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All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Microstructural and Superconducting Radiofrequency Properties of Multilayer Sequentially Sputtered Nb 3 Sn films

Nb 3 Sn is considered as a potential candidate for superconducting radiofrequency cavities for particle acceleration due to its higher transition temperature of 18.3 K and higher superheating field of 400 mT. Nb 3 Sn films can be grown inside the surface of a Nb cavity by sequentially sputtering multiple layers of Nb and Sn thin films followed by annealing at 950 °C for 3 h. We report on the properties of Nb 3 Sn films grown on Nb substrates by magnetron sputtering. The films’ crystal structure, surface morphology, and composition were characterized by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The films had a polycrystalline Nb 3 Sn structure with a fine-grain surface and an atomic Sn composition of ~23%. The RF surface resistance of the films was measured for different temperatures at 7.4 GHz to understand the feasibility of this method for the SRF application. The RF surface resistance of the films was 5 mΩ at 12 K, which is about 2 orders of magnitude higher than 60 μΩ previously measured in Nb 3 Sn films grown by Sn vapor diffusion. Finally, the sputtered film had a superconducting transition at 17.2 K, which is also lower than 17.9 K observed in Nb 3 Sn film prepared by vapor diffusion.

43 PARTICLE ACCELERATORS↗
DOE OSTI2020

Physically Based Modeling of PEMFC Cathode Catalyst Layers: Effective Microstructure and Ionomer Structure–Property Relationship Impacts

Abstract This work presents a pseudo-two-dimensional proton exchange membrane fuel cell (PEMFC) model incorporating Nafion ionomer structure–property relationships in the cathode catalyst layer (CL) to capture and explain losses at low Pt loading. Structural data from neutron reflectometry and thin film Nafion conductivity measurements predict variations in the oxygen diffusion coefficient and ionic conductivity with changing CL ionomer thickness and Pt loading. By including these structure–property relationships, predicted polarization curves agree closely with previously published experimental data from cells with Pt loadings between 0.025 and 0.2 mg/cm2. Results demonstrate that structure–property relationships based on physically measurable ionomer and CL properties provide a feasible interpretation of PEMFC CL phenomena for a range of Pt loadings and help explain previously unaccounted-for losses at low Pt. Results also show that simulations must account for surface species coverage variations in order to properly capture the kinetic losses. Finally, results suggest that an increase in ionomer thickness surrounding the C/Pt surfaces may lead to improved cell performance due to improved ionic conductivity.

Electrochemistry↗
DOE OSTI2022

Hydroxyapatite/TiO 2 Nanomaterial with Defined Microstructural and Good Antimicrobial Properties

Due to the growing number of people infected with the new coronavirus globally, which weakens immunity, there has been an increase in bacterial infections. Hence, knowledge about simple and low-cost synthesis methods of materials with good structural and antimicrobial properties is of great importance. A material obtained through the combination of a nanoscale hydroxyapatite material (with good biocompatibility) and titanium dioxide (with good degradation properties of organic molecules) can absorb and decompose bacteria. In this investigation, three different synthesis routes used to prepare hydroxyapatite/titanium dioxide nanomaterials are examined. The morphology and semiquantitative chemical composition are characterized by scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX). The obtained materials’ phase and structural characterization are determined using the X-ray powder diffraction method (XRD). The crystallite sizes of the obtained materials are in the range of 8 nm to 15 nm. Based on XRD peak positions, the hexagonal hydroxyapatite phases are formed in all samples along with TiO 2 anatase and rutile phases. According to SEM and TEM analyses, the morphology of the prepared samples differs depending on the synthesis route. The EDX analysis confirmed the presence of Ti, Ca, P, and O in the obtained materials. The IR spectroscopy verified the vibration bands characteristic for HAp and titanium. The investigated materials show excellent antimicrobial and photocatalytic properties.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2024

Microstructural Coarsening Kinetics and Mechanical Property Changes in Long-Term Aged Sn–Pb–Sb Solder Joints

