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NASA NTRS2008

Development and Characterization of the Bonding and Integration Technologies Needed for Fabricating Silicon Carbide Based Injector Components

Advanced ceramic bonding and integration technologies play a critical role in the fabrication and application of silicon carbide based components for a number of aerospace and ground based applications. One such application is a lean direct injector for a turbine engine to achieve low NOx emissions. Ceramic to ceramic diffusion bonding and ceramic to metal brazing technologies are being developed for this injector application. For the diffusion bonding technology, titanium interlayers (coatings and foils) were used to aid in the joining of silicon carbide (SiC) substrates. The influence of such variables as surface finish, interlayer thickness, and processing time were investigated. Electron microprobe analysis was used to identify the reaction formed phases. In the diffusion bonds, an intermediate phase, Ti5Si3Cx, formed that is thermally incompatible in its thermal expansion and caused thermal stresses and cracking during the processing cool-down. Thinner interlayers of pure titanium and/or longer processing times resulted in an optimized microstructure. Tensile tests on the joined materials resulted in strengths of 13-28 MPa depending on the SiC substrate material. Nondestructive evaluation using ultrasonic immersion showed well formed bonds. For the joining technology of brazing Kovar fuel tubes to silicon carbide, preliminary development of the joining approach has begun. Various technical issues and requirements for the injector application are addressed.

Halbig,Michael C.↗

DOE OSTI2021

Downselection of Cladding Materials for Zirconium Hydride Moderator

This report complete Milestone M3.1.1 — “Cladding downselection: Team will report to ARPA-E on at least two down-selected cladding options—one metallic and one ceramic.” In this milestone, we systematically assess FeCrAl alloys and SiC-based cladding options for a zirconium hydride (ZrHx) moderator in terms of their neutronics, radiation stability, hydrogen permeability, chemical compatibility, and fabricability. The analysis shows that FeCrAl alloys are excellent candidate cladding materials for a ZrHx moderator given their proven radiation stability, acceptable compatibility with ZrHx, and industrially established fabricability. The relative high hydrogen permeability is manageable by introducing a thin layer of an Al 2 O 3 hydrogen permeation barrier on the external surface. The SiC-cladded ZrHx moderator is promising because of its outstanding neutronics performance, excellent radiation stability, and extremely low intrinsic hydrogen permeability. However, potential interactions of SiC and Zr and the challenge in achieving a hermetic SiC-based cladding require further investigation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Polymer coatings on zirconia microspheres via rotating flow fluid dynamics

Conventional tristructural isotropic (TRISO) coatings for nuclear fuels require multi-step and expensive formation processes; any breakage of the coatings may lead to fission species release. Polymer derived ceramic (PDC) coatings can be a suitable alternative to address these issues. In this study, allylhydridopolycarbosilane (SMP-10) coatings were created on yttria stabilized zirconia (YSZ) microspheres using a Rotating Flow Fluid Dynamics (RFFD) coating method. The effects of curing temperature, rotation speed, and coating cycle/time on the coating were analyzed. Surface functionalization of YSZ microspheres with NaOH resulted in good adhesion between the polymer precursor and the YSZ kernel particles. Spectroscopy analysis revealed complete curing of SMP-10 coated YSZ at 160 °C. Rotation speed and coating time significantly affect the coating characteristics. After 3 cycles at lower rotation speed (50 rpm) for 10 min each, the coating obtained was uniform and homogeneous. In comparison, the coating showed almost 10 times less eccentricity at a high rotation speed of 300 rpm. Compared with the coatings prepared at 300 rpm condition, the coatings have higher sphericity and lower eccentricity at 50 rpm. Overall, this study provides a novel and effective route for fabricating and curing SMP-10 precursor coatings on YSZ microspheres.

