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DOE OSTI2023

Data-Driven Optimization of the Processing Window for 316H Components Fabricated Using Laser Powder Bed Fusion

The Advanced Materials and Manufacturing Technologies Program is focused on accelerating the development and deployment of advanced materials and components fabricated via additive manufacturing with a specific focus on laser powder bed fusion (LPBF). As an initial case study, the program has selected 316H stainless steel (SS) as an initial material around which to develop a code case development strategy. This strategy involves two parallel approaches: (1) an equivalency approach whereby round-robin testing across multiple collaborating laboratories demonstrates repeatability in processing and direct comparisons with conventional wrought 316H material and (2) a revolutionary approach to code qualification combining in situ data collection and high-fidelity modeling to capture, predict, and bound the performance of LPBF 316HSS components. As part of this campaign, this work package has initiated an extensive process optimization campaign across three laboratories, each printing variations of LPBF 316HSS using three different LPBF units (Concept Laser, EOS, and Renishaw). In FY23, ORNL has focused on unique experimental designs spanning wide ranges in energy inputs and turning knobs such as scan speed, laser power, hatch spacing, layer thickness, spot size, scan rotation, and more. On the Concept Laser M2, 72 different combinations of processing variables were investigated with duplicate samples and different powder compositions. In total, 252 samples were printed with combined in situ sensing data. A parallel design of experiments was conducted on the Renishaw AM400 with an additional 390 printed specimens for analysis. All 642 miniature specimens, each with unique features included in each print to capture geometry-related heterogeneity, were subjected to high-throughput x-ray computed tomography (XCT) analysis to enable the downselection of specific processing parameters of interest. Then, using electrical discharge machining (EDM), miniature tensile specimens were extracted for mechanical testing and microscopy investigations. From the analysis performed in FY23, it was found that powder composition drastically affects the resulting microstructure and mechanical performance of 316SS. Specifically, changing from 316L to 316HSS powder results in a wide range of grain sizes with varying degrees of preferred grain orientation, which increases as a function of energy density. It was also found that due to stored heat in thin fin–type features, large microstructural differences can be seen within one part printed with one set of processing parameters. These variations in microstructure features, including grain size, the nanoscale dislocation structure, and grain texture, will all affect the irradiation performance and high-temperature mechanical performance of LPBF 316HSS parts. Two sets of concept laser processing parameters, spanning both refined and columnar grain structures, were scaled to print larger 316H builds for campaign testing (high-temperature creep and irradiation). In addition, at least two optimized processing parameter sets were identified for the Renishaw AM400 for round-robin testing in FY24 with Argonne National Laboratory. Future work includes printing samples using identical parameters identified by partner institutions, providing material for corrosion and high-temperature mechanical testing, and continuing evaluations of heterogeneity in larger printed parts.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Data-Driven Optimization of the Processing Window for 316H Components Fabricated Using Laser Powder Bed Fusion

36 MATERIALS SCIENCE↗

DOE OSTI2026

High Temperature High Vacuum Mechanical Property Assessment of Zirconium Nuclear Fuel Cladding

This report presents the mechanical characterization of a specific Zry-4 cladding batch serving as the foundation for a diverse range of fuel performance research at Oak Ridge National Laboratory (ORNL). This effort supports research needs for the U.S. Department of Energy (DOE), particularly regarding evaluating accident tolerant fuel (ATF) cladding coating concepts, expanding understanding of cladding response to loss-of-coolant accidents (LOCA) transients, refining post-critical heat flux (CHF) limits (t@T), and upcoming irradiation campaigns. The central objective was to define the baseline performance of the substrate Zircaloy-4 (Zry-4) material leveraged across ORNL Advanced Fuel Campaign (AFC) efforts through controlled high-temperature vacuum tensile testing. This work begins to address gaps in existing models where implementation based on nominal heat-treatment labels, such as stress relief annealed (SRA), often fail to capture the interplay of recovery, recrystallization, and grain growth. To quantify this, data was benchmarked against the Pacific Northwest National Laboratory (PNNL) stress strain model to determine where this material falls in comparison to assumed values for materials in the same heat treatment regime. Analysis of the tensile data revealed that this specific SRA batch exhibits a transitional microstructural state best described by an effective cold-work (CW) parameter of 0.09, diverging from the previous estimation of 0.5 for SRA materials. Additionally, comparative testing of Cr coated specimens demonstrated no distinct difference in axial strength relative to the bare substrate. This suggests that the strengthening benefits of Cr coatings observed in burst scenarios are driven by residual stress mechanisms acting solely in the hoop direction.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2017

