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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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All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Effects of high-dose neutron irradiation at light-water reactor relevant temperature on the mechanical properties of SiC/SiC composites

For this study, the neutron dose-dependent evolutions and the underlying mechanisms of properties of SiC fiber-reinforced SiC matrix (SiC/SiC) composites at a temperature relevant to light-water reactors (∼600 K) were investigated and analyzed. Chemical vapor infiltrated (CVI) SiC/SiC composites reinforced with Hi-Nicalon Type S or Tyranno SA3 fiber were neutron-irradiated to doses up to 30 dpa. The irradiated composites retained their flexural strengths. The thermal diffusivity and dimensional changes were mostly retained from 2.0 to 30.2 dpa. Discrepancies in irradiation responses among CVI SiC/SiC composites from different sources were found. Additional microstructural analysis using Raman spectroscopy and numerical analysis on irradiation effect on residual stress were used to explain how the microstructural variables, especially of carbon interphases, affect the mechanical properties in the 30–40 dpa dose range.

Continuous fiber-reinforced ceramic matrix composi↗
DOE OSTI2018

Development of a mechanistic thermal aging model for Grade 91

This report provides a summary on understanding and predicting the effects of long-term thermal aging on microstructure and tensile properties of G91 to corroborate the ASME Code rules in strength reduction due to elevated temperature service. The research is to support the design and long-term operation of G91 structural components in sodium-cooled fast reactors (SFRs). The report is a Level 2 deliverable in FY18 (M2NT-18AN050502061), under the Work Package NT-18AN05050206, “G91 Code Extension Testing” performed by the Argonne National Laboratory (ANL), as part of the Advanced Materials Development Program for Fast Reactors. The thermal aging study of G91 involves three types of thermally-aged specimens: (1) specimens machined from two heats of G91, G91-H1 and H30176 that have been tested for the Advanced Materials Development Programs in the past years. These specimens were aged at 550, 600, and 650°C for times up to ~64,000 h; (2) specimens fabricated from the heads of the archived crept specimens (13 in total) of six heats of G91, H5349, H30394, H30383, H10148, H30176. These specimens were aged at 427 - 538°C and for times up to 132,647 h; (3) specimens made from a tube removed from the Kingston coal-fired power plant after exposure for 155,000 h at 550°C. These three sets of specimens provide a comprehensive data set for understanding and predicting the effect of long-term thermal aging on microstructure and tensile properties of G91. Microstructural analysis of the thermally-aged G91 revealed that thermal aging causes significant microstructural changes: (1) the tempered martensite formed during tempering is unstable, and suffers significant recovery during aging, manifested by an increase in subgrain width, a decrease in subgrain length, and a decrease in subgrain aspect ratio (i.e. subgrains become more equiaxed) as the aging temperature and time increase. The subgrain recovery is facilitated by the reduction of dislocation density within subgrains; (2) M23C6 carbides in the as-received G91 are distributed along grain and subgrain boundaries and play an important role as pinning obstacles against subgrain coarsening. M23C6 carbides coarsen during aging, and the coarsening of M23C6 carbides reduces the pinning force on the boundaries; (3) MX carbonitrides in the as-received G91 are distributed uniformly within subgrains, providing the precipitation hardening effect. They coarsen with increasing aging temperature and time, but the coarsening rate is low; (3) a new phase, the Laves phase intermetallic forms during aging. The formation of the Laves phase removes the Mo solutes from the matrix, reducing the solid solution strengthening effect. The Laves phase particles grow rapidly once they are nucleated, and they precipitate primarily along boundaries. They may have a pinning effect on boundaries, but should provide little to the alloy strength. The evolution of each microstructural constituent during thermal aging can be well described by individual microstructural models. The estimated activation energy for MX coarsening was 175 kJ/mol, equivalent to the activation energy for boundary and core diffusion in a-Fe, while the estimated activation energy for subgrain coarsening was significantly lower, ~96 kJ/mol. Thermal aging of G91 results in the reduction in the yield stress and the ultimate tensile strength but has an insignificant effect on the uniform and total elongations. The reduction in tensile strength is more pronounced as the aging temperature and time increases. The in situ tensile tests with high-energy X-rays revealed that sub-boundary strengthening plays a dominant role, and the strengthening role of M23C6 particles may be accounted for by subgrian boundary hardening, and three strengthening mechanisms can be superimposed to describe the tensile strength of G91: subgrain boundary hardening, MX precipitation hardening, and Mo solid solution strengthening. A microstructure – strength model was establ