Ravi, Nivetha [University of Alabama, Birmingham]↗

DOE OSTI2024

Integrated protonic ceramic electrochemical cell for sustainable energy economy using water-energy nexus framework

Reliance on fossil fuels will continue for the next decades even though there are global pushes away from it to mitigate the overarching climate challenge, most especially by its highest consumers and availability. While there is a hastening global shift away from fossil fuel, integrating its assets into this technology helps limit the risk and future losses of stranded assets and reduce the cost of investment in the new technologies. Moreover, the generation of electricity from intermittent renewable sources like solar and wind has witnessed a significant surge in recent years, leading to a pressing demand for practical energy storage systems. Electrical energy storage is anticipated to play a pivotal role in the future global energy system, facilitating load-leveling operations to support the greater integration of renewable and distributed generation. Reversible electrochemical cells (RECs) offer a promising option for addressing the fossil fuel assets integration and energy storage challenges through the interconversion between electrical and chemical energy and concurrent utilizing carbon emission. In their electrolysis mode, the RECs convert electricity into durable, storable, and portable valuable chemical fuels such as syngas and methane. Conversely, the produced chemical fuels can be used as reactants in the fuel cell mode to generate electricity on demand with minimal (hydrocarbons) or zero when H2 or NH3 is used emissions. However, a challenging goal for this type of technology remains to achieve optimal operation and high roundtrip efficiencies, which has hindered the deployment of previous electrochemical cells. This dissertation demonstrates how reversible protonic ceramic electrochemical cells (RePCECs) can be integrated with fossil fuel power plants and renewable energy sources as a potential energy storage system. In this work, integrated RePCEC systems are designed and examined using computational modeling at scales to determine appropriate system configurations and operating conditions that achieve high roundtrip efficiencies. Cell level design of the PCEC is the first approach, several cells are assembled for the stack level model that is integrated into combined cycle powerplant and solar photovoltaic for the system level model. After critical literature review, this answered the operational and integration research questions proposed to address these challenges. The designed systems perform two functions, utilizing captured CO2 and storing renewable energy through co-electrolysis of steam and CO2. The co-electrolysis reaction involves endothermic water electrolysis and exothermic methanation reaction. To enhance high roundtrip efficiency, there is a need for thermal balance and management in the electrolysis mode. This involves operating the RePCEC stack under conditions that favor methane production to balance out heat needed by water electrolysis, it crucial for the RePCEC system operation. Methanation is enhanced by low temperatures. Leveraging on fabricated BCZYYb-electrolyte RePCEC, the cell model designed revealed that the optimum temperature for methane production is 450℃ at atmospheric pressure. Thus, to achieve optimum system performance, operating in the temperature range 450-525℃ is recommended at the given configuration, combining between the optimum temperature for methane production and temperature for the optimum stack roundtrip efficiency. Configuration with carbon capture system and purge stream is the optimum configuration from the seven conceptualized and evaluated. The modeling outcomes include a thermodynamic examination of integrated RePCEC systems, calibration of cell and stack level models, and steady-state simulation and integration into a 600MW combined cycle power plant retrofitted with two two-stage membrane-based carbon capture system and a wastewater treatment and recovery unit. At 100% powerplant loading, the stack and system roundtrip efficiencies are 72% and 51.37% respectively. Adding a purge stream for produced hydrogen at the system downstream improves the efficiencies to 74 and 55.48% respectively. At atmospheric pressure and 525℃, the system model suggests that a stack roundtrip of 82% is achievable, and overall system efficiency increases by reducing the energy consumption by the balance of plant components for steam generation and storage. Economic analysis of the process gives levelized cost of methane as $2.24/MMBtu lower than the conventional production route that range between $3.46/MMBtu and $9.85/MMBtu. The lifecycle analysis shows that the global warming potential for the production of methane and hydrogen from the RePCEC system is 3.83 kg CO2 eq which is lower than 9.35 kg CO2 eq emission during steam methane reforming for hydrogen production. This answered both the environmental and economic concerns in the raised research question. The proposed RePCEC configuration and analysis carried out in this dissertation to address the surge in renewable energy and challenges with PCEC technology hold significant potential in achieving large-scale energy storage while simultaneously reducing carbon emissions. These advancements, coupled with suitable governmental policies and incentive programs, have the potential to economically disrupt the natural gas industries by using RePCEC systems for methane production, thereby making them more favorable for eventual implementation and commercialization.

