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DOE OSTI2023

Dual-Purpose Canister Filling Demonstration Project Progress Report at ORNL, 2023

The US DOE Office of Nuclear Energy is investigating the feasibility of direct disposal of dual-purpose canisters (DPCs) in a hypothetical geological repository to offset the potential requirement to repackage spent nuclear fuel (SNF) from existing DPCs into smaller, disposal-ready canisters. Oak Ridge National Laboratory (ORNL) is currently evaluating the feasibility of filling void space in loaded DPCs with an engineered material to prevent a criticality event caused by groundwater/moderator intrusion. Metal alloys are being investigated as a filler material because of their relatively low viscosities when molten, which may facilitate their injection via an existing drainpipe that runs almost the full length of the DPC. ORNL’s strategy for evaluating filler viability includes simulations and physical demonstrations of filling and casting behavior, as well as evaluations of materials for compatibility in the repository environment. Filling of DPCs in this manner is expected to mitigate the risk associated with a post-closure criticality event during the repository performance assessment time frame (10,000 years or greater). Efforts in this fiscal year focused on (1) destructive analysis of experimental filler castings made in FY 2022, (2) a report outlining a conceptual design of a DPC filling facility (Fortner et al., 2023, M3SF 23OR010305044/ ORNL/SPR-2023/2921, May 31, 2023), (3) a report on affected features, events, and processes (FEPs) due to DPC filling (Price et al., 2023, M3SF-23SN010305093, issuance pending), (4) developing and testing a more practical alloy filler based upon a Sn-Al eutectic, and (5) modeling the heating and cooling dynamics of a DPC subjected to molten metal filling. The preliminary results from each of these tasks support the feasibility of filling DPCs with metal as a strategy against the possibility of criticality in the repository. The FY 2022 casting was found to penetrate even very small orifices in the mold and internal structures. Preliminary testing of the Sn-Al eutectic indicate little interaction of the melt with Zircaloy cladding. Thermal modelling shows that a filled DPC will cool to manageable temperatures within 2-3 days, which is likely manageable in a facility.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Fabrication and Testing of Solid-Solution Strengthened Corrosion Resistant Alloys For Service in Molten Fluoride Environments

The demand for higher system thermal efficiencies requires the operation of power generation cycles and heat conversion systems at progressively higher temperatures. As the system operating temperature increases, existing materials may not provide adequate mechanical properties or environmental compatibility or both. There is an increasing commercial interest in the development and deployment of liquid-fueled Molten Salt Reactors (MSRs). Hastelloy®N, the highest performing candidate MSR structural alloy, is not capable of operations at temperatures above 700°C, thus limiting the performance of these systems. Using an Integrated Computational Materials Engineering (ICME)-approach and small laboratory scale heats, ORNL developed a class of patented alloys covered by U.S. Patent 9, 435, 011 B2, “Creep-resistant, Cobalt-free alloys for high temperature, liquid-salt heat exchanger systems,” similar to Hastelloy®N in that they are primarily solid solution strengthened. In contrast to precipitation strengthened alloys, the microstructure of solid solution alloys and hence the high temperature mechanical properties are stable for extended periods of time allowing long reactor operating life. The new alloys have shown to possess good resistance to liquid fluorides at temperatures up to 850°C and have significantly improved creep properties when compared to Hastelloy®N. The purpose of the CRADA project was for ORNL to collaborate with Haynes International- a materials producer, MetalTek International- a foundry, and Kairos Power – an advanced reactor developer – to scale-up selected alloys, evaluate their properties, and identify one solid solution strengthened alloy that can meet the property requirements for the reactor being developed by Kairos Power and other similar liquid fluoride-salt cooled reactors. As part of the project, eight alloys were down-selected and fabricated in larger industrial scale heats by Haynes International. Resistance to molten salt was evaluated in flowing FLiNaK and FLiBe by Kairos Power using their Rotating Cage Loop (RCL) system. Accounting for iron deposition during these tests, the new alloys displayed very low net mass change showing excellent corrosion performance in molten salt. Creep properties evaluated at ORNL were found to be better than that of Hastelloy®N and 316 stainless steel. Long-term stabilities of the alloys evaluated by Haynes International showed that these alloys have excellent thermal stability in the temperature range 704.4-815.6°C, with the change in strength and ductility being less than 10-15% after a 4000-hour exposure at 815.6°C. Autogenously Gas Tungsten Arc Welding (GTAW) welded samples showed less than 10% change in yield strength / ultimate tensile strength / total elongation compared to the basemetal, indicating that the alloys have excellent weldability. Three parts were successfully investment-cast using one alloy with very little voiding showing feasibility of fabricating parts using the casting process. This project enabled extensive interaction between the material producer Haynes International, casting supplier MetalTek, and reactor developer Kairos Power. This facilitated testing of materials and components produced using the newly developed alloys by the end-user. This allowed the generation of critical dataset required for down-selection of a few promising alloys for further development. This data is also currently being shared with other reactor designers for them to evaluate the suitability of this alloy for their reactor design. The availability of this alloy will ultimately enable the design and development and deployment of MSRs with increased temperature of operation and thus, improved efficiencies.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2025

