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At least 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
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 OSTI2025

Manufacturability and performance response of developed Ni-based alloys for reactor environments

Under the Advanced Materials and Manufacturing Technologies program, two Ni-based alloys fabricated by laser powder bed fusion (LPBF) at Oak Ridge National Laboratory and by laser powder directed energy deposition (LP-DED) at Idaho National Laboratory have been evaluated: γ′-strengthened Haynes 282 and solution-strengthened Inconel 625. Printing defects were observed in the LPBF 282 alloy fabricated using a Renishaw AM250 machine, likely due to particle spattering during printing. For both the LPBF and LP-DED 282 alloys, annealing at 1,180°C for 1 h resulted in partial recrystallization and a bimodal grain distribution, and subsequent aging for 4 h at 800°C led to the formation of a high density of nano-size γ′-strengthening precipitates. Creep testing performed at 750°C revealed lower creep life and ductility for the LPBF and LP-DED 282 compared with wrought 282. X-ray computed tomography combined with optical and scanning electron microscopy microstructural characterization revealed crack formation in the LPBF 282 alloy during creep testing, initiated either from printing defects or from creep cavitation at grain boundaries. Creep cavitation and cracking at grain boundaries were also observed for the LP-DED 282 alloy, and optimization of the printing strategies and postheat treatments will be needed to fabricate high-performance 282 components for high-temperature nuclear applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Manufacturability and performance response of developed Ni-based alloys for reactor environments

Under the Advanced Materials and Manufacturing Technologies program, two Ni-based alloys fabricated by laser powder bed fusion (LPBF) at ORNL and laser powder directed energy deposition (LP-DED) at INL have been evaluated: γ′-strengthened Haynes 282 and solution-strengthened Inconel 625. Printing defects were observed in the LPBF 282 alloy fabricated using a Renishaw AM250 machine, likely due to particle spattering during printing. For both the LPBF and LP-DED 282 alloys, annealing at 1,180°C for 1 h resulted in partial recrystallization and a bimodal grain distribution, while subsequent aging for 4 h at 800°C led to the formation of a high density of nano size γ′-strengthening precipitates. Creep testing performed at 750°C revealed lower creep life and ductility for the LPBF and LP-DED 282 compared with wrought 282. X-ray computed tomography combined with optical and scanning electron microscopy microstructural characterization revealed crack formation in the LPBF 282 alloy during creep testing, initiated either from printing defects or from creep cavitation at grain boundaries. Creep cavitation and cracking at grain boundaries were also observed for the LP-DED 282 alloy, and optimization of the printing strategies and post heat treatments will be needed to fabricate high performance 282 components for high temperature nuclear applications.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

SEM/EBSD Characterization of Baffle-Former Bolts Designated for High Energy X-ray Microscopy Studies at the Advanced Photon Source

This report documents the microstructural and surface characterization of two high-fluence baffle-former bolts (BFBs) harvested from a commercial pressurized water reactor (PWR) after nearly four decades of service. These bolts experienced extreme conditions including high neutron fluence, elevated temperatures, corrosive primary water, and sustained mechanical loads, all of which contribute to degradation mechanisms such as irradiation-assisted stress corrosion cracking (IASCC). Using scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), the study assessed bulk and near-surface microstructures, grain boundary characteristics, and in-service oxide layers. The results revealed significant differences between bolts exposed to 41 dpa and 29 dpa, including differences in recrystallization extent, deformation structures, and oxidation morphology. These findings establish critical baseline data for integration with advanced synchrotron-based high-energy X-ray microscopy (HEXM) and computational crystal plasticity models. Ultimately, the work supports improved mechanistic understanding and predictive capability regarding the long-term performance of reactor core internal components.

Lach, Tim [Oak Ridge National Laboratory (ORNL), O↗
DOE OSTI2024

Microstructure and Mechanical Properties of Ni-based Alloys Fabricated by Laser Powder Bed Fusion

