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The Material Test Reactors Fifth Workshop reviews the successes and failures of material test protocols and lessons learned. This presentation introduces the Annular Core Research Reactor (ACRR), the history of nuclear reactors at Sandia National Labs and the experiment review process. Included are actual examples of experimental activities at ACRR.
Material test reactors (MTRs) are used to irradiate nuclear fuels and materials to develop data for how they endure neutron bombardment in or near reactor cores. Most historic MTRs, and all that remain operational in the US today, are water-cooled types and produce a thermalized neutron flux. New irradiation facilities are needed which can produce neutron energy spectra relevant to fast and fusion reactor environments. Construction of these facilities will take several years of steadfast funding to complete, which poses a formidable schedule challenge for current fast and fusion reactor developers. Irradiation designs which modify the neutron energy spectra delivered to test specimens in thermal spectrum MTRs, an approach referred to as “spectral tailoring”, can be used to approximate several relevant phenomena in the materials needed to enable fast and fusion reactor technologies. This approach is imperfect, but still valuable in the present situation. Here, the two highest flux MTRs operational in the United States, the Advanced Test Reactor (ATR) and High Flux Isotope Reactor (HFIR), have rich histories, ongoing developments, and new potentials for spectral tailoring that will be reviewed and discussed in this paper.
Ceria (CeO 2 ) particles with low to ultra-low loading of nickel dopant were produced using an aerosol-based, droplet-to-particle synthesis via an in-line calcination technique. This aerosol-based synthesis method enables the production of particles with a monodisperse size distribution. These produced and well-characterized, multi-element, ceria-based particles demonstrate a material exemplar for multi-method analytical testing. They were prepared from a cerium nitrate feedstock where low loading nickel dopant was added at target Ni/(Ni + Ce) atomic percents of 1 %, 0.1 %, and 0.01 %, using a nickel nitrate spike. This methodology proved to produce ceria particles doped with a dynamic range of low to ultra-low loadings of nickel over a 24-h period, with consistent size distribution, morphology, and composition. The successful incorporation of nickel was demonstrated with bulk and single particle inductively coupled plasma mass spectroscopy and revealed notable particle-to-particle elemental homogeneity. X-ray photoelectron spectroscopy demonstrated the presence of a high concentration of nickel dopant incorporated preferentially toward the surface of the particles, and that this dopant aided oxidation of surface Ce(III) atoms to Ce(IV). These particle test materials were then validated through X-ray absorption near edge spectroscopy, comparing the ultra-low 0.01 % Ni and low 1 % Ni-doped ceria samples. This revealed a more-reduced oxidation state of the nickel with an increase in dopant concentration. Finally, this work demonstrates a synthesis and systematic characterization scheme to produce multi-method analytical test particulates.
The increasing demand for sustainable battery technologies requires effective recycling strategies for end-of-life lithium-ion battery cathodes. In this study, virtual materials testing, a well-established framework for modeling conventionally manufactured NMC-based cathodes, is applied to partially recycled cathodes. To this end, virtual cathodes consisting of mixtures of pristine and recycled NMC particles are utilized to systematically analyze structure–property relationships depending on mixing ratios and different spatial arrangement strategies. For this purpose, a stochastic 3D model is developed that is capable of generating virtual cathodes with arbitrary volume fractions of active materials and mixing ratios of pristine and recycled NMC particles. Particularly, the stochastic 3D model can mimic the different size distributions of pristine and recycled particles that are observed in image data. Additionally, the model allows the structuring of pristine and recycled NMC either uniformly mixed or layer-wise arranged, mimicking single- and dual-layer cathodes. Subsequently, a systematic computational analysis is conducted to assess the influence of increasing active material ratios of recycled particles, ranging from 0 % to 100 %, while maintaining a constant overall active material volume fraction. The impact of particle mixing on cathode performance is evaluated by examining transport-relevant geometrical descriptors and effective properties, such as geodesic tortuosity, specific surface area, and tortuosity factor.
