the evolution of $ϵ$ and $α'$ martensite and strength during compressive loading of additively manufactured 304L stainless steel

In this paper, the effect of heat-treatment and build orientation on martensitic phase transformation in additively manufactured (AM) 304L stainless steel is studied and compared with conventionally produced wrought material. The relationships between observed martensitic transformations and material microstructures and their effects on mechanical strength are established through experimental observations. In situ high-energy X-ray powder diffraction measurements were performed to monitor the evolution of $ϵ$ and $α'$ martensite during compressive loading of stainless steel. Electron backscatter diffraction (EBSD) was used to provide insight on initial grain morphology, crystallographic misorientation within grains, and crystallographic texture. Heat treatment alters the microstructure of AM samples creating different initial conditions. This difference in starting microstructure resulted in variability in martensitic transformation during compressive deformation. The rate of martensitic transformation decreased for AM samples treated with temperatures up to 1100°C, after which the AM microstructures recrystallized, resulting in increased rate of martensitic transformation for those samples treated at higher temperatures. It was also observed that aligning the axis of compression with the AM build direction resulted in a lower rate of strain-induced martensite formation as opposed to aligning the compression axis perpendicular to it. More favorable distribution of crystal orientations in the latter loading orientation promoted martensitic transformation. These and additional experimental observations from EBSD in terms of kernel average misorientation, mean grain orientation spread, and mean crystallite size reveal strong microstructural effects on strength of additively manufactured metallic materials.

304L stainless steel↗
DOE OSTI2020

Build Orientation Dependent Microstructure in Polymer Laser Sintering: Relationship to Part Performance and Evolution with Aging

Laser sintering (LS) is widely used to produce functional polymeric parts; however, the resulting parts are often limited by their porous structure, and performance of the part may be strongly anisotropic. Relating the structural features of parts to build process conditions or powder feedstock has been explored previously. In contrast, little is known regarding how the unique internal structures of LS parts evolve and relate to their performance later in their life cycle, for example, after use in a real-world operating environment. In this study, a tightly controlled LS build process and measurement campaign by standard X-ray computed tomography (XCT), supported by high-resolution synchrotron XCT, was used to benchmark the internal microstructure (e.g. porosity) as a function of four different build orientations in printed polyamide-12 (PA-12) parts. The initial performance of the parts after printing was characterized by tensile testing and dynamic mechanical analysis (DMA). Arrays of PA-12 parts in different build orientations were exposed to steam (under pressure) and air across multiple temperature and time points for the purposes of accelerated aging through oxidative and hydrolytic breakdown. Exposing parts to steam dramatically altered the internal microstructure and functional properties such as the glass transition temperature, tensile properties, and damping behavior. Notably, post-aging XCT revealed large microstructural changes after only 40 h of steam treatment relative to the as-printed specimens. Furthermore, pore reorganization and changes in crystallinity occurred regardless of whether the steam temperature was aggressive enough to induce a significant loss in mechanical properties. The build orientation dependence on the aging rate was minimal with the relative trend in performance persisting across most metrics among the different orientations even after aging.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Fiber orientation effects on ultra-high performance concrete formed by 3D printing

Despite the growing interest in 3D concrete printing, its current progress is limited by reinforcing methods. Inclusion of steel fibers is a potential reinforcing solution; however, the effect of printing process on orientation of the fibers is still unknown. This study aims to quantitatively investigate the orientation distribution of steel fibers in 3D printed ultra-high performance concrete. The effects of extrusion nozzle size, Cartesian print speed, and fiber volume fraction on the orientation of fibers were evaluated using digital image analysis. The consequent effects of the fiber orientation on the mechanical properties of the 3D-printed specimens were also determined. The results were compared with those of the conventionally mold-cast specimens. The results revealed that the smaller nozzle size and higher fiber volume fraction significantly enhanced the fiber alignment parallel to the printing direction. This preferential fiber alignment led to superior mechanical performance of the printed specimens to the mold-cast specimens.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Monitoring steel fibre orientation in self-compacting cementitious composite slabs during pouring with dynamic X-ray radiography

This paper presents a new technique based on dynamic X-ray radiography that can be used to assess fibre orientation during pouring of steel fibre reinforced cementitious composites. Synthetic examples were used to assess the suitability and robustness of the technique, which was shown to provide reliable measurements of fibre orientation even when the signal-to-noise ratio is relatively high. A study was then carried out on the effect of formwork aspect ratio, time/duration of pouring, and rebar placement on the fibre orientation while pouring self-compacting cementitious composite slabs. Results demonstrated the ability of the technique in monitoring the movements of fibres while pouring, and the strong effect of the flow in inducing preferential fibre alignment within the slabs. Fibre orientation was found to vary progressively over time and could take about half of the duration of pouring to fully stabilise.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of orientation on the directional and hemispherical emissivity of hyperbolic metamaterials

