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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 235 records · Page 13

Atomic-scale polarization switching in wurtzite ferroelectrics

Ferroelectric wurtzites have the potential to revolutionize modern microelectronics because they are easily integrated with multiple mainstream semiconductor platforms. However, the electric fields required to reverse their polarization direction and unlock electronic and optical functions need substantial reduction for operational compatibility with complementary metal-oxide semiconductor (CMOS) electronics. To understand this process, we observed and quantified real-time polarization switching of a representative ferroelectric wurtzite (Al 0.94 B 0.06 N) at the atomic scale with scanning transmission electron microscopy. The analysis revealed a polarization reversal model in which puckered aluminum/boron nitride rings in the wurtzite basal planes gradually flatten and adopt a transient nonpolar geometry. Independent first-principles simulations reveal the details and energetics of the reversal process through an antipolar phase. Furthermore, this model and local mechanistic understanding are a critical initial step for property engineering efforts in this emerging material class.

36 MATERIALS SCIENCE↗

GRinding Automated Classification Engine

This work is an ML-driven framework for automated surface analysis of microscopy images. We create a training dataset by imaging stainless steel samples to benchmark four developed deep neural network architectures. These models, based on a YOLOv8n-cls backend, integrate image features and process metadata using various fusion methods to distinguish between acceptable and unacceptable surface finishes. This code is associated with publication "Classifying Alloy Surface Preparation Quality with Metadata-Infused Machine Learning for Rapid Alloy Discovery" for project APEX LDRD-ER (25-ERD-039)

Gongora, AldairE [Lawrence Livermore National Labo↗

SR19021 Tritium Aging of Regenerated LANA.75 (Final Project Report)

The Savannah River Tritium Enterprise (SRTE) has used the metal hydride LaNi 4.25 Al 0.75 (LANA.75) in the Tritium Facilities for over two decades. LANA.75 beds store significant quantities of tritium but have a limited service life due to the radiolytic decay of tritium to He-3 within the metal matrix. It has been shown that heating tritium-aged LANA.75 under vacuum can reverse tritium aging effects, eliminating the heel of trapped hydrogen, and restoring the reversible capacity. Additional investigation is needed to ensure there are no unexpected changes to the hydride before this restoration technique is employed in full scale beds in the Tritium Facilities. This project was to be comprised of three distinct scopes: obtain tritium aging data on the sample regenerated in 2018, regenerate a tritium-aged sample at 600 °C, and perform thermal stability testing on a non-tritiated sample. Isotherms were collected on the previously regenerated sample after approximately two years of tritium aging. Isotherms were collected at 80, 100, and 120 °C. As expected, there was a decrease in the plateau pressure, an increase in plateau slope, and a portion of the “heel” of tritium trapped in the metal had been reestablished. Unexpectedly, it appeared that the plateau had shortened at the higher tritium to metal ratios as well. This is typically seen in older samples. The second scope, to regenerate a second tritium-aged LANA.75 sample, was not completed. A Task Technical and Quality Assurance Plan was written and approved, a high temperature test cell was fabricated, several pre-job briefs were held, and the hydride sample was passivated with air. Despite these successes, the hydride sample was not recovered from the legacy test cell. The third scope was to perform thermal stability testing on a “cold” LANA.75 sample. A non-tritiated sample of LANA.75 was held at 750 °C under vacuum for 200 hours to simulate exposure to multiple regeneration evolutions. Hydride isotherm performance, chemical composition, crystallinity, particle size, and morphology are compared between the pre- and post-regeneration samples. No significant changes were observed in composition, crystallinity, or particle size. Comparison of before and after isotherms showed that performance improved rather than deteriorated during the evolution. Scanning Electron Microscopy (SEM) analysis showed small growths on the particle surface after exposure to regeneration conditions. Additional testing will be required to determine the cause of these growths.

