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DOE OSTI2025

Molecular-resolution imaging of ice crystallized from liquid water by cryogenic liquid-cell TEM

Despite the ubiquity of ice, a molecular-resolution image of nanoscopic defects or microstructures in ice crystallized from liquid water has never been obtained. This is mainly due to the difficulties in preparing and preserving crystalline ice samples that can survive under high-resolution imaging conditions. Here, we report the stabilization and Å-resolution electron imaging of ice Ih crystallized from liquid water by developing cryogenic liquid-cell transmission electron microscopy (CRYOLIC-TEM). We combine lattice mapping with molecular dynamics simulations to reveal that ice formation is highly tolerant to nanoscale defects such as misoriented subdomains and trapped gas bubbles, which are stabilized by molecular-scale structural motifs. Importantly, bubble surfaces adopt low-energy nanofacets and create negligible strain fields in the surrounding crystal. These bubbles can dynamically nucleate, grow, migrate, dissolve, and coalesce under electron irradiation and be monitored in situ near a steady state. This work improves our understanding of water crystallization behaviors at a molecular spatial resolution.

Materials science↗

DOE OSTI2022

Hole Trapping in Halide Perovskites Induces Phase Segregation

Metal halide perovskites have garnered a great deal of attention for their applications in photovoltaics, LEDs, and radiation detection. The ease of solution processing high-quality perovskite semiconductors with large absorption coefficients and tolerance to native defects is decidedly attractive. Additionally, the ability to precisely tune the band gap of halide perovskites through compositional alloying of the halide ion is of particular interest for a range of applications, especially for tandem solar cells. However, under steady state light irradiation, an initially homogeneous mixed halide perovskite (MHP) will form local domains that are rich in one halide ion (e.g., Br or I). This light-induced phase segregation in MHPs forms iodide-rich domains that act as charge carrier traps and lowers the efficiency of perovskite-based devices. Thus, phase segregation poses a serious challenge to the implementation of MHPs in real-world device settings. Interestingly, when a phase segregated MHP film is placed in the dark, entropic driving forces become dominant and the segregated perovskite remixes and returns to its initially homogeneous state. Several key mechanistic details of phase segregation have been elucidated over the years. However, there are still aspects of halide segregation that are not clear, and there is ongoing debate in the literature as to what are the key factors that contribute to the mechanism. This Account discusses recent results that point to the specific role of hole trapping in phase segregation. Interestingly, generation of holes through above-band-gap excitation or through electrochemical injection increases ion migration and leads to phase segregation. The thermodynamic and redox properties of halide perovskites provide a strong driving force for hole trapping and oxidation of iodide species in MHPs. However, mobile halide species within the perovskite lattice take time to migrate and generate halide-rich domains. When in contact with a nonpolar solvent, the migration of iodine species is further extended to expulsion of iodine from the perovskite film. Thus, the mobility of halides and their susceptibility to hole-induced oxidation play a crucial role in determining the long-term stability of metal halide perovskites. Strategies to gain kinetic control over ion migration to slow phase segregation are needed to overcome these hurdles and achieve stable mixed halide perovskites. Modification of the perovskite composition through introduction of different cations or halide ions, or introduction of low-dimensional perovskite phases may suppress phase segregation. Furthermore, in achieving stability and improving the efficiency of perovskite solar cells and light emitting devices with minimal impacts, suppression of segregation remains the key factor.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Six micrometer period wide-gap permalloy magnetic bubble devices

This report describes the progress made toward the goal of developing a 1 Mbit bubble memory chip, based on a 6 micron period wide-gap permalloy technology. Characterization of the functions showed that the guard-rail, generator, swap, write-line, read-line and after several revisions, the replicator and the expander-detector performed acceptably in preliminary testing. Several investigations were initiated to solve the problem of low minor loop yield. A dual-spacing process, which allows the minor loop propagation elements to be more tightly coupled to the garnet film was developed. Several new propagate structures, intended to be more tolerant of small defects were also conceived.

