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Tailoring Carbide Dispersed Steels: A Path to Increased Strength and Hydrogen Tolerance
The use of transition metal carbides is reported for use as a hydrogen trapping mechanism for ferritic and austenitic steel materials. The program combined computational modeling and simulations to guide experiments towards candidate metal carbide traps, both for interfacial and interior trapping. It was found that interfacial trapping is less effective than interior trapping, with the group IVB transition metal carbides being the most effect internal traps with a loss of carbon. The sub-stoichiometric rocksalt structure accommodate the hydrogen atoms in its octahedral interstices. Using percolation theory, carbon loss of approximately 25% or more was sufficient to ensure an interconnected network of vacancies for such trapping from the surface to the internal sites within the carbide. Using this as a guide, the program developed a means to provide a uniform dispersion of ZrC nanoparticles with either Fe or 304L micron-scale powders which was then consolidated by direct current sintering. Electrolytic hydrogen diffusivity studies confirmed the reduction of hydrogen diffusion in the matrix with increasing ZrC content, which was a linear response over the sample range studied (0.01 to 1.0 wt.%). The consolidated material was micro-tensile tested in either a non-hydrogen or hydrogen charge condition and compared to a control with no carbides. Additions up to 0.05 wt.% ZrC increased the yield strength with no loss in ductility in either the non-hydrogen or hydrogen tested condition. ZrC concentrations above this amount further increased the yield strength at the expense of ductility. While these samples had a lower absolute ductility value prior to failure, the relative change in ductility between the non-hydrogen and hydrogen charge states was less for the carbides than that of the control. Metal-rich ZrC nanoparticles were fabricated through a conformal coating process yielding ZrC0.66 particles that were then incorporated into a metal matrix. Notch fatigue testing in a hydrogen environment was conducted where the number of cycles to failure was found to be less in the control than that of the carbide addition. However, the spread in experimental data and the number of samples tested limits a conclusive outcome based on defects noticed in the gauge section of all the powder processed samples. The collective outcomes of this report provide further insight into the mechanisms by which carbides act as hydrogen traps; a means to process such carbides through powder metallurgy; and their associated mechanical performance in either a non-hydrogen or hydrogen-charged condition.
Brittle-ductile transitions in a metallic glass
Recent computational and laboratory experiments have shown that brittle-ductile transitions in the notch toughnesses of metallic glasses such as Vitreloy 1 are strongly sensitive to the initial effective disorder (or “fictive”) temperature. Glasses with lower effective temperatures are weak and brittle; those with higher effective temperatures are strong and ductile. The analysis of this phenomenon presented here examines the onset of fracture at the tip of a notch as predicted by the shear-transformation-zone theory of spatially varying plastic deformation. The central ingredient of this analysis is an approximation for the dynamics of the plastic zone formed by stress concentration at the notch tip. As a result, this zone first shields the tip but then, with increasing stress, expands suddenly, producing a discontinuous transition between brittle and ductile failure in satisfactory agreement with the numerical and experimental observations.
Robust Dissimilar Metal Friction Welded Spool for Enhanced Capability for Steam Power Components (Final Program Report)
This project successfully demonstrated the feasibility and advantages of producing durable, friction-welded dissimilar-metal spools, both with and without transition pieces, as well as the use of advanced oxidation-protective coatings for steam power applications. The work encompassed the optimization and full-scale production of NFA tubing, overcoming manufacturing and processing challenges to achieve enhanced strength, creep, and fatigue properties validated by extensive microstructural characterization. Optimized welding techniques were developed and refined for joining dissimilar materials, resulting in defect-free welds optimized for both low- and high-pressure boiler circuits. Systematic evaluation of welding parameters, coupled with heat treatments, ensured reliable performance and minimized weld defects such as banding and cracking. Comprehensive mechanical and non-destructive testing, including tensile, bend, fatigue, and CT scanning, confirmed the superior integrity and durability of the friction-welded joints under representative service conditions. To address oxidation-related degradation, a range of protective alloy coatings—such as IN625, APMT, Duplex 2507, and FeCrAlY—were selected and evaluated for their ability to counteract oxide notch formation at dissimilar metal interfaces. These coatings demonstrated improved oxidation resistance and long-term stability under thermal cycling, thereby extending weld service life. Thermal cyclic testing and long-term studies captured the phase stability and diffusion behavior of coated and uncoated configurations. Validated models for low-cycle fatigue (LCF), creep, and thermal mechanical fatigue (TMF) were developed to predict component life and failure modes. These models confirmed that friction-welded configurations exhibited significantly enhanced performance compared to conventional gas-tungsten arc welding (GTAW), with up to 7× improvement in creep resistance and at least 2× enhancement in fatigue properties. The introduction of a tailored transition piece further reduced thermally induced strains, enhancing fatigue life. The results demonstrate a robust pathway for retrofitting existing steam fleet components and upgrading future equipment to deliver substantially improved cold-start cycling behavior and reduction of unplanned outages due to premature weld failures.