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2014

WETTING AND REACTIVE AIR BRAZING OF BSCF FOR OXYGEN SEPARATION DEVICES

Reactive air brazes Ag-CuO and Ag-V2O5 were evaluated for brazing Ba0.5Sr0.5Co0.8Fe0.2O(3-δ) (BSCF). BSCF has been determined in previous work to have the highest potential mixed ionic/electronic conducting (MIEC) ceramic material based on the design and oxygen flux requirements of an oxy-fuel plant such as an integrated gasification combined cycle (IGCC) used to facilitate high-efficiency carbon capture. Apparent contact angles were observed for Ag-CuO and Ag-V2O5 mixtures at 1000 °C for isothermal hold times of 0, 10, 30, and 60 minutes. Wetting apparent contact angles (θ<90°) were obtained for 1%, 2%, and 5% Ag-CuO and Ag-V2O5 mixtures, with the apparent contact angles between 74° and 78° for all compositions and furnace dwell times. Preliminary microstructural analysis indicates that two different interfacial reactions are occurring: Ag-CuO interfacial microstructures revealed the same dissolution of copper oxide into the BSCF matrix to form copper-cobalt-oxygen rich dissolution products along the BSCF grain boundaries and Ag-V2O5 interfacial microstructures revealed the infiltration and replacement of cobalt and iron with vanadium and silver filling pores in the BSCF microstructure. The Ag-V2O5 interfacial reaction product layer was measured to be significantly thinner than the Ag-CuO reaction product layer. Using a fully articulated four point flexural bend test fixture, the flexural fracture strength for BSCF was determined to be 95 ± 33 MPa. The fracture strength will be used to ascertain the success of the reactive air braze alloys. Based on these results, brazes were fabricated and mechanically tested to begin to optimize the brazing parameters for this system. Ag-2.5% CuO braze alloy with a 2.5 minute thermal cycle achieved a hermetic seal with a joint flexural strength of 34 ± 15 MPa and Ag-1% V2O5 with a 30 minute thermal cycle had a joint flexural strength of 20 ± 15 MPa.

Ag-CuO↗
DOE OSTI2022

TEM Specimen Manufacturing to Support Analysis of IASCC Mechanisms in Irradiated Austenitic Steels – Light-Water– Relevant Materials

The present report describes the manufacturing of samples for advanced microstructure studies of mechanisms of irradiation-assisted stress corrosion cracking (IASCC) in the materials of light-water reactor (LWR) internal components. The samples were manufactured via FIB (focused ion beam milling) from 4-point-bend specimens subjected to oxidation and mechanical loading in a simulated LWR environment (primary water, PW). The corrosion tests were conducted at the University of Michigan (UM), and the tested specimens were transported to ORNL to perform FIB work. Finally, the manufactured FIB specimens were shipped back to the UM for microstructure characterization. Section 1 in the report provides a brief introduction; Section 2 describes materials, their in-service and irradiation history, and the geometry of specimens for IASCC testing. Section 3 documents typical work steps (specimen mapping) and reports the number of manufactured FIB objects. Section 4 briefly describes the preliminary results of microstructure analysis performed at the University of Michigan and highlights the key findings. The summary and conclusions section discusses future possible future steps and generalizes the obtained results, their unique character, and their importance for the nuclear industry.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2018

Electrically-Assisted Tubing Processes for Enhancing Manufacturability of Oxide Dispersion Strengthened Structural Materials for Nuclear Reactor Applications

