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Results for “SCANNING ELECTRON MICROSCOPY”

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 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Hollow Ptychography: Toward Simultaneous 4D Scanning Transmission Electron Microscopy and Electron Energy Loss Spectroscopy

With the recent development of high-acquisition-speed pixelated detectors, 4D scanning transmission electron microscopy (4D-STEM) is becoming routinely available in high-resolution electron microscopy. 4D-STEM acts as a “universal” method that provides local information on materials that is challenging to extract from bulk techniques. It extends conventional STEM imaging to include super-resolution techniques and to provide quantitative phase-based information, such as differential phase contrast, ptychography, or Bloch wave phase retrieval. However, an important missing factor is the chemical and bonding information provided by electron energy loss spectroscopy (EELS). 4D-STEM and EELS cannot currently be acquired simultaneously due to the overlapping geometry of the detectors. Here, the feasibility of modifying the detector geometry to overcome this challenge for bulk specimens is demonstrated, and the use of a partial or defective detector for ptycholgaphic structural imaging is explored. Here, results show that structural information beyond the diffraction-limit and chemical information from the material can be extracted together, resulting in simultaneous multi-modal measurements, adding the additional dimensions of spectral information to 4D datasets.

4D-scanning transmitting electron microscopy (STEM↗
DOE OSTI2020

Failure analysis of field-failed bypass diodes

Defective bypass diodes are often found as the largest factor leading to power loss in solar modules. Here, we report on failure mechanisms by investigating shunted bypass diodes from a rooftop installation, using a combination of multiple characterizations including current–voltage analysis, thermal-runaway testing, X-ray computed tomography, lock-in thermography, focused ion-beam cross-section imaging, chemical decapsulation, optical microscopy, and scanning electron microscopy with energy-dispersive X-ray spectroscopy. Differing from static discharge typically associated with lightning strikes on modules, we found diode failure by the mechanism of thermal damage under continuous, long-term overstress in forward bias. Our conclusion is based on evidence of energy dissipated—the small to medium extent of melt-through on the Schottky diode face. The diode failure shows distortions or roughening of the Schottky diode metal-semiconductor interface with the die attach, and some failures are accompanied by die-attach solder melting. We propose that nonuniform irradiance on the modules caused diode shunting due to extended periods of heat dissipation in the modules, because modules in this string were placed in two different orientations. In contrast, a second parallel module string of the same module type on the same rooftop with a unique plane of array did not show any diode failures. The thermal damage failure of melt-through was caused by the long-term current generated by overstressing of diodes that may have had crystalline and impurity defects.

14 SOLAR ENERGY↗
DOE OSTI2020

High-efficiency single-junction p-i-n GaAs solar cell on roll-to-roll epi-ready flexible metal foils for low-cost photovoltaics

We demonstrate the fabrication and characterization of high-efficiency, single-junction p-i-n GaAs solar cells, on flexible metal foil with epi-ready buffer via roll-to-roll fabrication. Single-junction p-i-n GaAs solar cells were fabricated using metal–organic chemical vapor deposition (MOCVD). Furthermore, an efficiency greater than 13% was obtained at 1 sun, which is the highest reported efficiency on GaAs photovoltaics directly deposited on metal tapes. This exceeds our previously reported study showcasing 11.5% efficiency on single-junction p-n solar cell structure. Improved morphology of p-i-n structure compared with p-n is explained by atomic force microscopy (AFM), scanning electron microscopy (SEM), and helium ion microscopy (HIM) measurements. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) analysis showed reduced Zn diffusion in p-i-n cell compared with the p-n cell. We attribute the improvement in efficiency of p-i-n cells on flexible metal tapes to the quality of the junction, surface morphology, controlled diffusion of species within the active layers, and increase in absorption due to the optimized intrinsic layer thickness.