Fabrication and Testing of Solid-Solution Strengthened Corrosion Resistant Alloys For Service in Molten Fluoride Environments

The demand for higher system thermal efficiencies requires the operation of power generation cycles and heat conversion systems at progressively higher temperatures. As the system operating temperature increases, existing materials may not provide adequate mechanical properties or environmental compatibility or both. There is an increasing commercial interest in the development and deployment of liquid-fueled Molten Salt Reactors (MSRs). Hastelloy®N, the highest performing candidate MSR structural alloy, is not capable of operations at temperatures above 700°C, thus limiting the performance of these systems. Using an Integrated Computational Materials Engineering (ICME)-approach and small laboratory scale heats, ORNL developed a class of patented alloys covered by U.S. Patent 9,435,011 B2, “Creep-resistant, Cobalt-free alloys for high temperature, liquid-salt heat exchanger systems,” similar to Hastelloy®N in that they are primarily solid solution strengthened. In contrast to precipitation strengthened alloys, the microstructure of solid solution alloys and hence the high temperature mechanical properties are stable for extended periods of time allowing long reactor operating life. The new alloys have shown to possess good resistance to liquid fluorides at temperatures up to 850°C and have significantly improved creep properties when compared to Hastelloy®N. The purpose of the CRADA project was for ORNL to collaborate with Haynes International- a materials producer, MetalTek International- a foundry, and Kairos Power – an advanced reactor developer – to scale-up selected alloys, evaluate their properties, and identify one solid solution strengthened alloy that can meet the property requirements for the reactor being developed by Kairos Power and other similar liquid fluoride-salt cooled reactors. As part of the project, eight alloys were down-selected and fabricated in larger industrial scale heats by Haynes International. Resistance to molten salt was evaluated in flowing FLiNaK and FLiBe by Kairos Power using their Rotating Cage Loop (RCL) system. Accounting for iron deposition during these tests, the new alloys displayed very low net mass change showing excellent corrosion performance in molten salt. Creep properties evaluated at ORNL were found to be better than that of Hastelloy®N and 316 stainless steel. Long-term stabilities of the alloys evaluated by Haynes International showed that these alloys have excellent thermal stability in the temperature range 704.4-815.6°C, with the change in strength and ductility being less than 10-15% after a 4000-hour exposure at 815.6°C. Autogenously Gas Tungsten Arc Welding (GTAW) welded samples showed less than 10% change in yield strength / ultimate tensile strength / total elongation compared to the basemetal, indicating that the alloys have excellent weldability. Three parts were successfully investment-cast using one alloy with very little voiding showing feasibility of fabricating parts using the casting process. This project enabled extensive interaction between the material producer Haynes International, casting supplier MetalTek, and reactor developer Kairos Power. This facilitated testing of materials and components produced using the newly developed alloys by the end-user. This allowed the generation of critical dataset required for down-selection of a few promising alloys for further development. This data is also currently being shared with other reactor designers for them to evaluate the suitability of this alloy for their reactor design. The availability of this alloy will ultimately enable the design and development and deployment of MSRs with increased temperature of operation and thus, improved efficiencies.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Enabling Bipolar Membrane Manufacturing Using Microscopy