The overall goal of this project is to enhance the formability of Nanostructured Ferritic Alloys (NFAs) such that high-strength thin-walled claddings can be successfully and economically manufactured for use in future nuclear reactors. Specifically, four objectives were identified: Objective #1 – to achieve a good understanding of the mechanical behavior and resulting microstructure of 14YWT made from the powder form subjected to various Electrically- Assisted (EA) loading conditions. Objective #2 – to conduct EA-flat rolling of 14YWT completed and the prioritization/selection of two alternative designs of EA tube rolling processes. Objective #3 – to design and assemble a new EA tube rolling machine. Objective #4 – to conduct rolling using the new EA rolling machine. The above objectives were achieved and the findings can be further applied to establish other innovative fabrication processes. Specifically, the major accomplishments are summarized as: The use of an EA forming process was investigated to reduce the forming force of ODS ferritic steels. The effect of a continuous electric current on 14YWT during plastic deformation was evaluated. EA uniaxial tension tests show that the electric current is able to reduce the flow stress of 14YWT. 14YWT exhibits a ductility minimum at a current density of 34.5 A/mm2 which is consistent with fractography results. Hardness measurements and TEM results indicate that oxide particles are stable during the EA process. By following the tests, microstructure analysis was performed on the sample in its as-received state and after current treatment. The microstructures are stable when subjected to high current density. The related thermal model was developed to predict the Joule heating temperatures. The temperatures were compared with the experimental results. At last, a temperature-dependent hardening model was used to explore the mechanisms acting during EA deformation. Since the model can accurately predict the yield strength of 14YWT under EA conditions without the incorporation of non-thermal effects, it can be concluded that the reduction in yield strength is due to the Joule heating generated under continuous current loading conditions. An oven-heated pure thermal tension test was conducted to confirm this conclusion. The new EA tube rolling machine has been completely developed. The related work includes: (1) forming process design; (2) analysis of the effect of roll-tube contact geometry on rolling force; (3) analysis of machine performance under mechanical loading; (4) design of machine electrical setting path and insulation; (5) multi-pass process analysis; (6) design of power transmission system (axial/radial/torque feeding mechanisms), roll bearing system, cooling system, workpiece feeding mechanism, and other related mechanical connection support components; (7) design and optimization of roll profiles/dimensions; (8) analysis and simulation of the rolling process; (9) development of engineering drawings and fabrication; (10) assembly and calibration of the EA tube rolling machine; (11) design and integration of the electrical control system; (12) hardware integration for high power supply electrically-assisted rolling process; (13) induction heating system integration; (14) experimental tests for the new rolling process. Through the process from conceptual design to final machine calibration and experimental tests, there are many technical and physical works that have been implemented and improved for the best performance of the innovative prototype.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2017

High-Speed Friction Stir Welding of AA7075-T6 Sheet: Microstructure, Mechanical Properties, Micro-texture, and Thermal History

Friction-stir-welding (FSW) is a cost-effective and high quality joining process for aluminum alloys (especially heat-treatable allo ys) that has been applied successfully in the aerospace industry. However, the full potential of FSW on more cost-sensitive applications is still limited by the production rate, namely the welding speed of the process. The majority of literature evaluating FSW of aluminum alloys is based on welds made in the range of welding speeds around hundreds of millimeters per minute, and only a handful are at a moderate speed of 1 m/min. In this study we present a microstructural analysis of friction stir welded AA7075-T6 blanks with welding speeds up to 3 m/min. Textures, microstructures, mechanical properties, and weld quality are analyzed using TEM, EBSD, metallographic imaging, and Vickers hardness. Results are coupled with welding parameters to aid in the understanding of the complex material flow and texture gradients within the welds in an effort to optimize welding parameters for high speed processing.