07 ISOTOPE AND RADIATION SOURCES↗

Quality Control Methods for Measurement of UCO Kernel Composition and SiC Microstructure

Quality control (QC) is critically important to tristructural-isotropic (TRISO) particle fuels owing to the complexity of and reliance on the fuel form to contain fission products during irradiation. Characterization methods for particle fuel QC have decades of history and have continued to develop as new insights into fuel performance inform revised fuel specifications and as advances in underlying technologies expand the possibilities of what may be characterized. Two relatively new methods for characterization of TRISO fuels have been published in open literature: optical microscopy image analysis for mixed uranium carbide/uranium oxide (UCO) kernel composition analysis and automated grain boundary detection in backscattered electron (BSE) images of the silicon carbide (SiC) layer in TRISO particles for grain size characterization. Suggestions and guidelines for the application of these methods to TRISO fuel qualification are provided in this report.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Computer vision models and advanced TEM imaging for microstructures of irradiated AM316 stainless steels

Advancements were made in automating microscopy-based material characterization, particularly in studying irradiation effects on additively manufactured (AM) materials using machine learning (ML) and computer vision (CV). These automation efforts address the challenges of analyzing complex microstructures, accelerating the detection of irradiation-induced defects. Two CV models were developed at Argonne National Laboratory (ANL) to enhance transmission electron microscopy (TEM) analysis of irradiated AM 316 stainless steel. The first model focused on the detection of irradiation-induced dislocation loops, which contribute to material hardening and embrittlement. These loops, categorized as faulted or perfect, were automatically detected and classified using a Mask R-CNN model trained on TEM images from both in-situ and ex-situ ion irradiation experiments. The model achieved high accuracy, with precision, recall, and F1 scores of 0.839, 0.734, and 0.776, respectively, demonstrating its effectiveness in analyzing dislocation loops in irradiated AM materials. The second CV model was developed to analyze the size and wall thickness of dislocation cells in laser powder bed fusion (LPBF) 316 stainless steel. Using a U-Net++ architecture with EfficientNet as the encoder, the model was trained on TEM images to segment and measure cell size and wall thickness.

36 MATERIALS SCIENCE↗

Designing carbon wetting layers with inorganic salts as additives for enhanced adhesion and molten sodium wettability in electrochemical application

ß” alumina solid-state electrolyte (BASE) is considered one of the most promising materials for sodium batteries due to its high ionic conductivity and exceptional stability with molten sodium. However, at lower operating temperatures, the poor physical contact at the liquid-solid interface between molten sodium and BASE results in high interfacial resistance. In this study, we explore the optimization of carbon wetting layers with various salt additives to enhance adhesion and improve molten sodium wettability. Using a spray-coating method, carbon layers incorporating sodium hexametaphosphate (Na6(PO3)6, SHMP) as an additive demonstrate superior adhesion, mechanical stability, and enhanced wettability with molten sodium. Scanning Electron Microscopy (SEM) analysis reveals that SHMP preserves the porous carbon network required for efficient sodium transport while minimizing structural defects such as cracks and voids. Electrochemical testing using Na symmetric cells confirms that SHMP-modified layers significantly reduce interfacial resistance and overpotential, outperforming No salts counterparts. These findings highlight that the strategic incorporation of suitable additives, such as SHMP, in the design of microscale carbon layers could significantly enhance the performance of molten sodium batteries at lower operating temperatures.

Han, Henry H.↗

Covalent integration of polymers and porous organic frameworks

Covalent integration of polymers and porous organic frameworks (POFs), including metal-organic frameworks (MOFs), covalent organic frameworks (COFs) and hydrogen-bonded organic frameworks (HOFs), represent a promising strategy for overcoming the existing limitations of traditional porous materials. This integration allows for the combination of the advantages of polymers, i.e., flexibility, processability and chemical versatility etc., and the superiority of POFs, like the structural integrity, tunable porosity and the high surface area, creating a type of hybrid materials. These resulting polymer-POF hybrid materials exhibit enhanced mechanical strength, chemical stability and functional diversity, thus opening up new opportunities for applications across a large variety of fields, such as gas separation, catalysis, biomedical applications, environmental remediation and energy storage. In this review, an overview of synthetic routes and strategies on how to covalently integrate different polymers with various POFs is discussed, especially with a particular focus on methods like polymerization within, on and among POF structures. To investigate the unique properties and functions of these resultant hybrid materials, the characterization techniques, including nuclear magnetic resonance spectroscopy (NMR), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), gas adsorption analysis (BET) and computational modeling and machine learning, are also presented. The ability of polymer-POFs to manipulate the pore environments at the molecular level affords these materials a wide range of applications, providing a versatile platform for future advancements in material science. Looking forward, to fully realize the potential of these hybrid materials, the authors highlight the scalability, green synthesis methods, and potential for stimuli-responsive polymer-POF materials as critical areas for future research.