14 SOLAR ENERGY↗
DOE OSTI2021

Characterizing mechanical and microstructural properties of novel montmorillonite-rich polyethylene composites

Montmorillonite (MMT) clays are important industrial materials used as catalysts, chemical sorbents and fillers in polymer–clay nanocomposites. The layered structure of these clays has motivated research into further applications of these low-cost materials, including use as ion exchange media and solid-state ionic conductors. In these applications, the mechanical properties of MMT are key when considering long-term, reliable performance. Previous studies have focused on the mechanical properties of nanocomposites with MMT as the minority component or pure MMT thin films. In this work, the microstructure and mechanical properties of pure MMT and majority MMT/polyethylene composites pressed into dense pellets are examined. Characterization methods such as X-ray diffraction, atomic force microscopy and scanning electron microscopy together with nanoindentation reveal important structure–property relationships in the clay-based materials. Here, utilizing these techniques, we have discovered that MMT processing impacts the layered microstructure, chemical stability and, critically, the elastic modulus and hardness of bulk MMT samples. Particularly, the density of the pellets and the ordering of the clay platelets within them strongly influence the elastic modulus and hardness of the pellets. By increasing pressing force or by incorporating secondary components, the density, and therefore mechanical properties, can be increased. If the layered structure of the clay is destroyed by exfoliation, the mechanical properties will be compromised. Understanding these relationships will help guide new studies to engineer mechanically stable MMT-based materials for industrial applications.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Radiation-induced alteration of sandstone concrete aggregate

This study investigates the alteration of felsic sandstone-type rock, which is used as a coarse aggregate in concrete, subject to the effects of gamma-ray and neutron irradiation. The effects of three gamma-ray doses (27, 55, and 108 MGy) and four neutron fluence levels (1.22, 2.19, 6.99, and 14.30 × 10 19 n/cm 2 , $E$ ≥ 0.01 MeV) were investigated. Quartz and albite were found to be the major rock-forming minerals, with microcline intermediates, chlorite, and muscovite as the minors. Gamma rays caused no significant changes to the physical properties of the sandstone aggregates, even at high doses (108 MGy). In contrast, neutron irradiation caused alterations that became more pronounced at higher neutron fluences. The solid was confirmed to expand through metamictization of the rock-forming minerals. Quartz and muscovite were the most affected phases, whereas albite and microcline intermediates were only slightly affected, and chlorite was almost unaffected. The decrease in density was measured by He and water pycnometry, and this value was almost reproduced by calculations using the rock-forming mineral composition of the pristine sample measured using X-ray powder diffraction/Rietveld analysis and the cell volume change of the major forming minerals. In addition, light optical microscopy and scanning electron microscopy images confirmed the presence of intergranular and intragranular cracks. Intergranular cracks appeared to have initiated from the quartz grains, which expanded significantly. The intragranular cracks were frequently observed in the albite and microcline intermediates. These cracks can be described as radial cracks starting from the expanding quartz, caused by enforced displacement for deformation consistency with quartz expansion. The crack area ratio quantified by SEM image analysis corresponds to the discrepancy of the volume expansion difference calculated by He or water pycnometry and dimensional change measurements. In conclusion, an evaluation of solid expansion and crack openings in aggregates is important to estimate concrete degradation.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Effect of 316 stainless steel powder processing conditions on microstructure

One parameter that has both economic and performance effects in the manufacturing of steel parts is the powder feedstock used. 316 L steel powder can be produced through water atomization or gas atomization, where both the powder size and the atomization process determine the cost of powder feedstock. Gas atomized powder is spherical and has a lower oxygen content than water atomized powder, making it the preferred choice for performance, but comes at a higher financial cost. Here, in this study, various 316 L powder batches are characterized to understand physical properties and microstructural variations. Density and flowability were determined using gas pycnometry and Hall flow tests. Powder morphology and porosity were qualitatively analyzed via optical microscopy and scanning electron microscopy, Finally, transmission electron microscopy was used to determine changes in phases present. Spherical gas atomized powder of 30–100 μm contained Mn$-$Si rich oxides both on the surface and within the matrix. Meanwhile, irregular water atomized powder 30 μm in diameter contained silicon oxides without manganese. All powder particles contained a nickel rich cellular structure which was shown to support the formation of additional phases. While literature has observed general microstructural features across 316 L powder particles, transmission electron microscopy (TEM) in this study has identified variations in precipitation and cell structures. Information regarding morphology, flowability, density, and phase distributions can be applied to understand variations in part consolidation, which will in turn show which powder aspects are significant for production.