Zhang, Jingyi↗
DOE OSTI2013

Edward's sword? - A non-destructive study of a medieval king's sword

Non-destructive and instrumental methods including photon activation analysis were applied in an examination of an ancient sword. It was tried to find indication of forgery or, if authentic, any later processing and alteration. Metal components of the hilt and the blade were analysed by instrumental photon activation. Non-destructive metallurgical studies (hardness measurements, microscopic microstructure analysis) are briefly described, too. The results of these investigations did not yield indication of non-authenticity. This stood in agreement with the results of stylistic and scientific studies by weapon experts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Effect of Oxide Additives on Phase Evolution and Tribological Behavior of Zirconia-Toughened Alumina Composite

Four different zirconia-toughened alumina added with different pairs of oxides (CeO{sub 2}, TiO{sub 2}, CuO, ZnO and SnO{sub 2}) were prepared through the co-precipitation technique. Conventional sintering resulted in relative densities ≥96%. Phase analyses of these composites were performed by x-ray diffraction. Vicker’s hardness and tribological behavior of all ZTA composites were studied. Microstructure analysis of polished and worn surfaces was carried out to understand and correlate the mechanical/tribological behavior with the microstructure. A different wear mechanism is observed in ZTA containing CeO{sub 2} and TiO{sub 2} which resulted in considerable improvement in tribological behavior with a minimum specific wear rate of 9 × 10{sup −7} mm{sup 3}/Nm.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Magnesium Alloy ZK60 Tubing made by Shear Assisted Processing and Extrusion (ShAPE)

ZK60 Magnesium tubing has been friction extruded from as-cast billets and T5 conditioned bars using Shear Assisted Processing and Extrusion (ShAPE). Tubes having an outer diameter of 50.8 mm and wall thickness of 1.9 mm were extruded with >20 times less ram force compared to conventional extrusion due to the unique shearing conditions and tooling inherent to ShAPE. Microstructures of the as-cast billet and T5 bar feedstock materials were significantly different from each other in terms of grain size, texture, and second phase distribution; yet the resulting microstructures after ShAPE were remarkably similar. An average grain size of 4-5 microns, 20o tilt of basal texture away from the extrusion axis, and refined second phases having a uniform distribution were achieved independent of the feedstock material. Hardness for as-extruded and artificially aged tubes are presented with isotropic behavior explained by detailed microstructural analysis. This work suggests that bulk ZK60 magnesium alloys extrusions may be fabricated in a single step, with microstructures that are unobtainable with conventional extrusion.

Friction Stir Extrusion, Friction Consolidation an↗
DOE OSTI2020

Fabrication of UN-Mo CERMET Nuclear Fuel Using Advanced Manufacturing Techniques

Ceramic-metallic nuclear fuels are a candidate fuel for nuclear thermal propulsion systems due to their high heat transport properties, which are necessary in very high-temperature environments. The conventional fabrication of uranium nitride–molybdenum fuel has been thoroughly studied in the past, but modern manufacturing techniques have presented a unique opportunity for further development within this field. This work demonstrates the use of advanced manufacturing techniques to produce nuclear fuel pellets composed of uranium nitride microspheres encased in a molybdenum matrix. Binder jetting is used to print molybdenum disks that are filled with uranium nitride microspheres and afterward sintered using spark plasma sintering. Two fuel pellets were fabricated to demonstrate the methodology and to provide a baseline analysis of the effects of temperature and pressure processing conditions. Characterization of the sintered fuel pellets includes detailed microstructural analysis and thermal conductivity measurements.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

STEM imaging of irradiation induced defects in Eurofer97 steel variants irradiated in the EUROfusion collaboration

Ten exploratory variants of Eurofer97 reduced activation ferritic martensitic (RAFM) steel were irradiated in HFIR to ~2.94 – 32.4 dpa, 300±30 °C as a part of the EUROfusion collaboration. The irradiations were performed in rabbit capsules. ES21-22 capsule were used for irradiating SS-J3 tensile samples while M4CVN bend bar samples were irradiated in ES31-35 capsules. The mechanical properties and multi-length scale characterization of the microstructures of these ten steels, designated as H, I, P, J, K, L, M, N, O, P and reference E, in the nonirradiated form was reported in "Mechanical properties and microstructure characterization of unirradiated Eurofer-97 steel variants for the EUROfusion project, ORNL/SPR-2018/882," while their irradiated properties and some microstructure analysis was reported in "Post-irradiation examination of Eurofer97 steel variants irradiated to 2.5 dpa, ~300 °C in HFIR for the EUROfusion program, ORNL/SPR-2020/1440." Here, additional microstructures using TEM/STEM and STEM-EDX of the irradiated steels is presented. Characterization was performed at the Low Activation Materials Development and Analysis (LAMDA) laboratory.