Hossain, Md Amjad↗

Styrene-Based Elastomer Composites with Functionalized Graphene Oxide and Silica Nanofiber Fillers: Mechanical and Thermal Conductivity Properties

The mechanical and thermal conductivity properties of two composite elastomers were studied. Styrene–butadiene rubber (SBR) filled with functionalized graphene oxide (GO) and silica nanofibers, and styrene–butadiene–styrene (SBS) block copolymers filled with graphene oxide. For the SBR composites, GO fillers with two different surface functionalities were synthesized (cysteamine and dodecylamine) and dispersed in the SBR using mechanical and liquid mixing techniques. The hydrophilic cysteamine-based GO fillers were dispersed in the SBR by mechanical mixing, whereas the hydrophobic dodecylamine-based GO fillers were dispersed in the SBR by liquid mixing. Silica nanofibers (SnFs) were fabricated by electrospinning a sol–gel precursor solution. The surface chemistry of the functionalized fillers was studied in detail. The properties of the composites and the synergistic improvements between the GO and SnFs are presented. For the SBS composites, GO fillers were dispersed in the SBS elastomer at several weight percent loadings using liquid mixing. Characterization of the filler material and the composite elastomers was performed using x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy, scanning electron microscopy, thermogravimetric analysis, dynamic mechanical analysis, tensile testing, nanoindentation, thermal conductivity and abrasion testing.

36 MATERIALS SCIENCE↗

Near-Field Passive Wireless Sensor for High-Temperature Metal Corrosion Monitoring

This work focuses on the fabrication and evaluation of a passive wireless sensor for the monitoring of the temperature and corrosion of a metal material at high temperatures. An inductor–capacitor (LC) resonator sensor was fabricated through the screen printing of Ag-based inks on dense polycrystalline Al 2 O 3 substrates. The LC design was modeled using the ANSYS HFSS modeling package, with the LC passive wireless sensors operating at frequencies from 70 to 100 MHz. The wireless response of the LC was interrogated and received by a radio frequency signal generator and spectrum analyzer at temperatures from 50 to 800 °C in real time. The corrosion kinetics of the Cu 110 was characterized through thermogravimetric (TGA) analysis and microscopy images, and the oxide thickness growth was then correlated to the wireless sensor signal under isothermal conditions at 800 °C. The results showed that the wireless signal was consistent with the corrosion kinetics and temperature, indicating that these two characteristics can be further deconvoluted in the future. In addition, the sensor also showed a magnitude- and frequency-dependent response to crack/spallation events in the oxide corrosion layer, permitting the in situ wireless identification of these catastrophic events on the metal surface at high temperatures.

36 MATERIALS SCIENCE↗

Program for plasma-sprayed self-lubricating coatings

A method for preparing composite powders of the three coating components was developed and a procedure that can be used in applying uniform coatings of the composite powders was demonstrated. Composite powders were prepared by adjusting particle sizes of the components and employing a small amount of monoaluminum phosphate as an inorganic binder. Quantitative microscopy (image analysis) was found to be a convenient method of characterizing the composition of the multiphase plasma-sprayed coatings. Area percentages and distribution of the components were readily obtained by this method. The adhesive strength of the coating to a nickel-chromium alloy substrate was increased by about 40 percent by a heat treatment of 20 hours at 650 C.

Walther, G. C.↗

Characterization of microcomposite polyimide films

Thermally stable microcomposite polyimide films were prepared by the homogeneous incorporation of either a soluble metal salt or a metal complex into a poly(amide-acid)/N,N-dimethylacetamide solution. The thermal processing of films solvent cast onto glass substrates and cured in an appropriate atmosphere yields films containing not only a fairly uniform dispersion of submicrometer particles, but also a new surface layer of metal or metal oxide. These polymeric systems have been characterized using X-ray photoelectron spectroscopy, Auger electron spectroscopy with depth profiling via argon ion etching, transmission electron microscopy of ultramicrotomed cross-sections, scanning electron microscopy, elemental analysis, thermal analysis, and variable temperature electrical resistivity determinations. The data from these techniques were used cooperatively to develop a model for these microcomposite polyimide films.