Chemical segregation↗
DOE OSTI2020

Experimental evaluation of direct current magnetron sputtered and high-power impulse magnetron sputtered Cr coatings on SiC for light water reactor applications

Two types of physical vapor deposition Cr coatings were deposited on chemical vapor deposited SiC coupons using conventional direct current magnetron sputtering (DCMS) and high-power impulse magnetron sputtering (HiPIMS) to mitigate the corrosion of SiC, an advanced fuel and structural material in light water nuclear reactor cores. Coating microstructure was characterized using scanning electron microscopy and scanning transmission election microscopy. X-ray diffraction analysis was conducted for phase identification and qualitative analysis of residual stresses. The mechanical integrity of the coatings was evaluated using scratch testing, micro-indentation, and nano-indentation tests. Additionally, the microstructure of the DCMS coating consisted of fine columnar grains with nanoscale intercolumnar channels, while the HiPIMS microstructure was denser and free of any columnar defects. The DCMS coating showed a small tensile residual stress, while the HiPIMS coating was under compressive stress. Both types of coatings showed good mechanical integrity in terms of ductility and adhesion to the substrate. Corrosion performance of the coatings was assessed with a 30-day high temperature water autoclave test. Both types of coatings formed a protective Cr 2 O 3 surface layer 20-30 nm thick during the autoclave test. In the DCMS coating, the columnar defects provided permeation pathways for water penetration resulting in oxide formation in the intercolumnar regions in the interior of the coating. Overall, both types of Cr coatings offer promise for the mitigation of hydrothermal corrosion of SiC in light water reactor operating environments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

An Impedance Humidity Sensor Based on CVD Grown WSe 2 2D Films

2D materials-based planar devices have been sought after for gas and humidity sensor applications owing to their high sensitivity due to their ultrathin nature and increased surface area. Herein, 2D WSe 2 films-based planner devices were fabricated to evaluate their performance for potential application in humidity sensors. The structure and morphology of the WSe 2 sensing films were studied by Raman spectroscopy, photoluminescence, optical microscopy, and scanning electron microscopy (SEM) techniques. The relative humidity-dependent sensing performances of the 2D WSe 2 films were evaluated using current–voltage (I–V), relative impedance, and complex total impedance (electrochemical impedance spectroscopy, EIS) techniques. This sensor showed a very stable and repeatable performance investigated over the period of 18 months. The response and recovery times of the WSe 2 -based impedance sensors were found to be 40 and 30 s, respectively. The WSe 2 sensor exhibits a 2 ± 1% minimum hysteresis at a lower humidity level (50% RH) and around 8 ± 2% maximum hysteresis at relative humidity level (70% RH). This value of hysteresis is in the acceptable range during the initial investigation of any material to explore its potential for application in humidity sensors. The density functional theory (DFT) analysis was performed with the interaction from water molecules of the WSe 2 sample for a better understanding of the sensing mechanism of devices.

2D- WSe2↗
DOE OSTI2020

Engineering the Microstructure and Morphology of Explosive Films via Control of Interfacial Energy