25 ENERGY STORAGE↗

NASA NTRS2008

Bonding and Integration Technologies for Silicon Carbide Based Injector Components

Advanced ceramic bonding and integration technologies play a critical role in the fabrication and application of silicon carbide based components for a number of aerospace and ground based applications. One such application is a lean direct injector for a turbine engine to achieve low NOx emissions. Ceramic to ceramic diffusion bonding and ceramic to metal brazing technologies are being developed for this injector application. For the diffusion bonding, titanium interlayers (PVD and foils) were used to aid in the joining of silicon carbide (SiC) substrates. The influence of such variables as surface finish, interlayer thickness (10, 20, and 50 microns), processing time and temperature, and cooling rates were investigated. Microprobe analysis was used to identify the phases in the bonded region. For bonds that were not fully reacted an intermediate phase, Ti5Si3Cx, formed that is thermally incompatible in its thermal expansion and caused thermal stresses and cracking during the processing cool-down. Thinner titanium interlayers and/or longer processing times resulted in stable and compatible phases that did not contribute to microcracking and resulted in an optimized microstructure. Tensile tests on the joined materials resulted in strengths of 13-28 MPa depending on the SiC substrate material. Non-destructive evaluation using ultrasonic immersion showed well formed bonds. For the joining technology of brazing Kovar fuel tubes to silicon carbide, preliminary development of the joining approach has begun. Various technical issues and requirements for the injector application are addressed.

Halbig, Michael C.↗

NASA NTRS2015

Ultra High Temperature (UHT) SiC Fiber (Phase 2)

Silicon-carbide fiber-reinforced silicon-carbide ceramic matrix composites (SiCSiC CMC) are emerginglightweight re-usable structural materials not only for hot section components in gas turbine engines, but also for controlsurfaces and leading edges of reusable hypersonic vehicles as well as for nuclear propulsion and reactor components. Ithas been shown that when these CMC are employed in engine hot-section components, the higher the upper usetemperature (UUT) of the SiC fiber, the more performance benefits are accrued, such as higher operating temperatures,reduced component cooling air, reduced fuel consumption, and reduced emissions. The first generation of SiCSiC CMC with a temperature capability of 2200-2400F are on the verge of being introduced into the hot-section components ofcommercial and military gas turbine engines.Today the SiC fiber type currently recognized as the worlds best in terms ofthermo-mechanical performance is the Sylramic-iBN fiber. This fiber was previously developed by the PI at NASA GRC using patented processes to improve the high-cost commercial Sylramic fiber, which in turn was derived from anotherlow-cost low-performance commercial fiber. Although the Sylramic-iBN fiber shows state-of-the art creep and rupture resistance for use temperatures above 2550oF, NASA has shown by fundamental creep studies and model developmentthat its microstructure and creep resistance could theoretically be significantly improved to produce an Ultra HighTemperature (UHT) SiC fiber.This Phase II Seedling Fund effort has been focused on the key objective of effectively repeating the similar processes used for producing the Sylramic-iBN fiber using a design of experiments approach to first understand the cause of the less than optimum Sylramic-iBN microstructure and then attempting to develop processconditions that eliminate or minimize these key microstructural issues. In so doing, it is predicted that that theseadvanced process could result in an UHT SiC fiber with 20 times more creep resistance than the Sylramic-iBN fiber,which in turn would allow SiCSiC CMC to operate up to 2700oF and above, thereby further enhancing the performancebenefits of SiCSiC components in aero-propulsion engines. It was also envisioned that the fiber processes developedduring Phase II efforts would not only reduce production costs for the UHT fiber by using low-cost precursor fibers andcombined processes, but also allow the UHT fibers to be directly produced in preforms of the precursor fibers, possibly atthe facilities of the CMC fabricator.

SiC Ceramic Fiber↗

NASA NTRS1986

Brayton cycle solarized advanced gas turbine

Described is the development of a Brayton Engine/Generator Set for solar thermal to electrical power conversion, authorized under DOE/NASA Contract DEN3-181. The objective was to design, fabricate, assemble, and test a small, hybrid, 20-kW Brayton-engine-powered generator set. The latter, called a power conversion assembly (PCA), is designed to operate with solar energy obtained from a parobolic dish concentrator, 11 meters in diameter, or with fossil energy supplied by burning fuels in a combustor, or by a combination of both (hybrid model). The CPA consists of the Brayton cycle engine, a solar collector, a belt-driven 20-kW generator, and the necessary control systems for automatic operation in solar-only, fuel-only, and hybrid modes to supply electrical power to a utility grid. The original configuration of the generator set used the GTEC Model GTP36-51 gas turbine engine for the PCA prime mover. However, subsequent development of the GTEC Model AGT101 led to its selection as the powersource for the PCA. Performance characteristics of the latter, thermally coupled to a solar collector for operation in the solar mode, are presented. The PCA was successfully demonstrated in the fuel-only mode at the GTEC Phoenix, Arizona, facilities prior to its shipment to Sandia National Laboratory in Albuquerque, New Mexico, for installation and testing on a test bed concentractor (parabolic dish). Considerations relative to Brayton-engine development using the all-ceramic AGT101 when it becomes available, which would satisfy the DOE heat engine efficiency goal of 35 to 41 percent, are also discussed in the report.

