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  1. Creep-rupture behavior of alloy 740H weldment with alloy 263 filler metal.

    The creep-rupture behavior of weldments of alloy 740H fabricated using shielded metal arc welding with a commercially available filler metal based on alloy 263 and a post-weld heat treatment of 800 °C/4 h was studied at 650, 750, and 850 °C. Stress levels were chosen to reach extended rupture lifetimes (up to over 71,000 h) relevant for long-term applications and pressure vessels and piping code qualifications. All ruptures occurred within the weld zones of the cross-weld specimens except for one case at 850 °C for which the ruptured region covered both the weld and heat-affected zone. The effect of the welding process on creep lifetimemore » was quantitatively evaluated using weld strength reduction factors (WSRFs) which represented, for a given rupture time and temperature, the ratio of the applied creep-rupture stress of the weldment to that of alloy 740H base metal. These factors were 0.78-0.88, 0.82-0.89, and 0.64-0.75 at 650, 750 and 850 °C, respectively. Accordingly, with two exceptions at 850 °C with lower applied stresses, the creep failures were attributed to the lower strength of the weld zone relative to the alloy 740H base metal. Importantly, the failure location and WSRF depended on the microconstituents, microstructure, and stabilities of the weld and base metals at the creep temperatures, rather than welding-induced chemical inhomogeneities or defects. The weld strength reduction of these weldments was very similar to the expected ratio of creep-rupture strength of alloy 263 to that of alloy 740H.« less
  2. Flash electropolishing for TEM: Reducing FIB-induced defects in tungsten with protocols for new materials

    Focused ion beam (FIB) milling has become the dominant approach for site-specific transmission electron microscopy (TEM) specimen preparation; however, FIB damage remains a critical limitation for reliable microstructural characterisation, particularly in radiation effects studies. Tungsten is especially susceptible to FIB damage due to its high nuclear stopping power, which promotes the formation and strong diffraction contrast of FIB-induced ‘black spot’ defects that are indistinguishable from very fine irradiation-induced loops/defects resulting from low to intermediate temperature neutron irradiation. In this work, flash electropolishing is systematically evaluated as a post-FIB treatment for minimising preparation-induced artefacts for TEM analysis of tungsten-based alloys. Usingmore » a range of non-, ion-, and neutron-irradiated tungsten materials, the effectiveness of flash electropolishing has been assessed through direct comparison with conventional FIB and plasma-FIB preparation including low-energy Ga, Ar, Xe ion cleaning. The results demonstrate that flash electropolishing effectively removes FIB-damaged layers and ‘black spot’ defects, thereby enabling reliable observation of irradiation-induced dislocation structures. Key processing parameters governing flash electropolishing quality – including lamella thickness, applied voltage, polishing duration, electrolyte chemistry, and cathode geometry – have been systematically evaluated, and clear criteria were established for determining when flash electropolishing is required to ensure reliable microstructural analysis. This work also provides practical guidance for implementing flash electropolishing as an artefact-controlled specimen-preparation approach for TEM characterisation of FIB-produced specimens. The systematic protocol can be extended to other, non-tungsten materials.« less
  3. In-service corrosion and grain boundary oxidation in neutron-irradiated 316 stainless steel baffle-former bolts

    Reactor core internal components such as baffle-former bolts (BFBs) are subjected to significant mechanical stress, corrosive environment, and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and of the bolts. In this work, characterization was performed on the oxidized surface of stainless steel BFBs harvested from a commercial pressurized water reactor (PWR) after 40 years of operation. The analysis shows that a complex multilayered surface oxide with six identified layers formed that is different from 2-layer structure commonly observed in model experiments. The oxide varies by compositionmore » – predominantly Fe, Cr, and Ni, grain size, and phase, and has features resembling both unirradiated and radiation/ corrosion experiments likely due to the low radiation flux compared to ion-irradiation or the test reactor radiation. In addition, grain boundary oxidative attack featured a pathway for Fe and other elements to move from the metal matrix to the outermost oxide. In conclusion, the results help assess PWR lifetime extension, put into context previous experimental studies, and provide input for designing experiments combining radiation and corrosion effects.« less
  4. Strength and ductility of additively manufactured 316L stainless steel: Impact of neutron irradiation and data variability

