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DOE OSTI2013

Embedded Piezoresistive Microcantilever Sensors Functionalized for the Detection of Methyl Salicylate

Sensors designed to detect the presence of methyl salicylate (MeS) have been tested. These sensors use a sensor platform based on the embedded piezoresistive microcantilever (EPM) design. Sensing materials tested in this study included the polymer poly (ethylene vinyl acetate), or PEVA as well as a composite sensing material consisting of the enzyme SA-binding protein 2, or SABP-2. The SABP-2 was immobilized within a biocompatible Hypol gel matrix. The PEVA-based sensors exhibited slower but reversible responses to MeS vapors, recovering fully to their initial state after the analyte was removed. SABP-2 sensors exhibited faster overall response to the introduction of MeS, responding nearly instantly. These sensors, however, do not recover after exposures have ended. Sensors using the SABP-2 sensing materials act instead as integrating sensors, measuring irreversibly the total MeS dose obtained.

36 MATERIALS SCIENCE↗

DOE OSTI2015

NEET Enhanced Micro Pocket Fission Detector for High Temperature Reactors - FY15 Status Report

A new project, that is a collaboration between the Idaho National Laboratory (INL), the Kansas State University (KSU), and the French Atomic Energy Agency, Commissariat à l'Énergie Atomique et aux Energies Alternatives, (CEA), has been initiated by the Nuclear Energy Enabling Technologies (NEET) Advanced Sensors and Instrumentation (ASI) program for developing and testing High Temperature Micro-Pocket Fission Detectors (HT MPFD), which are compact fission chambers capable of simultaneously measuring thermal neutron flux, fast neutron flux and temperature within a single package for temperatures up to 800 °C. The MPFD technology utilizes a small, multi-purpose, robust, in-core parallel plate fission chamber and thermocouple. As discussed within this report, the small size, variable sensitivity, and increased accuracy of the MPFD technology represent a revolutionary improvement over current methods used to support irradiations in US Material Test Reactors (MTRs). Previous research conducted through NEET ASI1-3 has shown that the MPFD technology could be made robust and was successfully tested in a reactor core. This new project will further the MPFD technology for higher temperature regimes and other reactor applications by developing a HT MPFD suitable for temperatures up to 800 °C. This report summarizes the research progress for year one of this three year project. Highlights from research accomplishments include: A joint collaboration was initiated between INL, KSU, and CEA. Note that CEA is participating at their own expense because of interest in this unique new sensor. An updated HT MPFD design was developed. New high temperature-compatible materials for HT MPFD construction were procured. Construction methods to support the new design were evaluated at INL. Laboratory evaluations of HT MPFD were initiated. Electrical contact and fissile material plating has been performed at KSU. Updated detector electronics are undergoing evaluations at KSU. A project meeting was held at KSU to discuss the roles and responsibilities between INL and KSU for development of the HT MPFDs. Provide input to various irradiation programs for installation of the MPFD technology in irradiation tests. As documented in this report, FY15 funding has allowed the project to meet year one planned accomplishments to develop a HT MPFD that offers US MTR users enhanced capabilities for real-time measurement of flux and temperature with a single detector. In addition, the accomplishments of this project have attracted funding from other Department of Energy Office of Nuclear Energy (DOE-NE) programs for additional applications. The work in those programs will build on current activities completed in this NEETASI HT MPFD project, but the MPFD will be specifically tailored to meet their program needs.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2024

Corrosion Testing of Bubbler Materials for LAW Vitrification (Rev. 0)

This work involved crucible-scale corrosion tests using coupons of selected materials in the baseline glass formulations for the seven LAW Sub-Envelopes. The tests were performed with Inconel 690 and MA 758; per the Test Plan, selected tests were also performed with a proprietary high temperature alloy supplied by SRTC. Coupons of these materials were tested for their corrosion resistance to LAW baseline glasses in two test series: the first series was with a baseline glass only, the second series was with a baseline glass and an added salt layer.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Digital image correlation and infrared thermography data for seven unique geometries of 304L stainless steel