Chirovsky, L. M. F.↗

NASA NTRS1991

Analysis of foil bearings for high speed operation in cryogenic applications

The general objective of this project is to develop analysis tools which are required for the design of foil bearings to be used in cryogenic applications. During the second year of this project, a general analysis approach and code for journal bearings operating under steady state conditions will be completed. This will be followed by the initiation of an investigation into transient behavior of foil bearings to determine their performance in rotor systems. Foil bearings have been proposed as an alternative to rolling element bearings for use in cryogenic turbopumps in liquid propellant rocket engines. This type of bearing offers several advantages over rolling element bearings since they would use the cryogenic pump fluid for a lubricant and have structural flexibility. These bearings have the potential of high reliability and long life. The bearing surface is constructed of a 'foil' which resists deflection by a combination of bending, membrane, and elastic foundation effects. The relative motion between the rotating shaft and the foil causes pressure in the fluid film to develop. This pressure deflects the the foil surface away from the shaft. Once a full fluid film is established between the foil and the rotor shaft, contact no longer takes place and there is no subsequent wear of the surfaces. The flexible foil structure of the bearing allows it to compensate for minor tolerance and manufacturing defects. This same flexibility also has a significant effect on the dynamic performance of the rotor-bearing system.

Carpino, Marc↗

DOE OSTI2026

Radiation Tolerance of Nanoporous Gadolinium Titanate

Defect sinks play a crucial role in reducing radiation-induced damage accumulation, but their effectiveness varies. This study directly compares the efficacy of grain boundaries and pores (free surfaces) in gadolinium titanate (Gd 2 Ti 2 O 7 ) using in situ ion irradiation transmission electron microscopy (TEM). A unique sample configuration is developed, where each of the three distinct regions, each containing only one primary sink of interest, is in the same TEM lamella for simultaneous irradiation. Regular assessments of crystallinity in each region via nanobeam electron diffraction show that, at both room temperature and 600°C, free surface (pore) defect sinks are more effective than grain boundaries in capturing radiation-induced defects and delaying the onset of amorphization. These findings have significant implications for further microstructural engineering and the design of radiation-resistant microstructures.

36 MATERIALS SCIENCE↗

NASA NTRS1996

Structural Integrity Evaluation of the Lear Fan 2100 Aircraft

An in-situ nondestructive inspection was conducted to detect manufacturing and assembly induced defects in the upper two wing surfaces (skin s) and upper fuselage skin of the Lear Fan 2100 aircraft E009. The effects of the defects, detected during the inspection, on the integrity of the structure was analytically evaluated. A systematic evaluation was also conducted to determine the damage tolerance capability of the upper wing skin against impact threats and assembly induced damage. The upper wing skin was divided into small regions for damage tolerance evaluations. Structural reliability, margin of safety, allowable strains, and allowable damage size were computed. The results indicated that the impact damage threat imposed on composite military aircraft structures is too severe for the Lear Fan 2100 upper wing skin. However, the structural integrity is not significantly degraded by the assembly induced damage for properly assembled structures, such as the E009 aircraft.

Composites↗

NASA NTRS1999

Damage Tolerance of Large Shell Structures

Progressive damage and fracture of large shell structures is investigated. A computer model is used for the assessment of structural response, progressive fracture resistance, and defect/damage tolerance characteristics. Critical locations of a stiffened conical shell segment are identified. Defective and defect-free computer models are simulated to evaluate structural damage/defect tolerance. Safe pressurization levels are assessed for the retention of structural integrity at the presence of damage/ defects. Damage initiation, growth, accumulation, and propagation to fracture are included in the simulations. Damage propagation and burst pressures for defective and defect-free shells are compared to evaluate damage tolerance. Design implications with regard to defect and damage tolerance of a large steel pressure vessel are examined.

Minnetyan, L.↗

DOE OSTI2022

Role of chemical disorder on radiation-induced defect production and damage evolution in NiFeCoCr

Understanding chemical disorder in many concentrated solid solution alloys (CSAs) at the levels of electrons and atoms has attracted increasing attention as a path forward to reveal and identify underlying mechanisms for extraordinary mechanical properties and improved radiation tolerance. Single-phase NiFeCoCr CSA is a common base for many high-entropy alloys (HEAs) that have shown improved mechanical strength and radiation tolerance. In this study, defect production and damage evolution in NiFeCoCr under ion irradiation at room temperature to dose over 20 dpa are determined using ion channeling technique along both <100> and <110> directions utilizing multiple probing beam energies. The results obtained from the multi-axial and multi-energy channeling analysis are compared with those previously obtained for Ni crystals irradiated under similar conditions. The influence of chemical complexity on defect production and clustering at early-stage under room temperature irradiation up to dose of 1 dpa is discussed based on positron annihilation spectroscopy results. Defect structure evaluation in Ni and NiFeCoCr is also discussed based on transmission electron microscopy results over a prolonged irradiation at both room and elevated temperatures. Compared with chemically complex NiFeCoCr, larger dislocation loops thus less lattice strain are expected to form in pure Ni. Moreover, the role of chemical disorder in this CSA is also investigated based on ab initio calculations using large supercells. Finally, to understand the impact of chemical complexity effect on defect structure evolution, this integrated research effort attempts to link the relatively large charge redistribution due to difference in valence electron counts resulting from alloying different 3d transition metal elements, moderate lattice distortion arising from similar adaptable atomic size, and notable suppressed or delayed damage evolution in NiFeCoCr.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Microstructural Engineering of Cu-Rich Nanoprecipitate formation in NiCoFeCrCu0.12 High-Entropy Alloy via Severe Plastic Deformation for Enhanced Irradiation Tolerance

