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DOE OSTI2025

Electron ptychography reveals a ferroelectricity dominated by anion displacements

Sodium niobate, a lead-free ferroic material, hosts delicately balanced, competing order parameters, including ferroelectric states that can be stabilized by epitaxial strain. Here we show that the resulting macroscopic ferroelectricity exhibits an unconventional microscopic structure using multislice electron ptychography. This technique overcomes multiple scattering artefacts limiting conventional electron microscopy, enabling both lateral spatial resolution beyond the diffraction limit and recovery of three-dimensional structural information. These imaging capabilities allow us to separate the ferroelectric interior of the sample from the relaxed surface structure and identify the soft phonon mode and related structural distortions with picometre precision. Unlike conventional ferroelectric perovskites, we find that the polar distortion in this material involves minimal distortions of the cation sublattices and is instead dominated by anion displacements relative to the niobium sublattice. We establish limits on film thickness for interfacial octahedral rotation engineering and directly visualize a random octahedral rotation pattern, arising from the flat dispersion of the associated phonon mode.

ferroelectrics and multiferroics↗

NASA NTRS1992

Correlation of deformation mechanisms with the tensile and compressive behavior of NiAl and NiAl(Zr) intermetallic alloys

To identify the mechanisms controlling strength and ductility in powder-extruded NiAl and NiAl + 0.05 at. pct Zr, tensile and compressive testing was performed from 300 to 1300 K for several grain sizes. Grain size refinement significantly increased yield stress in both alloys and, in some cases, slightly lowered the ductile-to-brittle transition temperature (DBTT), although no room-temperature tensile ductility was observed even in the finest grain size specimens. The small Zr addition increased the DBTT and changed the low-temperature fracture mode from intergranular in NiAl to a combination of intergranular and transgranular in the Zr-doped alloy. Scanning electron microscopy of compression specimens deformed at room temperature revealed the presence of grain-boundary cracks in both alloys. These cracks were due to the incompatibility of strain in the polycrystalline material, owing to the lack of five independent slip systems. The tendency to form grain-boundary cracks, in addition to the low fracture stress of these alloys, contributed to the lack of tensile ductility at low temperatures.

Bowman, R. R.↗

NASA NTRS1995

Effect of Processing Route on Strain Controlled Low Cycle Fatigue Behavior of Polycrystalline NiAl

The present investigation examines the effects of manufacturing process on the total axial strain controlled low cycle fatigue behavior of polycrystalline NiAl at 1000 K, a temperature above the monotonic Brittle-to-Ductile Transition Temperature (BDTT). The nickel aluminide samples were produced by three different processing routes: hot isostatic pressing of pre- alloyed powders, extrusion of prealloyed powders, and extrusion of vacuum induction melted ingots. The LCF behavior of the cast plus extruded material was also determined at room temperature (below the BD77) for comparison to the high temperature data. The cyclic stress response, cyclic stress-strain behavior, and strain-life relationships were influenced by the alloy preparation technique and the testing temperature. Detailed characterization of the LCF tested samples was conducted by optical and electron microscopy to determine the variations in fracture and deformation modes and to determine any microstructural changes that occurred during LCF testing. The dependence of LCF properties on processing route was rationalized on the basis of starting microstructure, brittle-to-ductile transition temperature, deformation induced changes in the basic microstructure, deformation substructure, and synergistic interaction between the damage modes.

Rao, K. Bhanu Sankara↗

NASA NTRS1974

The effect of microstructure on the fracture toughness of titanium alloys

The microstructure of the alpha titanium alloy Ti-5Al-2.5Sn and the metastable beta titanium alloy Beta 3 was examined. The material was from normal and extra low interstitial grade plates which were either air-cooled or furnace-cooled from an annealing treatment. Beta 3 was studied in alpha-aged and omega-aged plates which were heat treated to similar strength levels. Tensile and plane strain fracture toughness tests were conducted at room temperature on the alpha-aged material. The microstructure and fracture mechanisms of alloys were studied using optical metallography, electron microscopy, microprobe analyses, and texture pole figures. Future experiments are described.