36 MATERIALS SCIENCE↗
DOE OSTI2023

EDS-PhaSe: Phase Segmentation and Analysis from EDS Elemental Map Images Using Markers of Elemental Segregation

Scanning electron microscopy (SEM), combined with energy-dispersive spectroscopy (EDS), is an extensively used technique for in-depth microstructural analysis. Here, we present the EDS-Phase Segmentation (EDS-PhaSe) tool that enables phase segmentation and phase analysis using the EDS elemental map images. Importantly, it converts the EDS map images into estimated composition maps for calculating markers of selective elemental redistribution in the scanned area and creates a phase-segmented micrograph while providing approximate fraction and composition of each identified phase. EDS-PhaSe offers two unique advantages. Firstly, it enables the direct processing of EDS elemental map images without requiring any raw or proprietary data/software, thereby allowing the analysis of EDS results available in the published literature as images. Secondly, it enables segmentation and analysis of phases even when the phase contrast is missing in backscattered micrographs, assisting in correlating the XRD and SEM-EDS data as shown in this work for a AlCoCrFeNi high-entropy alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Studying Unirradiated TRISO-coated Particles from the Second Advanced Gas Reactor Experiment

Combined precession electron diffraction and point resolved chemical imaging have been used to provide an analysis of the material structure and chemical information of unirradiated uranium oxy-carbide (14.0 wt% enriched) kernelled tristructural isotropic-coated (TRISO) coated particle fuel. The detailed microstructural analysis includes examination of the structure associated with kernel, IPyC and SiC layers, as well as the IPyC-SiC interface. The analysis serves as a baseline for future studies on the potential effects of fission product and defect release through intact SiC layers and possible grain restructuring with irradiation. The baseline microstructure is thereby identified to understand the subtle effects of fabrication that may influence fission product precipitate release associated with different fuel types. Results indicated a Si:C gradient in the SiC layer which could influence fission transport reactivity and the high resolution imaging at the IPyC-SiC interface shows the gradual chemical composition change at this interface.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Hydrothermal synthesis of vanadium pentoxide nanowires

Nanowires of V{sub 2}O{sub 5} were prepared via hydrothermal route using NH{sub 4}VO{sub 3} as precursor in the presence of sulfuric acid at 120°C for 24 h. This synthesis process is free of any templates and reducing agents. Thermal analysis showed a phase change at 350°C and the samples were annealed at 500°C. The XRD analysis showed the monoclinic phase for the as-prepared and orthorhombic phase of V{sub 2}O{sub 5} when annealed at 500°C. Characteristic Raman peaks also expressed the same structural features. Microstructure analysis by SEM showed the nanowire structure of V{sub 2}O{sub 5} with thickness in the range of 20–50 nm and length in micrometers. The possible mechanisms of formation of the nanowires were schematically explained based on the layered structure of V{sub 2}O{sub 5}.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

The relationship between low-temperature toughness and secondary crack in low-carbon bainitic weld metals

Highlights: • The crack propagation plane was identified with the decreasing possibility of {110}/{100}, {112} and {123}. • Crack path deviates at some middle-angle misorientation boundaries with high strain concentration. • The most effective barrier to arrest crack in Ni0 and Ni2 is the boundaries of inter-Bain in a CPP packet, while in Ni4 the boundaries of inter-CPP and intra-Bain packets impede crack propagation. - Abstract: This paper aims to reveal the relationship among low-temperature toughness, microstructure and secondary crack from both microstructural and crystallographic perspectives. Instrumented Charpy tests were carried out in the upper platform, transition temperature range, as well as at lower temperatures. Quantitative fractographic analysis, microstructural characterization and secondary crack observation were conducted on half of the impact specimen. Crystallographic features were identified in the secondary crack proximity, e.g. variant selection, orientation relationship, cleavage plane of the corresponding crack matrix. Some results in literature are confirmed. Nickel addition is beneficial to hindering crack propagation as a result of microstructure improvement. The most effective barrier for crack propagation is high-angle misorientation boundaries between Bain packets and the boundaries of ferrite matrix with the microstructure of granular bainite. Additionally, high-angle misorientation boundaries between closed-packed plane packets arrest cracks in the mixed microstructure of fine lath bainite and intricate acicular ferrite. Most preferred crack propagation planes are {110} and {100} in our low carbon bainitic weld metals, with the decreasing possibility of {112} and {123}.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Localized Deformation Investigation in Irradiated Materials via Electron Microscopy, EBSD, and In-Situ Mechanical Testing