Rancourt, J. D.↗

Sequentially evaporated thin Y-Ba-Cu-O superconductor films: Composition and processing effects

Thin films of YBa2Cu3O(7-beta) have been grown by sequential evaporation of Cu, Y, and BaF2 on SrTiO3 and MgO substrates. The onset temperatures were as high as 93 K while T sub c was 85 K. The Ba/Y ratio was varied from 1.9 to 4.0. The Cu/Y ratio was varied from 2.8 to 3.4. The films were then annealed at various times and temperatures. The times ranged from 15 min to 3 hr, while the annealing temperatures used ranged from 850 C to 900 C. A good correlation was found between transition temperature (T sub c) and the annealing conditions; the films annealed at 900 C on SrTiO3 had the best T sub c's. There was a weaker correlation between composition and T sub c. Barium poor films exhibitied semiconducting normal state resistance behavior while barium rich films were metallic. The films were analyzed by resistance versus temperature measurements and scanning electron microscopy. The analysis of the films and the correlations are reported.

Valco, George J.↗

Natural aging and reversion behavior of Al-Cu-Li-Ag-Mg alloy Weldalite (tm) 049

This study was initiated to understand the natural aging and reversion behavior of Weldalite (trademark) 049 in tempers without cold work. Of particular interest are: (1) the microstructural basis for the high strength in the T4 condition; (2) an explanation of the reversion phenomenon; and (3) the effect of re-aging at room temperature after a reversion treatment. Mechanical properties were measured and transmission electron microscopy (TEM) analysis performed at various stages of microstructural development during aging, reversion, and subsequent re-aging.

Gayle, Frank W.↗

Fluorescent-Antibody Measurement Of Cancer-Cell Urokinase

Combination of laboratory techniques provides measurements of amounts of urokinase in and between normal and cancer cells. Includes use of fluorescent antibodies specific against different forms of urokinase-type plasminogen activator, (uPA), fluorescence microscopy, quantitative analysis of images of sections of tumor tissue, and flow cytometry of different uPA's and deoxyribonucleic acid (DNA) found in suspended-tumor-cell preparations. Measurements provide statistical method for indicating or predicting metastatic potentials of some invasive tumors. Assessments of metastatic potentials based on such measurements used in determining appropriate follow-up procedures after surgical removal of tumors.

Morrison, Dennis R.↗

Measuring the metastatic potential of cancer cells

Cancer cells must secrete proteolytic enzymes to invade adjacent tissues and migrate to a new metastatic site. Urokinase (uPA) is a key enzyme related to metastasis in cancers of the lung, colon, gastric, uterine, breast, brain, and malignant melanoma. A NASA technology utilization project has combined fluorescence microscopy, image analysis, and flow cytometry, using fluorescent dyes, and urokinase-specific antibodies to measure uPA and abnormal DNA levels (related to cancer cell proliferation) inside the cancer cells. The project is focused on developing quantitative measurements to determine if a patient's tumor cells are actively metastasizing. If a significant number of tumor cells contain large amounts of uPA (esp. membrane-bound) then the post-surgical chemotherapy or radiotherapy can be targeted for metastatic cells that have already left the primary tumor. These analytical methods have been applied to a retrospective study of biopsy tissues from 150 node negative, stage 1 breast cancer patients. Cytopathology and image analysis has shown that uPA is present in high levels in many breast cancer cells, but not found in normal breast. Significant amounts of uPA also have been measured in glioma cell lines cultured from brain tumors. Commercial applications include new diagnostic tests for metastatic cells, in different cancers, which are being developed with a company that provides a medical testing service using flow cytometry for DNA analysis and hormone receptors on tumor cells from patient biopsies. This research also may provide the basis for developing a new 'magic bullet' treatment against metastasis using chemotherapeutic drugs or radioisotopes attached to urokinase-specific monoclonal antibodies that will only bind to metastatic cells.