Tin-lead-antimony (50Sn–47Pb–3Sb wt.%) soldered assemblies were mechanically tested approximately 30 years after initial production and found to have solder joints of reduced strength. The microstructure of this solder alloy exhibits a ternary eutectic structure with Sn-rich, Pb-rich, and SnSb phases. Accelerated aging was performed to evaluate solder microstructural coarsening and associated strength of laboratory solder joints to correlate these properties to the “naturally aged” solder joints. Isothermal aging was conducted at room temperature, 55, 70, 100, and 135 °C and aging times that ranged from 0.1 to 365 days. The coarsening kinetics of the Pb-rich phase were determined through optical microscopy and image analysis methods established in previous studies on binary Sn–Pb solder. A kinetic equation was developed with time exponent n of 0.43 and activation energy of 24000 J/mol, suggesting grain boundary diffusion or other fast diffusion pathways controlling the microstructural evolution. Compression testing and Vickers microhardness showed significant strength loss within the first 20–30 days after soldering; then, the microstructure and mechanical properties changed more slowly over long periods of time. Further, by combining accelerated aging data and the microstructure-based kinetics, strength predictions were made that match well with the properties of the actual soldered assemblies naturally aged for 30 years. However, aging at the highest temperature of 135 °C produced anomalous behavior suggesting that extraneous aging mechanisms are active. Therefore, data obtained at this temperature or higher should not be used. Overall, the combined microstructural and mechanical property methods used in this study confirmed that the observed reduction in strength of ~ 30-year-old solder joints can be accounted for by the microstructural coarsening that takes place during long-term solid-state aging.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Determining the Effects of Neutron Irradiation on the Structural Integrity of Additively Manufactured Heat Exchangers for Very Small Modular Reactor Applications, DOE Final Report (Project # 19-16980)

Auburn University (AU) teamed with the University of Missouri Research Reactor (MURR) and Kansas State University (KSU) to determine how to best use laser-powder bed fusion (L-PBF) additive manufacturing (AM) methods for generating radiation resistant nickel-based superalloys, Inconel alloy 625 and 718, for special purpose reactor (SPR) or very small modular reactor (vSMR) heat-exchangers (HeXs). Compact, conformal, and durable HeXs that are tolerant of extreme environments are needed for supporting the technical maturity of next-generation, portable compact reactors. AM is an enabler for realizing this new wave of HeXs – providing a means to make customizable hot and cold stream architectures with novel flow path geometries (e.g., tortuous channels with non-uniform, asymmetric cross-sections) and reduced layer-to-layer contact resistance (i.e., no separate bonding procedure required). AM further enables a more time/cost efficient means for fabricating SPRs by reducing the number of suppliers required for HeX assembly and allowing for on-site HeX fabrication. The project aim has been to better understand how neutron irradiation affects the microstructure and properties of additively manufactured nickel-based superalloys, to accelerate their safe, reliable use in the modular reactor industry. The major objective was to qualify/quantify the microstructure and microhardness of nickel-based superalloys (including Inconel 718 and 625) additively manufactured via the L-PBF process in the neutron-dosed (irradiated) and non-irradiated states over a course of 3 years. Effects of build orientation during L-PBF and post-AM heat treatments on neutron resistance, microstructure and mechanical properties were also investigated. Neutron damage mechanisms via hardening were characterized. This project combined subject-matter experts in AM, mechanical/microstructure metallic part characterization, and neutron irradiation, as well as unique assets and capabilities at AU and MURR at MU, to ensure project results translated to effectively addressing known gaps in nuclear science and engineering. Parts were fabricated using L-PBF systems readily available at AU. Specimens were then irradiated using MURR facilities; a manipulator equipped hot cell was also used to measure material hardness after dosing. MURR, a 10 MW, light-water nuclear reactor, is the largest, highest powered, highest-flux university owned research reactor in the U.S. The major findings in this project provide evidence that AM can serve as an alternative way to build structural components for future advanced small modular reactors using advanced materials like Inconel 625 (IN625) or Inconel 718 (IN718). After full spectrum neutron irradiation, vertically as-built AM IN625 samples were observed to display better resistance towards radiation-induced-hardening defects relative to traditionally machined metals. A Vickers microhardness tester, using settings of 1 kgf and dwell time of 15 seconds per indentation, was used to measure hardness in this study. The as-built, vertically printed samples experienced 1.2% of radiation hardening vs. 5.25% radiation hardening observed in wrought IN625. Another set of IN625 and IN718 samples were exposed to fast neutron irradiation. It was observed that IN718 showed more resistance towards radiation hardening compared to IN625 samples indicating IN718 had a better performance. Results showed that the IN718 samples experienced less change (-2.5 to 3.24 %) in microhardness. On the other hand, IN625 samples underwent more (0.9 to 7.21%) change in microhardness after fast neutron irradiation. AM IN625 samples were irradiated using an ion (proton) beam in cyclotron. The mechanical properties of AM samples post irradiation were compared with wrought samples. The irradiated region on the samples were tested using nano-hardness indention. It was observed that the beam current and time used in this study generated an annealing effect and thus reduced the hardness of the samples. The sum of the project results provide precious insight into how one may minimize radiation hardening in AM materials while maintaining material property constraints. Results should assist engineers in selecting an appropriate heat treatment for AM nickel-based superalloys for increased radiation resistance. Results should increase confidence levels for adopting AM for building nuclear reactor components which perform the same or better than conventionally manufactured components. Fast neutron irradiation testing provided an accelerated means of obtaining radiation effects without making materials radioactive and difficult to handle.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2019

