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At least 19 records

Microstructural characterization of cold-worked 316 stainless steel flux thimble tubes irradiated up to 100 dpa in a commercial Pressurized Water Reactor

Two flux thimble tubes (FTT) made of 15% cold-worked 316 stainless steel (SS) were harvested from Ringhals Pressurized Water Reactor (PWR) Unit 2, with peak damages of 76 and 100 displacements per atom (dpa) after 29 and 34 years’ service, respectively. Specimens sectioned from parent tubes were comprehensively characterized with nominal damage levels of ~0, ~41, ~74, 76, and 100 dpa at a nominal temperature range of 285-323 °C. Both FTTs contained helium and hydrogen gases as transmutation products. The helium follows a production rate of ~9.8 appm/dpa, while environmental factors complicate hydrogen production obscuring an exact H/dpa ratio. Irradiation-induced dislocation loops, nano-cavities, solute clusters, and microsegregation were all observed. The dislocation loops and nano-cavities indicated saturation at 41 dpa. The solute clusters continued to evolve with Ni-Si clusters formed at 41 dpa, and Ni-Si-Mn-P clusters formed at 74 and 100 dpa, but neither clusters exhibited distinct diffraction patterns at any damage levels. Solute clusters were observed to frequently be co-located with dislocation loops, but fully decorated loops were rarely detected. Significant radiation-induced segregation (RIS) was observed around grain boundaries at all damage levels. The modified inverse Kirkendall (MIK) model captured the RIS behavior of major elements. Large cavities within or around an Mn-S rich region were observed for the first time. Through all the damage levels, void swelling is always below 0.05%, making significant dimensional change unlikely in core internals when used at similar conditions. Meanwhile, the role of overwhelming nanocavities, presumably helium bubbles, should be considered in other potential degradation mechanisms, including irradiation-assisted stress corrosion cracking, embrittlement, and loss of fracture toughness, which remain the concerns for extended operation of nuclear power plants.

Post Irradiation Examination, Isotope Dilution Mas↗

Deformation band corrosion as a result of applied stress and cold-work in 304 stainless steel in simulated pressurized water reactor primary water conditions

Stainless steels like 304SS are commonly used in pressurized water reactor primary water environments due to their excellent resistance to stress corrosion cracking (SCC). However, SCC susceptibility has been observed in cold-worked 304SS. Cold-rolling introduces a high density of defects, such as deformation bands or dislocations, into the microstructure; applied stress, even if macroscopically below the yield stress, can result in regions with high localized stresses. Cold-worked and non-cold-worked samples were exposed to 360 °C simulated PWR primary water for 1500 h with and without active loading. Corrosion susceptibility of dislocations and deformation bands induced by cold-rolling and/or applied stress was studied using high-resolution (analytical) transmission electron microscopy. Deformation bands were generated in all specimens examined in the study. Penetrative oxidation was observed in some deformation bands in each specimen. The depth of penetrative deformation band oxidation frequently exceeded the depth of grain boundary oxidation in all specimens. However, deformation band oxides generally were narrowly confined to the deformation band plane. Highly Ni-rich regions were observed beyond all oxidation fronts. Surface oxides were thicker in the specimens exposed under active loading. In conclusion, the implications of these findings at surfaces for deformation bands intersecting stress corrosion crack paths are discussed.

EFTEM↗

Unveiling the Interplay: Cold Work, Recrystallization, and Flux Expulsion in SRF Cavities

The fabrication of SRF cavities from sheet materials includes deep-drawing, electron beam welding, chemical and mechanical polishing, high-temperature heat treatment, and material diffusion. The performance of these cavities is frequently limited by magnetic flux trapping giving rise to additional rf loss. In this presentation, we thoroughly examine how recrystallization influences flux expulsion in SRF cavities, using cold-worked niobium sheets from various suppliers. Our findings reveal that cold-worked sheets enhance flux expulsion, especially at lower heat treatment temperatures, by promoting improved recrystallization. In particular, a traditionally fabricated Nb cavity half-cell from an annealed poly-crystalline Nb sheet after an 800 C heat treatment leads to a bi-modal microstructure that ties in with flux trapping and inefficient flux expulsion. This non-uniform microstructure is related to varying strain profiles along the cavity shape. A novel approach to prevent this non-uniform microstructure is presented by fabricating a 1.3 GHz single cell Nb cavities with a cold-worked sheet and subsequent heat treatment leading to better flux expulsion after 800 C/3h

Dhakal, P. [Old Dominion Univ., Norfolk, VA (Unite↗

Microstructure development in a cold worked SRF Nb sheet undergoing 700°C-900°C/3h heat treatments.