Physical vapor deposition of organic explosives enables growth of polycrystalline films with a unique microstructure and morphology compared to the bulk material. This study demonstrates the ability to control crystal orientation and porosity in pentaerythritol tetranitrate films by varying the interfacial energy between the substrate and the vapor-deposited explosive. Additionally, variation in density, porosity, surface roughness, and optical properties is achieved in the explosive film, with significant implications for initiation sensitivity and detonation performance of the explosive material. Various surface science techniques, including angle-resolved X-ray photoelectron spectroscopy and multiliquid contact angle analysis, are utilized to characterize interfacial characteristics between the substrate and explosive film. Optical microscopy and scanning electron microscopy of pentaerythritol tetranitrate surfaces and fracture cross sections illustrate the difference in morphology evolution and the microstructure achieved through surface energy modification. X-ray diffraction studies with the Tilt-A-Whirl three-dimensional pole figure rendering and texture analysis software suite reveal that high surface energy substrates result in a preferred (110) out-of-plane orientation of pentaerythritol tetranitrate crystallites and denser films. Low surface energy substrates create more randomly textured pentaerythritol tetranitrate and lead to nanoscale porosity and lower density films. This work furthers the scientific basis for interfacial engineering of polycrystalline organic explosive films through control of surface energy, enabling future study of dynamic and reactive detonative phenomena at the microscale. Results of this study also have potential applications to active pharmaceutical ingredients, stimuli-responsive polymer films, organic thin film transistors, and other areas.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Liquid Crystal Films as Active Substrates for Nanoparticle Control

Organizing nanoparticles in a controlled way allows us to monitor their optical properties. It is particularly interesting to organize them on top of liquid crystal films to take advantage, in a second step, of the easy actuation of liquid crystals with external parameters such as temperature, electric fields, and so forth. We show that despite their fluidity, nematic and smectic films allow the formation of well-ordered hexagonal domains of gold spherical nanoparticles (AuNPs) at their surface, but we also show that both nematic films and AuNP domains impact each other. Using optical microscopy, atomic force microscopy (AFM), scanning electron microscopy (SEM), and spectrophotometry, we compare nematic, polymer-stabilized nematic, and smectic films with AuNP domains made of NPs of diameter 6 nm. On the liquid crystal films, depressions are revealed below the AuNP domains, whereas the AuNP domains appear well-organized but with a hexagonal period shortened with respect to AuNP monolayers formed on hard substrates. We interpret these features by the anchoring tilt imposed by the AuNP domains on the liquid crystal molecules. The smectic-A layers characteristic of the nematic surface transform into smecticC layers, which induce the formation of depression. Here, the energy penalty associated with the local smectic-A/smectic-C transition induces the shortening of the AuNP domain period in order to decrease the AuNP domain surface. The observed large depth of the polymer-stabilized nematic depressions below AuNP domains may be explained either by an increased size of the polymer-stabilized smectic layers close to the surface or by an increased number of polymer-stabilized smectic liquid crystal smectic layers close to the surface with respect to pure nematic films.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Chemical Vapor Deposition-Grown Hexagonal Boron Nitride and Graphene for Tandem Dielectric Capacitive Polymer Devices

To address the low energy density of polymeric capacitors, this work explores how tandem combinations of antagonistic properties can enhance energy storage. We introduce multilayer architecture integrating chemical vapor deposition (CVD)-grown ≈2 nm hexagonal boron nitride (hBN) and graphene with ferroelectric polyvinylidene fluoride (PVDF) and linear polyetherimide (PEI) layers to suppress leakage paths, reduce loss, and promote Maxwell–Wagner–Sillars polarization. Raman spectroscopy, X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), and plasma focused ion beam (PFIB) analyses confirm robust material integration. In conclusion, for the tandem device, E BD ≈600 V/μm, while individual layers show lower values (PVDF|Graphene (Gr)|PVDF ≈ 50 V/μm and PEI|hBN|PEI ≈ 275 V/μm), yielding an overall ≈6000% enhancement and demonstrating the effectiveness of the 2D multilayer design.

Chemical vapor deposition (CVD)↗
DOE OSTI2025

Uptake of polystyrene nanospheres by wheat and Arabidopsis roots in agar, hydroponics, and soil