    Here, this article presents the mechanical properties of additively manufactured (AM) 316L stainless steel processed via the laser powder bed fusion (LPBF) method, focusing on the effects of neutron irradiation on mechanical properties and the variability in strength and ductility data. The rapid melting-solidification process and multiple heating-cooling cycles inherent in LPBF typically result in a fine, metastable microstructure with significant local variability. AM 316L builds of varying thicknesses were fabricated, and SS-J3 miniature tensile specimens were machined from six different locations. These specimens were irradiated with fast neutrons to doses of 2 and 10 dpa at target temperatures ofmore » 300 °C and 600 °C. Post-irradiation tensile tests were conducted at room temperature, 300 °C, and 600 °C. Compared to conventional 316L stainless steel, AM 316L exhibited higher initial strength but lower ductility. Irradiation at 300 °C caused significant hardening and prompt necking at yield, with limited uniform ductility, although embrittlement was not observed up to 10 dpa. While neutron irradiation, particularly at 600 °C, increased the variability in strength and ductility data, no clear dependence of mechanical properties on build thickness or sampling location was found—contrary to the conventional perception that AM materials may exhibit high property variability. Furthermore, we observed that the variability in property data for LPBF-processed 316L was relatively low compared to that of wrought 316L stainless steel. This reduced variability in AM 316L steel may be attributed to its highly metastable, stress-containing microstructure, which is discussed in the context of general tensile property variations.« less
  5. Impact of post-irradiation annealing on mechanical performance of irradiated 718 alloy

    Here, the effect of post-irradiation annealing on solution-annealed 718 alloy was investigated using advanced mechanical testing, fractography, scanning electron microscopy, and transmission electron microscopy. Specimens were extracted from a proton beam window operated at the Spallation Neutron Source, irradiated with 940 MeV protons to a maximum dose of approximately 9.7 displacements per atom (dpa) at a calculated temperature not exceeding 110 °C while in service. Helium and hydrogen concentrations reached about 1700 and 6900 atomic parts per million (appm), respectively. Despite irradiation and high tensile strength (yield stress over 1 GPa), the material exhibited significant ductility. Annealing at 500 °C,more » 700 °C, and 900 °C for 30 min resulted in an appreciable decrease in yield strength and an increase in ductility for annealing treatments at 500 °C and 900 °C relative to the strength and ductility of the as-irradiated material. The presence of helium and hydrogen led to cavity formation and cleavage-like brittle features on fractured surfaces; however, high-magnification imaging revealed the presence of small-scale ductile dimples, indicating that the fracture mechanism remained mixed. The annealed specimens retained total elongation levels of 14–33 %, and there was no sudden drop in ductility after heat treatments. The ductility level in the irradiated and annealed material is notable despite the presence of helium and hydrogen.« less
  6. Creep performance and microstructure of grade 91 steel weldments with integrated welding and thermal processing

    Ferritic-Martensitic steel welds typically require post weld heat treatment (PWHT) to restore toughness and high temperature performance. This off-line thermal process reduces disparities between weld and base metal, but can cause distortion, cracking, or simply be impractical due to assembly size and joint non-uniformity. Here we show integrated welding and thermal processing applied to modified 9Cr-1Mo (Grade 91) steel, favored for advanced power generation applications, performed in real time through the addition of a secondary heat source near the primary weld head. Optimal integrated processing reduces weld fusion and heat affected zone hardness by 125 HV, approaching performance of conventionalmore » 730 °C, 60 min PWHT processing. Microstructures and mechanical performance are compared for mechanized GTAW welds, with equivalent lifetimes noted in cross-weld creep rupture tests up to 234 MPa at 550 °C, and up to 104 MPa at 650 °C. The integrated process was validated on a Grade 91 pressure vessel with multipass cold wire feed GTAW. After 550 °C, 71.4 bar thermomechanical cyclic testing, the maximum weld hardness is <350 HV.« less
  7. Microstructure, stored energy, and stability of H/He-filled nanocavities in low temperature irradiated Inconel 718