The Advanced Materials and Manufacturing Technologies (AMMT) program is aiming at the accelerated incorporation of new materials and manufacturing technologies into nuclear-related systems. Complex Ni-based components fabricated by laser powder bed fusion (LPBF) could enable operating temperatures at T > 700°C in aggressive environments such as molten salts or liquid metals. However, available mechanical properties data relevant to material qualification remains limited, in particular for Ni-based alloys routinely fabricated by LPBF such as IN718 (Ni- 19Cr-18Fe-5Nb-3Mo) and Haynes 282 (Ni-20Cr-10Co-8.5Mo-2.1Ti-1.5Al). Creep testing was conducted on LPBF 718 at 600°C and 650°C and on LPBF 282 at 750°C. finding that the creep strength of the two alloys was close to that of wrought counterparts. with lower ductility at rupture. Heat treatments were tailored to the LPBF-specific microstructure to achieve grain recrystallization and form strengthening γ' precipitates for LPBF 282 and γ' and γ" precipitates for LPBF 718. In-situ data generated during printing and ex-situ X-ray computed tomography (XCT) scans were used to correlate the creep properties of LPBF 282 to the material flaw distribution. In- situ data revealed that spatter particles are the potential causes for flaws formation in LPBF 282. with significant variation between rods based on their location on the build plate. XCT scans revealed the formation of a larger number of creep flaws after testing in the specimens with a higher initial flaw density. which led to a lower ductility for the specimen.

Dryepondt, Sebastien↗
DOE OSTI2024

Chloride-Induced Stress Corrosion Cracking of Friction Stir-Welded 304L Stainless Steel: Effect of Microstructure and Temperature

Dry storage canisters of used nuclear fuels are fabricated using SUS 304L stainless steel. Chloride-induced stress corrosion cracking (CISCC) is one of the major failure modes of dry storage canisters. The cracked canisters can be repaired by friction stir welding (FSW), a low-heat input ‘solid-phase’ welding process. It is important to evaluate the ClSCC resistance of the friction stir welded material. Stress corrosion cracking (SCC) studies were carried out on mill-annealed base materials and friction stir welded 304L stainless U-bend specimens in 3.5% NaCl + 5 N H2SO4 solution at room temperature and boiling MgCl2 solution at 155 °C. The engineering stress on the outer fiber of the FSW U-bend specimen was ~60% higher than that of the base metal (BM). In spite of the higher stress level of the FSW, both materials (FSW and BM) showed almost similar SCC failure times in the two different test solutions. The SCC occurred in the thermo-mechanically affected zone (TMAZ) of the FSW specimens in the 3.5% NaCl + 5 N H2SO4 solution at room temperature, while the stirred zone (SZ) was relatively crack-free. The failure occurred at the stirred zone when tested in the boiling MgCl2 solution. Hydrogen reduction was the cathodic reaction in the boiling MgCl2 solution, which promoted hydrogen-assisted cracking of the heavily deformed stirred zone. The emergence of the slip step followed by passive film rupture and dissolution of the slip step could be the SCC events in the 3.5% NaCl + 5 N H2SO4 solution at room temperature. However, the slip step height was not sufficient to cause passivity breakdown in the fine-grained SZ. Therefore, the SCC occurred in the partially recrystallized softer TMAZ. Overall, the friction-stirred 304L showed higher tolerance to ClSCC than the 304L base metal.

304L austenitic stainless steel↗
DOE OSTI2020

Dynamic Shear Deformation of a Precipitation Hardened Al 0.7 CoCrFeNi Eutectic High-Entropy Alloy Using Hat-Shaped Specimen Geometry

Lamellar eutectic structure in Al 0.7 CoCrFeNi high-entropy alloy (HEA) is emerging as a promising candidate for structural applications because of its high strength-ductility combination. The alloy consists of a fine-scale lamellar fcc + B2 microstructure with high flow stresses > 1300 MPa under quasi-static tensile deformation and >10% ductility. The response to shear loading was not investigated so far. This is the first report on the shear deformation of a eutectic structured HEA and effect of precipitation on shear deformation. A split-Hopkinson pressure bar (SHPB) was used to compress the hat-shaped specimens to study the local dynamic shear response of the alloy. The change in the width of shear bands with respect to precipitation and deformation rates was studied. The precipitation of L1 2 phase did not delay the formation of adiabatic shear bands (ASB) or affect the ASB width significantly, however, the deformed region around ASB, consisting of high density of twins in fcc phase, was reduced from 80 μm to 20 μm in the stronger precipitation strengthened condition. We observe dynamic recrystallization of grains within ASBs and local mechanical response of individual eutectic lamellae before and after shear deformation and within the shear bands was examined using nano-indentation.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Transient Microstructure Evolutions and Local Properties of Dual-Phase 980 MPa Grade Steel Via Friction Stir Spot Processing