This study demonstrates a defect-engineering approach for controlling Cu-rich precipitates in FeNiCrCoCu0.2 high-entropy alloys (Cu-HEAs), delivering a novel pathway for next-generation nuclear reactor materials with superior irradiation resistance. This work establishes that severe plastic deformation (SPD) processing via Shear Assisted Processing and Extrusion (ShAPE) and Friction Stir Layer Deposition (FSLD) creates dense dislocation networks and subgrain boundaries that fundamentally alter precipitation behavior under identical thermal treatments. Atom probe tomography (APT) indicates that SPD produces a metastable, atomically homogeneous solid solution that, upon moderate heat treatment (500°C/10 hour), develops remarkedly stronger Cu clustering than the as-cast counterpart. High-temperature exposure (800°C/100 h) produces near-pure Cu precipitates (~90 at% Cu) with significantly enhanced defect-sink efficacy in SPD-processed alloys: precipitate sizes of 50-60 nm and number densities of 2.7-3.8 × 10¹7 m?³, compared to 89 nm and 0.44 × 10¹7 m?³ in as-cast materials. Collectively, the findings establish defect-mediated precipitation control as a scalable, high-impact route to tailor sink density and distribution in HEAs, enabling microstructures optimized for irradiation tolerance and mechanical robustness in nuclear reactor environments.

Meher, Subhashish↗

DOE OSTI2024

Molecular-Resolution Electron Imaging of Defects and Dynamics at the Ice-Water Interface

Water crystallization into hexagonal ice (type I h ) is one of the most critical processes relevant to the Earth’s environment and human activities. However, despite recent breakthroughs in imaging non-equilibrium condensed ice structures, the ice-water interface has never been imaged at a molecular resolution. This is primarily due to the low stability of the hydrogen bonds in ice under high-resolution microscopy conditions and a lack of methods to prepare compatible samples. Here, this presentation describes the first molecular-resolution imaging of ice crystallized from liquid water and the ice-water interface using high-resolution transmission electron microscopy (HRTEM). By encapsulating deionized (DI) water between two amorphous carbon (a-C) TEM grids and subsequently freezing it with liquid N 2 on a cryo sample stage, we generated two types of ice: non-equilibrium, condensed ice from the atmosphere and encapsulated ice from the DI water (Fig. 1A). Condensed ice usually shows irregular, spherulitic shapes (Fig. 1B). Selected area electron diffraction (SAED) shows that they are a mixture of cubic and hexagonal crystals (Fig. 1C). On the contrary, encapsulated ice forms thin films that contain large-area single-crystalline regions of hexagonal ice oriented along the [0001] zone axis (Fig. 1D). Differential electron energy-loss spectroscopy (EELS) confirmed the high purity of the encapsulated ice free from organic contaminations that are common in other encapsulation methods for HRTEM such as graphene liquid cells. These single-crystalline areas are robust under the electron beam up to ~100 e/Å 2 s. Aberration-corrected HRTEM imaging in these areas achieved a line resolution of ~1.3 Å (Fig. 1E and F). This platform allows us to study near-equilibrium ice structures and dynamics at an unprecedented spatial resolution (Fig. 2). For example, we discovered subdomain-rich regions near the defective crystal edges despite the structure appearing single-crystalline according to diffraction criteria. These subdomains connect via low-angle grain boundaries with flat energy landscapes as a function of tilt angles (according to simulations), showing the high tolerance of ice to defect structures. When we tuned the sample temperature and electron flux rate, we observed radiolysis-controlled bubble generation and dissolution in ice single crystals near a steady state of bubble dynamics. Furthermore, rich beam-induced melting and recrystallization dynamics were observed at the ice-water interface with lattice resolution. These data represent the first observation of the ice-water phase transformation at the sub-nanometer level. In summary, the methods developed in this work enabled molecular-resolution observations of ice and the ice-water interface and shed light on the microstructures and phase transformation pathways. Finer control on the temperature, electron irradiation profile, and imaging detector could eventually lead to real-time observation of ice nucleation in water and address long-standing questions in the nucleation pathways.