Here, we investigate the spectral directional and hemispherical emissivity of hyperbolic metamaterials with arbitrary orientation of the optic axis. The 4 x 4 matrix method is combined with coordinate rotational transforms to circumvent projection operations. The two hyperbolic bands of hexagonal boron nitride (hBN) are examined in detail to elucidate the influence of the orientation of the optic axis on the emissivities for both transverse magnetic (TM) and transverse electric (TE) waves. The results show that the orientation of the optic axis can greatly affect the hemispherical emissivity in the two hyperbolic bands of hBN. The directional emissivity varies periodically with the azimuthal angle when TM and TE waves are coupled, resulting in conversion of polarization in the medium. For both TM and TE waves, the matching of impedance and admittance at the surface of the material is better for smaller tilting angle in the type I hyperbolic band, but the opposite is true in type II hyperbolic band where the matching becomes better for larger tilting angles. As the tilting angle increases, the hemispherical emissivity decreases in the type I hyperbolic band but increases in the type II hyperbolic band. Our conclusions can be extended to other hyperbolic materials. Therefore, this work may provide valuable guidance on characterization, measurement and tailoring of the directional and hemispherical emissivity for hBN and other hyperbolic materials with arbitrary orientation and application of such materials for manipulation of radiative heat transfer.

36 MATERIALS SCIENCE↗
DOE OSTI2019

10% Efficiency Cu(In,Ga)Se2 Solar Cell with Strongly (220)/(204) Oriented Cu-Poor Absorber Layers Sputtered Using Single Quaternary Target

Cu-poor CIGS thin films were fabricated by RF magnetron sputtering from a single quaternary target with the composition of Cu0.7In0.7Ga0.3Se2, in an effort to improve the cell efficiency of CIGS solar cells. The Cu-poor thin films with the ([Cu]/[In]+[Ga]) composition ratios of 0.70-0.77 were obtained showing that the composition of the target can be transferred to the film. It was also observed that the strongly (220)/(204) preferred orientation appeared at the substrate temperatures higher than 600 degrees C, which is known to be essential for achieving high-quality CIGS solar cells. This result indicates that the Cu-Se compounds present in trace amounts of CIGS films hinder the (112) orientation and promotes the growth of the (220) orientation. As a result, the CIGS absorber layer with the Cu-poor composition and the (220)/(204) preferred orientation exhibited a drastically improved cell efficiency of 10.02%.

14 SOLAR ENERGY↗
DOE OSTI2023

Orientation matters: Measuring the correct surface of polyamide membranes with quartz crystal microbalance

The surface of polyamide reverse osmosis (RO) membranes which regulates interface-dominated phenomena, such as partitioning and fouling, is the one facing the feed during operation. However, the opposite surface of the polyamide selective layer, the one facing the permeate and in contact with the polysulfone porous support, is commonly analyzed in quartz crystal microbalance (QCM) measurements due to limitations of state-of-the-art transfer methodologies. Such measurements on the back surface cannot be generalized because the polyamide layer is chemically and morphologically asymmetric. Herein, we introduce a simple method to coat QCM sensors with polyamide active layers in the correct orientation (i.e., exposing their front surface) and show that interface-dominated phenomena differ significantly between orientations. We start by describing a transfer protocol to coat any surface with a polyamide layer on its front surface orientation. We then systematically analyze the chemical and morphological differences between the two surfaces of the polyamide layer of a commercial RO membrane. Finally, we demonstrate that interface-dominated phenomena depend on the orientation by showing that NaCl partitioning at pH 6 was 1.3 to 2.3-fold higher on the front surface and that organic fouling with humic acid occurred at a lower rate on this surface. The new method presented herein enables measurements on the front surface of polyamide RO membranes, which should be the standard in any future QCM studies.

Fouling behavior↗
DOE OSTI2020

Spatially Resolved Mapping of Three-Dimensional Molecular Orientations with ~2 nm Spatial Resolution through Tip-Enhanced Raman Scattering

We record local optical field images of silver nanocubes (75 nm) using tip-enhanced Raman (TER) spectral imaging. The images that we observe are consistent with several recent reports from our group, but here, we demonstrate sub-2 nm spatial resolution in local optical field nanoimaging under ambient laboratory conditions. This is achieved by scanning the substrate (nanocube on Si) relative to a 4-thiobenzonitrile (TBN)-functionalized Ag-coated TER probe. The spatial resolution that we obtain necessitates that only a few molecules govern the recorded optical response; molecular orientation becomes an important consideration in such measurements. We model the orientation through geometry optimization of a TBN molecule chemisorbed onto an Ag79 cluster (sphere with a ~1 nm diameter). Using the computed orientation of the cluster-bound molecule, we then model the optical response using formalism that accounts for the orientation of the molecule relative to vector components of the local optical fields. We find optimal agreement between experiment and theory. In effect, this work reveals the parallels between single-molecule Raman scattering and high-spatial-resolution TER spectroscopy, even when the images themselves cannot be used to visualize a single molecule in real space.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Using Grazing-Incidence Small-Angle Neutron Scattering to Study the Orientation of Block Copolymer Morphologies in Thin Films