Source record↗

NASA NTRSDate not supplied

TechEdSat 7, 10, 13, 15: Exo-brake Experiments on the ISS, First Virgin Orbit, and First Firefly-Alpha Test Flights.

The TechEdSat flight series (TES-n), developed by the Nano Orbital Workshop (NOW) group at NASA Ames, has been studying cube satellite re-entry technologies with a focus on Exo-Brake drag device research. An exo-atmospheric braking device, the Exo-Brake uses the tenuous upper atmosphere acting in a free molecular flow regime to enable controllable adjustment of the drag profile of the host spacecraft, currently enabling rapid disposal of small spacecraft after mission conclusion, and eventual targeted de-orbit to a desired entry point at the Von Karman line, or approximately 100km in altitude. The TES-7 mission, flown on the first successful Virgin Orbit flight January 17, 2021, was injected into a 500km, 61-degree inclination orbit, with an expected orbital lifetime of approximately ten years. After successful deployment of a unique hydrogen gas-cell inflation design ‘disposal’-type Mylar Exo-Brake intended to rapidly de-orbit the spacecraft, the maximum expected orbital lifetime of the TES-7 spacecraft was successfully reduced from ten years to 1.3 years, an 87% reduction in orbit lifetime via a passive, fuel-less system. The subsequent TES-13 mission utilized a new, less complex ‘disposal’-type Exo-Brake design made from collapsible rigid struts rather than inflated struts to reduce the engineering, construction, and safety complexities introduced by the prior hydrogen gas inflation design. The rigid strut Exo-Brake design is stowed via rotational compression and deploys using only stored spring energy once released via electronic actuator. This new rotation compression storage design has become the new Exo-Brake design standard used on TES missions thanks to its simplicity. Following on the success of this new Exo-Brake design demonstrated by TES-13, the design was further refined to enabled active manipulation of the Exo-Brake effective drag area though a winch-like system. Both the TES-10 and TES-15 spacecraft were equipped with geometrically similar Exo-Brake devices capable of such active drag modulation, with the intent of studying the operational impact of having such devices on cube satellite missions. To increase the survival time of the Exo-Brake at low altitudes and thus gain more experiment time and better guidance capability, TES-15 was equipped with a modulated Exo-Brake constructed from 3M™ Nextel™ 440 ceramic oxide fiber, the same fabric material used in the Space Shuttle TPS system, rather than Mylar. After launching on Alpha Flight 2 October 1st, 2022, Firefly’s first successful launch, TES-15 met the same modulation restrictions as TES-10, with modulation prohibited above 200km to avoid possible collision with other spacecraft. In this case, a low deployment orbit caused an extremely short mission life, which, coupled with delayed spacecraft identification, exacerbated collision concerns and caused performance data of the high-temperature Exo-Brake design to be inconclusive. As such, the Nano Orbital Workshop has taken a new approach of only conducting modulated Exo-Brake research on missions deploying below ISS altitude to avoid collision avoidance restrictions, and is working to improve spacecraft identification and location reporting techniques to increase experiment durations. Upcoming TES mission will therefore use one of two classes of Exo-Brake depending on their target altitude, as to be described in the submission.

M Murbach↗

NASA NTRSDate not supplied

TechEdSat 7, 10, 13, 15: Exo-brake Experiments on the ISS, First Virgin Orbit, and First Firefly-Alpha Test Flights

