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Quantifying Microstructure Variability in Laser Powder Bed Fusion 316 L Stainless Steel Microstructures with Spatial Statistics
Here, we have explored data-driven methods for material microstructure quantification that improve sensitivity to microstructural changes compared to traditional approaches. The methods integrate multiple microstructural properties, including grain morphology, crystallographic orientation, and material phase information. The simpler method employs maps of the Euclidean distance transformation metric to evaluate the morphology of grain boundary networks. The more intensive approach employs generalized spherical harmonic mapping for crystallographic orientations, per-pixel phase information, and a variational auto-encoder for dimensionality reduction and results in a multidimensional clustering of by microstructure similarity. Applied to an experimental dataset of additively manufactured steel, both methods detected slight variations in samples produced under nominally identical processing conditions. Both methods were able to distinguish between samples from multiple (nominally identical) builds, while the generalized spherical harmonics-based method could additionally cluster data samples rotated at two orientations on the build plate. The improved sensitivity of the methods, demonstrated through comparison with traditional microstructure characterization techniques, offers advantages for microstructure quantification and comparisons in advanced manufacturing applications.
Effect of heat treatment on creep behavior of 316 L stainless steel manufactured by laser powder bed fusion
The objective of this study is to understand the thermal stability of microstructure and its effect on the creep behavior of additively-manufactured 316L stainless steel (AM 316L SS). Creep specimens were fabricated from rods printed by a laser powder bed fusion process. Six different heat treatments, namely 650 °C/1 h, 700 °C/1 h, 750 °C/1 h, 800 °C/1 h, 900 °C/1 h and 1050 °C/1 h were applied to the creep specimens. The heat-treated specimens were creep-tested under the same condition, 550 °C/275 MPa to evaluate the effect of post-build heat treatment on the creep behavior of AM 316L SS. In the temperature range of 650-750 °C, dislocation density within cells, and cell size and wall thickness were affected by the heat treatment, while elemental segregation at boundaries remained unchanged and Mn-enriched Si oxide particles remained stable. In the temperature range of 750-900 °C, concurrent changes were observed in dislocation cell structures, elemental segregation and oxide particles. The 1050 °C-heat treatment removed cell structures and boundary solute segregations, leading to formation of equiaxed grains; Mn-enriched Si oxide particles in the as-built specimen were replaced by more stable Mn-enriched Cr oxides. The creep life of AM 316L SS increased after the heat treatment at 650 °C and then decreased with increasing temperature up to 900 °C where cell/subgrain structures still existed. The creep rate and creep elongation followed an opposite trend. The creep rate can be correlated with the structural parameters of cell/subgrain size and cell wall/boundary thickness and can be rationalized by different strengthening mechanisms of dislocation cells and subgrains. The heat treatment affected strongly the primary and secondary creep but had a minimal effect on the tertiary creep of AM 316L SS.
Comparing the deformation mechanism in 316 L stainless steel fabricated by hybrid and additive manufacturing
This study rationalizes the relatively higher elongation with minimal strength drop of 316L stainless steel (316LSS) manufactured using the hybrid approach in comparison to a fully additive approach followed by machining. It was found that twinning was the dominant deformation mechanism in 316LSS produced by both additive and hybrid approaches. Additionally, the relatively lower fraction of twins in the as-fabricated state of hybrid approach compared to a fully additive approach resulted in delaying the onset of steady-state strain hardening rate to higher strain levels, thereby resulting in an overall increase in elongation to failure.