Plant uptake of micro- and nanoplastics can lead to contamination of food with plastic particles and subsequent human consumption of plastics. There is evidence that plant roots can take up micro and nanoplastics; however, most of this evidence stems from experiments conducted with plants grown in hydroponics or agar systems where uptake of nanoparticles by roots is more favorable than when plants were grown in soil. Here, we discern the root uptake and accumulation of polystyrene nanospheres in plants grown in different growth media: agar, hydroponics, and soil. In addition, we tested the impacts of nanospheres on plant biomass and plant stress. Wheat and Arabidopsis thaliana were grown in agar, hydroponics, and soil media and exposed to polystyrene nanospheres. Three different nanospheres were used (40 nm and 200 nm carboxylate-modified and 200 nm amino-modified polystyrene) and uniformly mixed into the growth media. Plants were grown for 7 to 10 days and the roots were then examined for the presence of nanospheres by confocal laser scanning microscopy and scanning electron microscopy. Plant stress was evaluated by measuring reactive oxygen species (ROS). We observed the 40 nm nanospheres inside the plant roots, but the 200 nm nanospheres only adhered to the root cap cells showing no uptake into the roots. Furthermore, confocal images indicated that root uptake of nanospheres was favored in hydroponic solutions as compared to agar and soil media. Plant biomass was generally not affected by the nanospheres, except for hydroponically grown Arabidopsis thaliana, where biomass was significantly reduced. Small sized (40 nm) and positively charged (200 nm amino-modified) nanospheres showed higher ROS accumulation in plants than negatively charged 200 nm carboxylate-modified nanospheres. In conclusion, this study provides evidence that polystyrene nanospheres can be taken up into the interior of plant roots and cause plant stress, but these impacts are less pronounced in media where the plastic particles are less mobile, like in agar and soil media as compared to hydroponic systems.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Chemical imaging of individual stratospheric particles sampled over North America

The increasing size, severity, and frequency of wildfires have led to dramatic increases in particulate matter concentrations in the troposphere. Severe wildfires can generate intense convective systems capable of transporting large quantities of biomass burning organic aerosols (BBOA) to the upper troposphere and lower stratosphere (UTLS). Chemically complex organic matter and light-absorbing carbonaceous material is introduced into stratospheric regions that were historically isolated from direct surface emissions. In this study, stratospheric particles were sampled over North America during the Dynamics and Chemistry of the Summer Stratosphere (DCOTSS) campaign, an aircraft-based research project designed to characterize convective perturbation in the UTLS. Particle samples collected from six research flights during summer 2022 were analyzed using Computer-Controlled Scanning Electron Microscopy and Scanning Transmission X-ray Microscopy to investigate particle size distributions, morphology, chemical composition, and mixing state of stratospheric particles along transects across the continental United States and adjacent Pacific Ocean airspace. Analysis revealed that all sampled particles contained detectable levels of carbon, with most exhibiting organic volume fractions of 0.37 ± 0.20. Notably, about 5% of the particles also contained soot inclusions, which indicates the presence of refractory black carbon transported to stratospheric altitudes and provides direct evidence of wildfire-derived black carbon reaching the UTLS. Typical particle morphology exhibits organic shells over soot and inorganic cores and suggests secondary processing and aging of BBOA during transport to and within the UTLS. These findings provide compelling evidence that wildfire emissions play a critical role in affecting the long-term composition and radiative properties of stratospheric particles.

Sharpe, Steven [Purdue Univ., West Lafayette, IN (↗
DOE OSTI2024

Improving Nb 3 Sn cavity performance using centrifugal barrel polishing

Abstract In this study we will show a new method of polishing for Nb 3 Sn cavities known as centrifugal barrel polishing (CBP). Using this method, Nb 3 Sn coated samples are polished to a surface roughness comparable to a traditional Nb cavity after electropolishing. We also investigate different methods of cleaning the Nb 3 Sn surface after CBP to remove residual abrasive particles. The polished Nb 3 Sn surface is analyzed using confocal laser microscopy, and scanning electron microscopy is used to image the surface and measure the surface roughness after polishing. Transmission electron microscopy is also used for high resolution analysis of the surface after polishing. Finally, we show that CBP can improve the performance of a Nb 3 Sn superconducting radiofrequency cavity.