74 ATOMIC AND MOLECULAR PHYSICS↗

DOE OSTI2025

Defect-engineered GaN high electron mobility transistors for enhanced radiation tolerance

This study explores the radiation resilience of GaN high-electron-mobility transistors (HEMTs) under various preconditioning treatments—pristine, electro-pulsed, electrically overstressed, and 60 Co gamma-irradiated—with a focus on enhancing survivability in high-radiation environments. Key findings emphasize the gate region’s central role in radiation sensitivity, with increased defect concentrations leading to reduced sensitivity—as determined from reduced single-event transient intensities during pulsed-laser studies—and impacting charge-transport dynamics. Notably, the most sensitive region shifted as a function of bias state, with the drain side of the gate being most sensitive under negative gate bias and the source side under unbiased conditions due to two-dimensional electron gas disruptions. These insights clarify the mechanisms influencing radiation sensitivity in microelectronics and highlight the potential of defect and strain engineering to enhance the radiation hardness of GaN HEMTs across various operational states, providing valuable guidance for applications in space, defense, and other radiation-rich environments.

36 MATERIALS SCIENCE↗

NASA NTRS1994

Software fault tolerance in computer operating systems

This chapter provides data and analysis of the dependability and fault tolerance for three operating systems: the Tandem/GUARDIAN fault-tolerant system, the VAX/VMS distributed system, and the IBM/MVS system. Based on measurements from these systems, basic software error characteristics are investigated. Fault tolerance in operating systems resulting from the use of process pairs and recovery routines is evaluated. Two levels of models are developed to analyze error and recovery processes inside an operating system and interactions among multiple instances of an operating system running in a distributed environment. The measurements show that the use of process pairs in Tandem systems, which was originally intended for tolerating hardware faults, allows the system to tolerate about 70% of defects in system software that result in processor failures. The loose coupling between processors which results in the backup execution (the processor state and the sequence of events occurring) being different from the original execution is a major reason for the measured software fault tolerance. The IBM/MVS system fault tolerance almost doubles when recovery routines are provided, in comparison to the case in which no recovery routines are available. However, even when recovery routines are provided, there is almost a 50% chance of system failure when critical system jobs are involved.

Iyer, Ravishankar K.↗

DOE OSTI2026

Pixelated plastic scintillator array manufacturing using fast-, photo-curable resin

Pixelated plastic scintillator arrays can serve as high efficiency and high resolution neutron imaging detectors. Manufacturing these arrays is intensive in both time and labor. This article presents a fabrication method based on additive manufacturing for two-dimensional plastic organic scintillator arrays using a custom-built automated assembly machine and a custom photocurable resin that has significant non-aromatic acrylate oligomer content. The process involves two main stages: fully autonomous production of one-dimensional layered arrays, followed by semi-autonomous cutting and stacking to form two-dimensional pixel arrays. One-dimensional arrays were manufactured at a rate of around 4 layers per hour with minimal defects and tight dimensional tolerances, while two-dimensional arrays up to 7 x 7 pixels and 70 mm in length were completed in approximately 3.5 hours. Final arrays exhibited dimensional deviations of less than 0.5 mm. Two-dimensional arrays read out by a multi-anode photomultiplier tube demonstrated per-pixel position resolution and pulse-shape discrimination, enabling gamma–neutron interaction separation in mixed radiation environments.

36 MATERIALS SCIENCE↗

DOE OSTI2022

High Performance Circuit Pastes for Solid Oxide Fuel Cell Applications: Final Technical Report

Using a combination of in-plane electrical conductivity measurements, electrical contact resistance measurements, tensile fracture tests, double shear lap fracture tests, rapid thermal cycling adhesion tests, in situ wetting angle measurements, 3D X-ray tomography, reduction-oxidation (RedOx) cycling, scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDAX), Density Functional Theory (DFT) modeling, Molecular Dynamics (MD) modeling, and Phase Field modeling, this project determined that a new brazing technique developed by the PIs (specifically the use of nickel particles to direct the wetting and spreading of molten silver) could be used to produce well-adhered, >97% dense, electrically-conductive circuits, current collectors, and/or electrical contacts on a variety of ceramic and ceramic-coated substrates (specifically lanthanum strontium manganite, yttria stabilized zirconia, sapphire, Cr2O3-passivated stainless steel, and Al2O3-passivated stainless steel). Compared to other silver-based alternatives, Ag:Ni led to less manufacturing defects and was more tolerant of the extreme environments (isothermal high-temperature aging) and occasional abuse (rapid thermal cycling and RedOx cycling) encountered during Solid Oxide Fuel Cell and/or Solid Oxide Electrolysis Cell operation. Further, in some situations (such as when to produce Ag:Ni electrical contacts to Al2O3-protected stainless steel) the Ni particles also improved operation by acting as chemical getters that removed electrically-insulating, surface-segregating substrate impurities (i.e. by lowering the contact resistance with the underlying substrate).

