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At least 703 records · Page 39

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NASA NTRS1980

Microstructure of the interplanetary magnetic field near 4 and 5 AU

Interplanetary magnetic field fluctuations near 4 and 5 AU are investigated on the basis of Pioneer 10 and 11 vector magnetic field measurements in order to identify extant wave modes and propagation directions as functions of frequency in the range 0.00004 to 0.009 Hz. Analysis of the approximately 500 spectral matrices as functions of frequency obtained from each spacecraft indicates the distributions of maximum variance directions to be peaked along the normal to the plane of the minimum variance direction and the mean magnetic field, as would be expected for a planar, small-amplitude Alfven wave with a minimum variance direction close to the wave vector. It is thus inferred that single small-amplitude Alfven waves are occasionally present in the temporal and frequency bands analyzed, however waves with wave vectors not well approximated by the minimum variance direction, Alfven wave ensembles, finite-amplitude waves and nonplanar fluctuations may also be present. Observations are also noted to suggest the predominance of the Alfven mode over the fast and slow modes, however do not support theoretical models of outward propagating plane Alfven waves of solar origin.

Parker, G. D.↗

DOE OSTI2026

Uncertainty quantification for competing failure mechanisms in unidirectionally reinforced carbon–carbon composites

Microstructure-informed finite element models play a key role in the carbon–carbon composite design process. Variability in manufacturing process parameters and experimental limitations introduce model parameter uncertainty. This study quantifies the effect of model parameter uncertainty on transverse tensile fracture behavior and proposes a methodology to predict the failure mode based on competing microscale damage mechanisms. Finite element simulations incorporate fiber–matrix interface debonding with cohesive zones and matrix damage with a smeared crack band approach in a unidirectional carbon–carbon composite. Results from a variance-based global sensitivity analysis identifies interfacial and matrix damage parameters as the primary source of variability in fracture behavior. Sobol’ indices indicate that matrix and cohesive zone strengths contribute 94% of the variance in the effective ultimate stress. A local analysis elucidates the relationship between these constituent strength parameters and failure mode by estimating the probability of cohesive, matrix, and mixed-mode dominated failure. Based on the results for 4000 simulations, 93% exhibit mixed-mode or interfacial dominated failure, which underscores the crucial role of fiber–matrix interface debonding in the transverse tensile failure of carbon–carbon composites. These uncertainty quantification results facilitate more efficient model calibration and provide a framework for microstructure-informed failure predictions in the face of manufacturing-induced uncertainty.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Comprehensive characterization of the irradiation effects of glassy carbon

Carbon materials have become increasingly diverse, finding applications in high-temperature and high-radiation environments. Glassy carbon, an allotrope known for its exceptional chemical inertness and desirable mechanical properties. However, understanding neutron irradiation effects in glassy carbon has proven challenging, primarily because of its unique nanopore structure. Here, this study presents a highly detailed microstructural characterization investigation of neutron-induced changes in glassy carbon, revealing how changes in nanopore structure and crystallinity impact the irradiation-induced shrinkage. Aberration-corrected scanning transmission electron microscopy (STEM) reveals pore closure that leads to material densification in the irradiated samples. Dimensional analysis combined with comparison to historical data suggest significant length shrinkage to occur. Neutron and in situ electron irradiation experiments suggest that glassy carbon transforms into so-called carbon onions, supporting the concept of shrinkage saturation. Investigating irradiation temperature effects using STEM, electron energy loss spectroscopy, x-ray diffraction, and Raman spectroscopy revealed partial amorphization at 210 °C–230 °C and preserved order in glassy carbon at 860 °C, coinciding with pore closure. Thermal property measurements were also conducted to assess the effects of densification and other changes in the atomic structure of glassy carbon. The results of this study have broad implications in the deployment of glassy carbon to nuclear environments, based around the observed changes in the thermal properties, and demonstrates the operational window for the onset of densification.