Bulk Nb for TESLA shaped SRF cavities is a mature technology, with high gradient (>35 MV/m) and high Q cavities (>1010, ~2K) routinely fabricated. Significant advances are in order to push Q?s to 1011 (~2K), and involve modifications to the sub-surface Nb layers by impurity doping (N, O). In order to achieve the lowest surface resistance any trapped flux needs to be expelled for cavities to reach high Q?s. There is clear evidence that cavities fabricated from polycrystalline sheets meeting current specifications require higher temperatures beyond 800oC leads to better flux expulsion, and hence improves Q. Recently, cavities fabricated with a non-traditional Nb sheet with initial cold work due to cold rolling expelled flux better after 800°C/3h heat treatment than cavities fabricated using fine-grain polycrystalline Nb sheets. Here, we analyze the microstructure development in Nb from the vendor supplied cold work non-annealed sheet that was fabricated into an SRF cavity as a function of heat treatment building upon the methodology development to analyze microstructure being developed by the FSU-MSU-UT-Austin- JLAB collaboration. The results indicate correlation between full recrystallization and better flux expulsion.

Balachandran, S.↗

Modification of Ni-20Cr corrosion dealloying behavior in molten fluorides via cold work induced plastic deformation

The corrosion dealloying behavior of cold-worked (CW) Ni20Cr alloy (wt%) was studied in molten LiF-NaF-KF (or FLiNaK) salts at 600 °C, equal to a homologous temperature (TH) of 0.52. Alloys were cold-rolled to achieve reductions of thickness of 10%, 30%, and 50% introducing plastic deformation and a high density of dislocations. Potentiostatic holds (Eapplied) were applied in two different electrode potential regimes. At 1.75VK+/K$${\text{V}}_{{\text{K}}^{+}/{\text{K}}}$$, Cr dealloying to Cr(II) and Cr(III) is predominant, while at 1.90 VK+/K$${\text{V}}_{{\text{K}}^{+}/{\text{K}}}$$, both Ni and Cr are oxidized in molten FLiNaK at 600 °C. In these potential regimes, dealloyed Ni20Cr displayed bicontinuous porosity within the grain interior and at grain boundaries, driven by the high driving force for Cr dissolution and sustained by defect mediated outward solid state diffusion of Cr in parallel with surface diffusion of Ni. The bicontinuous porous structure developed was observed to undergo further coarsening and densification of the Ni-rich ligaments at a higher electrode potential. The main effect of CW observed is the introduction of plastic deformation and dislocation substructures that serve as short-circuit paths for Cr solid state diffusion to surfaces exposed to FLiNaK. This modified the evolution of the bicontinuous porous structure which increased with CW substantially. Kinetic analysis reveals that the Cr dealloying at +1.75 VK+/K$${\text{V}}_{{\text{K}}^{+}/{\text{K}}}$$ and 1.90 VK+/K$${\text{V}}_{{\text{K}}^{+}/{\text{K}}}$$ is initially charge transfer controlled, except for the 50% CW condition at 1.90 VK+/K$${\text{V}}_{{\text{K}}^{+}/{\text{K}}}$$, where the process becomes limited by slow Cr defect mediated bulk diffusion. The rate determining factors are explored and compared to experimental results.

Chan, Ho Lun↗

MAGNETIC FLUX EXPULSION IN SUPERCONDUCTING RADIO-FREQUENCY NIOBIUM CAVITIES MADE FROM COLD WORKED NIOBIUM

Trapped residual magnetic field during the cool down of superconducting radio frequency (SRF) cavities is one of the primary sources of RF residual losses leading to lower quality factor. Historically, SRF cavities have been fabricated from high purity fine grain niobium with grain size ~50 to 100 µm as well as large grain with grain size of the order of few centimeters. Non-uniform recrystallization of fine-grain Nb cavities after the post fabrication heat treatment leads to higher flux trapping during the cool down, and hence the lower quality factor. We fabricated two 1.3 GHz single cell cavities from cold-worked niobium from different vendors and processed along with cavities made from SRF grade Nb. The flux expulsion and flux trapping sensitivity were measured after successive heat treatments in the range 800 to 1000°C. The flux expulsion from cold-worked fine-grain Nb cavities improves after 800°C/3h heat treatments and it becomes similar to that of standard fine-grain Nb cavities when the heat treatment temperature is higher than 900°C.

Khanal, B. D.↗

MAGNETIC FLUX EXPULSION IN SUPERCONDUCTING RADIO-FREQUENCY NIOBIUM CAVITIES MADE FROM COLD WORKED NIOBIUM

Trapped residual magnetic field during the cool down of superconducting radio frequency (SRF) cavities is one of the primary sources of RF residual losses leading to lower quality factor. Historically, SRF cavities have been fabricated from high purity fine grain niobium with grain size ~50 to 100 µm as well as large grain with grain size of the order of few centimeters. Non-uniform recrystallization of fine-grain Nb cavities after the post fabrication heat treatment leads to higher flux trapping during the cool down, and hence the lower quality factor. We fabricated two 1.3 GHz single cell cavities from cold-worked niobium from different vendors and processed along with cavities made from SRF grade Nb. The flux expulsion and flux trapping sensitivity were measured after successive heat treatments in the range 800 to 1000°C. The flux expulsion from cold-worked fine-grain Nb cavities improves after 800°C/3h heat treatments and it becomes similar to that of standard fine-grain Nb cavities when the heat treatment temperature is higher than 900°C.