Draft ASME Boiler and Pressure Vessel Code Cases and Technical Bases for Use of Alloy 617 for Constructions of Nuclear Component Under Section III, Division 5
The American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code currently only allows five materials for use in construction of nuclear components for high temperature service. These are: 2.25Cr-1Mo and V-modified 9Cr-1Mo steels, Types 304 and 316 stainless steels and the high nickel Alloy 800H. Since 2005, the US high temperature gas-cooled reactor program has been characterizing elevated temperature mechanical properties of Alloy 617 as the leading candidate construction material for the intermediate heat exchanger. After analysis of these experimental results, along with historical data and additional results available through the Generation IV International Forum, Very High Temperature Reactor, Materials Program Management Board Materials Handbook, a draft ASME Code Case to allow nuclear construction with Alloy 617 for temperatures up to 1750°F (954°C) has been developed. This report contains the Code Case for Low Temperature Service Construction of Section III, Division 5, Subsection HB, Subpart A, Class A and Subsection HC, Subpart A, Class B components, which has been approved in Section II, Materials, and Section III, Rules for Construction of Nuclear Facility Components. Supporting technical justification for the low temperature Code Case is also included. This Code Case allows use of Alloy 617 up to 800°F (425°C). This report also contains an updated draft of a Section III, Division 5, Subsection HB, Subpart B, Class A Code Case for Alloy 617 to qualify it for use in construction of nuclear components up to 1750°F (954°C) for service life up to 100,000 hours. The draft contained in Appendix 4, subject to editorial revision and approval by the ASME Special Task Group on Alloy 617 Code Qualification, will be submitted for approval by letter ballot by the appropriate ASME Committees. The technical justification supporting the Code Case is presented in Appendix 5 of this report. This background document is part of the information package that will be submitted with the Code Case for ballot.
An Initial Evaluation of the Elevated-Temperature Cyclic Properties of Optimized 316H Stainless Steel Fabricated by Powder Metallurgy Hot Isostatic Pressing
Powder metallurgy hot isostatic pressing (PM-HIP) is a mature advanced manufacturing technology, which can consolidate metallic powder under high temperature and pressure to generate near-net shape components. This process can lower production costs and reduce component lead times for nuclear reactor construction and can be readily deployed in the near term for microreactor components because of their smaller size. The purpose of this work is to continue the evaluation of elevated-temperature cyclic material properties for PM-HIP 316H stainless steel. Prior scoping results have shown that the commercially procured PM-HIP stainless-steel materials have reduced creep-fatigue performance compared to wrought 316 stainless steels. To better understand how PM-HIP processed material properties compare to traditional manufacturing methods, additional billets of PM-HIP 316H stainless steel were procured and tested. This testing is necessary to understand how elevated-temperature properties are influenced by the PM-HIP process and what data are needed for incorporating PM HIP 316H into the American Society of Mechanical Engineers Boiler Pressure Vessel Code, Section III, Division 5 for high temperature reactor construction. Specifically, an additional PM-HIP 316H stainless steel billet with lower oxygen and nitrogen concentrations was fabricated by the Nuclear Advanced Manufacturing Research Centre of the United Kingdom and tested to understand if elevated-temperature cyclic properties can be improved. The creep-fatigue resistance of the material from this new billet did not show appreciable improvement compared to prior testing.
Mechanical and Corrosion Response of 316SS in Supercritical CO 2
The supercritical carbon dioxide (s-CO 2 ) Brayton cycle is currently being explored as a replacement for the steam Rankine cycle due to its potential for higher efficiency and lower cycle cost. 316 stainless steel is a candidate alloy for use in s-CO 2 up to roughly 600 °C, but the mechanical effects of prolonged exposure of base and welded material in s-CO 2 have not been analyzed. The potential for carburization makes this an important concern for the implementation of 316 and similar austenitic stainless steels in the s-CO 2 environment. In this study, welded and base material of two types of 316–316L and 316H–were exposed in either s-CO 2 or argon at 550 °C or 750 °C for 1000 h. 550 °C s-CO 2 exposure yielded a thin (< 1 µm) Cr oxide with occasional nodules of duplex Fe oxide and Fe–Cr spinel that were up to 5 microns thick. However, tensile results from s-CO –2 exposure matched those of 550 °C thermal aging in Ar, indicating that no mechanically detrimental carburization occurred in either 316 variant after 1000 h exposure. Conversely, 750 °C s-CO 2 exposure produced roughly 10 × the oxide thickness, with a more substantial Fe oxide (3–5 µm) on the majority of the surface and nodules of up to 40 µm thick. In comparison to aged samples, tensile testing of 750 °C CO 2 -exposed samples revealed ductility loss attributed to carburization. As a result, projections of 316L performance in s-CO 2 indicate that mechanically detrimental carburization—equal to that shown here for 750 °C, 1000 h—will likely be present after 7–14 years of service at 550 °C.