36 MATERIALS SCIENCE↗

DOE OSTI2026

High hardness and oxidation-resistant Cr-containing medium entropy ZrTaW diboride

This study reports the successful synthesis of a Cr-containing (Zr 0.30 Ta 0.34 Cr 0.06 W 0.30 )B 2 medium-entropy boride (MEB) via an in-situ reactive borothermal reduction route from oxide precursors. High-energy ball milling was employed to homogenize the precursor mixture prior to reactive densification. X-ray diffraction confirmed the formation of a predominantly AlB₂-type hexagonal diboride structure together with a secondary (W X , M 1-X )B monoboride phase. Microstructural characterization revealed compositional heterogeneity and localized W-rich regions associated with the secondary phase. The synthesized medium-entropy boride exhibited enhanced mechanical properties, which are attributed to lattice distortion and solid-solution strengthening effects. Thermogravimetric analysis revealed complex multistage oxidation behavior, and the oxidation resistance was compared with conventional ultra-high-temperature diborides. The results demonstrate the strong relationship between oxide-derived processing, compositional complexity, phase evolution, and oxidation behavior, highlighting the potential of medium-entropy borides for high-temperature structural applications

36 MATERIALS SCIENCE↗

NASA NTRS1978

The room-temperature dissociation of the compound Au3Si

Three gold-18.6 at.% silicon specimens which were solidified by quenching from above the liquidus temperature have been reexamined after being stored at room temperature for about 8 years. It was found that the 'metastable' compound Au3Si formed on quenching had begun to dissociate by a surface nucleated, solid-state reaction. The reaction front had advanced about 0.2 mm from the surface, leaving a rim of dissociation products. These dissociation products were studied using optical and scanning electron microscopy, electron beam microprobe analysis and an X-ray micro-diffraction technique. It was concluded that the reaction produces elemental gold and silicon, as at higher reaction temperatures, but that the scale of dispersion is so extremely fine that the resulting microstructure cannot be resolved by scanning electron microscopy.

Bhattacharya, D.↗

NASA NTRS1995

Modeling and characterization of through-the-thickness properties of 3D woven composites

The through-the-thickness properties of three-dimensionally (3D) woven carbon/epoxy composites have been studied. The investigation aimed at the evaluation and development of test methodologies for the property characterization in the thickness direction, and the establishment of fiber architectures were studied: layer-to-layer Angle Interlock, through-the-thickness Orthogonal woven preform with surface pile was also designed and manufactured for the fabrication of tensile test coupons with integrated grips. All the preforms were infiltrated by the resin transfer molding technique. The microstructures of the composites were characterized along the warp and fill (weft) directions to determine the degree of yarn undulations, yarn cross-sectional shapes, and microstructural dimensions. These parameters were correlated to the fiber architecture. Specimens were designed and tested for the direct measurement of the through-the-thickness tensile, compressive and shear properties of the composites. Design optimization was conducted through the analysis of the stress fields within the specimen coupled with experimental verification. The experimentally-derived elastic properties in the thickness direction compared well with analytical predictions obtained from a volume averaging model.

Hartranft, Dru↗

NASA NTRS2011

Characterizing TPS Microstructure: A Review of Some techniques

I. When seeking to understand ablator microstructure and morphology there are several useful techniques A. SEM 1) Visual characteriza3on at various length scales. 2) Chemical mapping by backscatter or x-ray highlights areas of interest. 3) Combined with other techniques (density, weight change, chemical analysis) SEM is a powerful tool to aid in explaining thermo/structural data. B. ASAP. 1) Chemical characteriza3on at various length scales. 2) Chemical mapping of pore structure by gas adsorption. 3) Provides a map of pore size vs. pore volume. 4) Provided surface area of exposed TPS. II. Both methods help characterize and understand how ablators react with other chemical species and provides insight into how they oxidize.

Gasch, Matthew↗

DOE OSTI2025

Novel Synthesis and Characterization of Uranium-Zirconium Carbonitride by Direct Casting

UZrCN has exhibited thermophysical properties beneficial to high temperature reactor applications such as nuclear thermal rockets. The present work investigates a novel liquid phase synthesis method involving the admission of nitrogen gas during arc melting of uranium, zirconium, and carbon. Initial microstructural examinations using SEM indicated that the samples remain heterogenous with zirconium-rich cores in a uranium-rich matrix. Heterogeneity resulted from large differences in melting temperature of the major constituents and rapid solidification. Additional EDS, combustion analysis, and inert gas fusion analysis proved that the core regions have both uranium and zirconium and establish that carbon and nitrogen are retained during the fabrication process. XRD clarifies that the light elements did not form compounds with the uranium matrix but rather incorporated into the core region forming a sub-stoichiometric UZrCN. Heat treatment performed on equimolar U-Zr-C resulted in an increase in the homogenous phase present with an XRD pattern reflecting a ternary UZrCN despite small amounts of segregation in the final button.