Bipolar membranes (BPMs) used for water treatment suffer from interface instabilities, causing premature failure and decreased performance. Recent research has highlighted the impacts of membrane morphology on mechanical behavior and performance. Improved material performance of thin film membranes requires enhanced transport properties coupled with better control of the mechanical characteristics to avoid premature failure of the film. Thus, morphology is a key parameter when developing and evaluating novel membrane materials. Microscopy offers unique advantages for nano-scale characterization of thin film membrane interfaces and morphologies. In this study, the interface junction of BPMs was evaluated using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). BPMs were fabricated using (1) hot pressing lamination, (2) bench-scale solution casting, and (3) roll-to-roll sequential casting (R2R). Both commercial and in-house fabricated ion exchange membranes were used in the BPMs. The BPMs were comprised of a cation exchange membrane and an anion exchange membrane with a catalyst layer sandwiched in between. Cross sectional SEM and EDX images of the membrane interface junction were compared among the different fabrication techniques and materials. The bench cast catalyst layers were nonuniform compared to the R2R and hot pressed membranes, demonstrating the importance of precise catalyst application conditions. Different thicknesses of the BPMs and individual membrane layers revealed that polymer solution concentration needs to be optimized during manufacturing. This work shows that microscopy can identify key processing parameters that affect BPM interface junction quality at the microscale to enable manufacturing of high performance BPMs.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Enabling Roll-to-Roll Manufacturing of Bipolar Membranes Using Microscopy

36 MATERIALS SCIENCE↗

NASA NTRS1973

Fabrication and life testing of thermionic converters

An unfueled converter containing a chloride-fluoride duplex tungsten emitter of 4.78 eV vacuum work function was tested for 46,647 hours at an emitter temperature of 1973 K and an electrode power output of about 8 watts/sq cm. The test demonstrated the superior and stable performance of the (110) oriented tungsten emitter at high temperatures. Three 90 UC-10 ZrC(C/U = 1.04, tungsten additive = 4 wt %) fueled converters were fabricated and tested at an emitter temperature of 1873 K. Converter containing chloride-arc-cast duplex tungsten cladding showed temperature thermionic performance and slower rate of performance drop than converter containing chloride-fluoride duplex tungsten cladding. This is believed to be due to the superior fuel component diffusion resistance of the arc-cast tungsten substrate used in the fuel cladding. It was shown that a converter containing a carbide fueled chloride-arc-cast duplex tungsten emitter with an initial electrode power output of 6.80 watts/sq cm could still deliver an electrode power output of 6.16 watts/sq cm after 18,632 hours of operation at an emitter temperature of 1873 K.

Yang, L.↗

NASA NTRS1951

Experimental Investigation of Air-Cooled Turbine Blades in Turbojet Engine. 7: Rotor-Blade Fabrication Procedures

An experimental investigation was conducted to determine the cooling effectiveness of a wide variety of air-cooled turbine-blade configurations. The blades, which were tested in the turbine of a - commercial turbojet engine that was modified for this investigation by replacing two of the original blades with air-cooled blades located diametrically opposite each other, are untwisted, have no aerodynamic taper, and have essentially the same external profile. The cooling-passage configuration is different for each blade, however. The fabrication procedures were varied and often unique. The blades were fabricated using methods most suitable for obtaining a small number of blades for use in the cooling investigations and therefore not all the fabrication procedures would be directly applicable to production processes, although some of the ideas and steps might be useful. Blade shells were obtained by both casting and forming. The cast shells were either welded to the blade base or cast integrally with the base. The formed shells were attached to the base by a brazing and two welding methods. Additional surface area was supplied in the coolant passages by the addition of fins or tubes that were S-brazed. to the shell. A number of blades with special leading- and trailing-edge designs that provided added cooling to these areas were fabricated. The cooling effectiveness and purposes of the various blade configurations are discussed briefly.

Long, Roger A.↗

NASA NTRS1976

An oxide dispersion strengthened Ni-W-Al alloy with superior high temperature strength

An experimental oxide dispersion strengthened (ODS) alloy, WAZ-D, derived from the WAZ-20 composition was produced by the mechanical alloying process. Cast WAZ-20 is strengthened by both a high refractory metal content, and 70 volume percent of gamma prime. The ODS alloy WAZ-D was responsive to variables of alloy content, of attritor processing, of consolidation by extrusion, and of heat treatment. The best material produced had large highly elongated grains. It exhibited tensile strengths generally superior to a comparable cast alloy. The ODS alloy exhibited high temperature stress rupture life considerably superior to any known cast superalloy. Tensile and rupture ductility were low, as was intermediate temperature rupture life. Very low creep rates were noted and some specimens failed with essentially no third stage creep. Also the benefit derived from the oxide dispersion, far out-weighed that from the elongated microstructure alone.