Khanal, B. D.↗

Tradeoffs and Variability of Mechanical Properties in Cold Worked 21-9-6 Stainless Steel Bars

Sub-standard yield stress in a batch of 21-9-6 stainless steel (Nitronic 40) bars was observed while other batches passed requirements. This material requires enhanced property uniformity due to its application in critical components and therefore has tighter restrictions on alloying elements. Using tensile testing, this study investigates the distribution of yield and ductility across bar geometry for three lots of material and is corroborated alongside Vickers microhardness profiles.

Estrada, Micah Garnet Watson↗

Microstructural Engineering of Mn-Alloyed Austenitic Steel for Hydrogen Storage and Delivery

Austenitic stainless steels are commonly used for hydrogen storage and transportation. These alloys have a high nickel (Ni) content, which increases alloy cost. In this study, high manganese (Mn) austenitic alloys were evaluated as potential lower cost alternatives. Two heats of high Mn alloys with different stacking fault energies (SFE) of ~29 mJ·m -2 and 49 mJ·m -2 were acquired. Additionally, a new vanadium (V)-microalloyed high Mn alloy was designed to achieve a SFE of 47 mJ·m -2 to minimize planar slip deformation mechanisms. Post-processing via cold working in conjunction with aging was also performed on the V-microalloyed high Mn steel. Hydrogen embrittlement sensitivity was investigated using circumferential notch tensile specimens cathodically charged with hydrogen in a 0.05M NaOH electrolytic solution. The alloys were compared to a cold-worked 316L stainless steel, which exhibited no strength loss due to hydrogen. The high Mn alloys with SFE of ~29 mJ·m 2 and 49 mJ·m -2 had notch strength losses of 11 and 6 pct, respectively. The V-microalloyed high Mn steel in the as-hot-rolled condition had a notch strength loss of 17 pct. Furthermore, the V-microalloyed high Mn steel in the cold worked and aged condition indicated no notch strength loss in hydrogen, which was comparable to the performance of the 316L stainless steel.

36 MATERIALS SCIENCE↗

Magnetic properties of equiatomic CrMnFeCoNi

Magnetic, specific heat, and structural properties of the equiatomic Cantor alloy system are reported for temperatures between 5 and 300 K, and up to fields of 70 kOe. Here magnetization measurements performed on as-cast, annealed, and cold-worked samples reveal a strong processing history dependence and that high-temperature annealing after cold working does not restore the alloy to a “pristine” state. Measurements on known precipitates show that the two transitions, detected at 43 and 85 K, are intrinsic to the Cantor alloy and not the result of an impurity phase. Experimental and ab initio density functional theory computational results suggest that these transitions are a weak ferrimagnetic transition and a spin-glass-like transition, respectively, and magnetic and specific heat measurements provide evidence of significant Stoner enhancement and electron-electron interactions within the material.

36 MATERIALS SCIENCE↗

EVALUATION OF FLUX EXPULSION AND FLUX TRAPPING SENSITIVITY OF SRF CAVITIES FABRICATED FROM COLDWORK NB SHEET WITH SUCCESSIVE HEAT TREATMENT

The main source of RF losses leading to lower quality factor of SRF cavities is due to the residual magnetic flux trapped during cooldown. The loss due to flux trapping is more pronounced for cavities subjected to impurities doping. The flux trapping and its sensitivity to rf losses are related to several intrinsic and extrinsic phenomena. To elucidate the effect of recrystallization by high temperature heat treatment on the flux trapping sensitivity, we have fabricated two 1.3 GHz single cell cavities from cold-worked Nb sheets and compared with cavities made from standard fine-grain Nb. Flux expulsion ratio and flux trapping sensitivity were measured after successive high temperature heat treatments as well as after low temperature, 120 0C baking. The cavity made from cold worked Nb showed better performance after 800 0C/3hr heat treatment and similar behavior when heat treated with additional 900 0C and 1000 0C compared to standard fine-grain Nb cavity. In this contribution, we present the summary of flux expulsion, trapping sensitivity and results from RF tests at 2 K.