Friction stir processing is a novel solid-state process to modify microstructures and their properties by intense, localized plastic deformation. However, little research has been reported for microstructure evolutions of advanced high-strength steels during the process. The present work focuses on the study of transient microstructure changes and local mechanical properties for friction stir spot processed dual-phase (DP) 980 MPa grade steel (DP980) under different peak temperatures. A pinless silicon nitride ceramic tool was used to produce relatively simple material deformation and flow near the tool. Friction stir spot processed steel samples were characterized by optical and electron microscopies. Furthermore, Vickers microhardness and nano-indentation measurements were used to study local mechanical properties for correlation with microstructures. A swallow layer of refined grains (<0.6 µm) was obtained with a low peak temperature (under 400 °C), whereas higher peak temperatures (>Ac 1 ) led to a change in grain size with different microstructures (fine-grained DP or martensite). Electron back-scattered diffraction characterizations revealed a large deformation in the as-received microstructures (mixture of ferrite and tempered martensite) induced by friction stir spot processing, leading to recrystallization and grain refinement around the stirred zone. Also, nano-indentation measurements showed a higher hardness than the hardness of the as-received DP980. Friction stir processing with different process conditions effectively changed microstructures and local mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Evaluation of Equiatomic CrMnFeCoNiCu System and Subsequent Derivation of a Non-Equiatomic MnFeCoNiCu Alloy

Investigation into non-equiatomic high-entropy alloys has grown in recent years due to questions about the role of entropy stabilization in forming single-phase solid solutions. Non-equiatomic alloys have been shown to retain the outstanding mechanical properties exhibited by their equiatomic counterparts and even improve electrical, thermal, and magnetic properties, albeit with relaxed composition bounds. However, much remains to understand the processing–structure–property relationships in all classes of so-called high-entropy alloys (HEAs). Here, we are motivated by the natural phenomena of crystal growth and equilibrium conditions to introduce a method of HEA development where controlled processing conditions determine the most probable and stable composition. This is demonstrated by cooling an equiatomic CrMnFeCoNiCu alloy from the melt steadily over 3 days (cooling rate ~4 °C/h). The result is an alloy containing large Cr-rich precipitates and an almost Cr-free matrix exhibiting compositions within the MnFeCoNiCu system (with trace amounts of Cr). From this juncture, it is argued that the most stable composition is within the CrMnFeCoNiCu system rather than the CrMnFeCoNi system. With further optimization and evaluation, a unique non-equiatomic alloy, Mn 17 Fe 21 Co 24 Ni 24 Cu 14 , is derived. The alloy solidifies and recrystallizes into a single-phase face-centered cubic (FCC) polycrystal. In addition to possible applications where Invar is currently utilized, this alloy can be used in fundamental studies that contrast its behavior with its equiatomic counterpart and shed light on the development of HEAs.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Microstructural Transitions during Powder Metallurgical Processing of Solute Stabilized Nanostructured Tungsten Alloys

Exploiting grain boundary engineering in the design of alloys for extreme environments provides a promising pathway for enhancing performance relative to coarse-grained counterparts. Due to its attractive properties as a plasma facing material for fusion devices, tungsten presents an opportunity to exploit this approach in addressing the significant materials challenges imposed by the fusion environment. Here, we employ a ternary alloy design approach for stabilizing W against recrystallization and grain growth while simultaneously enhancing its manufacturability through powder metallurgical processing. Mechanical alloying and grain refinement in W-10 at.% Ti-(10,20) at.% Cr alloys are accomplished through high-energy ball milling with transitions in the microstructure mapped as a function of milling time. We demonstrate the multi-modal nature of the resulting nanocrystalline grain structure and its stability up to 1300 °C with the coarser grain size population correlated to transitions in crystallographic texture that result from the preferred slip systems in BCC W. Field-assisted sintering is employed to consolidate the alloy powders into bulk samples, which, due to the deliberately designed compositional features, are shown to retain ultrafine grain structures despite the presence of minor carbides formed during sintering due to carbon impurities in the ball-milled powders.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Structure Analysis of Natural Wangdaodeite—LiNbO3-Type FeTiO3

This paper reports the first structure refinement of natural wangdaodeite, LiNbO3-type FeTiO3 from the Ries impact structure. Wangdaodeite occurs together with recrystallized ilmenite clasts in shock melt veins which have experienced peak shock pressures of between 17 and 22 GPa. Comparison of natural and synthetic wangdaodeite points toward a correlation between the distortion of ferrate- and titanate-polyhedra and the c/a ratio of the unit cell. The Raman spectrum of wangdaodeite is calculated based on the refined structure. Comparison to the reported spectrum of the type-material shows that the Raman peak at 738–740 cm−1 is indicative for this phase, whereas other features in type-wangdaodeite are tentatively assigned to disordered ilmenite.