Microstructural banding of directed energy deposition-additively manufactured 316L stainless steel
The microstructures of 316 L stainless steel created by rapid solidification are investigated here by comparing the similar microstructures of individual hatches of directed energy deposition additive manufacturing (DED-AM) and those of single, laser surface-melted tracks formed on a solid plate. High recoil pressure, which is exponentially dependent on the laser beam power density, induces convection of the melt pool, which causes formation of microstructural bands in the as-solidified microstructure. The microstructural bands are associated with changes in the chromium concentration and are a significant component of the inhomogeneous microstructure of DED-AM.
Neutron Irradiation Experiments
This presentation discusses the ongoing and upcoming neutron irradiation experiments within the Advanced Materials and Manufacturing Technologies (AMMT) program for the 2024 AMMT program review meeting. Ongoing and upcoming neutron irradiation of additively manufactured 316 stainless steel and A709 in the High Flux Isotope Reactor and Advanced Test Reactor are described.
Voltammetry measurements in lithium chloride-lithium oxide (LiCl–Li 2 O) salt: An evaluation of working electrode materials
Instrumentation to provide process monitoring (PM) and safeguards for the oxide reduction (OR) step in the electrochemical processing of used oxide nuclear fuel is necessary to ensure equipment is operated as declared. Cyclic voltammetry (CV) has been proposed for real-time monitoring of the operation of an OR process for safeguards purposes. In this study, different materials including 316 stainless steel (SS), tantalum (Ta), molybdenum (Mo), tungsten (W), platinum (Pt), and iridium (Ir) were evaluated as potential working electrode (WE) materials based on their chemical inertness, corrosion resistance, and sensitivity in detecting Li 2 O and other chloride salts in the OR electrolyte. Of the electrodes evaluated, 316 SS, Ir, and Pt all performed reasonably well in the LiCl-Li 2 O electrolyte. Here, stainless steel was operated in the cathodic potential and had reasonable corrosion resistance and is relatively inexpensive. Iridium could be operated in both the cathodic and anodic potentials and was the most corrosion resistant of those evaluated. Platinum is limited to the anodic potential range, had reasonable corrosion resistance, and was the most sensitive to Li 2 O concentrations in the salt. In the development of a stand-alone safeguards instrumentation, our recommendation is a CV sensor fitted with both Ir and Pt WEs. The results in this study may also be helpful for anode material selection in other electrometallurgy industries, such as molten salt electrolysis.
Corrosion Compatibility of Stainless Steels and Nickel in Pyrolysis Biomass-Derived Oil at Elevated Storage Temperatures
Corrosion compatibility of stainless steels and nickel (Ni200) was assessed in fast pyrolysis bio-oil produced from pyrolysis of high ash and high moisture forest residue biomass. Sample mass change, ICP-MS and post-exposure electron microscopy characterization was used to investigate the extent of corrosion. Among the tested samples, type 430F and type 316 stainless steels (SS430F and SS316) and Ni200 (~98.5% Ni) showed minimal mass changes (less than 2 mg∙cm−2) after the bio-oil exposures at 50 and 80 °C for up to 168 h. SS304 was also considered to be compatible in the bio-oil due to its relatively low mass change (1.6 mg∙cm−2 or lower). SS410 samples showed greater mass loss values even after exposures at a relatively low temperature of 35 °C. Fe/Cr values from ICP-MS data implied that Cr enrichment in stainless steels would result in a protective oxide layer associated with corrosion resistance against the bio-oil. Post exposure characterization showed continuous and uniform Cr distribution in the surface oxide layer of SS430F, which showed a minimal mass change, but no oxide layer on a SS430 sample, which exhibited a significant mass loss.
Direct Imaging of Hydrogen‐Driven Dislocation and Strain Field Evolution in a Stainless Steel Grain
Hydrogen embrittlement (HE) poses a significant challenge to the durability of materials used in hydrogen production and utilization. Disentangling the competing nanoscale mechanisms driving HE often relies on simulations and electron-transparent sample techniques, limiting experimental insights into hydrogen-induced dislocation behavior in bulk materials. This study employs in situ Bragg coherent X-ray diffraction imaging to track three-dimensional (3D) dislocation and strain field evolution during hydrogen charging in a bulk grain of austenitic 316 stainless steel. Tracking a single dislocation reveals hydrogen-enhanced mobility and relaxation, consistent with dislocation dynamics simulations. Subsequent observations reveal dislocation unpinning and climb processes, likely driven by osmotic forces. Additionally, nanoscale strain analysis around the dislocation core directly measures hydrogen-induced elastic shielding. These findings experimentally validate theoretical predictions and offer mechanistic insights into hydrogen-driven dislocation behavior. The quantified nanoscale phenomena serve as critical inputs for multiscale modeling frameworks to predict bulk material responses and accelerate the development of HE-resistant alloys.