Effects of Notches on the Intermediate Creep-Rupture Life of Alloy 617 Weldment
A Code Case has recently been completed that adds Alloy 617 to Section III, Division 5 of the American Society of Mechanical Engineers Boiler and Pressure Vessel Code, which covers high temperature nuclear components. However, additional information is needed to address concerns raised by the Nuclear Regulatory Commission that are not covered by the Code Case. The effects of notches (geometric discontinuities) and multiaxial stress on the expected creep life of a component are among these concerns. This report covers the current state of testing of Alloy 617 notched specimens at Idaho National Laboratory, with particular focus on intermediate length (8,000 – 20,000 hours) creep tests of Alloy 617 weld metal. While most of this testing is ongoing, the current state of the tests indicate that the multi-axial stress state imposed by the notch geometry does not negatively impact the creep rupture life of the Alloy 617 weld metal. While the weld metal is notch strengthening in short-term (1,000 – 2,000 hours) testing, it is not clear if this characteristic will continue to hold for intermediate and long-term testing. Ongoing tests will provide additional information to address this concern of a crossover from notch strengthening to notch weakening for intermediate and long-term creep lives.
Assessment of Different Approaches for Measuring Shear Fracture Appearance in Charpy Tests
In this work, different approaches for establishing shear fracture appearance (SFA) on tested Charpy specimens were assessed and compared, namely (in order of increasing expected accuracy) estimates based on characteristic forces from instrumented Charpy tests, optical measurements using image analysis software, and measurements performed with the aid of a scanning electron microscope. Comparisons between different SFA values for 129 instrumented Charpy tests currently included in the National Institute of Standards and Technology database allowed us to establish the relationships between the different available approaches and formulate recommendations for the revision of the standards ASTM E2298-18, Standard Test Method for Instrumented Impact Testing of Metallic Materials, and ISO 14556:2015, Metallic Materials — Charpy V-Notch Pendulum Impact Test — Instrumented Test Method, which currently provide four empirical correlations that can be used to estimate SFA.
Thermal Frequency Drift of 3D Printed Microwave Components
Fabrication of microwave slot array antennas and waveguide bandpass and notch filters using 3D printing has significant advantages in terms of speed and cost even for parts with high mechanical complexity. One disadvantage of Stereolithography (SLA) 3D printed, copper plated microwave components is that some SLA resins have a high Coefficient of Thermal Expansion (CTE), quoted in micrometers per meter per degree or 10 -6 per degree. Compared to typically used metals such as aluminum (CTE 24 × 10 -6 ·K -1 ) and copper (CTE 17 × 10 -6 ·K -1 ), SLA resin can have CTE above 100 × 10 -6 ·K -1 . Resonant structures experience significant frequency drift with temperature changes on the order of 10–50 °C. The issue of 3D printed microwave structures changing frequency characteristics significantly with temperature shift has not been addressed or reviewed in current literature. We measured and simulated the effect of temperature change on a slot array, cavity notch filters, and post loaded waveguide bandpass filters. We tested several types of SLA resin, different plating techniques, and also Direct Metal Laser Sintering (DMLS) and Binder Infusion metal 3D printing. Performance as a function of temperature is presented for these alternatives.