Effect of Ca and Sm Combined Addition on the Microstructure and Elevated-Temperature Mechanical Properties of Mg-6Al Alloys

In the present study, the microstructure and elevated-temperature mechanical properties of Mg-6Al, Mg-6Al-4Ca, Mg-6Al-4Sm and Mg-6Al-2Ca-2Sm alloys were investigated. The experimental results showed that the microstructure and elevated-temperature mechanical property of Mg-6Al alloy changed obviously with the different elements addition. By analyzing the results of optical microscope, x-ray diffraction analysis, scanning electron microscope, and transmission electron microscope, it could be determined that there was only Mg{sub 17}Al{sub 12} phase in Mg-6Al alloy, there were Al{sub 2}Ca and (Mg, Al){sub 2}Ca phases in Mg-6Al-4Ca alloy, there were Al{sub 2}Sm and Mg{sub 17}Al{sub 12} phases in Mg-6Al-4Sm alloy, and there were (Mg, Al){sub 2}Ca, Al{sub 2}Ca and Al{sub 2}Sm phases in Mg-6Al-2Ca-2Sm alloy. In addition, the addition of alloying elements including Ca and Sm, especially the composite addition, could significantly improve the tensile properties of Mg-6Al alloy. Compared to Mg-6Al alloy, the tensile strengths of Mg-6Al-2Ca-2Sm alloy at 448, 473 and 498 K were enhanced by 50.32, 87.92, and 94.99%, respectively. Furthermore, when the stretching temperatures were 448 and 473 K, the fracture pattern of Mg-6Al-2Ca-2Sm alloy was the mixture of intergranular fracture and trans-crystalline fracture. However, when the stretching temperature was 498 K, the fracture pattern of Mg-6Al-2Ca-2Sm alloy was the intergranular fracture.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Synthesis of porous Ti–50Ta alloy by powder metallurgy

Highlights: • The proposed preview milling with the next sintering enables the homogeneous porous Ti50Ta (wt).% alloy to be obtained • The α and β nanocrystalline phases were prepared by ball milling. • For the longest sintering time there is complete diffusion of preview milled initial powders • The press and sinter route is proved to be a promising alternative for melted Ti-based biomaterials. - Abstract: The aim of the present study was to assess the possibility of producing porous Ti50Ta (wt%) alloys using powder metallurgy by characterizing the material properties. The influence of the sintering time on the microstructure, mechanical properties, and corrosion behaviour of the produced alloy was investigated. The samples were examined using scanning electron microscopy (SEM), transmission electron microscopy (TEM), optic microscopy, X-ray diffraction (XRD) and nanoindentation methods. The XRD results confirmed that nanocrystalline α and β phases were formed during high-energy ball milling. A longer sintering time of 72 h allowed complete interdiffusion of the elements in the pre-milled initial powders. The sintering time significantly influenced the microstructure and porosity. Additionally, the corrosion resistance of the Ti-Ta samples in Ringer's solution was characterized and differences were observed between the samples sintered at different temperatures. The open-circuit potential (E{sub OCP}) and the corrosion potential (E{sub CORR}) of all samples were similar. The sintered Ti50Ta (wt%) alloy showed better corrosion resistance than equivalent Ti or Ta reference samples. We concluded that these alloys had suitable properties for medical implant applications in the future.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Japan-US Joint Research Project PHENIX (2013–2018); Heat Transfer Tests, Neutron Irradiation and Post-Irradiation Examinations for Development of He-Cooled Tungsten Divertor