36 - MATERIALS SCIENCE↗

DOE OSTI2025

On Uranium-Zirconium Carbonitride Formation by Direct Casting - A Novel Synthesis Study

36 - MATERIALS SCIENCE↗

DOE OSTI2025

Redox-Induced Microstructure and Phase Dynamics in Nickel: Insights from In Situ Synchrotron X-ray Diffraction

Using in situ synchrotron X-ray diffraction, we interrogate the microstructural and phase evolution of polycrystalline nickel (Ni) during redox cycling in O 2 , H 2 , and H 2 O environments. Oxidation in O 2 promotes strong (111) texturing in both the NiO overlayer and the underlying Ni substrate. However, this crystallographic alignment is lost following reduction in H 2 and subsequent reoxidation, demonstrating irreversible microstructural changes. H 2 exposure leads to proton dissolution into the Ni lattice, triggering a localized phase transition from face-centered cubic (FCC) to hexagonal close-packed (HCP) Ni in hydrogen-saturated regions. In H 2 O-containing atmospheres, dissociative H 2 O adsorption produces protons that permeate the NiO layer, forming γ-NiOOH within the NiO lattice and HCP Ni beneath the NiO overlayer as protons accumulate. Kinetic analysis via the Johnson-Mehl-Avrami–Kolmogorov model uncovers distinct growth mechanisms: preoxidized Ni surfaces follow one-dimensional (1D) kinetics for NiO, γ-NiOOH, and HCP growth, whereas pristine Ni exhibits three-dimensional (3D) kinetics due to island-like nucleation and growth of NiO. Furthermore, these results highlight the critical interplay between H 2 O dissociation, hydrogen permeation, and redox-driven phase transformations, with practical implications in engineering nickel-based catalysts and hydrogen storage systems through controlled microstructural and phase evolution.

36 MATERIALS SCIENCE↗

NASA NTRS2006

High-Performance Scanning Acousto-Ultrasonic System

A high-performance scanning acousto-ultrasonic system, now undergoing development, is designed to afford enhanced capabilities for imaging microstructural features, including flaws, inside plate specimens of materials. The system is expected to be especially helpful in analyzing defects that contribute to failures in polymer- and ceramic-matrix composite materials, which are difficult to characterize by conventional scanning ultrasonic techniques and other conventional nondestructive testing techniques. Selected aspects of the acousto-ultrasonic method have been described in several NASA Tech Briefs articles in recent years. Summarizing briefly: The acousto-ultrasonic method involves the use of an apparatus like the one depicted in the figure (or an apparatus of similar functionality). Pulses are excited at one location on a surface of a plate specimen by use of a broadband transmitting ultrasonic transducer. The stress waves associated with these pulses propagate along the specimen to a receiving transducer at a different location on the same surface. Along the way, the stress waves interact with the microstructure and flaws present between the transducers. The received signal is analyzed to evaluate the microstructure and flaws. The specific variant of the acousto-ultrasonic method implemented in the present developmental system goes beyond the basic principle described above to include the following major additional features: Computer-controlled motorized translation stages are used to automatically position the transducers at specified locations. Scanning is performed in the sense that the measurement, data-acquisition, and data-analysis processes are repeated at different specified transducer locations in an array that spans the specimen surface (or a specified portion of the surface). A pneumatic actuator with a load cell is used to apply a controlled contact force. In analyzing the measurement data for each pair of transducer locations in the scan, the total (multimode) acousto-ultrasonic response of the specimen is utilized. The analysis is performed by custom software that extracts parameters of signals in the time and frequency domains. The computer hardware and software provide both real-time and postscan processing and display options. For example, oscilloscope displays of waveforms and power spectral densities are available in real time. Images can be computed while scanning continues. Signals can be digitally preprocessed and/or post-processed by filtering, windowing, time-segmenting, and running-waveform-averaging algorithms. In addition, the software affords options for off-line simulation of the waveform-data-acquisition and scanning processes. In tests, the system has been shown to be capable of characterizing microstructural changes and defects in SiC/SiC and C/SiC ceramic-matrix composites. Delaminations, variations in density, microstructural changes attributable to infiltration by silicon, and crack-space indications (defined in the next sentence) have been revealed in images formed from several time- and frequency-domain parameters of scanning acousto-ultrasonic signals. The crack-space indications were image features that were not revealed by other nondestructive testing methods and are so named because they turned out to mark locations where cracking eventually occurred.

Roth, Don↗

NASA NTRS1981

Failure analysis of a tool steel torque shaft

A low design load drive shaft used to deliver power from an experimental exhaust heat recovery system to the crankshaft of an experimental diesel truck engine failed during highway testing. An independent testing laboratory analyzed the failure by routine metallography and attributed the failure to fatigue induced by a banded microstructure. Visual examination by NASA of the failed shaft plus the knowledge of the torsional load that it carried pointed to a 100 percent ductile failure with no evidence of fatigue. Scanning electron microscopy confirmed this. Torsional test specimens were produced from pieces of the failed shaft and torsional overload testing produced identical failures to that which had occurred in the truck engine. This pointed to a failure caused by a high overload and although the microstructure was defective it was not the cause of the failure.