Characterization and testing of advanced plasma-facing materials (PFMs) for Fusion Pilot Plants (FPP) is being conducted at the DIII-D National Fusion Facility through the ongoing two-year FPP Candidate Materials Thrust. Year one tested 17 novel materials utilizing the Divertor Materials Evaluation System (DiMES), with samples analyzed pre- and post-experiment via SEM, EDS, and confocal microscopy. Repeatable reference discharges were developed to ensure uniformity between experiments, including a new strike-point rastering scenario to provide more uniform heat/particle flux across DiMES during ELMing H-mode discharges. Various sample geometries and temperatures were used to achieve FPP-relevant conditions, including samples angled 10° towards the incident plasma flux and pre-heating up to 500 °C. The first exposure of liquid lithium (Li) capillary porous structures in a tokamak demonstrated uniform emission of Li vapor and suppression of Li droplets in H-mode when preheated to 350 °C. Dispersoid-strengthened W with 1 wt% TaC, TiC, and ZrC exposed to H-mode showed cracking and dispersoid ejection for all varieties except TiC, providing a clear down-selection. Ultra-high temperature ceramic materials TiB 2 and ZrB 2 showed minimal degradation under L-mode exposure. Silicon carbide (SiC) fiber composites showed arcing along edges, while CVD SiC remained pristine. Atmospheric plasma-sprayed W and SiC coatings endured H-mode exposure without macroscopic delamination; SiC exhibited granular ejection, while W showed increased outgassing. Additional W-based alloys were stress tested in H-mode, including Ni-based W heavy alloys, W f SiC f /W composites, W multi-principle element alloys, and functionally-graded W/SiC, to varying degrees of success.
As the US fusion materials community awaits the selection and design of a fusion prototypical neutron source (FPNS), a risk reduction exercise has been conducted to (i) provide an updated materials performance evaluation using state-of-the-art computational materials modeling, (ii) expand on legacy analysis based on pure Fe to other relevant fusion structural materials types, and (iii) ensure that materials response under FPNS operational conditions is consistent with referential fusion reactor conditions. The current paper describes the efforts undertaken to assemble a comprehensive computational methodology that includes neutronics, primary damage calculations, atomistic simulations of displacement cascades, chemical inventory evolution calculations, and a computational thermodynamic analysis of emerging phases during irradiation. Our work extends existing studies in pure Fe to reduced-activation ferritic/martensitic steels, tungsten, silicon carbide, and vanadium alloys. We focus on the single-beam deuteron/lithium-stripping neutron source behind the IFMIF-DONES concept, which we assess against ITER, two DEMO designs, and an ideal pure 14-MeV flux. Our analysis indicates that, within standard uncertainties inherent to the models employed, the DONES concept adequately captures fusion conditions in the four materials analyzed. Our work is intended as a comprehensive irradiation damage analysis of fusion-representative neutron sources, to be used for further neutron source evaluation and fusion facility operation.
Next generation gas turbines will reduce carbon emissions by improving their cycle efficiencies and implementing hydrogen as a low-carbon fuel. The combined-cycle efficiency can be improved by increasing the combustor outlet temperature and decreasing the cooling air required for hot-section parts. Ultra-high temperature ceramic matrix composites (CMC) can survive increasingly extreme environments due to their strong mechanical properties at expected conditions. The introduction of CMCs in high-hydrogen flame environments requires testing at realistic conditions that mimic the thermochemical and fluid mechanic states in gas-turbine combustors. In this work, we describe a new experiment that has been designed to test high-temperature materials in a combustor-relevant environment. Its trapped-vortex combustor chamber design allows for high levels of fuel flexibility and wide flame stability limits. Testing of monolithic silicon carbide (SiC) samples in this environment was done to characterize the heat transfer to material samples over a wide range of operating conditions, including variations in fuel composition and thermal power. Heat flux measurements were verified in non-reacting and reacting environments after which they were benchmarked with previous literature to verify the operation of the facility with heated air. Testing in combustor-relevant conditions shows high levels of heat flux to the material samples in the combustor, particularly downstream of the anchored flame.