The goal of the Japan-US joint research project PHENIX (2013–2018) is to understand the feasibility of He-cooled W divertor for DEMO applications. To achieve this goal, the project has three major objectives: (1) to understand heat transfer in a divertor module cooled with high-temperature and high-pressure He gas, (2) to establish database on thermomechanical properties of W materials after high temperature (~500, ~800 and ~1100 °C) neutron irradiation with fusion-relevant energy spectrum, and (3) to clarify tritium (T) trapping and permeation in neutron-irradiated W materials. Heat transfer tests for a He-cooled modular divertor with multi-jet (HEMJ) have been performed, and the problem of heat transfer degradation by re-laminarization was identified.The irradiation capsule with thermal neutron shielding was designed for high temperature neutron irradiation in the High Flux Isotope Reactor (HFIR), Oak Ridge National Laboratory (ORNL) with fusion-relevant transmutation. The expected damage level is 1–1.5 displacements per atom (dpa). Heat load resistance, thermal conductivity, mechanical properties and microstructures are examined in ORNL after the irradiation. Mechanical properties of W single crystal samples irradiated with neutrons in HFIR at 90– 850 °C without thermal neutron shielding were examined for comparison. Significant hardening was observed after irradiation to >1 dpa. Microstructural examinations revealed that the hardening was mainly caused by formation of irradiation-induced precipitates consisting of W, Re and Os. Comparison with new samples irradiated in the capsule with thermal neutron shielding will show the effects of irradiation temperatures and transmutation elements. Retention and permeation of hydrogen isotopes including T in neutron-irradiated samples are examined in Idaho National Laboratory, and permeation of H and D in samples damaged with surrogate irradiations (heavy ions, electrons, etc.) is measured in Sandia National Laboratories, Livermore, to study hydrogen-defect interactions in wider conditions. The measurement of D retention in the single crystal W sample after neutron irradiation to 0.1 dpa at 360 °C and subsequent plasma exposure at 400 °C showed significant trapping effects by radiation-induced defects.

Ueda, Yoshio↗
DOE OSTI2024

Promoting the regulatory acceptance of combined ion and neutron irradiation for material degradation in nuclear reactors

The Advanced Materials and Manufacturing Technologies (AMMT) program within the Department of Energy (DOE) Office of Nuclear Energy has developed its current recommendation for promoting the use of combined ion irradiation and neutron irradiation for the accelerated qualification of materials to be deployed in nuclear reactors. This plan is intended to provide a collaborative path forward that can be adopted by academia, national laboratories, and industry, and has been developed with input from the regulatory research arm of the U.S. Nuclear Regulatory Commission (NRC). To deploy new materials or materials manufactured with new technologies, such as additive manufacturing, materials must be evaluated for reactor-induced degradation from the combination of harsh temperatures, corrosive environments, and radiation fields. However, rapid deployment of materials necessitates accelerated testing methods rather than relying on years of neutron irradiation in a material test reactor. Ion irradiation has demonstrated success in reproducing material microstructure and select property evolution resulting from neutron irradiation with three to four orders of magnitude reduction in time and cost, making it an ideal candidate for accelerated irradiation testing. This presentation provides context governing both the scientific and regulatory aspects of the proposed goal. The discussion is aimed at a broad audience including researchers from industry, national laboratories, and academia. The recommended path forward is presented as a conceptual framework of specific steps. In brief, the strategy entails developing an integrated ion and neutron irradiation test plan for the material property of interest based on the fundamental tenet of the linkage of microstructure and properties in materials. Physics-based modeling interprets ion irradiation data and predicts neutron irradiation microstructure and properties with uncertainty bounds. The first round of testing is sufficient for an initial licensing application using a risk-informed approach, while a minimum required neutron irradiation test plan reduces cost and time requirements. A surveillance program with witness specimens in-reactor provides additional data over time to improve model predictions to higher damage levels and further reduce uncertainty bounds, which can be used for license extensions or longer lifetimes in new license applications.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

The Microstructure, and Mechanical and Corrosion Properties of As-Cast and As-Extruded Mg-2%Zn-x%Cu Alloys After Solution and Aging Heat Treatments