Adhesion measurement of highly-ordered TiO 2 nanotubes on Ti-6Al-4V alloy

Self-assembled nanotubular arrays on Ti alloys could be used for more effective implantable devices in various medical approaches. In the present work, the adhesion of TiO 2 nanotubes (TiO 2 NTs) on Ti-6Al-4V (Ti64) was investigated by laser spallation and scratch test techniques. At first, electrochemical anodization was performed in an ammonium fluoride solution dissolved in a 90:10 ethane-1,2-diol (ethylene glycol) and water solvent mixture. This process was performed at room temperature (23 °C) at a steady potential of 60 V for 1 h. Next, the TiO 2 nanotubes layer was heat-treated to improve the adhesion of the coating. The formation of self-organized TiO 2 nanotubes as well as the microstructural evolution, are strongly dependent on the processing parameters and subsequent annealing. From microscopic analysis, highly oriented arrays of TiO 2 nanotubes were grown by thermal treatment for 90 min at 500 °C. Further heat treatment above 500 °C led to the detachment of the nanotubes and the complete destruction of the nanotubes occurred at temperature above 700 °C. Scratch test analysis over a constant scratch length (1000 μm) indicated that the failure point was shifted from 247.4 to 557.9 μm while the adhesion strength was increased from ~862 to ~1814 mN after annealing at 500 °C. Finally, the adhesion measurement determined by laser spallation technique provided an intrinsic adhesion strength of 51.4 MPa for the TiO 2 nanotubes on the Ti64 substrate.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Improving microstructure of silicon/carbon nanofiber composites as a Li battery anode

We report the interfacial study of a silicon/carbon nanofiber (Si/CNF) nanocomposite material as a potentially high performance anode for rechargeable lithium ion batteries. The carbon nanofiber is hollow, with a graphitic interior and turbostratic exterior. Amorphous silicon layers were uniformly coated via chemical vapor deposition on both the exterior and interior surfaces of the CNF. The resulting Si/CNF composites were tested as anodes for Li ion batteries and exhibited capacities near 800 mAh g1 for 100 cycles. After cycling, we found that more Si had fallen off from the outer wall than from the innerwall of CNF. Theoretical calculations confirmed that this is due to a higher interfacial strength at the Si/Cedge interface at the inner wall than that of the Si/C-basal interface at the outer wall. Based upon the experimental analysis and theoretical calculation, we have proposed several interfacial engineering approaches to improve the performance of the electrodes by optimizing the microstructure of this nanocomposite.

Howe, Jane Y↗

DOE OSTI2017

Quantitative characterization of soil micro-aggregates: New opportunities from sub-micron resolution synchrotron X-ray microtomography

Soil microaggregates are the fundamental building block, at the micron scale, of the highly hierarchical structure of soils, and can exert a significant control on the local biological metabolism and microbial community partitioning. In this study we propose an analysis protocol for the morphometric characterization of complete soil microaggregates based on sub-micron resolution synchrotron X-ray microtomography. A comprehensive characterization of the aggregate morphology is the first step towards a complete characterization of the soil microaggregates, when trying to correlate morphometric parameters with physical and/or biological properties, or when building models (e.g., effective diffusivity, microbial distribution, etc.). In this study, we demonstrate our characterization approach on two single microaggregate samples from dramatically different soil environments: one from Kansas, primarily composed by inorganic particles, and one from Barrow (Alaska) dominated by plant fragments. A series of state-of-the-art morphometric analysis techniques have been employed providing quantitative results highlighting specific differences of the two samples. The role of the microstructure in a scenario microbial population development has been discussed and it has been found that the Barrow microaggregate seems to be more favorable, from a purely geometrical point of view, as also confirmed by a simple model presented in this work. Finally, the potential of this approach, when coupled with chemical and biological analysis for a fully comprehensive characterization of soil aggregates in the larger picture of enhanced biological activity, is evident.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Spark plasma sintering (SPS) densified U 3 Si 2 pellets: Microstructure control and enhanced mechanical and oxidation properties

