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Baldo, Peter

Publications and source records attributed to Baldo, Peter.

In-situ and ex-situ characterization of irradiated AM materials

This study investigates the irradiation performance of laser powder bed fusion (LPBF) 316L and 316H stainless steels (SS), and their wrought counterparts. While LPBF 316L has been more studied, LPBF 316H is relatively new, with little prior data on its irradiation behavior. The research involved fabricating, preparing, irradiating, and characterizing six materials: LPBF 316L (two variants), LPBF 316H (two variants), and wrought 316L and 316H. LPBF materials were subjected to various heat treatments, including solution annealing and stress relief, and were irradiated using in-situ and ex-situ ion techniques at temperatures of 300°C and 600°C, with doses ranging from 0.2 dpa to 25 dpa. Under ex-situ irradiation with 4 MeV Ni 2+ ions at 600°C, the dislocation cell structures in LPBF316L-1 and LPBF316H-1 gradually evolved into a uniform dislocation network. At a low irradiation dose (0.2 dpa), the cell structures were still partially visible. At 2 dpa, a uniform dislocation network formed, though remnants of the original cell structure were still discernible as contrast domains. At 5 dpa and 10 dpa, even the contrast domains vanished. For irradiation at 300°C, the cell structure was still clearly visible at 0.2 dpa for LPBF316L-1. For LPBF316H-1, the dislocation cell structure was less apparent at the same dose but was still recognizable. With further increase in dose at 300°C, the dislocation cell walls were completely replaced by irradiation-induced defects and no longer visible. Void formation was observed for irradiation at 600°C. At 2 dpa, no evident voids were observed in either LPBF316L-1 or LPBF316H-1.

36 MATERIALS SCIENCE↗

Report on the Integration of Experimental and Modeling Data for Initial Equivalence Study of Microstructural Evolution in Irradiated LPBF 316SS

Advanced materials and manufacturing technologies are poised to improve the safety and design characteristics of nuclear technologies and meet US energy, environmental, and economic needs. In particular, metal additive manufacturing (AM) provides an opportunity to produce novel materials and component geometries, but their use is not without hurdles arising from the inherent microstructure variability that can result from the layer-by-layer build approach. Given the greater possible microstructure variability in AM materials—and the dearth of materials test reactors—it is impractical to rely solely on neutron irradiation studies to produce data for materials qualification for every possibility. This work within the Advanced Materials and Manufacturing Technologies (AMMT) Environmental Effects technical area contributes to the rapid qualification framework by developing a science-driven framework for the accelerated qualification of materials for nuclear environments. A key product of the Environmental Effects technical area of the AMMT program is the Licensing Approach with Ions and Neutrons (LAIN). This approach recognizes that whether using existing materials in new environments, newly developed materials tailored for these environments, or new manufacturing methods, the traditional decades-long approach for materials qualification does not facilitate rapid deployment. In FY 2023, the AMMT program presented a conceptual framework of specific steps to fulfill several technical challenges associated with qualifying materials for performance in radiation environments on an accelerated time frame informed by the state of the art in materials science and a review of the current regulatory landscape. The objective of this section of the Environmental Effects technical area is to critically evaluate and refine the proposed qualification framework presented under AMMT by integrating the research results of the neutron irradiations, the ion irradiations, and modeling efforts. These ongoing efforts span across Argonne National Laboratory (ANL), Idaho National Laboratory (INL), and Oak Ridge National Laboratory (ORNL) and are closely coordinated.

36 MATERIALS SCIENCE↗

Preliminary results addressing material qualification using combined ion irradiation and modeling data

Additively-manufactured (AM) materials have attracted increasing attention in recent years as a new method to make novel and customized components. While AM and conventionally produced materials are compositionally similar, they do possess different microstructures, necessitating assessment of materials produced via AM for their behavior in reactor environments. Some microstructures unique to AM materials, such as compositional micro-inhomogeneity and dislocation cell structures, are of particular importance since they may lead to different radiation performance. The performance of AM materials for advanced nuclear reactor applications is of interest to the Advanced Materials and Manufacturing Technologies (AMMT) program under the Department of Energy Office of Nuclear Energy. The AMMT program aims to demonstrate its new accelerated development and qualification methods via laser powder bed fusion (LPBF) 316 stainless steel (SS). Focusing on material bearing both 316L and 316H specifications, we integrate ion irradiation and modeling. This year, we focus on answering foundational questions related to process variability, alloy chemistry variation, and microchemical segregation. Experimental results provide information and motivate questions to the modeling effort, which aims to develop the ability to model radiation-driven microstructural evolution in additively-manufactured 316 stainless steel under a variety of advanced reactor conditions, including different temperatures, neutron spectra, and fluxes, in a sort of "virtual experiment". We perform in-situ and ex-situ ion irradiations and microstructural characterizations to support the development of AM materials for reactor applications, develop a phase field model of radiation-induced segregation in additively manufactured material with high angle grain boundaries and dislocation cells, and investigate the effect of carbon and chromium content on point defect behavior.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

In-situ and ex-situ characterization of ion-irradiated AM materials

Additive manufacturing (AM) has attracted increasing attention in recent years as a new way of making high-quality components for nuclear reactors. While AM materials are compositionally similar to their conventionally produced counterparts, they do possess different microstructures, such as dislocation cells and chemical inhomogeneity, that can lead to different mechanical properties and performance behavior. In this study, the irradiation response of AM materials was investigated. In-situ and ex-situ ion irradiations were performed on AM316L and AM316H stainless steels (SS) at 300 and 600°C. The influence of the dislocation cell structure on the evolution of irradiation-induced dislocation loops was evident at 600ºC, but was much weaker at 300ºC. No voids were observed with the in-situ ion irradiation up to 10 dpa at both temperatures. Post-irradiation energy dispersive spectroscopy showed radiation-induced segregation (RIS) near grain boundaries and the formation of Cr-rich oxides throughout the matrix. The extent of segregation at dislocation cell walls varies with dose. Nanoindentation tests performed on the AM316L SS irradiated at 600ºC showed a complex dose dependence with softening at low doses and hardening at high doses.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Radiation induced amorphization of carbides in additively manufactured and conventional ferritic-martensitic steels: In-situ experiments on extraction replicas