Khanal, Bashu↗

The effect of heat treatment on the defect evolution in LPBF 316H stainless steel

This work investigates the effect of processing and heat treatment on defect evolution and irradiation response of laser powder bed fusion (LPBF) 316H stainless steel, with comparisons to LPBF 316L and wrought 316L/316H. Using in-situ and ex-situ ion irradiations across a wide parameter space—temperature (300–675 °C), dose (0.2–25 dpa), dose rate (10 -3 –10 -5 dpa/s), and helium co-implantation (20–2500 appm)—we correlated void swelling, dislocation loop evolution, and segregation behavior with pre-irradiation microstructures (as-built, stress-relieved, solution-annealed, and cold-worked). Results show that swelling is strongly controlled by dislocation density: intermediate densities maximize swelling, while solution annealing or cold working reduce susceptibility to levels comparable to wrought alloys. Low dose rates and helium both promote cavity nucleation and lower the incubation barrier, with helium suppressing the role of dislocation density and driving swelling behavior toward wrought-like response. Loop evolution in SA LPBF 316H resembles wrought 316L but shows localized denuded zones near low-angle grain boundaries. STEM-EDS mapping further revealed Ni segregation at voids and sparse Al-rich oxides, without evidence of Ni–Si precipitates. Collectively, these findings identify dislocation density, helium content, and dose rate as the factors governing swelling in LPBF 316H and provide mechanistic datasets for model validation, supporting LAIN and the qualification of AM austenitic steels for nuclear service.

316 stainless steel↗

Role of microstructure on flux expulsion of superconducting radio frequency cavities

The trapped residual magnetic flux during the cool-down due to the incomplete Meissner state is a significant source of radio frequency losses in superconducting radio frequency cavities. Here, in this study, we clearly correlate the niobium microstructure in elliptical cavity geometry and flux expulsion behavior. In particular, a traditionally fabricated Nb cavity half-cell from an annealed poly-crystalline Nb sheet after an 800 °C heat treatment leads to a bi-modal microstructure that ties in with flux trapping and inefficient flux expulsion. This non-uniform microstructure is related to varying strain profiles along the cavity shape. A novel approach to prevent this non-uniform microstructure is presented by fabricating a 1.3 GHz single cell Nb cavity with a cold-worked sheet and subsequent heat treatment leading to better flux expulsion after 800 °C/3 h. Microstructural evolution by electron backscattered diffraction-orientation imaging microscopy on cavity cutouts, and flux pinning behavior by dc-magnetization on coupon samples confirms a reduction in flux pinning centers with increased heat treatment temperature. The heat treatment temperature-dependent mechanical properties and thermal conductivity are reported. The significant impact of cold work in this study demonstrates clear evidence for the importance of the microstructure required for high-performance superconducting cavities with reduced losses caused by magnetic flux trapping.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Improving creep resistance of Al-0.27Zr-0.08Sn (wt%) via cold swaging while maintaining high electrical conductivity

This study investigates the effect of mechanical cold work (0, 50, and 90% cross-sectional area reduction via swaging) on the creep properties of cast aluminum alloys with high electrical conductivity including high-purity Al (HP-Al), Al-0.15Zr (Al-Zr), and Al-0.27Zr-0.08Sn (Al-Zr-Sn, wt%). The Al-Zr alloy is strengthened by Zr in solid solution while the Al-Zr-Sn alloy is additionally strengthened by Al3Zr nanoprecipitates (8 nm diameter). After 90% cold swaging, the alloys exhibit grains elongated along the swaging direction with their widths ranging between 8 and 152 μm perpendicular to the swaging direction. Creep testing at 200 °C shows that the minimum creep rate of all 90% swaged alloys shows high sensitivity to stress, which can be modeled via a threshold stress σth. Increasing swaging magnitude from 0 to 50 to 90% in Al-Zr-Sn improves the creep resistance without reducing electrical conductivity. The formation of subgrains, increased dislocation density, and columnar grain structure in swaged alloys all enhance creep resistance. HP-Al swaged to 90% exhibits much lower creep resistance (σth = 18 MPa) due to subgrain coarsening and the absence of precipitates compared to Al-Zr (σth = 40 MPa) and Al-Zr-Sn (σth = 40 MPa), which maintain stable subgrain structures and benefit from solid solution strengthening and Al3Zr nanoprecipitates, respectively. Although Al3Zr precipitates are known to stabilize the deformed microstructure by pinning grain-boundaries, this work demonstrates that Zr in solid solution alone can effectively stabilize the deformed microstructure resulting in enhanced creep resistance. This effect of Zr solute on stabilizing grain boundaries for creep performance was not previously well-defined in the literature. Despite similar creep performances of Al-Zr and Al-Zr-Sn, the latter shows 70% higher room-temperature microhardness and slightly improved electrical conductivity (56%IACS (International Annealed Copper Standard) vs. 57%IACS, respectively). This work provides new insights into creep mechanisms of cold-worked Al–Zr alloys that will guide the design of heat-resistant Al conductors for high-demand applications.

Coello ramirez, Ismael [Northwestern University,]↗