Dense U 3 Si 2 pellets with controlled grain structure and enhanced thermal-mechanical and oxidation properties are synthesized with spark plasma sintering (SPS). Microstructure and phase composition of the SPS densified pellets are characterized systematically using SEM, EDS, and XRD. Thermal-mechanical properties and oxidation behavior of the sintered silicide fuel pellets are analyzed by laser flash, indentation, and dynamic thermogravimetric analysis. Dense U 3 Si 2 pellets are consolidated by combining high energy ball milling and rapid sintering by SPS, and the microstructure structures are controlled from micron-sized (~5.7 μm grain size) for conventional silicide to a nanocrystalline matrix with an average grain size of ~280 nm. A dominant phase of distorted U 3 Si 2 was identified with lattice expansion due to residual thermal stress upon SPS consolidation and rapid cooling processes. Both micron-sized and nano-sized pellets show exceptional thermal transport properties, consistent with monolithic silicides reported in literature. The SPS-densified pellets possess simultaneously high hardness and fracture toughness. The SPS-densified silicide pellets also demonstrate exceptional oxidation performance with extended onset oxidation temperature above 500 °C and reduced oxidation kinetics, particularly for nano-sized pellets. A strong strain effect was proposed in which compressive stress in nano-sized pellets enhances the oxidation resistance of silicide fuels, as evidenced by the degradation of oxidation performance upon strain relaxation by isothermal annealing. The correlation among the sintering process – microstructure control – physical properties and fuel behavior is established. A new concept of strain engineering is proposed further properties optimization, enabling the development of potential oxidation and corrosion-resistant silicides with extended performance, the key technological challenge of U 3 Si 2 as the leading concept of accident tolerant fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Examining Constituent Redistribution in U-19Pu-10Zr Fuel as it Evolves with Local Burnup

While constituent redistribution is a known irradiation behavior in U-Pu-Zr fuel, new data have shown it is more complex than our current understanding and predictive capabilities. The size and composition of redistributed rings evolve as a function of pin composition, burnup, geometry, and irradiation temperature. In this work, we extract microstructural information from optical microscopy conducted on U-19Pu-10Zr pins (irradiated between 1.9 at. % and 11.6 at. % peak burnup). Both manual image analysis techniques and machine learning-assisted segmentation are used to quantify the thicknesses of the cladding, fuel-cladding interaction layers, and rings of fuel constituent redistribution in addition to pore distribution. These microstructural features and individual redistributed regions affect local thermomechanical properties, and identifying the relationship between burnup and constituent redistribution will improve accurate prediction of advanced reactor fuel performance.

Constituent Redistribution↗

DOE OSTI2011

Influence of slag chemistry on the hydration of alkali-activated blast-furnace slag - Part I: Effect of MgO

The hydration and the microstructure of three alkali activated slags (AAS) with MgO contents between 8 and 13 wt.% are investigated. The slags were hydrated in the presence of two different alkaline activators, NaOH and Na{sub 2}SiO{sub 3}.5H{sub 2}O (WG). Higher MgO content of the slag resulted in a faster reaction and higher compressive strengths during the first days. The formation of C(- A)-S-H and of a hydrotalcite-like phase was observed in all samples by X-ray diffraction (XRD), thermal analysis (TGA) and scanning electron microscopy (SEM) techniques. Increasing the MgO content of the slag from 8 to 13% increased the amount of hydrotalcite and lowered the Al uptake by C-S-H resulting in 9% higher volume of the hydrates and a 50 to 80% increase of the compressive strength after 28 days and longer for WG activated slag pastes. For NaOH activated slags only a slight increase of the compressive strength was measured.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Embedding Neural Thermal Scattering (NeTS) Modules in SERPENT for Higher Fidelity Advanced Reactor Analysis