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After several years of relatively low activity in the field of Light Water Reactor (LWR) fuel development, the Department of Energy again began to engage in developing new fuel technologies and irradiation performance data prompted by the Fukushima Daichi nuclear accidents. New competencies for irradiation testing in material test reactors in the United States began to be developed at this time using the Advanced Test Reactor (ATR), High Flux Isotope Reactor (HFIR), Massachusetts Institute of Technology Reactor (MITR), and the Transient Reactor Test Facility (TREAT). Capsules for testing fuel and cladding materials in ATR and HFIR were deployed, a Pressurized Water Reactor (PWR) condition loop for testing fuel rods was established in ATR, cladding corrosion studies were performed using a water loop in MITR, and TREAT pulse testing capabilities were commissioned for fuel rods in water capsules. The more recent and unexpected closure of the Halden Boiling Water Reactor (HBWR) also prompted further investments in Loss of Coolant Accident (LOCA) testing capabilities at TREAT. New configurations of these test devices show further potential in enhanced steam condition control and other investigations are building toward a flowing water loop for testing transient to dryout conditions. The closure of HBWR also prompted a major project currently underway to construct additional water loops in ATR where a novel approach is being pursued to enable Boiling Water Reactor (BWR) conditions. A meaningful collaborative project was awarded to MITR which, amidst an unexpected major overhaul of the reactor, has expanded cladding corrosion test capabilities at MITR. New explorations have led to methods for unique experiments at HFIR including channel box irradiations. New device developments are also bridging toward future potential for instrumented capsule irradiation tests in ATR and HFIR. Finally, a new project referred to as the System Physics Advanced Reactor Critical facility (SPARC) is gaining traction towards a large zero-power reactor able to produce physics validation data for LWR fuel bundle designs with increased enrichment and enhanced absorbers for 24-month operation cycles. This paper provides a brief summary of the status of these irradiation testbed capabilities with an emphasis on current efforts toward future capabilities to obtain new data and maximize the performance potential of LWR fuel technologies.
The Palisades Nuclear Generating Station included in its original surveillance program a surveillance capsule, designated A-60. The capsule was removed from its surveillance position in early 1995 and has been resident in the spent fuel pool since that time. It was harvested to perform characterization of surveillance specimens in this capsule in 2023. This capsule was irradiated to a fluence of 1.96x1020 n/cm2 (E> 1MeV) that is equivalent for more than 150 effective full power years for the current US reactor pressure vessel (RPV) fleet. This capsule contained several materials, including Charpy specimens of standard reference material (SRM) from Heavy-Section Steel Technology (HSST) A533-B Plate 01. To perform Charpy testing of this highly irradiated material, the new Charpy specimen transfer system was designed and implemented on Charpy impact testing machine in the hot cell to accommodate remote testing of these specimens. This new transfer system includes integrated environmental chamber to cool or heat Charpy specimens to the desired temperature. Testing of this highly irradiated material revealed very large shift of Charpy transition temperature, 188oC.
The Enhanced Linear Variable Intrinsic Sensor (ELVIS) was a 2024 breakthrough discovery by Idaho National Laboratory (INL) in terms of further innovating the usage of all linear variable differential transformers (LVDTs) and enhancing their performance in harsh environments. In irradiation tests conducted within material test reactors (MTRs), LVDTs with an internal temperature sensing capability can address several critical challenges. This report focuses on performance testing of the ELVIS III device with new hybrid LVDTs provided by the Institute for Energy Technology (IFE), which is the world’s sole supplier of nuclear-grade LVDTs. The ELVIS III device was evaluated in terms of temperature showcasing promising results comparable to a typical type-K thermocouple (TC).
The use of subsize specimens in nuclear materials testing has been a subject of ongoing interest due to radiation safety concerns and resource conservation needs. It is also of interest in additive manufacturing (AM), also known as 3D-printing, as subsize specimens can more accurately represent the behavior of the small, intricate geometries often produced using AM. A novel, extremely small geometry, called the Subsize Teeny (SST) was recently developed and is of interest for implementation. Given its extraordinarily small size and the complexities associated with subsize specimen testing, adequate vetting of this geometry is necessary to ensure data quality. Here, a variety of unirradiated nuclear structural materials were tested in the SST geometry and compared against the well-established SSJ3 geometry. In addition, two case studies implementing the SST as a screening geometry for AM materials were also conducted. The question of SST viability was found to be highly nuanced and will often be dependent on the context or application in question. It was determined, however, that the SST is a largely invalid geometry for exceptionally coarse-grained materials or in cases where the physical defect volume equals or exceeds 0.1 % or where the specimen machining parameters result in significant surface alterations. On the other hand, it was determined that the SST may be employed with confidence if the test material is nearly or totally free of physical defects, isotropic, demonstrates homogeneous plastic deformation, and possesses a fine-grained, nearly or totally homogeneous microstructure with at least twelve slip systems.