43 PARTICLE ACCELERATORS↗
DOE OSTI2022

A re-examination of the mechanism of whiting events: A new role for diatoms in Fayetteville Green Lake (New York, USA)

Whiting events—the episodic precipitation of fine-grained suspended calcium carbonates in the water column—have been documented across a variety of marine and lacustrine environments. Whitings likely are a major source of carbonate muds, a constituent of limestones, and important archives for geochemical proxies of Earth history. While several biological and physical mechanisms have been proposed to explain the onset of these precipitation events, no consensus has been reached thus far. Fayetteville Green Lake (New York, USA) is a meromictic lake that experiences annual whitings. Materials suspended in the water column collected through the whiting season were characterized using scanning electron microscopy and scanning transmission X-ray microscopy. Whitings in Fayetteville Green Lake are initiated in the spring within the top few meters of the water column, by precipitation of fine amorphous calcium carbonate (ACC) phases nucleating on microbial cells, as well as on abundant extracellular polymeric substances (EPS) frequently associated with centric diatoms. Whiting particles found in the summer consist of 5–7 μm calcite grains forming aggregates with diatoms and EPS. Simple calculations demonstrate that calcite particles continuously grow over several days, then sink quickly through the water column. In the late summer, partial calcium carbonate dissolution is observed deeper in the water column. Settling whiting particles, however, reach the bottom of the lake, where they form a major constituent of the sediment, along with diatom frustules. The role of diatoms and associated EPS acting as nucleation surfaces for calcium carbonates is described for the first time here as a potential mechanism participating in whitings at Fayetteville Green Lake. This mechanism may have been largely overlooked in other whiting events in modern and ancient environments.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2020

Intermediate-Term Thermal Aging Effect Evaluation for Grade 92 and 316L at The LWR Relevant Temperature

Life extension of the existing nuclear reactors imposes accumulated damages, such as higher fluences and longer period of corrosion, to structural materials, which would result in significant challenges to the traditional reactor materials such as type 304 and 316 stainless steels. Advanced alloys with superior radiation resistance will increase safety margins, design flexibility, and economics for not only the life extension of the existing fleet but also new builds with advanced reactor designs. The Electric Power Research Institute (EPRI) teamed up with Department of Energy (DOE) on the Advanced Radiation Resistant Materials (ARRM) program, aiming to develop and test degradation resistant alloys from current commercial alloy specifications by 2021 to a new advanced alloy with superior degradation resistance in light water reactor (LWR)-relevant environments by 2024. Based on a comprehensive microstructure and property screening performed in Phase-1 of the ARRM program, a total of five alloys, together with 316L and X-750 as references, were down-selected for Phase-2 neutron irradiation studies. Because thermal aging could exert a synergistic effect on neutron irradiation due to the low neutron damage rate on the order of 10 –7 displacements per atom per second (dpa/s), Grade 92 (one of the five down-selected alloys) and two heats of 316L were selected in this task to study the effect of aging at 350°C for 12.5–12.7 kh on microstructure and mechanical properties. The aging time is approximately corresponding to 5 dpa neutron irradiation, which can be served as a reference for the 5-dpa-irradiated samples of the alloys to help understand the independent neutron damage influence on microstructure and mechanical properties. Optical microscopy and scanning electron microscopy were used for microstructural characterization. Hardness, tensile, Charpy impact toughness, and fracture toughness in the ductile regime of the aged samples were examined. The aging of Grade 92 led to the formation of many Laves phase in sizes of ~100–200 nm and resulted in some reduction in hardness and yield/ultimate tensile strength with some increases in uniform and total plastic elongations, which may have helped the enhancement of Charpy impact toughness, e.g., ~4 J increase in upper-shelf energy and 20.5°C reduction in ductile-brittle transition temperature compared with the unaged condition. The fracture toughness of the aged Grade 92 showed decent toughness of ~303 MPa√m (K Jq ) with ~87 tearing modulus at 22°C, which reduced to ~241 MPa√m (~20% reduction) with ~75 tearing modulus at 300°C. The two heats of 316L are differentiated by their amounts of δ-ferrite, i.e., ~1 vol% in heat T1103 and ~4 vol% in heat N5B8. The two heats of 316L were subjected to 15% cold work (CW) as this condition is often used in nuclear reactors to help trapping radiation-induced defects and thus postpone the steady state swelling stage. The aging did not result in any noticeable microstructure changes, except for possible segregations at grain boundaries that need to be further investigated. The aging resulted in slight reduction in hardness of 316L-T1103 and slight increase in hardness of 316L-N5B8, which is consistent with their tensile testing results. The 15%CW might have introduced some inhomogeneity, resulting in large standard deviations in hardness, which were reduced after the aging. The aged 316L followed the same trend as the unaged condition for the strength and elongation results from the tensile testing. Minimum elongations appeared within ~300–600°C, above which the elongations seem to increase. Unlike the negligible or minor changes in microstructure, hardness and tensile results of the two heats of 316L, their fracture toughness showed noticeable difference. The aged 316L-T1103 showed good toughness of ~350 MPa√m with ~80 tearing modulus at 22°C, which reduced to ~271 MPa√m (~23% reduction) with ~83 tearing modulus at 300°C. In contrast, the aged 316L-N5B8 showed lower toughness of ~244 MPa√m with ~53 tearing modulus at 22°C, which reduced to ~180 MPa√m (~26% reduction) with ~31 tearing modulus at 300°C. The preliminary results indicate that the presence of high volume of δ-ferrite would noticeable impair fracture toughness although it may not influence hardness and tensile properties.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