Morrison, Dennis R.↗

A Sensitive Technique Using Atomic Force Microscopy to Measure the Low Earth Orbit Atomic Oxygen Erosion of Polymers

Polymers such as polyimide Kapton and Teflon FEP (fluorinated ethylene propylene) are commonly used spacecraft materials due to their desirable properties such as flexibility, low density, and in the case of FEP low solar absorptance and high thermal emittance. Polymers on the exterior of spacecraft in the low Earth orbit (LEO) environment are exposed to energetic atomic oxygen. Atomic oxygen erosion of polymers occurs in LEO and is a threat to spacecraft durability. It is therefore important to understand the atomic oxygen erosion yield (E, the volume loss per incident oxygen atom) of polymers being considered in spacecraft design. Because long-term space exposure data is rare and very costly, short-term exposures such as on the shuttle are often relied upon for atomic oxygen erosion determination. The most common technique for determining E is through mass loss measurements. For limited duration exposure experiments, such as shuttle experiments, the atomic oxygen fluence is often so small that mass loss measurements can not produce acceptable uncertainties. Therefore, a recession measurement technique has been developed using selective protection of polymer samples, combined with postflight atomic force microscopy (AFM) analysis, to obtain accurate erosion yields of polymers exposed to low atomic oxygen fluences. This paper discusses the procedures used for this recession depth technique along with relevant characterization issues. In particular, a polymer is salt-sprayed prior to flight, then the salt is washed off postflight and AFM is used to determine the erosion depth from the protected plateau. A small sample was salt-sprayed for AFM erosion depth analysis and flown as part of the Limited Duration Candidate Exposure (LDCE-4,-5) shuttle flight experiment on STS-51. This sample was used to study issues such as use of contact versus non-contact mode imaging for determining recession depth measurements. Error analyses were conducted and the percent probable error in the erosion yield when obtained by the mass loss and recession depth techniques has been compared. The recession depth technique is planned to be used to determine the erosion yield of 42 different polymers in the shuttle flight experiment PEACE (Polymer Erosion And Contamination Experiment) planned to fly in 2002 or 2003.

deGroh, Kim K.↗

Fungal degradation of fiber-reinforced composite materials

As described in a previous report, a fungal consortium isolated from degraded polymeric materials was capable of growth on presterilized coupons of five composites, resulting in deep penetration into the interior of all materials within five weeks. Data describing the utilization of composite constituents as nutrients for the microflora are described in this article. Increased microbial growth was observed when composite extract was incubated with the fungal inoculum at ambient temperatures. Scanning electron microscopic observation of carbon fibers incubated with a naturally developed population of microorganisms showed the formation of bacterial biofilms on the fiber surfaces, suggesting possible utilization of the fiber chemical sizing as carbon and energy sources. Electrochemical impedance spectroscopy was used to monitor the phenomena occurring at the fiber-matrix interfaces. Significant differences were observed between inoculated and sterile panels of the composite materials. A progressive decline in impedance was detected in the inoculated panels. Several reaction steps may be involved in the degradation process. Initial ingress of water into the resin matrix appeared to be followed by degradation of fiber surfaces, and separation of fibers from the resin matrix. This investigation suggested that composite materials are susceptible to microbial attack by providing nutrients for growth.

Environmental Microbiology↗

Crystal Growth of CdTe by Gradient Freeze in Universal Multizone Crystallizator (UMC)

In the case of unsealed melt growth of an array of II-VI compounds, namely, CdTe, CdZnTe and ZnSe, there is a tremendous amount of experimental data describing the correlations between melt conditions and crystal quality. The results imply that the crystallinity quality can be improved if the melt was markedly superheated or long-time held before growth. It is speculated that after high superheating the associated complex dissociate and the spontaneous nucleation is retarded. In this study, crystals of CdTe were grown from melts which have undergone different thermal history by the unseeded gradient freeze method using the Universal Multizone Crystallizator (UMC). The effects of melt conditions on the quality of grown crystal were studied by various characterization techniques, including Synchrotron White Beam X-ray Topography (SWSXT), infrared microscopy, chemical analysis by glow discharge mass spectroscopy (GDMS), electrical conductivity and Hall measurements.

Su, Ching-Hua↗