When a neutron born in fission thermalizes to the order of $k$ $B$ $T$, it’s de-Broglie wavelength and energy approach the order of inter-atomic spacing and elementary lattice oscillations, respectively. $S$($a,β,t$) or the scattering law, uuantify these temperature-dependent crystallographic contributions to total cross section (or reaction rate). In a Monte Carlo analysis, cumulative distribution functions (CDFs) of $S$($a,β,t$) are loaded to memory from “A Compact ENDF” (ACE) files for stochastically selecting thermal scattered neutron trajectories. In this work, novel neural thermal scattering (NeTS) modules for $S$($a,β,t$) CDFs are designed, trained, serialized and embedded within SERPENT using Python’s limited C-API for on-the-fly deployment of crystalline graphite $S$($a,β,t$) sampling. Torchscript tracing and Numba just-in-time (JIT) compilation streamline neural inference on NVIDIA GPUs with CUDA libraries. Demonstrations of bare sphere thermalization of fast and thermal sources show excellent agreement between embedded NeTS in SERPENT and MCNP. With an explicit model of the reactor, NeTS can predict on-the-fly changes in TREAT neutron spectra as a function of local temperature, which can serve to improve transient and accident predictions in a multiphysics analysis framework. This framework can be further extended to account on-the-fly for changes in local graphitic microstructure to scattering cross sections, and outlines a novel coupling of modern machine learning with state-of-the-art reactor physics methods.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2018

Interfacial design and strengthening mechanisms of AZ91 alloy reinforced with in-situ reduced graphene oxide

Highlights: • An in-situ process was developed to synthesize magnesium alloy composite reinforced by graphene. • Microstructure and phase composition of oxide films were investigated by OM, SEM, EDS and XRD analysis. • The interfacial structure of Mg composites reinforced with reduced graphene oxide was characterized. • The interfacial reaction mechanisms between GO (graphene oxide) and the Mg metal was studied. - Abstract: This work highlights to develop an in-situ process to disperse uniformly graphene possessing good interfacial bonds with the matrix of Mg alloy. A homogeneous distribution of graphene in the matrix has been successfully obtained through in-situ reduction of graphene oxide (RGO) by sintering process after the graphene oxide (GO) was uniformly dispersed in AZ91 powders. The interface product nano-sized MgO can significantly improve the interfacial bonding strength between RGO and α-Mg with analysis by transmission electron microscopy. The orientation relationships of ( 2-bar 00){sub MgO}//( 1-bar 10 2-bar ){sub α‐Mg} and [011]{sub MgO}//[2 4-bar 2 3-bar ]{sub α‐Mg} with the semi-coherent interface characteristics were clarified for the first time at the interface of MgO/α-Mg, suggesting a good lattice space matching. By employing such process, a composite containing 0.5 wt% of GO shows an 85.7% and 61.4% increase in yield strength and elongation, respectively, over unreinforced AZ91 alloy. The underlying strengthening mechanisms of in-situ reduced graphene oxide are discussed in detail.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2020

Multiscale-Informed Modeling of High Temperature Component Response with Uncertainty Quantification

This report summarizes a joint effort between Argonne National Laboratory, Idaho National Laboratory, and Los Alamos National Laboratory to develop and deploy constitutive models targeted at predicting the life of Grade 91 alloy components subjected to high temperature environments typical of those that structural components in advanced nuclear reactors would experience. Two distinct, but complementary constitutive modeling approaches have been taken here. The first employs a phenomenological viscoplastic model for which parameters have been calibrated based on experimental data for a wide range of Grade 91 alloy that has undergone a variety of processing. A Bayesian approach was used to derive distributions of uncertain parameters for this model based on this data set. The second approach is a reduced order model suitable for engineering-scale analysis that is based on the results of a large set of mesoscale simulations. Mesoscale models allow for the microstructure and composition of a particular alloy to be directly taken into account in the computation of the viscoplastic response, but are computationally expensive, which makes it impractical to directly call those models for the material constitutive response in an engineering-scale simulation. The reduced-order representation of the response of the underlying model used here allows for an engineering-scale model to take into account the characteristics of the underlying microstructure, while only incurring a reasonable computational expense. Both of these approaches have different strengths, and are applicable for different parts of the design/analysis process. The phenomenological models can be readily parameterized based on a set of experimental data for a given class of materials and used for scoping calculations. Once a specific material is chosen and adequately characterized, the reduced order models can accurately predict the response of that specific alloy, and because the models are based on predictive models of the underlying microstructure, they can be used to more confidently predict the response under conditions in regions where there is limited experimental data. Both of these models have been integrated in the Grizzly code, which is used here to perform proof-of-concept uncertainty quantification analyses of a simple component under prototypical conditions. The built- in stochastic analysis capabilities in the MOOSE framework that Grizzly is built on are used here to run large sets of simulations for this uncertainty quantification analysis. As would be expected, because the reduced order models are developed for a much more tightly defined alloy, they predict tighter distributions of the time to failure than the phenomenological models, which are calibrated to a broader set of data. Also important is that these simulations demonstrate that a reduced order modeling approach can be successfully deployed to propagate uncertainties from the material scale to practical engineering-scale component simulations.