Vanstone, R. H.↗

NASA NTRS2000

Assessment of Internal Fabric of Particulate Materials

Particle arrangement and distribution within a soil matrix has long been recognized as having significant influence on the mechanical behavior of cohesionless soils. It is well known that two soil specimens having the same grain type (e.g., quartz, feldspar, etc.), same grain size distribution and relative density (or void ratio) can display completely different mechanical behavior. Because of the different fabric configurations in the otherwise similar specimens, they are likely to have different mechanical properties such as stress-strain response, anisotropy, dilatancy, etc. Soil Fabric is defined as the arrangement of particles, particle groups and associated pore space. In the literature, fabric analysis techniques are mainly classified as destructive (e.g., specimen stabilization, thin-sectioning, and microscopy), and nondestructive techniques (e.g., magnetic resonance imaging, ultrasonic testing, x-ray radiography, and computed tomography). Quantifying the void ratio and its distribution is the main parameter used to describe the fabric of particulate materials. This paper presents a comprehensive literature review of fabric analysis techniques applied to particulate materials. In addition, the results of a comprehensive investigation to quantify void ratio of sand specimens will be presented and discussed. The sand used in the experiments in a natural, uniform rounded to sub-rounded silica sand known as F-75 banding sand with mean particle size of 0.22 mm. Uniform specimens and specimens subjected to different axial-strain levels tested under triaxial and biaxial conditions are examined to evaluate void ratio evolution and its distribution using destructive thin-sectioning and nondestructive Computed Tomography (CT) techniques. Details of a new innovative polygon generation technique called Voronoi tessellation used to quantify void ratio of microscopic images of sand grains will be presented and compared to classical Oda's method. Finally, frequency distribution of void ratio calculated using CT analysis will be presented and discussed.

Alshibi, Khalid A.↗

DOE OSTI2025

Development of an ultrahigh affinity, trimeric ACE2 biologic as a universal SARS-CoV-2 antagonist

Abstract Severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2), responsible for the COVID-19 pandemic, utilizes membrane-bound, angiotensin-converting enzyme II (ACE2) for internalization and infection. We describe the development of a biologic that takes advantage of the proximity of the N-terminus of bound ACE2 to the three-fold symmetry axis of the spike protein to create an ultrapotent, trivalent ACE2 entry antagonist. Distinct disulfide bonds were added to enhance serum stability and a single point mutation was introduced to eliminate enzymatic activity. Through surface plasmon resonance, pseudovirus neutralization assays, and single-particle cryo-electron microscopy, we show this antagonist binds to and inhibits SARS-CoV-2 variants. We further show the antagonist binds to and inhibits a 2003 SARS-CoV-1 strain. Collectively, structural insight has allowed us to design a universal trivalent antagonist against all variants of SARS-CoV-2 tested, suggesting it will be active against the emergence of future mutants.

Gonzales, Juliet (ORCID:0000000327219566)↗

NASA NTRS1984

High temperature low-cycle fatigue mechanisms in single crystals of nickel-based superalloy Mar-M 200

Twenty three high temperature low-cycle fatigue tests were conducted on single crystals of the nickel-based superalloy Mar-M 200. Tests were conducted at 760 and 870 C. SEM fractography and transmission electron microscopy were used to determine mechanisms responsible for the observed orientation dependent fatigue behavior. It has been concluded that the plastic characteristics of the alloy lead to orientation-dependent strain hardening and fatigue lives at 760 C. At 870 C, the elastic characteristics of the alloy dominated the behavior, even though the plastic strain ranges were about the same as they were at 760 C. This led to orientation-dependent fatigue lives, but the trends were not the same as they were at 760 C.

Milligan, W. W.↗

NASA NTRS1991

Deformation and failure mechanisms in metal matrix composites

An investigation was undertaken to determine the key deformation mechanisms and their interaction leading to failure of both 0 degree and 90 degree Ti 15-3/SCS-6 laminae under monotonic loading. The experimental results suggest that inelastic deformation in the 0-degree lamina is dominated by plastic deformation and that in the 90-degree lamina is dominated by both fiber-matrix debonding and plasticity. The loading-unloading response, monitoring of Poisson's ratio and microscopy were utilized to identify the key deformation mechanisms. The sequence of deformation mechanisms leading to failure are identified for both the 0 and the 90-degree specimens. The threshold strains for plasticity or damage which are referred to as 'microdeformation' in the 0 deg and 90 deg laminae are approximately 0.004 and 0.002, respectively, at room temperature. These strain levels may be considered critical in initiation based structural design with these composites.