58 GEOSCIENCES↗
DOE OSTI2021

Novel Poly-Si:Ga/SiOx Passivating Contacts through Non-Equilibrium Doping

Poly-Si/SiOx passivating contacts are one of the key enablers for high-efficiency, low-cost c-Si solar cells. In recent years, record devices have reached efficiencies of 26% in the laboratory and 25% in the industry. The current cell structure utilizing a tunneling oxide passivating contact structure with a back phosphorus-doped poly- Si/SiOx passivating contact and a front boron diffused emitter suffers from large emitter recombination. Thus, replacing the front B diffused emitter with a p-type passivating contact is a route to overcome this deficiency. This gives rise to front/back poly-Si based passivating contacts. To address the low passivation performance of the B-doped poly-Si passivating contacts, we replace B with Ga as a novel p-type dopant to avoid dopant accumulation in the tunneling oxide, which is known to lead to large degradation loss in passivation quality. Here, we introduce a non-equilibrium method via pulsed laser melting to thermally melt and recrystallize the poly-Si and redistribute the dopants, achieving doping concentrations above the solid solubility limit (~4E19 cm-3). We demonstrate a good passivation quality with an iVoc of 721 mV with an active Ga doping concentration in poly-Si >1020 cm-3. Furthermore, we show a low contact resistivity of 33.2 +/- 9.3 mO cm2 using a diode model calculation. Finally, cross-section scanning spreading resistance microscopy was performed to determine the resistance profile across the non-homogeneously doped poly-Si layer.

c-Si↗
DOE OSTI2022

Local Thermomechanical Processing for Improving Formability of High Strength Aluminum Sheets

Limited room temperature formability hinders the wide-spread use of high strength aluminum alloys in structural body-in-white parts. Stamping or extrusion at warm temperatures or from softer tempers are the current solutions. In this work, our approach is to start with age-hardened sheets from 7xxx and 6xxx family of alloys and improve their formability using local thermomechanical processing only in the regions demanding highest ductility in the forming processes. We achieved local formability improvements with friction stir processing and introduce another process named roller-bending as a concept and showed its feasibility through finite element simulations. Initial results from FSP indicated significant deformation in the processed zones with minimal sheet distortion. FSP also resulted in dynamically recrystallized, fine grained (d < 5 µm) microstructures in the processed regions with textures significantly different from the base material. This resulted in formability improvements of > 30% in 7085-T76 and > 50% in 6111-T6 alloys as measured by minimum bend radius (r/t) ratios established with V-bending tests performed at 90° and 180° bend angles. Based on the encouraging initial results, we envision applicability of these processes in both pre- and post-stamping stages through integration of the process tools as end-effectors to robotic arms.

Nasim, Wahaz↗
DOE OSTI2022

Measuring Very Low Radiation Doses in PTFE for Nuclear Forensic Enrichment Reconstruction

Every country that has made nuclear weapons has used uranium enrichment. Despite the centrality of this technology to international security, there is still no reliable physical marker of past enrichment that can be used to perform forensic verification of historically produced weapons. We show that the extremely low radioactivity from uranium alpha emissions during enrichment leaves detectable and irreversible calorimetric signatures in the common enrichment gasket material PTFE, allowing for historical reconstruction of past enrichment activities at a sensitivity better than one weapon's quantity of highly enriched uranium. Fast scanning calorimetry also enables the measurement of recrystallization enthalpies of sequentially microtomed slices, confirming the magnitude and the type of radiation exposure while also providing a detection of tampering and a method for analyzing field samples useful for treaty verification. This work opens the door for common items to be turned into precise dosimeters to detect the past presence of radioactivity, nuclear materials, and related activities with high confidence.