42 ENGINEERING↗

DOE OSTI2018

Combined curing as a novel approach to improve resistance of ultra-high performance concrete to explosive spalling under high temperature and its mechanical properties

Highlights: • The combined curing can significantly enhance the resistance of UHPC to explosive spalling under high temperature. • The combined curing can improve the mechanical properties of UHPC remarkably. • Both further hydration of residual cement and pozzolanic reaction are activated under a high temperature steam condition. - Abstract: The influence of a combined curing composed of precuring in hot water and heating in dry air on mechanical properties and explosive spalling of ultra-high performance concrete (UHPC) subjected to high temperature was investigated in this experiment. Meanwhile, the microstructure of UHPC was determined by means of X-ray diffraction (XRD) with Rietveld method, thermogravimetric analysis (TGA), scanning electron microscope (SEM) and mercury intrusion porosimetry (MIP). The results indicate that the combined curing improves the mechanical properties of UHPC remarkably. More importantly, it is quite efficient to enhance the resistance of UHPC to explosive spalling under high temperature, which should be a novel approach to prohibit spalling occurrence, different from adding polypropylene fiber. During dry air heating in the combined curing, a high temperature steam environment is established in the dense structure framework of UHPC formed in the preceding hot water curing. Both further hydration of residual cement and pozzolanic reaction of mineral admixtures can be activated during the dry air heating, leading to not only the formation of a large amount of dense hydrates (such as C-S-H gels, katoite, tobermorite and xonotlite, etc.), which accumulate in the aforementioned existing framework, but also the consumption of most of internal free water. Therefore, both mechanical properties of UHPC and its resistance to explosive spalling under high temperature can be enhanced significantly.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Nuclear forensic analysis of an unknown uranium ore concentrate sample seized in a criminal investigation in Australia

In early 2009, a state policing agency raided a clandestine drug laboratory in a suburb of a major city in Australia. While searching the laboratory, they discovered a small glass jar labelled “Gamma Source” and containing a green powder. The powder was radioactive. This paper documents the detailed nuclear forensic analysis undertaken to characterize and identify the material and determine its provenance. Isotopic and impurity content, phase composition, microstructure and other characteristics were measured on the seized sample, and the results were compared with similar material obtained from the suspected source (ore and ore concentrate material). While an extensive range of parameters were measured, the key ‘nuclear forensic signatures’ used to identify the material were the U isotopic composition, Pb and Sr isotope ratios, and the rare earth element pattern. These measurements, in combination with statistical analysis of the elemental and isotopic content of the material against a database of uranium ore concentrates sourced from mines located worldwide, led to the conclusion that the seized material (a uranium ore concentrate of natural isotopic abundance) most likely originated from Mary Kathleen, a former Australian uranium mine.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2019

Impact of irradiation induced dislocation loops on thermal conductivity in ceramics

Experimental work aimed at understanding the role of dislocation loops in limiting phonon mediated thermal transport in ceramics is presented. Faulted dislocation loops, having diameters of a few nanometers, were introduced by irradiating a polycrystalline cerium dioxide sample with 1.6 MeV protons at 700°C. XRD analysis indicated that irradiated samples retained their crystalline structure and exhibit very little lattice expansion suggesting a low concentration of point defects. Additionally, further microstructure characterization using transmission electron microscopy revealed that interstitial type faulted dislocation loops were primarily created as expected for these irradiation conditions. Thermal conductivity of the damaged layer was measured using a modulated thermoreflectance approach. Analysis of the experimental data using the classical Klemens-Callaway approach reveals that the conductivity reduction is primarily due to dislocation loops, while point defects and voids play only a minor role. These results provide experimental confirmation that faulted loops offer a unique arrangement for displaced atoms that leads to an unusually large reduction of thermal conductivity.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Magnetic hardening of Ce1+xFe11-yCoyTi with ThMn12 structure by melt spinning