Newaz, G.↗

NASA NTRS1990

Cosmos 1887: morphology, histochemistry, and vasculature of the growing rat tibia

Light microscopy, electron microscopy, and enzyme histochemistry were used to study the effects of spaceflight on metaphyseal and cortical bone of the rat tibia. Cortical cross-sectional area and perimeter were not altered by a 12.5-day spaceflight in 3-month-old male rats. The endosteal osteoblast population and the vasculature near the periosteal surface in flight rats compared with ground controls showed more pronounced changes in cortical bone than in metaphyseal bone. The osteoblasts demonstrated greater numbers of transitional Golgi vesicles, possibly caused by a decreased cellular metabolic energy source, but no difference in the large Golgi saccules or the cell membrane-associated alkaline phosphatase activity. The periosteal vasculature in the diaphysis of flight rats often showed lipid accumulations within the lumen of the vessels, occasional degeneration of the vascular wall, and degeneration of osteocytes adjacent to vessels containing intraluminal deposits. These changes were not found in the metaphyseal region of flight animals. The focal vascular changes may be due to ischemia of bone or a developing fragility of the vessel walls as a result of spaceflight.

Non-NASA Center↗

DOE OSTI2026

Programmable Phase Selection between Altermagnetic and Noncentrosymmetric Polymorphs of MnTe on InP via Molecular Beam Epitaxy

This dataset contains DFT input and output files supporting the theoretical modeling in the associated publication (ACS Appl. Mater. Interfaces 2026, 18, 15654-15664). The calculations model the interfacial energetics of two MnTe polymorphs — NiAs-MnTe (hexagonal, alpha phase) and ZnS-MnTe (cubic, gamma phase) — on InP(111) substrates with two surface terminations: In-terminated InP(111)A and P-terminated InP(111)B. This gives four interface configurations: NiAs on In-terminated (experimentally observed), NiAs on P-terminated (computed for comparison), ZnS on In-terminated (computed for comparison), and ZnS on P-terminated (experimentally observed). The dataset is organized into four calculation types, each covering all four polymorph/termination combinations: (i) Slabs: Pristine MnTe/InP heterostructure slabs used to compute total energies and interface energy densities (Eint) for all four configurations, as reported in Fig. 6 of the main text. (ii) Disorder: Same slab geometries with a P_Te + Te_P antisite defect pair introduced near the interface, used to assess chemical intermixing effects on interface stability (Fig. S8, SI). (iii) Strain: Pristine slab calculations with in-plane lattice parameters strained by -1% and +1% relative to the InP lattice constant, used to evaluate strain-dependent interface energetics (Fig. S9, SI). (iv) Charge_Density: Single-point calculations on the full heterostructure, the isolated InP slab, and the isolated MnTe slab at fixed geometry, used to compute differential charge density plots showing interfacial charge accumulation and depletion as a function of surface termination (Fig. S10, SI). Each calculation folder contains INCAR, KPOINTS, POSCAR, CONTCAR, OUTCAR, and POTCAR_info.txt (PAW potential information, excluding the full POTCAR due to VASP licensing restrictions). The calculations were performed using VASP 6.4.3 with PBE exchange-correlation, PAW potentials, a Hubbard correction of Ueff = 5 eV on Mn d-states, and A-type AFM spin initialization.

36 MATERIALS SCIENCE↗

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

thermoplastic↗

DOE OSTI2025

Phase segregation dynamics in mixed-halide perovskites revealed by plunge-freeze cryo-electron microscopy

Mixed-halide lead perovskites, with photoexcited charge-carrier properties suitable for high-efficiency photovoltaics, hold significant promise for high-efficiency tandem solar cells. However, phase segregation under illumination, where an iodide-rich phase forms carrier trap states, remains a barrier to application. This study employs plunge-freeze cryoelectron microscopy to visualize nanoscale phase segregation dynamics in CsPb(Br x I 1–x ) 3 films. By rapidly freezing the illuminated samples, we preserve transient photoexcited ion distributions for high-resolution structural and compositional analysis at the nanoscale. Cryogenic scanning transmission electron microscopy (STEM) techniques (electron energy loss spectroscopy [EELS] and 4D-STEM) captured the dynamics of photo-induced iodine migration from grain boundaries to centers, identified the buildup of anisotropic strain, and captured the heterogeneous evolution of this process within a single grain. These findings provide insight into microscopic phase segregation mechanisms and their dynamics, enhancing our understanding of mixed-halide perovskite photostability.