Glasgow, T. K.↗

NASA NTRS1976

Analysis of the survivability of the shuttle (ALT) fault-tolerant avionics system

An extension of the Complementary-Analytic-Simulative Technique (CAST) is presented which is applicable to the Shuttle Data Processing Subsystem (DPS). A two step process was used. The first step provides models, both analytic and simulative, for analysis of the Approach-Landing Test (ALT) configuration. The ALT modeling and analysis are presented. Since CAST had already been shown to be multicomputer systems, the emphasis was placed on extending the CAST concept so it is applicable to computer systems including the multiplicity of input and output devices found in a real-time control system application. The DPS mission-critical survivability for a six-hour mission was determined to be 0.999863 for the Shuttle ALT baseline configuration. Thus it can be said that for ALT, the survivability is adequate. However, the fact that orbiting missions of up to 30 days are planned illustrates the necessity of extending the ALT work to be applicable to OFT and actual mission scenarios. The above analysis led to the evaluation of three selected options which identified two areas of possible improvement. These improvements would result from use of a recovery technique which combines roll ahead with memory copy, and increased TACAN fault detectability.

Source record↗

NASA NTRS1977

Tensile and creep rupture properties of (16) uncoated and (2) coated engineering alloys at elevated temperatures

Sixteen test materials were supplied by NASA-Lewis Research Center as wrought bar or cast remelt stock. The cast remelt stock was cast into test blanks with two such materials being also evaluated after Jocoat coating was applied. Mechanical properties evaluated included tensile, modulus of elasticity, Poisson's Ratio, creep properties and creep rupture strength. Tests were conducted at temperatures applicable to the service temperature of the various alloys. This range extended from room temperature to 1000 C.

Fritz, L. J.↗

NASA NTRS1977

Containerless processing of beryllium

Melting and solidification of a beryllium alloy containing 1.5% BeO by weight in the weightless environment of space has produced cast beryllium with a relatively uniform dispersion of BeO throughout. Examination of the cast material shows that it is coarse grained, although the BeO is not heavily agglomerated in the flight specimen. Ground based comparison experiments show extreme agglomeration and segregation of BeO, resulting in large zones which are practically free of the oxide. Several postulated hypotheses for the failure to grain refine the beryllium are formulated. These are: (1) spherodization of the BeO particles during specimen preparation and during the molten phase of the experiment; (2) loss of nucleation potency through aging in the molten phase; and (3) inability of BeO to act as a grain refiner for beryllium. Further investigation with non spherodized particles and shorter dwell times molten may delineate which of these hypotheses are valid. The results of this flight experiment indicate that the weightless environment of space is an important asset in conducting research to find grain refiners for beryllium and other metals for which cast dispersions of grain refining agents cannot be prepared terrestrially due to gravitationally driven settling and agglomeration.

Wouch, G.↗

NASA NTRS1979

Evaluation of urethane for feasibility of use in wind turbine blade design

A preliminary evaluation was conducted of the use of cast urethane as a possible material for low-cost blades for wind turbines. Specimen test data are presented for ultimate tensile strength, elastic modulus, flexural strain, creep, and fatigue properties of a number of urethane formulations. Data are also included for a large-scale urethane blade section composed of cast symmetrical half-profiles tested as a cantilever beam. Based on these results, an analysis was conducted of a full-scale blade design of cast urethane that meets the design specifications of the rotor blades for the NASA/DOE experimental 100-kW MOD-0 wind turbine. Because of the low value of elastic modulus for urethane (around 457 000 psi), the design loads would have to be carried by metal reinforcement. Considerations for further evaluation are noted.

Lieblein, S.↗

NASA NTRS1980

Application of superalloy powder metallurgy for aircraft engines

In the last decade, Government/Industry programs have advanced powder metallurgy-near-net-shape technology to permit the use of hot isostatic pressed (HIP) turbine disks in the commercial aircraft fleet. These disks offer a 30% savings of input weight and an 8% savings in cost compared in cast-and-wrought disks. Similar savings were demonstrated for other rotating engine components. A compressor rotor fabricated from hot-die-forged-HIP superalloy billets revealed input weight savings of 54% and cost savings of 35% compared to cast-and-wrought parts. Engine components can be produced from compositions such as Rene 95 and Astroloy by conventional casting and forging, by forging of HIP powder billets, or by direct consolidation of powder by HIP. However, each process produces differences in microstructure or introduces different defects in the parts. As a result, their mechanical properties are not necessarily identical. Acceptance methods should be developed which recognize and account for the differences.