Connick, Rachel↗
DOE OSTI2020

A FEASIBILITY STUDY ON CRACK REPAIR IN AUSTENITIC STAINLESS STEEL DRY STORAGE CANISTERS USING ISOTHERMAL FRICTION STIR WELDING

In recent time, solid state crack repair techniques in spent nuclear fuel dry storage canisters (SNF-DSC) have garnered significant interest. Plates of austenitic stainless steels are usually arc welded to fabricate the cylindrical canisters which are prone to chloride-induced stress corrosion cracking. Friction stir welding (FSW) is considered to be a potential candidate for damage repair. In this work, electrical discharge machining was used to simulate cracks in 304L stainless steel plates of 12.7 mm thickness. Subsequently, isothermal FSW was carried out at two different temperatures (725 and 825°C) in order to repair the simulated crack. Microstructure-mechanical property correlations in FSWed plates were studied in detail. Significant grain refinement observed in the stir zone (SZ) was attributed to dynamic recrystallization occurring during FSW. A comparison of Vickers microhardness showed higher hardness and homogeneity in the 725°C SZ than its 825°C counterpart. The fraction of S3 boundary is found to be low in the SZ as compared to base metal (BM). Yield strength of the joints was found to be approximately 100 MPa higher than that of the BM accompanied by a drop in ductility by a factor of 2. Residual stress profile across 825°C weld was measured using x-ray diffraction.

Bhattacharyya, Madhumanti↗
DOE OSTI2020

Method for the preparation of uniform triaminotrinitrobenzene microparticles

A new, rapid and inexpensive synthesis method for monodispersed triaminotrinitrobenzene (TATB) microparticles based on micelle-confined precipitation that enables control of microscopic morphology. The morphology of the TATB microparticles can be tuned between quasi-spherical and faceted by controlling the speed of recrystallization. The method enables improved performance and production consistency of TATB explosives for military grade explosives and propellants

36 MATERIALS SCIENCE↗
DOE OSTI2021

Corrosion and creep resistant high Cr FeCrAl alloys

An alloy includes in weight % based upon the total weight of the alloy: 28-35% Cr; 2.5-4% Al; 0.8-2% Nb; 5.5-7.5% W; 0-0.5% Mo; 0-0.3% Ti; 0.1-0.3% Zr; 0.1-1% Si; 0-0.07% Y; 0-2% Mn; 0-1% Ni; 0-0.05% C; 0-0.015% B; 0-0.02% N; 0.02-0.04 Ce; balance Fe. The alloy includes a recrystallized, equi-axed grain structure, and forms an external alumina scale, and has strengthening particles including Fe2M (M: Nb, W, Mo, and Ti) type C14 Laves-phase, and a BCC ferritic matrix microstructure from room temperature to melting point with less than 1% FCC-phase, less than 1% martensite phase, less than 0.5 wt. % of carbides (MC and M23C6), and at least 1% tensile elongation at room temperature. The alloy provides a creep resistance of greater than 3000 to 15000 h creep rupture life at 750° C. and 50 MPa, or greater than 500 to 5000 h creep rupture life at 700° C. and 100 MPa.

Yamamoto, Yukinori↗
DOE OSTI2021

Colossal Grains for a New Structural Paradigm in Thin-Film Photovoltaics

II-VI based thin-film photovoltaics (PV) have experienced substantial commercial success on a foundation of fast large-scale deposition and processing. This type of processing, regardless of material type, nearly always results in small grain (nm to several um diameters) polycrystalline material that, if not for effective grain boundary (GB) and defect passivation, would severely limit PV performance. In the case of CdTe based PV technology, the nearly ubiquitous CdCl2 treatment is used, in part, to passivate the polycrystalline p-type absorber even though Cl is known to (and used to) compensate p-type II-VI materials. Given that VOC is still the most limited performance metric and it can only be improved through higher p-type absorber concentrations, CdCl2 treatments may be holding the technology back. In this talk, we will discuss results related to a process by which small grain CdSeTe material is rapidly transformed into very large grain material (100-1000um diameters, Fig. 1a). This explosive recrystallization, which we have termed colossal grain growth (CGG), occurs by a Cl free process with thin films (<10um) deposited using the same fast deposition techniques the industry has relied on for more than a decade. Our modeling suggests that GB recombination becomes significantly less important at these grain sizes and thus may eliminate the need for a CdCl2 treatment. This result is complimented by previous results of epitaxial growth at high rates on single crystal seed layers. Thin CdSeTe CGG seed layers can be used for rapid epitaxy of CdTe to complete a standard device stack (Fig.1b). This is an optimistic view and the current limitations and challenges related to this process and these materials will also be discussed, including alloy and substrate roughness sensitivity, intragrain material quality, and complex defect chemistry. These challenges are not insignificant but overcoming them may enable a new structural paradigm for thin-film PV.

CdTe↗