Testing Protocol Development for the Fracture Toughness of Parts Built with Big Area Additive Manufacturing
The mechanical testing of additively manufactured parts has largely relied on the existing standards developed for traditional manufacturing. While this approach leverages the investment made in current standards development, it inaccurately assumes that the mechanical response of additive manufacturing (AM) parts is identical to that of parts manufactured through traditional processes. When considering thermoplastic, material extrusion AM, the differences in response can be attributed to an AM part’s inherent inhomogeneity caused by porosity, interlayer zones, and surface texture. Additionally, the interlayer bonding of parts printed with large-scale AM is difficult to adequately assess, as much testing is performed such that stress is distributed across many layer interfaces; therefore, the lack of AM-specific standards to assess interlayer bonding is a significant research gap. To quantify interlayer bonding via fracture toughness, double cantilever beam (DCB) testing has been used for some AM materials, and DCB has been generally used for a variety of materials including metal, wood, and laminates. Mode I DCB testing was performed on thermoplastic matrix composites printed with Big Area Additive Manufacturing (BAAM). Of particular interest was the notch shape and deflection speed during testing. The results examine the differences when using two notch types and three deflection speeds. The testing method introduced by the following paper differentiates itself from the ones described in the standards used by modernizing the methodology. This was conducted with the introduction of Digital Image Correlation (DIC) to gather displacement and load data simultaneously without human intervention.
Pyrolysis Vacuum-Assisted Plasma Ionization Ion Mobility–Mass Spectrometry for Insoluble Polymer Analysis
Wire-based metal additive manufacturing utilizes the ability of additive manufacturing to fabricate complex geometries with high deposition rates (above 7 kg/h), thus finding applications in the fabrication of large-scale components, such as stamping dies. Traditionally, the workhorse materials for stamping dies have been martensitic steels. However, the complex thermal gyrations induced during additive manufacturing can cause the evolution of an inhomogeneous microstructure, which leads to a significant scatter in the mechanical properties, especially the toughness. Therefore, to understand these phenomena, arc-based additive AISI 410 samples were fabricated using robotic gas metal arc welding (GMAW) and were subjected to a detailed characterization campaign. The results show significant scatter in the tensile properties as well as Charpy V-notch impact toughness data, which was then correlated to the microstructural heterogeneity and delta (δ) ferrite formation. Post-processing (austenitizing and tempering) treatments were developed and an ~70% reduction in the scatter of tensile data and a four-times improvement in the toughness were obtained. The changes in mechanical properties were rationalized based on the microstructure evolution during additive manufacturing. Based on these, an outline to tailor the composition of “printable” steels for tooling with isotropic and uniform mechanical properties is presented and discussed.
Mitigating Scatter in Mechanical Properties in AISI 410 Fabricated via Arc-Based Additive Manufacturing Process
Wire-based metal additive manufacturing utilizes the ability of additive manufacturing to fabricate complex geometries with high deposition rates (above 7 kg/h), thus finding applications in the fabrication of large-scale components, such as stamping dies. Traditionally, the workhorse materials for stamping dies have been martensitic steels. However, the complex thermal gyrations induced during additive manufacturing can cause the evolution of an inhomogeneous microstructure, which leads to a significant scatter in the mechanical properties, especially the toughness. Therefore, to understand these phenomena, arc-based additive AISI 410 samples were fabricated using robotic gas metal arc welding (GMAW) and were subjected to a detailed characterization campaign. The results show significant scatter in the tensile properties as well as Charpy V-notch impact toughness data, which was then correlated to the microstructural heterogeneity and delta (δ) ferrite formation. Post-processing (austenitizing and tempering) treatments were developed and an ~70% reduction in the scatter of tensile data and a four-times improvement in the toughness were obtained. The changes in mechanical properties were rationalized based on the microstructure evolution during additive manufacturing. Based on these, an outline to tailor the composition of “printable” steels for tooling with isotropic and uniform mechanical properties is presented and discussed.