Marcus Murbach↗

NASA NTRS2005

Cooled Ceramic Matrix Composite Propulsion Structures Demonstrated

NASA's Next Generation Launch Technology (NGLT) Program has successfully demonstrated cooled ceramic matrix composite (CMC) technology in a scramjet engine test. This demonstration represented the world s largest cooled nonmetallic matrix composite panel fabricated for a scramjet engine and the first cooled nonmetallic composite to be tested in a scramjet facility. Lightweight, high-temperature, actively cooled structures have been identified as a key technology for enabling reliable and low-cost space access. Tradeoff studies have shown this to be the case for a variety of launch platforms, including rockets and hypersonic cruise vehicles. Actively cooled carbon and CMC structures may meet high-performance goals at significantly lower weight, while improving safety by operating with a higher margin between the design temperature and material upper-use temperature. Studies have shown that using actively cooled CMCs can reduce the weight of the cooled flow-path component from 4.5 to 1.6 lb/sq ft and the weight of the propulsion system s cooled surface area by more than 50 percent. This weight savings enables advanced concepts, increased payload, and increased range. The ability of the cooled CMC flow-path components to operate over 1000 F hotter than the state-of-the-art metallic concept adds system design flexibility to space-access vehicle concepts. Other potential system-level benefits include smaller fuel pumps, lower part count, lower cost, and increased operating margin.

Jaskowiak, Martha H.↗

NASA NTRS2009

Self-Assembling, Flexible, Pre-Ceramic Composite Preforms

In this innovation, light weight, high temperature, compact aerospace structures with increased design options are made possible by using self-assembling, flexible, pre-ceramic composite materials. These materials are comprised of either ceramic or carbon fiber performs, which are infiltrated with polymer precursors that convert to ceramics upon thermal exposure. The preform architecture can vary from chopped fibers formed into blankets or felt, to continuous fibers formed into a variety of 2D or 3D weaves or braids. The matrix material can also vary considerably. For demonstration purposes, a 2D carbon weave was infiltrated with a SiC polymer precursor. The green or unfired material is fabricated into its final shape while it is still pliable. It is then folded or rolled into a much more compact shape, which will occupy a smaller space. With this approach, the part remains as one continuous piece, rather than being fabricated as multiple sections, which would require numerous seals for eventual component use. The infiltrated preform can then be deployed in-situ. The component can be assembled into its final shape by taking advantage of the elasticity of the material, which permits the structure to unfold and spring into its final form under its own stored energy. The pre-ceramic composites are converted to ceramics and rigidized immediately after deployment. The final ceramic composite yields a high-temperature, high-strength material suitable for a variety of aerospace structures. The flexibility of the material, combined with its high-temperature structural capacity after rigidization, leads to a less complex component design with an increased temperature range. The collapsibility of these structures allows for larger components to be designed and used, and also offers the potential for increased vehicle performance. For the case of collapsible nozzle extensions, a larger nozzle, and thus a larger nozzle exit plane, is possible because interference with surrounding structures can be avoided in the collapsed state. The larger exit plane leads to an increase in expansion area ratio, which has the potential to increase thrust and overall rocket performance. In general, the use of advanced ceramic materials can lead to improved engine and vehicle performance. The ceramics can run hotter, so less cooling is required. Fuel to coolant ratios can be balanced more readily to reduce weight. Engine efficiency can also be increased with hotter combustion and exhaust temperatures. In addition, the ceramic composites themselves can reduce the component weight by as much as 50 percent, which can translate into greater payload for the vehicle

Jaskowiak, Martha H.↗

DOE OSTI2021

Moderate temperature sintering of BaZr 0.8 Y 0.2 O 3-δ protonic ceramics by A novel cold sintering pretreatment

The state-of-the-art protonic ceramic conductor BaZr 0.8 Y 0.2 O 3-δ (BZY20) requires an extremely high sintering temperature (≥1700 °C) to achieve the desired relative density and microstructure necessary to function as a proton conducting electrolyte. In this work, we developed a cold sintering pretreatment assisted moderate-temperature sintering method for the fabrication of high-quality pure BZY20 pellets. BZY20 pellets with high relative density of ~94% were fabricated with a final sintering temperature of 1500 °C (200 °C lower than the traditional sintering temperature). A comparison with BZY20 control samples indicated that the proper amount of BaCO 3 introduced on the BZY20 particle surface and the high green density achieved by cold sintering pretreatment were the main drivers for lowering the sintering temperature. The electrical conductivity measurement by electrochemical impedance spectroscopy showed that the as-prepared BZY20 pellets have a proton conductivity comparable to the state-of-the-art values. The cold sintering pretreatment outlined in this work has the potential to lower the sintering temperatures for similar types of protonic ceramic materials under consideration for a wide range of energy conversion and storage applications.