Dreshfield, R. L.↗

NASA NTRS1980

Mechanical properties of Al-mica particulate composite material

Cast aluminum alloy mica particle composites of varying mica content were tested in tension, compression, and impact. With 2.2 percent mica (size range 40-120 microns) the tensile and compression strengths of aluminum alloy decreased by 56 and 22 percent, respectively. The corresponding decreases in percent elongation and percent reduction are 49 and 39 percent. Previous work shows that despite this decrease in strength the composite with 2.5 percent mica and having an UTS of 15 kg/sq mm and compression strength of 28 kg/sq mm performs well as a bearing material under severe running conditions. The differences in strength characteristics of cast aluminum-mica particle composites between tension and compression suggests that, as in cast iron, expansion of voids at the matrix particle interface may be the guiding mechanism of the deformation. SEM studies show that on the tensile fractured specimen surface, there are large voids at the particle matrix interface.

Nath, D.↗

NASA NTRS1980

Development of low-cost directionally-solidified turbine blades

A low-cost directionally solidified (DS) casting of turbine blades of high stress rupture is discussed. The process uses an exothermically heated mold; a newly designed solid blade was cast for the high-pressure turbine of the TFE731-3 turbofan engine. Ni-based alloys Mar-M 247 and Mar-M 200 + Hf were used. The solid DS blade replaced a conventionally cast IN100 component; a 40% cost saving is expected, with a 2.4% reduction in the takeoff specific fuel consumption. The DS Mar-M 247 blade has been selected for production in the TFE731-3B-100, and advanced version of the TFE731-3.

Hoppin, G. S., III↗

NASA NTRS1982

Mechanical properties of low tantalum alloys

The mechanical property behavior of equiaxed cast B-1900 + Hf alloy as a function of tantalum content was studied. Tensile and stress rupture characterization was conducted on cast to size test bars containing tantalum at the 4.3% (standard level), 2.2% and 0% levels. Casting parameters were selected to duplicate conditions used to prepare test specimens for master metal heat qualification. The mechanical property results as well as results of microstructural/phase analysis of failed test bars are presented.

Kortovich, C. S.↗

NASA NTRS1983

Epoxy hydantoins as matrix resins

Tensile strength and fracture toughness of castings of the hydantoin resins cured with methylenedianiline are significantly higher than MY 720 control castings. Water absorption of an ethyl, amyl hydantoin formulation is 2.1 percent at equilibrium and Tg's are about 160 C, approximately 15 deg below the final cure temperature. Two series of urethane and ester-extended hydantoin epoxy resins were synthesized to determine the effect of crosslink density and functional groups on properties. Castings cured with methylenedianiline or with hexahydrophthalic anhydride were made from these compounds and evaluated. The glass transition temperatures, tensile strengths and moduli, and fracture toughness values were all much lower than that of the simple hydantoin epoxy resins. Using a methylene bishydantoin epoxy with a more rigid structure gave brittle, low-energy fractures, while a more flexible, ethoxy-extended hydantoin epoxy resin gave a very low Tg.

Weiss, J.↗

NASA NTRS1982

Creep-rupture behavior of 6 candidate stirling engine iron-base superalloys in high pressure hydrogen. Volume 1: Air creep-rupture behavior

Four wrought alloys (A-286, IN 800H, N-155, and 19-9DL) and two cast alloys (CRM-6D and XF-818) were tested to determine their creep-rupture behavior. The wrought alloys were used in the form of sheets of 0.89 mm (0.035 in.) average thickness. The cast alloy specimens were investment cast and machined to 6.35 mm (0.250 in.) gage diameter. All specimens were tested to rupture in air at different times up to 3000 h over the temperature range of 650 C to 925 C (1200 F to 1700 F). Rupture life, minimum creep rate, and time to 1% creep strain were statistically analyzed as a function of stress at different temperatures. Temperature-compensated analysis was also performed to obtain the activation energies for rupture life, time to 1% creep strain, and the minimum creep rate. Microstructural and fracture analyses were also performed. Based on statistical analyses, estimates were made for stress levels at different temperatures to obtain 3500 h rupture life and time to 1% creep strain. Test results are to be compared with similar data being obtained for these alloys under 15 MPa (2175 psi) hydrogen.

Bhattacharyya, S.↗