Effects of Geometric Discontinuities on Creep Behavior of Alloy 617
Due to the excellent long-term high-temperature performance of Alloy 617, the Alloy has been identified as the primary structural material for the intermediate heat exchanger of the Very High Temperature Reactor (VHTR). Both the base and welded alloy has been qualified to be used up to 950 °C up to 100,000 hours by the American Society of Mechanical Engineer (ASME) Boiler and Pressure Vessel Code (BPVC). The qualification properties of the material were exclusively determined by uniaxial creep tests. The components may, however, experience multiaxial stress conditions in service due to the reactor geometry. This study used notched creep tests to investigate the effect of geometric discontinuities on creep behavior of both the base and welded Alloy 617. The V-notch tests reveal that the geometric discontinuities do not reduce the creep rupture live under high and intermediate stress conditions. The U-notch tests show that a larger radius notch behave in a similar way as a straight gauge section of a uniaxial test. The creep rupture live of the welded alloy was slightly longer than the base metal.
12.5 kV GaN Super-Heterojunction Schottky Barrier Diodes
In this work, we report GaN super-heterojunction Schottky barrier diodes (SHJ-SBDs) with substantially improved performance. Metal-2DEG sidewall n-ohmic contacts were deployed to achieve low contact resistance of 0.75 Ω · mm, avoiding the risk of abnormally high contact resistance caused by inaccurate etch depth control. A pGaN notch formed near the cathode successfully eliminated excessive hole conduction caused by the sidewall n-ohmic contact. Isolation was improved by a high-energy Al implantation step. The resulting SHJ-SBD exhibited a breakdown voltage (BV) of 12.5 kV and a specific ON-resistance of 100.8 mΩ · cm 2 .
Comprehensive Toughness Dataset of Nuclear Reactor Structural Materials using Charpy V-Notch Impact Testing
Not Available
CHARACTERIZATION OF FATIGUE BEHAVIORS OF NOTCHED 316L DED AM SPECIMENS
ASME Codification of Additive Manufacturing • Integration of AM into ASME Codes and Standards • The ASME goal is to have AM requirements in ASME Code Cases preceding the 2025 Edition. • The ASME Special Committee on AM has drafted criteria for two Code Cases for Additive Manufacturing. • AM Construction of Pressure Equipment using the Direct Energy Deposition Process with Wire Feedstock. • Includes Gas Metal Arc Welding. • Time-independent material properties. • Status - Criteria endorsed by AM Committee. • AM Construction of Pressure Equipment using the Powder Bed Fusion AM Process. • Includes Laser and Electron Beam Energy Sources. • Austenitic and Nonferrous materials. • Time-independent material properties. • Status – Approval ballot circulating to the AM Committee.
2019 accomplishments: degradation of mechanical properties in structural metals and welds for FTS reservoirs
This report documents work in 2019 at SRNL in support of the Aging and Lifetimes program. Specimens for fracture toughness testing were prepared in prior years by thermally pre-charging samples, provided by Sandia National Laboratories, of welded types 304L and 21-6-9 stainless steels. These samples were pre-charged in 2017. The fracture toughness of the first aged specimens was measured and compared to historical data. The measurements of the 304L and 21-6-9 weld and particularly HAZ represent some of the first fracture data relevant to modern GTS reservoirs. This work represents an on-going collaboration between SRNL and SNL to understand tritium embrittlement of structural metals in Gas Transfer System reservoirs which informs lifetime assessments. Continued testing was conducted on ongoing historical studies, including the effects of very long-term aging, and the relative performance of differently forged stockpile relevant 304L and 316L samples. New samples were pre-charged with tritium and placed in a freezer for an aging study to allow helium to build into the material. The precharged samples consist of smooth and notched tensile samples of 304L stainless steel, as well as tube tensile samples of different thermal treatments supplied by Sandia National Laboratories. Their charging marks the beginning of a new sequence of studies to explore fundamental deformation mechanisms underpinning tritium embrittlement. At predesignated times, samples will be removed from aging and tested to provide data which will help develop an understanding of material degradation with increasing aging time. Also documented is progress in employing various advanced characterization techniques including high resolution electron microscopy, thermally programed desorption, and small angle x-ray scattering, as well as facilities renovations and equipment procurements in support of sustained tritium impacts on materials program at SRNL.