36 MATERIALS SCIENCE↗

NASA NTRS1997

Smoldering News From STS-77 Endeavour

The Microgravity Smoldering Combustion (MSC) experiment lifted off aboard the Space Shuttle Endeavour for its second flight in May 1996, as part of the STS-77 mission. This experiment is part of a series of studies focused on the smolder characteristics of porous combustible materials in a microgravity environment. Smoldering is a nonflaming form of combustion that takes place in the interior of combustible materials. Common examples of smoldering are nonflaming embers, charcoal briquettes, and cigarettes. The objective of this study is to provide a better understanding of the controlling mechanisms of smoldering in microgravity and normal Earth gravity (1g). As with other forms of combustion, gravity affects the availability of air and transport of heat, and therefore, the rate of combustion. The results of the microgravity experiments will be compared with identical ones carried out in 1g. In addition, they will be used to verify present theories of smolder combustion and will provide new insights into the process of smoldering combustion, enhancing our fundamental understanding of this frequently encountered combustion process and guiding improvements in fire safety practices. Two smoldering combustion tests with polyurethane foam were successfully accomplished during the STS-77 mission. The tests investigated smoldering combustion in a quiescent (no-flow) enriched oxygen environment, and in an air environment with a 2-mm/sec airflow through the fuel sample. The primary data from the tests are the ignition characteristics, spread rate, smolder reaction temperature, and products of combustion (solid and gas). On both the first mission on STS-69 and the second mission on STS-77, a smolder front propagated the length of the forced-flow samples, with the spread rate between the corresponding upward and downward 1g smolder rates. Neither of the quiescent cases propagated combustion (the first case was due in part to a problem with the experiment electronics). These results show a dramatic difference from the normal gravity results, where smolder propagation is very rapid and complete for both of these conditions. The experiment was conceived by Prof. A. Carlos Fernandez-Pello at the University of California-Berkeley. The MSC hardware was designed and built at the NASA Lewis Research Center by a team of civil servants and contractors from NYMA, Inc., and Aerospace Design & Fabrication, Inc. (ADF). The hardware consists of two sealed aluminum combustion chambers (each being a half a cylinder). The chambers hold the MSC test section, data acquisition electronics, power distribution electronics, and instrumentation. The hardware is fitted into a 5-ft(sup 3) Get-Away-Special (GAS) canister that is mounted in the shuttle cargo bay. The test section consists of a quartz cylinder that contains the polyurethane foam sample and an igniter. This igniter, which is an electrically heated wire sandwiched between two porous ceramic disks, is mounted in contact with the end of the foam sample. An array of 12 thermocouples placed axially and radially along the foam sample provide temperature histories, which are used to determine the rate of smolder propagation, and the characteristics of the reaction.

Koudelka, John M.↗

DOE OSTI2021

Multicomponent pyrochlore solid solutions with uranium incorporation – A new perspective of materials design for nuclear applications

Multicomponent pyrochlore solid solutions with and without uranium incorporation were fabricated and their thermal-mechanical properties were characterized. Multicomponent pyrochlore solid solutions without uranium exhibit comparable thermal conductivity and higher mechanical strength compared to baseline single component rare-earth titanate pyrochlore (A 2 Ti 2 O 7 ). Uranium incorporation reduces hardness as compared with single component compositions. High entropy pyrochlore with uranium displays the highest thermal conductivity within multicomponent pyrochlore solid solutions with significantly better mechanical properties than UO 2 . The measured thermal conductivity correlates well with A-site cation mixing entropy and a modified size disorder parameter, and thus the size disorder and mixing entropy could be good indicators for predicting thermal conductivity of multicomponent pyrochlore solid solutions. This work opens up the possibility of designing multicomponent oxide solid solutions by controlling their chemical disorder/mixing entropy to achieve acceptable thermal-mechanical properties, desired radiation and corrosion performance for potential nuclear waste form and inert matrix fuel applications.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