42 ENGINEERING↗

DOE OSTI2024

Embedding of Optical Fibers with Electric Field Assisted Sintering

The Electric Field Assisted Sintering (EFAS) technique was used for embedding the fibers, involving rapid heating via an electric current and pressure, reducing fiber exposure to high temperatures. Stainless steel guide tubes were inserted at the fiber-matrix junctions to prevent fiber breakage during the sintering process. The study varied key EFAS parameters—temperature (800°C to 980°C), pressure (40-50 MPa), and hold time (5-10 minutes)—to assess how they influenced fiber embedding. After embedding, the fibers were inspected using optical frequency domain reflectometry (OFDR) to evaluate optical losses and strain along the fiber length. The OFDR scans confirmed that the fibers remained intact, and subsequent transmission tests demonstrated no macroscopic fractures. The embedded samples were also analyzed using scanning electron microscopy (SEM) and X-ray computed tomography (CT) scans. These tests confirmed good bonding between the fiber and matrix with no cracking, though some porosity was present in samples fabricated at lower temperatures. At higher temperatures (980°C), the fiber-matrix bonding was continuous and defect-free, with metal coatings aiding in the bonding process. Elemental analysis showed interdiffusion between the fiber coatings and matrix materials, particularly between the gold coating and stainless steel. Helium leak tests revealed that lower sintering temperatures resulted in matrix porosity, causing leaks, but samples fabricated at 980°C were leak-tight.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

NASA NTRS1977

Correlation of creep rate with microstructural changes during high temperature creep

Creep tests were conducted on Haynes 188 cobalt-base alloy and alpha titanium. The tests on Haynes 188 were conducted at 1600 F and 1800 F for stresses from 3 to 20 ksi, and the as-received, mill-annealed results were compared to specimens given 5%, 10%, and 15% room temperature prestrains and then annealed one hour at 1800 F. The tests on alpha titanium were performed at 7,250 and 10,000 psi at 500 C. One creep test was done at 527 C and 10,000 psi to provide information on kinetics. Results for annealed titanium were compared to specimens given 10% and 20% room temperature prestrains followed by 100 hours recovery at 550 C. Electron microscopy was used to relate dislocation and precipitate structure to the creep behavior of the two materials. The results on Haynes 188 alloy reveal that the time to reach 0.5% creep strain at 1600 F increases with increasing prestrain for exposure times less than 1,000 hours, the increase at 15% prestrain being more than a factor of ten.

Young, C. T.↗

NASA NTRS1984

The influence of hold times on LCF and FCG behavior in a P/M Ni-base superalloy

The relative importance of creep and environmental interactions in high temperature fatigue behavior has been investigated for as-HIP Rene 95. Strain-controlled low cycle fatigue and load-controlled fatigue crack growth tests were performed at elevated temperatures in argon, followed by fractographic analyses of the fracture surfaces by scanning electron microscopy. Fatigue lives were drastically reduced and crack growth rates increased one hundred fold as a result of superposition of hold times on continuous cycling. A change in fracture mode with hold time also was noted. Chromium oxide was detected on the fracture surface by Auger electron spectroscopy. The drastic changes in fatigue resistance due to hold times were attributed primarily to environmental interactions with fatigue processes.

Choe, S. J.↗

NASA NTRS1992

Mechanisms of compressive failure in 3D composites

The present study of angle-interlock woven polymer matrix composite behavior under uniaxial monotonic compression notes these materials to be macroscopically ductile, with compressive strains in failure that can exceed 15 percent. Some of the tests conducted on stitched laminates indicated brittle behavior. Woven composite failure mechanisms have been studied by a combination of optical microscopy, moire interferometry, stereoscopy, and digital image comparisons; the critical failure event was in all cases a kink band formation in the primary load-bearing axial rows.

Cox, B. N.↗

NASA NTRS1996

Crack Development in Cross-Ply Laminates Under Uniaxial Tension

This study addresses matrix-dominated failures in carbon fiber/polymer matrix composite laminates in a cross-ply lay-up. The events of interest are interlaminar fracture in the form of transverse cracks in the 90' plies and longitudinal splitting in the 0 deg plies and interlaminar fracture in the form of 0/90 delamination. These events were observed using various nondestructive evaluation (NDE) techniques during static tensile tests. Acoustic emission (AE) x radiography, and edge view microscopy were the principal ones utilized in a real-time environment. A comparison of the NDE results with an analytical model based on the classical linear fracture mechanics concept of strain energy release rate as a criterion for crack growth was performed. The virtual crack closure theory was incorporated with a finite element model to generate strain energy release rate curves for the analytical case. Celion carbon fiber/polyimide matrix (G30-500/PMR-15) was the material tested with cross-ply lay-ups of (0(2)/90(6))s and (0(4)/90(4))s. The test specimens contained thermally induced cracks caused by the high-temperature processing. The analytical model was updated to compensate for the initial damage and to study further accumulation by taking into account the crack interactions. By correlating the experimental and analytical data, the critical energy release rates were found for the observable events of interest.

Gyekenyesi, Andrew L.↗