Reagan, J. R.↗

NASA NTRS1983

Failure analysis of a tool steel torque shaft

Reagan, J. R.↗

DOE OSTI2025

Multiscale Characterization of Additive Manufacturing Components with Computed Tomography, 3D X-ray Microscopy, and Deep Learning

Additive manufacturing (AM) facilitates the creation of complex-geometry parts, driving advancements in lightweight aerospace components, high-efficiency engine cooling channels, and customized medical implants. However, ensuring the quality and reliability of AM parts remains challenging due to internal defects, surface irregularities, porosity, and residual trapped powder, which are often inaccessible to traditional inspection methods. Recent developments in X-ray computed tomography (XCT) and 3D X-ray microscopy (XRM), particularly systems equipped with resolution-at-a-distance (RaaD™) capabilities, enable high-resolution, non-destructive evaluation of AM components across multiple scales, from sub-micrometer to macroscopic levels. This paper explores modern XCT and XRM techniques for multiscale characterization of AM parts, focusing on their ability to detect and analyze defects such as porosity, cracks, inclusions, and surface roughness, while offering insights into defect formation mechanisms, material properties, and process-induced variations. The integration of deep learning (DL) frameworks, including Simurgh, DeepRecon, and DeepScout, enhances XCT/XRM workflows by reducing scan times, improving resolution recovery, and enabling accurate defect detection even with limited projection data. These DL-based methods overcome limitations of traditional reconstruction techniques, enabling faster, more reliable characterization of dense materials like Inconel 718 and novel alloys such as AlCe. Applications include process parameter optimization, high-throughput quality control, and multistage AM process evaluation, with DL-enhanced workflows accelerating analysis times from weeks to days. Correlative imaging approaches further validate XCT and XRM data against scanning electron microscopy (SEM) images of physically sectioned samples, confirming the accuracy of DL-based reconstructions and enabling comprehensive defect analysis. While challenges remain in generalizing DL models to diverse materials and imaging conditions, improvements in resolution, noise reduction, and defect detection highlight the transformative potential of these methods. This multiscale and correlative approach enables precise identification and correlation of microstructural features with the overall performance of AM components. By integrating advanced XCT, XRM, and DL techniques, this paper demonstrates a significant leap forward in AM characterization, offering valuable insights into the relationships between processing parameters, microstructure, and part performance, and driving innovations that enhance the quality and reliability of AM products for demanding industrial applications.

Additive manufacturing↗

DOE OSTI2024

Metal Scrap Upcycling with Shear Assisted Processing and Extrusion (ShAPE)

The overarching objective of this project is to convert metal scraps, such as aluminum, titanium, and other alloys provided by the industry, into extruded tubing, wires, and rods. Upcycling of scrap will be accomplished using Shear Assisted Processing and Extrusion (ShAPE). This approach is a new solution for recycling. The specific aims of this project are as follows: 1. Receive metal scrap under a Material Transfer Agreement (MTA), in the form of billets, from select industry partners that meet the following requirements: outer diameter of 1.245 inches (+/-0.003 inches), inner diameter drilled with a 0.404-inch drill bit, and a length of 4.0 inches (+/-0.01 inches). The billet must be cast or compacted to greater than 98% density. If the industry partner does not have the capabilities to prepare the billets, PNNL can make introductions to third-party entities as needed. Industry partners will also provide a composition analysis as weight percent. 2. Extrude metal scrap via the ShAPE process at PNNL. 3. Evaluate and benchmark the extrudate material properties per the ASTM B557-15 – Testing Tubulars Standard or similar wire and rod standards. 4. Characterize the extrudate microstructure for any of the following: grain size, second phase composition, and texture. Additional testing may include corrosion per the ASTM B117 standard and electro-potential. 5. Deliver specimens to industry partners under an MTA for additional third-party evaluations. Industry partners will, in return, provide a non-proprietary report on any testing, including testing per the ASTM B557-15, ASTM B117, and other industry standards. 6. PNNL will develop data and insights to support intellectual property capture, a published non-proprietary technical report, research collaborations, and commercialization opportunities.