Material Testing 2.0 (MT2.0) is a paradigm that advocates for the use of rich, full-field data, such as from digital image correlation and infrared thermography, for material identification. By employing heterogeneous, multi-axial data in conjunction with sophisticated inverse calibration techniques such as finite element model updating and the virtual fields method, MT2.0 aims to reduce the number of specimens needed for material identification and to increase confidence in the calibration results. To support continued development, improvement, and validation of such inverse methods—specifically for rate-dependent, temperature-dependent, and anisotropic metal plasticity models—we provide here a thorough experimental data set for 304L stainless steel sheet metal. The data set includes full-field displacement, strain, and temperature data for seven unique specimen geometries tested at different strain rates and in different material orientations. Commensurate extensometer strain data from tensile dog bones is provided as well for comparison. We believe this complete data set will be a valuable contribution to the experimental and computational mechanics communities, supporting continued advances in material identification methods.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Foam Fracturing Study for Stimulation Development of Enhanced Geothermal Systems

This is a final technical report for the project: Foam Fracturing Study for Stimulation Development of Enhanced Geothermal Systems (EGS). The goal is to demonstrate the feasibility of foam fracturing in EGS applications. The project, led by Oak Ridge National Laboratory (ORNL), was conducted in collaboration with Temple University. The report describes the research activities with Task 1 at ORNL: foam fracturing testing system development and experimental study on foam fracturing, and Task 2 at Temple University: foam testing and foam characterization. Main findings are: 1. A foam fracturing test system has been developed at ORNL, which can be used to perform foam fracturing under pressure up to 6,000 psi. The system monitors foam density during fracturing online and is capable of testing materials in both monotonic and cyclic (up to 50 Hz) injections. 2. Foam fracturing tests were carried out on Charcoal black granite specimens with a blind borehole to the middle length. Two diameters of blind borehole were tested; G2 series: 9.53 mm and G3 series: 4.76 mm. N2-in-water foam was used with AOS as a surfactant. 3. There was a hole-size effect on fracture initiation pressure. The effect is smaller in the case of foam, which was influenced by the high penetrability of gas in foam. Breakdown pressure showed a behavior just as that of fracture pressure; namely an increased value for small hole samples, while the effect in water fracture was more impressive than in foam fracture. 4. Water mass was reduced in foam fracturing within similar range of breakdown pressures. In G2 series, it was decreased from 10.44 g for water fracturing to 5.17 g, representing more than 50% water reduction. Therefore, there is the potential to reduce water use in EGS stimulation through foam fracturing. 5. Use of cyclic injection has the potential to reduce the breakdown pressure and seismicity in EGS application. Experiments using 4-s cycle period found that specimens can be fractured with a low number of cycles. The fatigue pressure was approximately 64 - 77% of monotonic breakdown pressure for water fracturing and 58 - 94% of the breakdown pressure for foam fracturing. 6. A foam stability testing system has been developed that can test foam at 220 Deg C to 2,000 psi. Tested components of candidate foams included two gases: N2 and CO2; 4 surfactants: AOS, SDS, NP-40 and CTAC; 5 stabilizing agents: guar, bentonite clay, borate salt, silica NPs, and GO. 7. N2 and AOS provided the most stable performance over the tested ranges. Furthermore, the AOS foam with stabilizing agents of guar and borate salt (crosslinker) offered the highest half-life of 20 minutes at 200 Deg C and 1,000 psi. 8. Arrhenius equation and modified power law have been demonstrated to fit well the half-time vs. temperature and pressure data, respectively. These relations can be useful to provide the suggestion for future foam stability study. This submission contains the supporting data developed during the project: 1) A final technical report 2) Granite fracturing data in monotonic and cyclic injections with water and N2 foam Foam performance data in various temperatures and pressures, including half-time, is submitted separately.