Post Irradiation Examination of Pressurized Water Reactor Stainless Steel Internal Components
Internal structural components of pressurized water reactors (PWR), such as baffle former bolts, are subjected to significant neutron irradiation and mechanical stresses at elevated temperatures during plant operation. Over the long operation of the power plant, these conditions lead to potential degradation and reduced load-carrying capacity of these bolts. To understand property degradation more fully, to confirm the results of experimental irradiation programs, and to predict operational lifetime performance of structural materials in internal components, post irradiation examination of harvested materials from operating nuclear reactors is required. In this work, two high fluence 316 stainless steel baffle former bolts were retrieved from a commercial Westinghouse two-loop downflow type PWR and then sectioned for analysis via mechanical testing and microstructural characterization. The irradiation damage fluctuated along the bolt length with damage levels from 15 to 41 displacements per atom with the bolt head receiving approximately twice the neutron damage levels as that of the bolt thread section. Mechanical testing evaluations showed extensive irradiation hardening and a sharp decrease in fracture toughness in all parts of the bolt, though with limited variation along the bolt length. Microstructural characterization using analytical scanning transmission electron microscopy and atom probe tomography showed significant radiation induced precipitation, segregation, and dislocation loop and cavity formation. However, unlike the mechanical behavior, there was considerable variation along the bolt length but opposite of what may be expected, with more precipitation and cavity formation in the bolt thread where the neutron radiation dose is less than in the bolt head where the neutron radiation dose is higher. The cause of this variation is likely due to gradients in temperature, neutron energy spectra, and gamma irradiation.
Interaction of beryllium with 316H stainless steel in molten Li 2 BeF 4 (FLiBe)
The increased demand in renewable energy resources has led to a renewed interest in nuclear reactors including a new generation of molten salt reactors. One of the issues encountered in handling of molten chloride or fluoride salts is the inability of metals to form and retain a protective oxide surface layer, generally chromium oxide. The low chromium content, nickel-based alloy INOR-8, later marketed as Hastelloy N, was specifically developed to contain molten fluorides. This alloy had some deficiencies, but its composition resulted in it incurring far less chromium depletion by the molten fluoride salts than alloys like 316 stainless steel. For the next generation of molten salt reactors, an alloy with pressure vessel code approval and higher temperature capability than Hastelloy N is required. Consequently, several reactor designers have reportedly chosen to build the reactor containment vessel from 316H stainless steel. In order to minimize corrosion of the stainless steel by the molten fluoride salt (2LiF-BeF 2 ), it is proposed to add beryllium metal to the salt to react with impurities and provide a means to lower the oxidation potential thus making the salt less corrosive. Even so, there is a concern whether the beryllium would react with components of the stainless steel. To address this concern, static capsule tests were conducted in which selected amounts of beryllium were added to capsules containing 2LiF-BeF 2 (FLiBe) salt and 316H stainless steel and Hastelloy N samples. Following exposure, the samples were cleaned and examined using a variety of analysis techniques including, optical microscopy, SEM-EDS, XPS, LIBS, XRD and EPMA. Tensile samples were also exposed in capsules, and those were subjected to tensile testing. Notably, It was found that for the level of beryllium additions used in this study, intermetallic compounds were formed which could be detrimental to the long-term performance of the 316H stainless steel.