    The microstructure, trapped transmutation gases, stored energy, and mechanical behavior of samples from an irradiated Inconel 718 proton beam window were characterized using transmission electron microcopy, thermal desorption spectrometry (TDS), differential scanning calorimetry (DSC), and tensile testing. In the as-irradiated condition the microstructure contained a high number density of 1–3 nm gas-filled nanocavities. Emissions of trapped gases, H and He, during TDS correlated with peaks of the energy release curves from DSC examinations, which suggest these gases were likely stored in highly stable defect traps. The stored energy from radiation damage saturated at doses of a few dpa and didmore » not increase with increasing radiation dose, but the amount of stored H and He increased with increasing dose. Effects of post-irradiation annealing were studied as well. After exposure to 700 °C, the nanocavities grew only slightly to 2–4 nm in diameter, but after exposure to 900 °C, the cavities grew to 10–20 nm in diameter and electron energy-loss spectroscopy showed these cavities contained a core of He surrounded by a shell of H. Further, this study demonstrated that the irradiation defect structures containing H and He were remarkably stable during irradiation and after exposure up to 700 °C. The effect of the irradiation temperature, defect mobility, and interaction of H, He, and irradiation defects on mechanical behavior provides insight into the processes responsible for the unusual recovery in ductility with increasing radiation dose observed in Inconel 718 after high energy proton and spallation neutron irradiation.« less
  8. Understanding and removing FIB artifacts in metallic TEM samples using flash electropolishing

    Focused ion beam methods have often become a de facto choice for metallic materials that could also be easily electropolished. FIB preparation of TEM samples is widely used for radioactive materials, since the site specificity, coupled with the minuscule volume of material used for the TEM sample, can produce TEM samples with minimal to no detectable radioactivity. FIB preparation has problems however, as evidenced by artifacts such the subsurface black spots (clusters of vacancies and/or interstitials), dislocations, amorphous layers and phase changes, and must be accounted for when conducting TEM experiments. This study has two main objectives, first, presenting evidencemore » on two types of surface artifacts (moiré fringes and surface dislocations) observed in FIB prepared Fe-Cr alloys and pure Fe. This evidence will include similar artifacts produced in ferritic based systems using two other ion sputtering techniques: conventional Ar+ ion milling with a Gatan PIPS®, and an Ar+ based Fischione NanoMill®. The second objective documents our method of removing all of the FIB artifacts using flash electropolishing (FEP) of FIB TEM lamella, demonstrating our success in producing electropolished FIB lamella from an FeCr HT-9 alloy free of both the subsurface and surface artifacts. With the proper choice of parameters, TEM samples from FeCr alloys are comparable to those prepared by jet polishing of bulk TEM samples. These comparisons between FIB prepared and FEP FIB samples are done using both TEM imaging and diffraction contrast imaging STEM (DCI-STEM) on samples from an unirradiated and neutron irradiated Fe-Cr alloy. The observed black spot damage, moiré fringes and surface dislocations in the ion beam prepared samples are discussed in terms of how they could impact the microstructural analysis of irradiated metals.« less
  9. Characterization of the microstructure of yttrium hydride under proton irradiation

    High moderation per unit volume solid moderator materials like yttrium hydride (YHx) are necessary for compact nuclear microreactors. However, the phase stability and hydrogen transport processes of YHx under high-temperature irradiation are largely unknown. Proton irradiation was conducted on YHx at 300 °C and 580 °C to 0.2 dpa using 1 MeV or 2 MeV protons in a high-vacuum environment. The hydrogen concentration was determined before and after irradiation using elastic recoil detection analysis, and microstructural evolution was examined via post-irradiation scanning transmission electron microscopy and Raman spectroscopy. Dislocation loops and cavities were observed in all conditions; their distribution wasmore » correlated with the bombarding proton energy and ion irradiation temperature. This work revealed that hydrogen retention is proportional to the formation of traps for hydrogen gas atoms and identified pathways for hydrogen release. The relative contributions of bulk or fast diffusion paths, such as grain boundaries, delamination boundaries, and stacking faults are discussed; the primary mechanisms of hydrogen loss are likely based on diffusion, ruling out artefacts of the experimental design. In conclusion, the study suggests proton irradiation may be a strong surrogate to study hydrogen transport in hydride moderator materials under irradiation.« less
  10. Complexity of segregation behavior at localized deformation sites formed while in service in a 316 stainless steel baffle-former bolt

    Here, post-irradiation evaluation was performed on a 316 stainless steel baffle former bolt harvested after 40 years of service in a pressurized water reactor. Microstructure analysis revealed the presence of defect-free dislocation channels and strain-induced twins, indicative of loading at a stress level close to yield stress at least once while in service. Primary radiation-induced Ni/Si precipitates were destroyed during channel and twin formation, and secondary, significantly coarser Ni/Si precipitates formed along newly formed Σ3 boundaries during the continued irradiation. Additionally, an elevated phosphorus level was observed inside the strain-induced twin. Complex chemistry inside the strain-induced feature may overlap withmore » dislocation pileups and impact localized corrosion, material long-term performance, and safety.« less
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