In-situ irradiations using 1 MeV Kr 2+ ions in a transmission electron microscope were performed on extraction replica samples containing M 23 C 6 carbides and MX carbonitrides from two ferritic-martensitic (FM) steels: (i) 9%Cr-1%W-TaV based Eurofer97 and (ii) 9%Cr-1%Mo-VNb (all in wt.%) based additively manufactured (AM) Grade91 steel. The irradiations were performed between 100 and 773 K up to a maximum dose of ~2.4 displacements per atom (dpa). The M 23 C 6 carbides are highly susceptible to radiation induced amorphization (RIA), while the MX type nanoprecipitates are highly amorphization resistant across the entire irradiation temperature range. Between 100 and 423 K, RIA of M 23 C 6 carbides occurs very rapidly with critical amorphization doses ranging between ~0.35 and 0.9 dpa, increasing to higher doses at 573 K. Complete amorphization of the M 23 C 6 carbides up to doses of ~2.4 dpa is not possible at 773 K under the present irradiation conditions. The critical amorphization dose of M 23 C 6 carbides increases nearly exponentially with irradiation temperature. The critical temperature for the crystalline-to-amorphous phase transformation (T c→a ) of M 23 C 6 carbides irradiated as replica samples, i.e. without the surrounding metal matrix, was estimated to be ~812 K. Comparing the present results with neutron irradiation data on bulk samples reveals a decrease in the critical amorphization dose for M 23 C 6 and an increase of T c→a , highlighting the effect of dose rate on the amorphization behavior that is qualitatively consistent with literature on other non-metals. Changes in the minor chemistry of M 23 C 6 , such as presence or absence of W, V, Nb, Mo, seems to have little effect on the amorphization behavior. Here, in-situ irradiations on extraction replica samples provide a novel pathway to explore radiation tolerance of nanoprecipitates in nuclear structural materials

36 MATERIALS SCIENCE↗

Grain boundary strain as a determinant of localized sink efficiency

The opportunity to achieve radiation tolerance in crystalline materials hinges on understanding the structure and response of grain boundary sinks to irradiation. A common descriptor of grain boundary efficiency as a defect sink is the denuded zone, which is a defect free zone adjacent to the grain boundary dictated by its ability to absorb radiation induced defects. This descriptor is often used at the mesoscale, which requires an averaging of absorption events. In this paper, we resolve the defect sink efficiency as a function of interfacial strain with respect to grain boundary character, and correlate high levels of grain boundary strain to an enhanced absorption efficiency. Here, we also introduce a key relationship between localized strain in proximity with the grain boundary sink and the variation absorption efficiency associated with these regions, revealing the pitfalls of averaging absorption events along a grain boundary, and presenting a path forward toward improved models for denuded zones and localized grain boundary absorption phenomena.

36 MATERIALS SCIENCE↗

IVEM Contributions to CINR Penn State MT17-12797: In situ Ion Irradiation to Add Irradiation Assisted Grain Growth to the MARMOT Tool

In-situ TEM experiments were performed at the IVEM-Tandem Facility in Argonne National Laboratory to study the irradiation-induced grain growth of nanocrystalline UO 2 and CeO 2 thin films using 1 MeV Kr ions at various temperatures from 50K to 1073K. The grain growth kinetics was studied under both irradiation and thermal annealing conditions. Bright field and dark field TEM images and diffraction patterns were systematically recorded as a function of temperature, irradiation dose and annealing time. A comprehensive grain growth data of UO 2 was collected for further analysis and for the implementation to the MARMOT tool.

36 MATERIALS SCIENCE↗

Effect of sink strength on coherency loss of precipitates in dilute Cu-base alloys during in situ ion irradiation

In situ irradiations with 1 MeV Kr ions at 50~613 K up to a fluence of 6.25 × 10 14 ions/cm 2 (~1.25 displacements per atom, dpa) have been performed on pre-aged dilute Cu-0.9%Co, Cu-0.9%Fe and Cu-0.8%Cr alloys containing uniform matrix dispersions of coherent precipitates in order to study the effects of initial precipitate sink strength, damage dose and irradiation temperature on radiation-induced coherency loss of precipitates. Coherent precipitates with different point defect sink strengths (2πNd, where N and d are the precipitate density and diameter) were used in this work to examine potential differences in atomic relaxation during absorption of point defects. In all cases, irradiation to low doses (<~1 dpa) was very effective at inducing loss of precipitate coherency. At low sink strengths (~10 13 m -2 ), loss of precipitate coherency could be induced for doses ~0.01 dpa. This suggests there might be an efficient preferential medium-range strain-induced bias for absorption of interstitial defects due to tensile strains emanating from the undersized precipitates, which induces relatively rapid loss of coherency at low precipitate sink strengths. High precipitate sink strength (~10 14 m -2 ) conditions were relatively resistant to the radiation-induced loss of coherency (requiring higher doses approaching ~1 dpa) and this might be due to nearly equal numbers of interstitial and vacancy defects arriving at the precipitate interface for such high sink strength conditions. The precipitate coherency loss was observed to have a weak dependence on irradiation temperature. Molecular dynamics simulations confirm a strong effect of precipitate sink strength on the probability of interstitial absorption at precipitates.

36 MATERIALS SCIENCE↗