Porous CeO 2 /CuO Heterostructure for Efficient Hydrogen Evolution Reaction in an Acidic Medium
A composite electrocatalyst CeO 2 /CuO is fabricated for the hydrogen evolution reaction (HER) via a simple, facile, one‐step hydrothermal method, using F‐127 as a template and structure directing agent. The prepared composite CeO 2 /CuO shows top‐notch HER activities with a small overpotential of 98 mV at 10 mA cm −2 and just 160 mV overpotential to attain a current density of 50 mA cm −2 with good stability for 20 h in an acidic medium. The enhanced catalytic activities of CeO 2 /CuO nanocomposite are attributed to their synergetic interface interaction, which lead to improved conductivity, reactive sites, and oxygen vacancies in their lattices. This study aims to advance the development of earth‐abundant transition metal oxides–based electrocatalysts as economical, durable, and efficient HER electrocatalysts to replace noble metal–based materials in the future.
Multiscale dynamic experiments on fiber-reinforced composites with damage assessment using high-speed synchrotron X-ray phase-contrast imaging
We report fiber-reinforced composites (FRCs) have been widely used as protection materials to replace heavier metals. However, predictive capabilities for the impact-induced failure of FRCs have not been well-developed. In this work, we introduced an integrated technique to visualize the dynamic failure of FRCs, with the modified Kolsky bar loading and the high-speed synchrotron X-ray phase-contrast imaging (PCI). We summarize our experimental studies across the FRCs’ structural levels by using this integrated technique, including single-fiber tensile experiments, fiber/matrix debonding experiments, and single-edge notched bending experiments on composite laminates. It is revealed that the high-speed synchrotron X-ray PCI technique possesses sufficient spatial resolution to identify the failure behavior of a single fiber in the 10-μm scale level, as well as temporal resolution to identify the time sequence of internal dynamic damage evolution. The technique can penetrate through the opaque composite sample and provide real-time visualization of small-scale damaging mechanisms such as the embedded fiber’s sliding in the matrix and the fiber’s transverse debonding with the matrix. At an expanding scale, the technique can identify the crack initiation and track the cracking behavior inside a single ply or between different plies of a composite laminate. High-speed visualization inside the material by this integrated technique provides critical deformation and failure information to develop physical understanding of the damage inside composites under impact.
Intrinsic and extrinsic effects on the fracture toughness of ductile metallic glasses
The potential application of metallic glasses (MGs) as structural materials demands accurate measurements of their toughness and the understanding of the underlying factors affecting it. Currently, it is challenging to precisely measure the toughness of MGs, especially ductile MGs. Measured toughness values are widely scattered, even for MGs with identical compositions. That is attributed to the combined effect of intrinsic and extrinsic factors including processing, sample geometries, and loading conditions. A fundamental understanding of the influences of these elements is thus of great significance. In the present study, molecular dynamics simulations are performed to investigate the influence of intrinsic and extrinsic effects on the fracture toughness of CuZr MGs. In particular, focused is placed on the effects of cooling rate, notch shape and size, strain rate, and temperature. The results indicate that the fracture toughness of a MG scales with the cooling rate used to prepare it. This is attributed to increased free volume content generated at high cooling rates, which enhances plastic deformation and amplifies the associated energy dissipation during plastic deformation events. Fracture toughness also increases with the strain rate, arguably due to strain rate-induced crack extension delay. Overall, the results demonstrate that the largest fracture toughness are achieved when MG samples are fabricated at high cooling rates and subjected to high strain rate deformation. In addition, results suggest that the fracture toughness decreases with increasing temperature, due to the significant decrease in strength. Here, the correlations revealed between these crucial intrinsic and extrinsic parameters and the calculated MG fracture toughness support the development of a framework to understand the root of the discrepancies in the measurement of the toughness of MGs and provide insights into the design of tough MGs for structural applications.