High-Strength, High-Ductility, High Entropy Alloys with High-Efficiency Native Oxide Solar Absorbers for Concentrating Solar Power Systems
This EPSCoR Project has been investigating the synergy between the excellent high-temperature mechanical behavior of FeMnNiAlCr high entropy alloys (HEA) and the high solar absorptance of their native oxides for high efficiency concentrated solar thermal power (CSP) systems working at >700°C. While HEAs have attracted substantial interest in recent years, most investigations have focused on their applications as structural materials rather than functional materials. This EPSCoR project discovered that FeMnNiAlCr HEAs can potentially be applied synergistically as both a structural and functional material for high-efficiency concentrating solar thermal power (CSP) systems working at >700°C. The HEA itself would be used in high-temperature tubing to carry molten salts or supercritical CO 2 , while its surface oxide would act as a high-efficiency solar thermal absorber. With Fe and Mn being the major components in these HEAs (adding up to ~70 at.% of the alloy), these materials are much more cost-effective than the Ni-based superalloys currently being investigated for high-temperature CSP systems. Through this research, these Fe-Mn based HEAs have demonstrated yield strengths 2-3x greater than that of stainless steel at 700°C and a creep lifetime >800 h at 700ºC under a typical CSP tubing mechanical load of 35 MPa. Their Mn-rich surface oxides maintain a high optical-to-thermal conversion efficiency of ~87% under 1000x solar concentration ratio for 20 simulated day-night thermal cycles between 750ºC and room temperature. In preliminary corrosion studies, these HEAs have sustained immersion in unpurified bromide molten salts for 14 days at 750°C with <2% weight loss, in contrast to 70% weight loss from a 316 stainless steel reference. The simultaneous achievement of promising mechanical, optical, and thermochemical properties in this FeMnNiAlCr system opens the door to new applications of HEAs in solar energy harvesting. Partnerships with Ames Laboratory and Oak Ridge National Laboratory (ORNL) also advanced our understanding of the fundamental structure-property relationships through atomic scale material characterization and first-principles computational modeling. The key research results in this project can potentially be extended to other HEAs and their native oxides. In terms of applications, the proposed FeMnNiAlCr HEA/native oxide system could potentially exceed the mechanical and the optical performance of existing tubing and solar coating materials under EERE’s CSP program at lower cost, which also aligns well with the EPSCoR Science and Technology strategies of New Hampshire in boosting the deployment of renewable energy.
ASME Code Qualification Plan for LPBF 316 SS
This report describes a plan to qualify laser powder bed fusion (LPBF) 316 stainless steel for use with the American Society of Mechanical Engineers (ASME) Boiler & Pressure Vessel Code Section III, Division 5 rules for metallic components in high temperature nuclear reactors. Accomplishing this goal would make the material and manufacturing process available to vendors for inclusion in the next generation of advanced, high temperature reactors. The general approach adopted here is to treat LPBF 316 as if it was a completely new material and to develop a plan to qualify the material according to the current ASME practices. One key goal of this work is to explore and develop accelerated qualification approaches that might reduce the time required to qualify new materials by reducing the need for long term testing. However, the qualification plan here does not employ any accelerated qualification approaches to provide a limiting, bounding description of the number, duration, and types of testing required to qualify LPBF 316 without such techniques and to describe a comprehensive dataset that could be used to explore and validate accelerated qualification approaches in the future. The report addresses the fundamental challenges to qualifying Advanced Manufacturing (AM) materials for high temperature applications and summarizes the ASME Section III qualification process as well as current efforts to qualify LBPF and DED 316 for low temperature applications. The report then discusses specific issues, both material and logistical, related to qualifying PBF 316 steel. The final chapters of the report describe a complete test plan designed to generate sufficient data to qualify the material as well as a data management plan for how to store and manage the data to eventually provide the test data packaged needed to qualify the material with ASME.
A Rate Theory Model of Radiation-Induced Swelling in an Austenitic Stainless Steel
Many rate theory models of cavity (void) swelling have been published over the past 50 years, all having the same, or similar, structures. A rigorous validation of the models has not been possible because of the dearth of information concerning the microstructures that correspond with the swelling data. Whereas the lack of microstructure information is still an issue for historical swelling data, in the past 10–20 years data have been published on the evolution of the microstructure (point defect yields from collision cascades, cavity number densities, and dislocation densities/yield strengths) allowing certain gaps in information to be filled when considering historic swelling data. With reasonable estimates of key microstructure parameters, a standard rate theory model can be applied, and the model parameter space explored, in connection with historical swelling data. By using published data on: (i) yield strength as a function of dose and temperature (to establish an empirical expression for dislocation density evolution); (ii) cavity number densities as a function of temperature; and (iii) freely migrating defect (FMD) production as a function of primary knock-on atom (PKA) spectrum, the necessary parameter and microstructure inputs that were previously unknown can be used in model development. This paper describes a rate-theory model for void swelling of 316 stainless steel irradiated in the EBR-2 reactor as a function of irradiation temperature and neutron dose.