A recent study on the intrinsic magnetic properties of CeFe11-yCoyTi has revealed that substituting one Co for Fe retains the favorable magnetocrystalline anisotropy H-a found in the ternary Fe end member, while enhancing the Curie temperature T-c and saturation magnetization 4 pi M-s. These findings warrant further optimization around Co substitution y = 1 to try to exploit the hard magnetic properties of these Ce-based magnets. Both Ce and Co concentrations in Ce1+xFe11-yCoyTi have been optimized in the range of x = 0 0.2 and y = 0 1.5. It was found that Co substitution effectively enhances all hard magnetic properties, although the values are still lower than those predicted from the intrinsic magnetic properties. Specifically, Tc increases from 210 degrees C to 285-350 degrees C; 4 pi M-19 (magnetization at 19 kOe) from 8.9 kG to 10.5-11.5 kG, remanence B-r from 3.1 kG to 4.1-4.5 kG, and most importantly, H-ci from 1.1 kOe to 1.5 kOe. As a result, the room temperature energy product (BH)(max) has been increased by over 100% from 0.7 MGOe in Ce1.1Fe11Ti to 1.5 MGOe in Ce1.05Fe9.75Co1.25Ti. Microscopy analysis indicates that the addition of Co refines the grain size and promotes chemical homogeneity at the microscopic scale. The beneficial effect of Co on the microstructure contributes to the improved hard magnetic properties. (C) 2015 AIP Publishing LLC.

Zhou, C↗

DOE OSTI2014

The sequence of intermetallic formation and solidification pathway of an Al–13Mg–7Si–2Cu in-situ composite

The phase transformation sequence and solidification behaviour of an Al–13Mg–7Si–2Cu in-situ composite was examined using a combination of computer-aided cooling curve thermal analysis and interrupted quenching techniques. Five different phases were identified by analysing the derivative cooling curves, the X-ray diffraction profile, optical and scanning electron microscopy images and the corresponding energy dispersive spectroscopy. It has been found that the solidification of this alloy begins with primary Mg{sub 2}Si precipitation and continues with the formation of eutectic Al–Mg{sub 2}Si, followed by Al{sub 5}FeSi and simultaneous precipitation of Al{sub 5}Cu{sub 2}Mg{sub 8}Si{sub 6} and Al{sub 2}Cu complex intermetallic phases. The formation of the last three intermetallic compounds changes the solidification behaviour of these composites remarkably due to their complex eutectic formation reactions. The solidification of the alloy, calculated using the Factsage thermochemical analysis software, has demonstrated a good agreement with the experiments in terms of compound prediction, their weight fractions and reaction temperatures. - Highlights: • Solidification path of a commercial Al-13Mg-7Si-2Cu composite was characterized. • Five different phases were identified and then confirmed with EDS and XRD results. • Mg{sub 2}Si, Al-Mg{sub 2}Si,Al{sub 5}FeSi (β),Al{sub 5}Cu{sub 2}Mg{sub 8}Si{sub 6} (Q) and Al{sub 2}Cu(θ) precipitated respectively. • Solidification was predicted using the Factsage thermochemical analysis software.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Microstructurally resolved electrochemical evolution of mechanical- and irradiation-induced damage in nuclear alloys

Abstract There is a need for high-throughput, scale-relevant, and direct electrochemical analysis to understand the corrosion behavior and sensitivity of nuclear materials that are exposed to extreme (high pressure, temperature, and radiation exposure) environments. We demonstrate the multi-scale, multi-modal application of scanning electrochemical cell microscopy (SECCM) to electrochemically profile corrosion alterations in nuclear alloys in a microstructurally resolved manner. Particularly, we identify that both mechanically deformed and irradiated microstructures show reduced charge-transfer resistance that leads to accelerated oxidation. We highlight that the effects of mechanical deformation and irradiation are synergistic, and may in fact, superimpose each other, with implications including general-, galvanic-, and/or irradiation-activated stress-corrosion cracking. Taken together, we highlight the ability of non-destructive, electrochemical interrogations to ascertain how microstructural alterations result in changes in the corrosion tendency of a nuclear alloy: knowledge which has implications to rank, qualify and examine alloys for use in nuclear construction applications.

Chen, Xin↗