The effects of different Cu concentrations and heat treatment on the microstructure, mechanical and corrosion properties of the as-cast and hot-extruded Mg-2%Zn alloys were studied. The results showed that T6 heat treatment led to the dissolution of intermetallics and breaking the continuous networks of intermetallics. Also, the grain size of the base alloy decreased with further Cu additions after solution and aging heat treatments. Microstructural characterization indicated that Mg(Zn,Cu) and Mg(Zn,Cu){sub 2} intermetallics were formed which their volume fractions increased with exceeding Cu additions. Moreover, the addition of 3 wt.% Cu and T6 heat treatment increased the Brinell hardness of both as-cast and hot-extruded specimens reached to 94 HBN and 116 HBN, respectively. The optimum amounts of the ultimate tensile strength and elongation values obtained from 0.1 wt.% Cu addition for both conditions after T6 treatment which were 253 MPa, 11.5% and 263 MPa, 14.7%, respectively. However, more Cu addition (> 0.5 wt.%) deteriorated the tensile properties of the alloy due to the high volume fraction of intermetallics. The yield tensile strength increased continuously with different Cu additions for the cast and extruded alloys after solution and aging heat treatments. After T6 heat treatment, extruded alloys showed better anti-corrosion properties than those of the cast alloys, while the extruded Mg-2%Zn-0.1%Cu alloy exhibited the best anti-corrosion property. Further Cu addition increased the volume fraction of intermetallics and enhanced the corrosion rate which was due to the galvanic couple effect.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Study of Tribological Characteristics of Multi-pass SMAW Armox 500T Steel Joints

Study of tribological characteristics of multi-pass shielding metal arc-welded (SMAW) Armox 500T steel joints in comparison with its counterpart base metal was carried out. Series of dry sliding wear tests were carried out as a function of applied loads ranging from 30 to 120 N and sliding distances from 1000 to 6000 m at a constant sliding velocity using pin-on-disk tribometer. It was observed that specific wear rate and lost volume in SMAW joints significantly high compared to Armox 500T base metal in the range of loads and sliding distances considered in the present study. The scanning electron micrographs indicated that wear of Armox 500T base metal occurred due to micro-grooving and adhesion, on the other hand, micro-delamination was observed in SMAW joints. Microstructural investigations revealed that base metal exhibits superior tribological properties as compared to SMAW joints due to the formation of martensite lath in acicular form with coarse and fine precipitates.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure, fatigue, and impact toughness properties of additively manufactured nickel alloy 718

A complete understanding of processing-structure-property-performance relationship of additively manufactured (AM) components are critical from an application standpoint. Therefore, in the current investigation, a comprehensive microstructural characterization and mechanical properties (tensile, fatigue and impact toughness) evaluation of nickel alloy 718 AM by the laser powder bed fusion (L-PBF) technique have been performed. AM builds were made from powders manufactured via different atomization conditions. Although the standard post-heat treatment procedure led to the removal of severe interdendritic segregation both grain boundary and intra-grain precipitation of d phase occurred. Regardless of d phase presence, axial fatigue properties of both the AM builds were similar to design handbook wrought fatigue data. However, due to the d phase, impact toughness properties were comparable to the wrought material conditions that exhibited d phase. Fractured surfaces of Charpy impact samples exhibited crack propagation extensively along the boundaries decorated by d precipitates.

Komarasamy, Mageshwari↗
NASA NTRSDate not supplied

Integrated Process-Structure-Property Simulations for Additive Manufacturing Using the Open-Source Materialite Package

The microstructure and properties of additively manufactured (AM) metals are strongly dependent on process conditions. Therefore, process-structure-property (PSP) simulations are a useful tool for exploring process parameter space, studying process variations, and quantifying uncertainty in material properties. However, integrating process-structure and structure-property simulations often involves connecting multiple software packages. Each package may use unique data structures and require substantial domain knowledge. This presentation demonstrates PSP simulation capabilities of Materialite, an open-source package developed at NASA Langley Research Center. Materialite simplifies model linkages by using a common data structure and model interface, enabling straightforward simulation across a PSP model chain. Physics-based models, including kinetic Monte Carlo and crystal plasticity, are implemented within the package. The model interface is also intended to simplify implementation of new models and enable integration with external simulation tools. Example use cases include uncertainty quantification with PSP models and GPU-accelerated powder bed fusion AM process models.

additive manufacturing↗
DOE OSTI2022

Microstructural evolutions, phase transformations and hard magnetic properties in polycrystalline Ce–Co–Fe–Cu alloys

This work focuses on systematic studies of Ce–Co based 1:5 permanent magnet alloys of CeCo 4.4-x Fe x Cu 0.6 and CeCo 3.9-x Fe x Cu 1.2 (x = 0, 0.3, 0.6, 0.9, 1.2, 1.8) by varying Co:Fe. The overarching aim of this manuscript is to elucidate the hard-magnetic properties through a better understanding of phase formation by the structural, microstructural, and magnetic properties in these materials. Improved mutual solubility of Fe in the 1:5 phase has been observed with an extended homogeneity range by Cu substitution. For both composition series, Fe contents of x ≤ 0.6 show a homogeneous microstructure with a single 1:5 phase and good magnetic properties. The composition region 0.6 < x ≤ 0.9 appears to be near the boundary of solubility and evolution of other phases. At x = 1.8, it is found that the homogeneous 1:5 phase and magnetic hardness deteriorated due to the evolution of secondary phases such as 2:17, 2:7, and Fe–Co. Furthermore, the addition of Fe improved both the magnetization and Curie temperature via increased effective exchange interactions, while an increase in Cu content enhanced coercivity.