36 MATERIALS SCIENCE↗

NASA NTRS1986

Transition from a planar interface to cellular and dendritic structures during rapid solidification processing

The development of theoretical models which characterize the planar-cellular and cell-dendrite transitions is described. The transitions are analyzed in terms of the Chalmers number, the solute Peclet number, and the tip stability parameter, which correlate microstructural features and processing conditions. The planar-cellular transition is examined using the constitutional supercooling theory of Chalmers et al., (1953) and it is observed that the Chalmers number is between 0 and 1 during dendritic and cellular growth. Analysis of cell-dendrite transition data reveal that the transition occurs when the solute Peclet number goes through a minimum, the primary arm spacings go through a maximum, and the Chalmers number is equal to 1/2. The relation between the tip stability parameter and the solute Peclet number is investigated and it is noted that the tip stability parameter is useful for studying dendritic growth in alloys.

Laxmanan, V.↗

NASA NTRS2014

Focal Gray Matter Plasticity as a Function of Long Duration Bedrest: Preliminary Results

Long duration spaceflight (i.e., 22 days or longer) has been associated with changes in sensorimotor systems, resulting in difficulties that astronauts experience with posture control, locomotion, and manual control. It is unknown whether and how spaceflight impacts sensorimotor brain structure and function, and whether such changes may potentially underlie behavioral effects. Long duration head down tilt bed rest has been used repeatedly as an exclusionary analog to study microgravity effects on the sensorimotor system [1]. Bed rest mimics microgravity in body unloading and bodily fluid shifts. We are currently testing sensorimotor function, brain structure, and brain function pre and post a 70‐day bed rest period. We will acquire the same measures on NASA crewmembers starting in 2014. Here we present the results of the first eight bed rest subjects. Subjects were assessed at 12 and 7 days before‐, at 7, 30, and ~70 days in‐, and at 8 and 12 days post 70 days of bed rest at the NASA bed rest facility, UTMB, Galveston, TX, USA. At each time point structural MRI scans (i.e., high resolution T1‐weighted imaging and Diffusion Tensor Imaging (DTI)) were obtained using a 3T Siemens scanner. Focal changes over time in gray matter density were assessed using the voxel based morphometry 8 (VBM8) toolbox under SPM. Focal changes in white matter microstructural integrity were assessed using tract based spatial statistics (TBSS) as part of the FMRIB software library (FSL). TBSS registers all DTI scans to standard space. It subsequently creates a study specific white matter skeleton of the major white matter tracts. Non‐parametric permutation based t‐tests and ANOVA's were used for voxel‐wise comparison of the skeletons. For both VBM and TBSS, comparison of the two pre bed rest measurements did not show significant differences. VBM analysis revealed decreased gray matter density in bilateral areas including the frontal medial cortex, the insular cortex and the caudate nucleus from pre to in bed rest. Over the same time period, there was an increase in gray matter density in the cerebellum, occipital, and parietal cortices. The majority of these changes did not recover from during to post bed rest. TBSS analyses will also be presented. Extended bed rest, which is an analog for microgravity, can result in gray matter changes and potentially in microstructural white matter changes in areas that are important for neuromotor behavior and cognition. These changes did not recover at two weeks post bed rest. These results have significant public health implications, and will also aid in interpretation of our future data obtained pre and post spaceflight. Whether the effects of bed rest wear off at longer times post bed rest, and if they are associated with behavior are important questions that warrant further research.

Koppelmans, V.↗

NASA NTRS1990

A study of hydrogen environment effects on microstructure property behavior of NASA-23 alloy and related alloy systems

This work is part of the overall advanced main combustion chamber (AMCC) casting characterization program of the Materials and Processes Laboratory of the Marshall Space Flight Center. The influence of hydrogen on the tensile properties and ductility behavior of NASA-23 alloy were analyzed. NASA-23 and other referenced alloys in cast and hipped conditions were solution treated and aged under selected conditions and characterized using optical metallography, scanning electron microscopy, and electron microprobe analysis techniques. The yield strength of NASA-23 is not affected much by hydrogen under tensile tests carried at 5000 psig conditions; however, the ultimate strength and ductility properties are degraded. This implies that the physical mechanisms operating would be related to the plastic deformation process. The fracture surfaces characteristics of NASA-23 specimens tensile tested in hydrogen, helium, and air were also analyzed. These revealed surface cracks around specimen periphery with the fracture surface showing a combination of intergranular and transgranular modes of fracture. It is seen that the specimens charged in hydrogen seem to favor a more brittle fracture mode in comparison to air and helium charged specimens. The AMCC casting characterization program is to be analyzed for their hydrogen behavior. As a result of this program, the basic microstructural factors and fracture characteristics in some cases were analyzed.

Diwan, Ravinder M.↗