AGR-5/6/7 Final Release-to-Birth Ratio Data Analysis

AGR-5/6/7 is the last of a series of Advanced Gas Reactor (AGR) experiments conducted in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) in support of development and qualification of tristructural isotropic (TRISO) low-enriched fuel for use in the high-temperature gas cooled reactor (HTGR). AGR configuration and irradiation conditions are based on prismatic HTGR technology that is distinguished primarily through the use of helium coolant, a low-power-density ceramic core capable of withstanding very high temperatures, and TRISO-coated particle fuel. The AGR tests provide valuable irradiation-performance data to support fuel process development, qualify fuel for normal operation and accident conditions, and support development and validation of fuel performance and fission-product (FP) transport models and codes. Each AGR test consists of multiple independently controlled and monitored capsules containing fuel compacts placed in a graphite cylinder shrouded by a steel shell. Release-to-birth ratios (R/B) for fission-gas isotopes released from each capsule are calculated from release rates, measured by germanium detectors in the Fission Product Monitoring System (FPMS) installed downstream from each capsule, and birth rates calculated using numerical models of FG generation. The R/Bs are a critical measure of the ability of the fuel kernel, the particle coating layers, and the compact matrix to retain fission-gas atoms, preventing their release into the sweep-gas flow, and the impact of initially defective particles and/or particle-coating failures that occur during irradiation. For fission-gas isotopes, particle failure is defined as failure of all coating layers, allowing gaseous fission atoms to escape from a particle. During the first five cycles (162B ? 165A), R/Bs were stable in the 10-8?10-6 range, and no in-pile particle failures were observed, based on the gross gamma counts. The maximum R/B value of around 2 ? 10-6 for Kr-85m resulted from the presence of as-fabricated exposed kernels (based on the high exposed kernel fraction), the dispersed uranium, and high fuel particle temperatures in Capsule 1. Comparison of capsule-measured R/Bs from these early cycles to predictions using the previously developed AGR R/B model demonstrated FG release from the AGR-5/6/7 TRISO fuel was comparable to that of previous experiments. In addition, the Kr-85m R/B per-exposed-kernel values are comparable to R/B values obtained in AGR-3/4 irradiation experiment and four irradiation experiments performed during 1980s: (1) HRB-17/18, (2) COMEDIE-BD1, (3) HFR B1, and (4) HRB-21. In contrast, all measured R/B values are lower than predictions by the commonly used Richards and German models, which are intentionally conservative. A large number of in-pile particle failures occurred in Capsule 1 by the end of Cycle 166A. During the final four cycles (166A ? 168A), apparent damage to the Capsule 1 gas line appeared to cause FG leakage from that capsule into the other four capsules, resulting in an increase in fission gas (FG) detected in the effluent for all capsules. Isolation of the Capsule 1 gas line during the last three cycles also prevented measurement of its FG release. Thus, R/Bs in all capsules after Cycle 166A are highly uncertain because of undefined amount of leakage from Capsule 1, especially for long-lived isotopes. A few hundred in-pile particle failures were estimated for Capsule 1 before the end of Cycle 166A, but the total number of failures is unknown due to the lack of FG release data in the later cycles. Based primarily on evidence from the gross gamma counts during Cycle 168A, approximately 15 particles failed in Capsule 3 and four particles failed in Capsule 2. In-pile failures in Capsule 3 were anticipated because this capsule was designed to operate beyond the HTGR normal operating temperature range. In contrast, no in-pile failures were identified in the top two capsules (4 and 5) based on the absence of the typical spikes in gross gamma counts and low failure estimates using the AGR model, developed in INL/EXT-14-32970, for R/B of the short-lived isotopes (Kr-89 and Xe-137) with minimal leakage from Capsule 1.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Experimental system for studying temperature gradient-driven fracture of oxide nuclear fuel out of reactor

Temperature gradients in ceramic light water reactor (LWR) uranium dioxide (UO 2 ) nuclear fuel pellets generate thermal stresses that cause fractures in the fuel beginning early in the life of fresh fuel. The combination of heating due to fission and forced convective cooling on the exterior of LWR fuel rods generates a temperature profile that is difficult to replicate outside the reactor environment. In the present study, a state-of-the-art experimental set-up using electrical heating to replicate fission heating was built and surrogate fuel materials such as ceria (CeO 2 ) were used to validate the system. Cracking experiments were conducted on these surrogates by inducing reactivity-initiated-accident (RIA) like temperature gradients in the pellets via induction and direct resistance heating. Induction heating was done using copper coils and molybdenum susceptors which heated the surrogates to a threshold temperature that is sufficiently high for the fuel material to conduct current. Thereafter, direct resistance heating was used by a D.C. power supply to introduce volumetric heating to replicate LWR operating conditions analogous to fission heating. The pellets were held against nickel electrodes and mounted on a boron nitride test-stand. All the tests were carried out in a stainless-steel vacuum chamber. Simultaneous real-time dual imaging of the surrogate pellet surface has been implemented using an optical and infrared camera system which will be mounted along axial and perpendicular directions to the pellet surface respectively. A beam-splitter was used to split the incoming radiation from the sample into two halves. While one of the beams is transmitted from the splitter through a bandpass filter to obtain optical images, the other beam is reflected from the splitter to the thermal camera to capture full field temperature gradients of the as fabricated pellet surface during crack initiation and propagation. In the current series of tests, a 2-color pyrometer was used for recording and comparing the surface and centerline temperatures of the surrogate pellets in lieu of the thermal camera. A LabVIEW data acquisition system has been set up for collecting useful data during experiments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Characterization of Aluminum Metal Powders for Plutonium-238 Program