33 ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2019

Microstructural, Magnetic, Magnetocaloric, and Electrical Properties of Ni{sub 0.4}Mg{sub 0.3}Cu{sub 0.3}Fe{sub 2}O{sub 4} Ferrite Prepared Using Sol–Gel Method

Detailed investigations of the microstructural, magnetic, magnetocaloric, and electrical properties of Ni{sub 0.4}Mg{sub 0.3}Cu{sub 0.3}Fe{sub 2}O{sub 4} ferrite synthesized by sol-gel method have been investigated. XRD pattern indicates that sample has cubic spinel structure with Fd 3-bar m symmetry. The cation distribution of the sample has been determined by Rietveld refinement. Temperature dependence of magnetization shows that sample exhibits a second-order PM to FM phase transition at the Curie temperature T{sub C} = 690 K. From the M(μ{sub 0}H,T) data, we found that the maximum entropy change |ΔS{sub M}{sup max}| reaches value of about 1.56 J kg{sup − 1} K{sup − 1} and relative cooling power (RCP) of 136 J kg{sup − 1} at μ{sub 0}H = 5 T. From electrical conductivity curves, the estimated value of the activation energy is equal to 0.349 eV. The Nequist diagram at different temperatures reveals that the grain boundary contribution is responsible to the conduction process for the studied sample.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Post-build stress-relief optimization for laser powder bed fusion 316H stainless steel

Nuclear energy remains a critical component of a diversified and efficient energy portfolio, offering reliable, high-capacity, and low-carbon power. However, in the U.S., aging infrastructure and the slow qualification and deployment of advanced materials and manufacturing techniques hinder progress in next-generation reactor technologies. This study explores the application of laser powder bed fusion (LPBF) additive manufacturing for stainless steel 316H, with a focus on optimizing post-build heat treatments to enhance material properties for high-temperature nuclear applications. The research targets the optimization of stress-relief temperatures to alleviate postbuild residual stresses, ensuring improvements in the microstructural corelated properties. A series of microstructural and mechanical evaluations were performed on LPBF-printed SS-316H samples which were subjected to annealing at temperatures varying between 650 °C and 850 °C. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy analyses revealed that increasing the heattreatment temperature accelerated dislocation recovery. Vickers microhardness measurements showed an initial reduction in values, followed by stabilization over extended durations at all the temperatures. While higher temperatures facilitated faster recovery, they also promoted carbide precipitation along grain and solidification cell boundaries, narrowing the safe processing window. In contrast, heat treatment at 650°C preserved the cellular substructure and enabled controlled carbide precipitation over time. In conclusion, these findings highlight the importance of time–temperature optimization and suggest that 650°C for up to 2 h provides the most favorable balance between recovery and carbide control for a stress-relief treatment.

316 stainless steel↗
DOE OSTI2025

Structure–property relationships of reduced graphene oxide membranes intercalated with polycyclic aromatics

Graphene oxide (GO) membranes intercalated with various organic moieties have shown excellent potential for a range of water processing applications. However, microstructure–functional property relationships in these structurally disordered membranes are not well understood. We demonstrate a practical methodology for developing such relationships for GO membranes intercalated with molecular species, with polycyclic aromatic toluidine blue O (TBO) as an example functional intercalant. We use solid-state UV–vis absorbance and fluorescence measurements to quantitatively track the arrangements of TBO in a series of TBO-loaded reduced GO (rGO) membranes. This study reveals the evolution of diverse arrangements including TBO monomers, lateral and stacked dimers, and other aggregates, as a function of overall TBO loading. These microstructures are then correlated to changes in overall properties such as interlayer d-spacings, permeate fluxes, and solute rejections. The characterization of these different intercalant microstructures explains non-intuitive flux and rejection trends, which can circumvent flux and solute rejection trade-offs.

02 PETROLEUM↗