15 GEOTHERMAL ENERGY↗

DOE OSTI2023

Collaborative R&D with First Solar on Understanding Performance Limitations in CdTe (Project 1 "CdTe" - Mods 0-10, 13, 14-A1, 17)

This CRADA involves analyses on a variety of CdTe and CdTe-PV related materials, test structures, and solar cells produced at FSLR or NREL. Single-crystal (sx) material will be primarily MBE grown and provided by FSLR. Joint activities are focused on establishing the appropriate quality metrics as a basis for high performing sx devices and to study the dopability of the material. Polycrystalline (px) materials will be provided by NREL, FSLR, or fabricated jointly. Px activities are focused on the characterization of performance limiting mechanisms including bulk defects, grain boundaries, and the hetero-interface. A combination of growth, characterization, and theory will be applied. Analysis will include techniques that are well established in CdTe research at NREL (e.g., LIV/DIV/CV, AS/DLTS, LTPL, TRPL) as well as techniques that have not been widely applied to the PV part of CdTe technology (e.g., PCD, CL, uPL, SE).

14 SOLAR ENERGY↗

DOE OSTI2024

Nuclear Structural Component Relevant Properties of Nickel-Based Alloys Produced via Additive Manufacturing

Idaho National Laboratory initiated examination of nickel-based alloys manufactured via three different additive manufacturing methods for potential applications in nuclear, high temperature structural components. The three methods analyzed included laser powder bed fusion, blown powder laser directed energy deposition, and wire-fed gas metal arc directed energy deposition. With the rapid push towards additive manufacturing, codes do not exist that definitively define what is or is not tolerable for each process and application, such as with conventional, wrought products. This report contains the initial work to understand possible manufacturing methods for high temperature alloys, and specifically, void formation, microstructure evolution, corrosion, and mechanical properties. To generate mechanical test data, specimens were tested irrespective of voids and microstructures were analyzed to better understand how to negate/improve these issues. The preliminary results showed major decreases in mechanical performance for material tested. Test specimens will continue to be produced to further improve each additive manufacturing processes, quantify void acceptance, and better understand the most suitable high temperature alloys receptive to additive manufacturing and high temperature nuclear applications.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Solvari SR, Simplifying Residential Solar to 1 SKU, with Extended Testing

Accelerated weathering and material compatibility testing for polymeric and asphaltic materials. NLR will be testing the durability of the polymeric materials proposed for use in the supporting structures designed by TESCI solar. This will include the bare materials and coupons attached to asphalt shingles. The exposure will be in damp heat and separately heat, humidity and UV light, all followed by mechanical evaluation. Modification 1 is an extension of the first round of testing with both a continuation of some of the same testing and addition of new testing methods and materials. The testing of materials in the condition of A3 looking at mechanical durability will be continued looking at the materials used in the mounting brackets. We will be adding in testing of the silicone adhesive to the module and of the module itself. For the mounting brackets, testing will also be conducted at multiple temperatures and humidity levels to allow for extrapolation to the field.

14 SOLAR ENERGY↗

DOE OSTI2012

Characterization of the physical properties for solid granular materials

Accurate prediction of the behavior of a system is strongly governed by the components within that system. For multiphase systems incorporating solid powder-like particles, there are many different physical properties which need to be known to some level of accuracy for proper design, modeling, or data analysis. In the past, the material properties were determined initially as a secondary part of the study or design. In an attempt to provide results with the least level of uncertainty, a procedure was developed and implemented to provide consistent analysis of several different types of materials. The properties that were characterized included particle sizing and size distributions, shape analysis, density (particle, skeletal and bulk), minimum fluidization velocities, void fractions, particle porosity, and assignment within the Geldart Classification. In the methods used for this experiment, a novel form of the Ergun equation was used to determine the bulk void fractions and particle density. Materials of known properties were initially characterized to validate the accuracy and methodology, prior to testing materials of unknown properties. The procedures used yielded valid and accurate results, with a high level of repeatability. A database of these materials has been developed to assist in model validation efforts and future designs. It is also anticipated that further development of these procedures wil be expanded increasing the properties included in the database.