3013 Baseline Inner Container Report: Description, Imaging, and Analysis

This report presents consolidated findings from three microscopy studies of baseline Bagless Transfer Containers (BTCs), which are the inner containers used in DOE Standard 3013-compliant plutonium storage packages. The studies were conducted by Los Alamos National Laboratory (LANL), Savannah River National Laboratory (SRNL), and DNV, a subcontractor specializing in corrosion science. The baseline BTCs examined had not been exposed to corrosive environments, serving as control samples for comparison with destructively examined (DE) containers. Additionally, the Background section provides an overview of the BTC design, including manufacturing methods, material properties, and container configurations that may influence corrosion behavior. The primary objective of the LANL and SRNL studies was to establish reference characteristics of BTCs to distinguish manufacturing artifacts from corrosion-induced features observed in DE containers. Both laboratories used advanced microscopy techniques, including Wide Area Microscopy (WAMS), Laser Confocal Microscopy (LCM), Scanning Electron Microscopy (SEM), and Focused Ion Beam (FIB), to reveal that most surface anomalies were shallow and attributable to flow-forming processes, not corrosion. Subsurface impurities, identified as non-metallic inclusions, were also observed. DNV’s investigation focused on characterizing the mechanical and chemical properties of the BTC material to support crack growth modeling. Their findings indicate higher hardness and strength but reduced ductility—consistent with flow-formed 304L stainless steel and a higher-than-expected martensite content, in contrast to manufacturer claims. Ongoing and future studies, including Electron Backscatter Diffraction (EBSD), aim to further understand the microstructural factors influencing crack initiation and propagation. The combined studies provide a crucial baseline for distinguishing corrosion effects in DE containers, contributing to the safe and reliable long-term storage of plutonium-bearing materials.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Photocatalytic Generation of Singlet Oxygen by Graphitic Carbon Nitride for Antibacterial Applications

Carbon-based functional nanocomposites have emerged as potent antimicrobial agents and can be exploited as a viable option to overcome antibiotic resistance of bacterial strains. In the present study, graphitic carbon nitride nanosheets are prepared by controlled calcination of urea. Spectroscopic measurements show that the nanosheets consist of abundant carbonyl groups and exhibit apparent photocatalytic activity under UV photoirradiation towards the selective production of singlet oxygen. Therefore, the nanosheets can effectively damage the bacterial cell membranes and inhibit the growth of bacterial cells, such as Gram-negative Escherichia coli, as confirmed in photodynamic, fluorescence microscopy, and scanning electron microscopy measurements. The results from this research highlight the unique potential of carbon nitride derivatives as potent antimicrobial agents.

36 MATERIALS SCIENCE↗