36 MATERIALS SCIENCE↗

NASA NTRS2000

Integrated Design and Analysis Overview

The objectives of the project this viewgraph presentation summarizes (integrated design and analysis) include the following: (1) Develop methodology for assessing the effects of manufacturing defects; (2) Develop damage tolerance criteria and damage tolerance database for reusable launch vehicle cryogenic tank structures, including impact, pressure leakage, cryogenic permeation, and validated damage prediction tools; and (3) Develop repair technology.

Gates, Tom S.↗

NASA NTRS1996

Computational Simulation of Damage Progression of Composite Thin Shells Subjected to Mechanical Loads

Defect-free and defected composite thin shells with ply orientation (90/0/+/-75) made of graphite/epoxy are simulated for damage progression and fracture due to internal pressure and axial loading. The thin shells have a cylindrical geometry with one end fixed and the other free. The applied load consists of an internal pressure in conjunction with an axial load at the free end, the cure temperature was 177 C (350 F) and the operational temperature was 21 C (70 F). The residual stresses due to the processing are taken into account. Shells with defect and without defects were examined by using CODSTRAN an integrated computer code that couples composite mechanics, finite element and account for all possible failure modes inherent in composites. CODSTRAN traces damage initiation, growth, accumulation, damage propagation and the final fracture of the structure. The results show that damage initiation started with matrix failure while damage/fracture progression occurred due to additional matrix failure and fiber fracture. The burst pressure of the (90/0/+/- 75) defected shell was 0.092% of that of the free defect. Finally the results of the damage progression of the (90/0/+/- 75), defective composite shell was compared with the (90/0/+/- theta, where theta = 45 and 60, layup configurations. It was shown that the examined laminate (90/0/+/- 75) has the least damage tolerant of the two compared defective shells with the (90/0/+/- theta), theta = 45 and 60 laminates.

Gotsis, P. K.↗

DOE OSTI2020

The integral spliceosomal component CWC15 is required for development in Arabidopsis

Efficient mRNA splicing is a prerequisite for protein biosynthesis and the eukaryotic splicing machinery is evolutionarily conserved among species of various phyla. At its catalytic core resides the activated splicing complex Bact consisting of the three small nuclear ribonucleoprotein complexes (snRNPs) U2, U5 and U6 and the so-called NineTeen complex (NTC) which is important for spliceosomal activation. CWC15 is an integral part of the NTC in humans and it is associated with the NTC in other species. Here we show the ubiquitous expression and developmental importance of the Arabidopsis ortholog of yeast CWC15. CWC15 associates with core components of the Arabidopsis NTC and its loss leads to inefficient splicing. Consistent with the central role of CWC15 in RNA splicing, cwc15 mutants are embryo lethal and additionally display strong defects in the female haploid phase. Interestingly, the haploid male gametophyte or pollen in Arabidopsis, on the other hand, can cope without functional CWC15, suggesting that developing pollen might be more tolerant to CWC15-mediated defects in splicing than either embryo or female gametophyte.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

Carbon nanotube (CNT) metal composites exhibit greatly reduced radiation damage

Radiation damage of structural materials leads to mechanical property degradation, eventually inducing failure. Secondary-phase dispersoids or other radiation defect sinks are often added to materials to boost their radiation resistance. We demonstrate that a metal composite made by adding 1D carbon nanotubes (CNTs) to aluminum (Al) exhibits superior radiation resistance. In situ ion irradiation with transmission electron microscopy (TEM) and atomistic simulations together reveal the mechanisms of rapid defect migration to CNTs, facilitating defect recombination and enhancing radiation tolerance. The origin of this effect is an evolving stress gradient in the Al matrix resulting from CNT transformation under irradiation, and the stability of resulting carbides. Extreme value statistics of large defect behavior in our simulations highlight the role of CNTs in reducing accumulated damage. Furthermore, this approach to controlling defect migration represents a promising opportunity to enhance the radiation resistance of nuclear materials without detrimental effects.

36 MATERIALS SCIENCE↗