Here, we used grazing-incidence small-angle neutron scattering (GISANS) to probe the depth-dependent orientation of self-assembled morphologies of block copolymers. A hydrophobic–hydrophobic block copolymer, poly(solketal methacrylate)-block-polystyrene (PSM-b-PS), was synthesized and spin-coated into films tens of nanometers in thickness where the polymers adopted a disordered state. PSM-b-PS was then hydrolyzed by exposing the polymer thin film to trifluoroacetic acid vapor or embedding a photoacid generator in the film during spin coating, followed by exposure to UV light. The hydrolysis converted the block copolymer into a hydrophilic–hydrophobic block copolymer, poly(glycerol monomethacrylate)-block-polystyrene (PGM-b-PS), significantly increasing the segmental interaction parameter (χ) and causing microphase separation of the copolymers. GISANS was used to study the depth-dependent structure of the films and revealed that the orientation of the microphase-separated structure differed at the polymer–air and polymer–substrate interfaces. In the regions where the lamellae were parallel to the interfaces, the orientation propagated into the film from the interfaces. However, in the areas where the lamellae were perpendicular to the interfaces, the orientation did not persist with increasing distance from the interfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Correlating Crystallographic Orientation and Ferroic Properties of Twin Domains in Metal Halide Perovskites

Metal halide perovskite (MHP) solar cells have attracted worldwide research interest. Although it has been well established that grain, grain boundary, and grain facet affect MHPs optoelectronic properties, less is known about subgrain structures. Recently, MHP twin stripes, a subgrain feature, have stimulated extensive discussion due to the potential for both beneficial and detrimental effects of ferroelectricity on optoelectronic properties. Furthermore, connecting the ferroic behavior of twin stripes in MHPs with crystal orientation will be a vital step to understand the ferroic nature and the effects of twin stripes. In this work, we studied the crystallographic orientation and ferroic properties of CH 3 NH 3 PbI 3 twin stripes, using electron backscatter diffraction (EBSD) and advanced piezoresponse force microscopy (PFM), respectively. Using EBSD, we discovered that the orientation relationship across the twin walls in CH 3 NH 3 PbI 3 is a 90° rotation about ($\bar{11}0$), with the (030) and (111) directions parallel to the direction normal to the surface. By careful inspection of CH 3 NH 3 PbI 3 PFM results including in-plane and out-of-plane PFM measurements, we demonstrate some nonferroelectric contributions to the PFM responses of this CH 3 NH 3 PbI 3 sample, suggesting that the PFM signal in this CH 3 NH 3 PbI 3 sample is affected by nonferroelectric and nonpiezoelectric forces. If there is piezoelectric response, it is below the detection sensitivity of our interferometric displacement sensor PFM (<0.615 pm/V). Overall, this work offers an integrated picture describing the crystallographic orientations and the origin of PFM signal of MHPs twin stripes, which is critical to understanding the ferroicity in MHPs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Preferred crystallographic orientation of cellulose in plant primary cell walls

Abstract Cellulose, the most abundant biopolymer on earth, is a versatile, energy rich material found in the cell walls of plants, bacteria, algae, and tunicates. It is well established that cellulose is crystalline, although the orientational order of cellulose crystallites normal to the plane of the cell wall has not been characterized. A preferred orientational alignment of cellulose crystals could be an important determinant of the mechanical properties of the cell wall and of cellulose-cellulose and cellulose-matrix interactions. Here, the crystalline structures of cellulose in primary cell walls of onion ( Allium cepa ), the model eudicot Arabidopsis ( Arabidopsis thaliana ), and moss ( Physcomitrella patens ) were examined through grazing incidence wide angle X-ray scattering (GIWAXS). We find that GIWAXS can decouple diffraction from cellulose and epicuticular wax crystals in cell walls. Pole figures constructed from a combination of GIWAXS and X-ray rocking scans reveal that cellulose crystals have a preferred crystallographic orientation with the (200) and (110)/( $$1\bar 10$$ 1 1 ¯ 0 ) planes preferentially stacked parallel to the cell wall. This orientational ordering of cellulose crystals, termed texturing in materials science, represents a previously unreported measure of cellulose organization and contradicts the predominant hypothesis of twisting of microfibrils in plant primary cell walls.

36 MATERIALS SCIENCE↗