36 MATERIALS SCIENCE↗

DOE OSTI2025

High Temperature Gas Cooled Reactor Materials

Overview of high temperature materials testing within the ART Gas Cooled Reactor Program. Covers 800H weldment creep testing and Alloys 617 and 709 creep and creep-fatigue crack growth rate testing.

36 - MATERIALS SCIENCE↗

DOE OSTI2018

Fracture Resistance of Cast Stainless Steels after Thermal Aging for up to 10000 Hours

This work package, Cast Stainless Steel Aging, aims to achieve a comprehensive scientific understanding on the aging and failure phenomena in cast austenitic stainless steels (CASSs) using holistic experimental and modeling means and to provide a practical and science-based model to predict the degree of thermal degradation of CASS components in extended-term operations. The test materials in the project include four model CASSs (CF3, CF3M, CF8, and CF8M), four EPRI-provided CASSs (CF3, two CF8s, and CF8M), and two reference wrought materials (304L and 316L), which contain a wide variety of d-ferrite contents (2–33%). These materials have been thermally aged at two light water reactor (LWR)-relevant temperatures (290 and 330°C) and at two accelerated-aging temperatures (360 and 400°C) for up to three years. In the fiscal year, the fracture toughness testing and J-R curve calculation were completed for the ten CASS and wrought materials aged up to 10,000 hours. This report is to present the results of the static fracture (J-R) testing for the model and EPRI-provided CASS materials after thermal aging up to 10,000 hours. First, a new aging parameter (A) was defined to present the aging degradation of mechanical properties against the common variable. This definition is used to scale an aging time at a temperature to the effective aging time at a reference temperature based on Arrhenius equation, which is a rate theory equation for thermally activated mechanisms.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Imminent: Irradiation Testing of (Th,Pu)O{sub 2} Fuel - 13560

Commercial-prototype thorium-plutonium oxide (Th-MOX) fuel pellets have been loaded into the material test reactor in Halden, Norway. The fuel is being operated at full power - with instrumentation - in simulated LWR / PHWR conditions and its behaviour is measured 'on-line' as it operates to high burn-up. This is a vital test on the commercialization pathway for this robust new thoria-based fuel. The performance data that is collected will support a fuel modeling effort to support its safety qualification. Several different samples of Th-MOX fuel will be tested, thereby collecting information on ceramic behaviours and their microstructure dependency. The fuel-cycle reasoning underpinning the test campaign is that commercial Th- MOX fuels are an achievable intermediate / near-term SNF management strategy that integrates well with a fast reactor future. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2015

Final Technical Report: Electromagnetic Pump Insulation Materials Development and Testing (PLM-DOC-0005-2465) Report # DOEGEHB00613

Final Technical Report: Electromagnetic Pump Insulation Materials Development and Testing (Report # DOEGEHB00613) summarizes the information gathered from the analysis of the 160 m3/min EM Pump insulation that was tested in 2000-2002 and additional evaluations of new resilient, engineered insulation system evaluated and tested at both GRC and ANL. This report provides information on Tasks 1 and 2 of the entire project. This report also provides information in three broad areas: Historical and current data; Conclusions based on test data; and Insulation specifications for use in EM Pumps. The research for Task 2 builds upon Task 1: Update EM Pump Databank, which is summarized within this report. Where research for Task 3 and 4 Next-Generation EM Pump Analysis Tools identified parameters or analysis model that benefits Task 2 research, those items are noted within this report. The important design variables for the manufacture and operation of an EM Pump that the insulation research can evaluate are: space constraints; voltage capability of insulation system; maximum flux density through iron; flow rate and outlet pressure; efficiency and manufacturability. The development summary of the Electromagnetic Pump Insulation Materials Development and Testing was completed to include: Historical and current data; Conclusions based on test data; and Insulation specifications for use in EM Pumps.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Evaluation of High Temperature Elastomers for Geothermal Wells