This report describes the preliminary results of an analysis of dislocation defect structures in nondeformed and deformed austenitic stainless steels – materials of light water reactor internal components. The analysis was performed using an advanced modern approach: high-resolution electron backscatter diffraction (HR-EBSD). Work was performed at Oak Ridge National Laboratory’s Low Activation Materials Development and Analysis (LAMDA) facility. The report is divided into sections describing specific aspects of the project. Section 1 describes the necessity and importance of the defect microstructure analysis and demonstrates that there are very limited data regarding dislocation and defect population at the meso-level (i.e., a grain or group of interacting grains). Section 1 also introduces the HR-EBSD approach used in this research and provides a limited background. Section 2 describes the scanning electron microscope/EBSD systems available at the LAMDA facility, materials investigated in the present work, and hardware and software requirements for the HR-EBSD analysis. Section 3 provides preliminary HR-EBSD results for nonirradiated austenitic stainless steel in contrast to and in comparison with the conventional EBSD outcome. Section 4 describes the HR-EBSD results for austenitic stainless steel irradiated in a commercial-type nuclear power plant and subjected to in-situ mechanical testing. The analysis is focused on mapping and analyzing the geometrically necessary dislocations before and after deformation at small strain levels. As expected, the results will be beneficial for performing corrosion tests, including electrochemical microscopy, which is currently being performed within the Light Water Reactor Sustainability program at the University of California–Los Angeles (Dr. G. Sant). Section 5 summarizes the work performed, presents conclusions, and discusses future activities for this research.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2021

Machine Learning Based Software Package for Reproducible Data Analysis for Electron Microscopy

Advances in hardware and computation technologies are enabling large hyperspectral imaging during Electron Microscopy (EM), resulting in datasets being produced at rapidly increasing spatial and temporal resolutions. This presents exciting opportunities for microstructure analysis, but also poses great challenges in data analysis. Under this STTR program, QuesTek Innovations LLC, a leader in the field of integrated computational materials engineering (ICME), collaborated with Lawrence Livermore National Laboratory and Argonne National Laboratory. The team developed an open-source machine learning (ML) powered tool for EM data analysis of multiple systems and data types, and collected EM data for ML model development using the cutting-edge PicoProbe equipment at Argonne National Laboratory.

Lin, Yu↗
DOE OSTI2013

Observation of crystallization and characterizations on thiourea cadmium iodide: A semi-organic optical material

Graphical abstract: - Highlights: • Thiourea cadmium iodide (TCI) was grown by slow evaporation solution technique. • Morphology and growth rate of the grown compound are determined with the help of inverted microscope. • Optical band gap has been determined. • Microstructure analysis has been reported. • Electrical study has been reported and discussed. - Abstract: In this work, the single crystals of thiourea cadmium iodide were grown by slow evaporation solution technique in two different ratios 2:1 and 1:1. During the formation of their single crystals the morphological features and its live growth process were recorded with the help of inverted microscope. Structural studies of the grown crystals have been carried out by powder X-ray diffraction to confirm the crystal system and vibrational modes by Raman spectroscopy. The optical energy band gaps were investigated through UV–vis spectroscopy study. The surface morphology of the grown single crystals was analyzed by using Scanning Electron Microscope and thermal analysis was carried out by using thermogravimetric analysis. The electrical properties were also studied as a function of frequency and the obtained results are discussed.

36 MATERIALS SCIENCE↗