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Linear plasma devices (LPD) utilizing a helicon plasma source, a high density light ion source, can generate impurities due to progressive erosion of the radio frequency (RF) transmission window caused by rectified sheath voltage. These source-born impurities can entrain and be transported by the plasma toward a target, affecting plasma-material interaction studies. Earlier work on material testing in Prototype-Materials Plasma Exposure eXperiment at ORNL revealed significant source impurity deposition on downstream targets. However, using a similar RF source, no target impurity deposition is observed in Plasma Interaction Surface Component Experimental Station (PISCES)-RF despite evidence of RF window erosion in the source region, thereby motivating the present work. Experimentally, using various magnetic field configurations upstream of the PISCES-RF plasma source and seeding titanium (Ti) impurities at various axial locations, impurity transport and deposition along the machine axis were investigated. It was found that Ti deposition was localized to the side of the plasma source where the Ti impurity was seeded. In contrast, aluminum (Al) deposition, originating from the sputtering of the helicon window, occurred predominantly upstream of the plasma source, suggesting an asymmetry in the axial transport of eroded RF window material. These observations suggest a stagnation of the parallel plasma flow immediately downstream of the plasma source, with impurity ions remaining unmagnetized near the source upstream. Al deposition in magnetic field-free regions in PISCES-RF indicates that sputtered Al impurities likely remained neutral due to their large ionization mean-free path under PISCES-RF conditions. Plasma modeling and simulation supported this, indicating that Al-neutrals transport toward the helicon source upstream for low electron density cases. It was found that the Larmor radius of the Al ions was greater than the plasma radius towards the source upstream and remained weakly magnetized in PISCES-RF, meaning that plasma source-born impurities are not efficiently entrained in the plasma flow. These findings provide critical insights into impurity transport in helicon plasma-based LPDs.
Nuclear materials testing is essential for understanding changes in reactor environments, but traditional methods are costly and time-consuming. High-Throughput Experimentation (HTE) enables rapid screening and optimization of material properties by significantly increasing the number of specimens in the experiment. In this work, HTE methods were employed to irradiate novel materials at the Advanced Test Reactor (ATR) at Idaho National Laboratory. A total of 367 sub-sized tensile specimens were irradiated using the standard capsule design. To facilitate HTE, automated systems such as the Automated Mechanical Testing System were implemented for mechanical testing within hot cell environments, thereby reducing the need for manual interaction with hot cell manipulators and significantly lowering both the cost and duration of experiments. Digital image correlation (DIC) was used to measure displacement during mechanical testing, providing precise, non-contact measurement capabilities. The methodologies developed in this research will support the advancement of HTE techniques for future nuclear materials testing experiments at ATR. This approach allows for more efficient and cost-effective evaluation of new materials, ultimately leading to improved reactor performance, enhanced safety, and extended longevity within the nuclear industry.
This Perspective builds upon insights from the National Institute of Standards and Technology (NIST)-organized workshop, “Materials and Metrology Needs for Advanced Semiconductor Packaging Strategies,” held at the 35th annual Electronics Packaging Symposium in Binghamton, NY, on September 5, 2024. It outlines critical challenges and opportunities related to polymer-based “soft” materials in advanced semiconductor packaging, with emphasis on polymer science, measurement science (metrology), and the strategic development of Research-Grade Test Materials (RGTMs). These efforts, led by the NIST CHIPS team, aim to advance the fundamental understanding of structure-property-processing relationships, promote standardized guidelines and innovative methods for material characterization, and accelerate the development, qualification, and adoption of next-generation packaging materials. The Perspective also distills key insights from the panel discussion with industry experts, emphasizing the need for close collaboration among materials scientists, process engineers, and metrology experts to enable a holistic strategy, further highlighting the importance of cross-sector partnerships among industry, academia, and government to address pressing challenges in packaging materials and processes.