This report describes the extension of a performance screening study of elastomers for geothermal well applications. Elastomeric O-rings were subjected to compression while submerged in water at elevated temperatures and pressure to determine performance under more aggressive conditions. Following the experiment, the elastic moduli of the O-ring cross-sections were assessed for any changes which may affect O-ring function down-hole. All materials showed susceptibility to thermo-oxidative degradation at high temperatures and pressures. Type I FKM had the least amount of compression set of all materials tested at 150ºC while Kalrez FFKM O-rings had the least amount of edge hardening of all materials, regardless of aging temperature. Prior visual observation of materials aged in simulated environments revealed an unusual trend with EPDM and FEPM materials: the degradation and disintegration of these polymers in an oxidative thermal cycle environment, but the ability to maintain mechanical performance and shape during oxidative thermal cycling in the presence of steam. EPDM and FEPM were subjected to additional testing at SNL in order to better understand this aging anomaly. No abnormalities were observed in the chemical (oxidation rates, FTIR spectra, solvent uptake, gel content, and weight loss vs. temperature) or physical (modulus profiles) measurements that could explain the visually observed aging differences. SNL validated this observation through a secondary controlled aging test using only EPDM, where, once again, it was shown that thermo-oxidative conditions appear to cause more degradative damage (enhanced embrittlement) than did thermo-oxidative coupled with hydrolytic environments. From these data we conclude that water may favorably interfere with normal thermo-oxidative degradation processes via some type of inhibition pathway which has yet to be identified.

15 GEOTHERMAL ENERGY↗

DOE OSTI2020

An Overview of the Hybrid Illinois Device for Research and Applications Material Analysis Test-stand (HIDRA-MAT)

The Hybrid Illinois Device for Research and Applications (HIDRA) at the University of Illinois at Urbana-Champaign is a toroidal plasma device that enables fusion plasma-material interaction testing with both stellarator and tokamak plasmas. HIDRA’s long-pulse steady state stellarator plasmas provide a testbed for plasma facing component (PFC) plasma exposures. The HIDRA Material Analysis Test-stand (HIDRA-MAT) is a material characterization module attached to HIDRA that is being designed and fabricated to include thermal desorption spectroscopy and laser induced breakdown spectroscopy systems for in-vacuo PFC characterization. A specialized rotatable sample holder positions the sample for liquid metal droplet application from a liquid metal droplet injector on HIDRA-MAT. Early experiments look to investigate the effect liquid lithium has on porous tungsten samples’ retention of H, D, and He after plasma exposure. Preliminary results from a dual residual gas analyzer system show the ability to differentiate D2 and He in HIDRA-MAT. Finally, this work aims to advance the understanding of liquid metal PFCs and further the design and development of new fusion PFCs and technologies.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Fatigue and Creep-Fatigue Evaluation of Alloy 709 at 760 and 816°C

A significant research and development effort is underway to support the qualification of Alloy 709 as a Class A construction material in the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code, Section III, Division 5, High Temperature Reactors. This initiative includes a comprehensive Alloy 709 code qualification plan aimed at generating extensive material testing data crucial for compiling the code case data package. The data package is essential in establishing material-specific design parameters for Alloy 709 to be used as Section III, Division 5 Class A construction material for fast reactors, molten salt reactors and gas-cooled reactors. An ASME Section III, Division 5 material code case requires the evaluation of mechanical properties from a minimum of three commercial heats, covering anticipated compositional ranges. A key part of the data package involves fatigue and creep-fatigue testing at elevated temperatures, needed for developing the fatigue design curves and the damage envelope of the creep-fatigue interaction diagram (D-diagram). This paper summarizes the strain-controlled fatigue testing on three commercial heats of Alloy 709 at 760 and 816°C with strain ranges between 0.25% and 3%. The fatigue failure data are used to generate a preliminary fatigue design curve. Additionally, the creep-fatigue testing results at 816°C with tensile hold times of 10, 30, and 60 minutes are presented in support of developing the D-diagram for Alloy 709.