As part of radioisotope thermoelectric generator (RTG) production for power sources in deep space exploration, Oak Ridge National Laboratory (ORNL) produces plutonium-238 ( 238 Pu). To produce 238 Pu, neptunium-237 ( 237 Np) targets are fabricated at ORNL and subsequently irradiated at the High Flux Isotope Reactor (HFIR) at ORNL and the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL). Specifically, current flowsheets utilize neptunium dioxide ( 237 NpO 2 ) targets. Aluminum (Al) powder is blended with 237 NpO 2 target material to improve thermal conductivity during irradiation. The current composition of 237 NpO 2 /Al pellets (i.e., cermets, or ceramic–metallics) is 20% 237 NpO 2 , 70% Al, and 10% void space. Al powders utilized by the 238 Pu program are high-fired under vacuum before blending into targets. The primary objective of this work is to measure the physical, chemical, and thermal properties of Al before and after the high-firing process. Properties of interest include the morphology, surface texture, particle size, crystal phase(s), and thermal conductivity of the material. These properties are measured with existing materials characterization equipment at ORNL, including powder x-ray diffraction (pXRD), scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS), laser flash analysis (LFA), and thermogravimetric analysis (TGA). A secondary objective of this work is to compare the Al powders before and after the high-firing procedure to determine the effects of high-firing on chemical, physical, and thermal properties and to determine the efficacy of the high-firing process.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Integrated TBC/EBC for SiC Fiber Reinforced SiC Matrix Composites for Next Generation Gas Turbines (Final Report)

In this ambitious project, a significant challenge preventing widespread use of ceramic matrix composites in hot section components of gas power generating turbines was addressed. Hot section components made from SiC fiber reinforced SiC matrix composites (SiC/SiC composites), have the potential to achieve a combined cycle energy efficiency of above 65%. To achieve this efficiency, the temperature of the combustion gases on the turbine component surface is expected to reach as high as ~1700ºC (3100ºF). However, SiC/SiC composites suffer from volatilization at high temperature under high velocity steam environment – typical in a turbine hot chamber. This integrated collaborative project, between two research groups at Clemson University and a team of engineers and scientists at GE Gas Power, focused on design, fabrication and evaluation of a new graded environmental barrier coating. Using the excellent compositional tailorability of polymer derived ceramics (PDCs), we developed an integrated EBC/BC that smoothly transitions from bottom SiC/SiC bond interface to hermetic sesquioxide (Y 2 O 3 ) top surface. This smooth compositional transition avoided the sharp CTE mismatch at interfaces to greatly reduce the thermal stress. The developed EBC is compatible with and bonds well with the bond coat that GE uses. The top hermetic oxide surface ensures low oxygen transportation and volatilization rates under the high velocity steam environment. The graded microstructure with increasing sesquioxide concentration also decreases the amount of Si and C elements near the top hermetic sesquioxide layer. Coatings made using a process suitable for manufacturing – atmospheric plasma spraying was demonstrated. The microstructure of coatings made using this process were fully characterized. Finally, the performance of these coatings was investigated under the most demanding conditions for this application. Specifically, high temperature, high velocity steam exposure; thermal shock test; and thermal cycling tests. The graded coatings performed exceptionally well in all these tests. Specific suggestions for future development in this area have also been identified. In addition to the excellent technical progress, this project helped initiate a robust collaboration between the research groups at Clemson and GE Gas Power. It also provided a high-quality learning and mentoring opportunity for the three post-doctoral research associates and two UG students at Clemson University who worked on this project. All proposed tasks, sub-tasks were completed, and all milestones achieved.

03 NATURAL GAS↗