H-13 tools steel’s relative hardness, resistance to thermal fatigue, and high tolerance of thermal shock, make it very desirable for use in forging, pressing, casting, and extrusion processes[1]. H-13 is however typically quite expensive when compared to many other steel compositions. It is therefore desirable to encase a lower cost steel composition with H-13. This configuration allows for the benefits of H-13 tooling to be realized, at a considerably reduced cost. To demonstrate the viability of this concept, a casting tool was fabricated using a Wire Arc Additive Manufacturing (WAAM) process. Initial materials testing was conducted on a multi-material wall which consisted of one section of H-13 tool steel, and one section of 410NiNmo. These tests included scanning electron microscopy, energy dispersive X-ray spectroscopy, and hardness testing. This testing generated favorable results and subsequently a casting tool was fabricated for evaluation. Utilization of a Multi-Material WAAM process to fabricate large tooling in this manner could yield significant improvements in material cost, manufacturing agility, and supply chain complexity.
Hermetic machinery utilizing gas bearings for MW-scale supercritical CO 2 (sCO 2 ) machinery applications can have significantly lower power loss and enable improved cycle efficiency compared to conventional machinery with oil-lubricated bearings. Active magnetic bearings (AMBs) are another option anticipated to have similar power loss and load capacity to gas bearings as well as offering larger mechanical tolerances, the ability to tune properties, and high reliability due to lack of mechanical wear. AMBs also have proven commercial experience at MW-scale, though environments for high-temperature sCO 2 power cycle machinery conditions are novel. Besides the potential impact of AMBs for sCO 2 turbomachinery, the technology also offers promising benefits for steam and gas turbines for power generation, compressors and expanders for industrial heat and power, and in other oil and gas and space applications. The goals of this project were to conceptual design an AMB and perform material testing. Conceptual designs for radial and thrust AMBs were produced based on a hermetically-sealed sCO 2 machinery waste-heat recovery (WHR) application for sizing and loads, and choosing a target design temperature of 540°C useful for high-temperature sCO 2 turbines for concentrating solar power (CSP) applications. Conceptual designs were initially developed for multiple radial and thrust AMBs with spreadsheet-based calculations before selecting one of each to develop further using higher-fidelity design methods for magnetic and structural performance. It was found that the radial AMB at 540°C was feasible, but the thrust AMB needed to be limited to 315°C for high-speed operation. The decision for a reduced-temperature thrust AMB was the result of several significant conclusions: 1) Hiperco 50A, originally chosen for good magnetic performance at high temperature, had insufficient strength for high-speed operation, so it was replaced with 17-4 PH. 2) The reduced magnetic performance from 17-4 PH yielded a larger bearing size, reducing the strength margin. 3) This ultimately led to a creative design implementing a more-compact E-core topology, compared to the original (conventional) C-core, and an integral shaft-disk with Hirth joint connection. These conceptual designs are unique for the size and temperature in CO 2 , relevant for MW-scale CSP applications. Long term, high temperature test data was generated for several materials, filling a void in the current body of literature. Corrosion and magnetic performance measurements were produced for PM materials (Alnico 5-7C, Alnico 9C, and SmCo) with and without nickel-coating for environments of high-temperature CO 2 up to 550°C at atmospheric pressure and 450°C at 103 bar for up to 6,000 hours. Corrosion measurements were also produced for Hiperco 50, a SM material relevant for AMB laminations, with and without C5 coating. Comparisons were also made for 450°C and 550°C, atmospheric pressure air exposures up to 5,000 hours. Results generally show that coatings can be effective at improving oxidation resistance of the bare materials, and Alnicos generally outperformed SmCo after high-temperature exposure. In addition to technical feasibility demonstrated by the design, economic feasibility was demonstrated by updating the TEA from the reference machine, re-evaluating it with CAPEX and OPEX to reflect estimated changes from process-lubricated bearings to AMBs. AMBs were shown to be comparable in performance to process-lubricated bearings, still showing a notable improvement over conventional machinery architecture with oil-lubricated bearings.