Wang, Yanli↗

DOE OSTI2026

Impact of Molten Gallium on the Microstructure and Corrosion Behavior of Aluminum and Uranium-Aluminum Alloys for Used Nuclear Fuel Reprocessing

Test reactors around the world utilize highly enriched uranium fuel to achieve high neutron fluxes for materials testing. Once spent, the remaining uranium is a valuable resource for subsequent fuel fabrication. However, some of these test reactor cores consist of curved plate-type fuel elements, fabricated using aluminum alloy 6061 (AA6061) cladding to encapsulate a uranium-aluminum alloy (UAlx) fuel matrix. These assemblies require non-standard reprocessing approaches for uranium recovery, as aluminum dissolves readily in acidic solutions, generating large volumes of waste and complicating downstream chemical separations. In this work, we investigate a novel chemical decladding strategy based on the interaction between AA6061/UAlx and molten gallium (Ga). Ga is known to induce severe degradation of aluminum metal through liquid metal embrittlement (LME), even at relatively low Ga concentrations. By penetrating the aluminum crystal lattice, Ga disrupts grain cohesion and facilitates fracture or dissolution of the aluminum matrix. Thermodynamic analysis of the Al–Ga binary phase diagram suggests that Ga may offer a viable pathway to selectively weaken or dissolve the AA6061 cladding, and potentially the aluminum component of the UAlx fuel matrix within. To this end, parametric experiments were performed at 50 °C and 100 °C across a range of Al–Ga atomic fractions. At lower Al fractions, the AA6061 was completely molten after 2 hours of exposure to the Ga metal. In contrast, samples with higher Al fractions (0.9 Al, 0.1 Ga) contained residual solids after 2 hours, which were characterized by microstructural examination using electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). These Al-Ga compositions were also evaluated using FactSage thermodynamic modeling to further elucidate the relationship between phase diagram behavior and LME.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Report on the Integration of Experimental and Modeling Data for Initial Equivalence Study of Microstructural Evolution in Irradiated LPBF 316SS

Advanced materials and manufacturing technologies are poised to improve the safety and design characteristics of nuclear technologies and meet US energy, environmental, and economic needs. In particular, metal additive manufacturing (AM) provides an opportunity to produce novel materials and component geometries, but their use is not without hurdles arising from the inherent microstructure variability that can result from the layer-by-layer build approach. Given the greater possible microstructure variability in AM materials—and the dearth of materials test reactors—it is impractical to rely solely on neutron irradiation studies to produce data for materials qualification for every possibility. This work within the Advanced Materials and Manufacturing Technologies (AMMT) Environmental Effects technical area contributes to the rapid qualification framework by developing a science-driven framework for the accelerated qualification of materials for nuclear environments. A key product of the Environmental Effects technical area of the AMMT program is the Licensing Approach with Ions and Neutrons (LAIN). This approach recognizes that whether using existing materials in new environments, newly developed materials tailored for these environments, or new manufacturing methods, the traditional decades-long approach for materials qualification does not facilitate rapid deployment. In FY 2023, the AMMT program presented a conceptual framework of specific steps to fulfill several technical challenges associated with qualifying materials for performance in radiation environments on an accelerated time frame informed by the state of the art in materials science and a review of the current regulatory landscape. The objective of this section of the Environmental Effects technical area is to critically evaluate and refine the proposed qualification framework presented under AMMT by integrating the research results of the neutron irradiations, the ion irradiations, and modeling efforts. These ongoing efforts span across Argonne National Laboratory (ANL), Idaho National Laboratory (INL), and Oak Ridge National Laboratory (ORNL) and are closely coordinated.

36 MATERIALS SCIENCE↗