Results for “SiC Temperature Monitor”

DOE OSTI2025

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Passive Temperature Sensors for Nuclear Applications

In April 2007, the Department of Energy (DOE) designated the Advanced Test Reactor (ATR) a National Scientific User Facility (NSUF) to advance US leadership in nuclear science and technology. By attracting new users from universities, laboratories, and industry, this program supports basic and applied nuclear research to help address the nation's energy security needs. In support of this program, the Idaho National Laboratory (INL) established in-house capabilities to develop, fabricate, test, and qualify new and enhanced temperature sensors for irradiation testing. This effort is continuing today through the DOE?s Advanced Sensors and Instrumentation (ASI) program. Although most efforts emphasize sensors capable of providing real-time data, selected tasks have been completed to enhance passive sensors for irradiations where instrumentation leads cannot be included. These sensors include silicon carbide (SiC) monitors, melt wires and the sublime temperature monitor. SiC monitors are available to detect peak irradiation temperatures between 200°C and 800°C in reactor locations where instrumentation leads cannot be used. SiC monitors may be evaluated using specialized equipment installed at INL?s Measurement Sciences Laboratory (MSL). A melt wire inventory is also maintained at MSL. This inventory contains wires for specific use in irradiation experiments ranging in temperatures from 30°C to 1500°C. Melt wires and SiC monitors have had decades of research and application. Recent research has produced a passive monitor known as the sublime temperature monitor. This passive sensor has the capability of recording temperature gradients. This paper will discuss passive temperature sensors currently being researched and implemented under the ASI program.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Passive Temperature Sensors for Nuclear Applications

Thermocouples are generally used to provide real-time temperature indications in instrumented tests performed at material and test reactors. Passive temperature monitors, such as Silicon Carbide (SiC) and melt wires, may be included in such tests as an independent technique of detecting peak temperatures experienced during irradiation. In less expensive static (drop-in) capsule tests, which have no leads attached for real-time data transmission, melt wires, and SiC temperature monitors (TMs) are essentially the only possibility for peak temperature indication. A melt wire involves placing materials (wires) of a known composition and melting temperature in a test. An inventory is maintained at Material Science Laboratory (MSL) for melt wires ranging in temperatures from 30°C to 1500°C. Unfortunately, melt wires are limited in that it can only detect whether a single temperature is or is not exceeded (melt wire melted or not). SiC TMs, which can also be used to detect peak irradiation temperatures, are advantageous because a single monitor can allow to determine the peak temperature reached within a relatively broad range (100 – 1200°C) resulting in accuracies within ±20°C. Irradiation temperature is determined by measuring a property change after isochronal annealing or during a continuously monitored annealing process using specialized equipment at MSL. Recent research has produced a passive monitor known as sublime temperature monitor. This passive sensor has the capability of recording temperature gradients and pinpointing exactly where a temperature is located along that gradient. Long measurement lengths are achieved with very high accuracy in the location of desired temperature measurements (±2 mm over a 1 m span); however, this sensor has not been deployed in a nuclear reactor. This article will focus only on passive temperature sensors currently being researched and implemented under the Advanced Sensors and Instrumentation (ASI) program at Idaho National Laboratory (INL).

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Design Report on the MiniFuel Instrumented Test Apparatus for Understanding Radiation Effects

Most nuclear fuels irradiations at Oak Ridge National Laboratory (ORNL) over the past decade have been conducted using MiniFuel—a static capsule design employing subscale fuel specimens to collect separate-effects irradiated fuel performance data. Irradiation conditions for MiniFuel experiments are predicted pre-test using reactor physics, and thermal models are verified post-irradiation via SiC dilatometry and various spectrometry methods. Relevant fuel performance parameters are also observed post-irradiation in a hot cell, thereby providing a single data point for each parameter representing the cumulative effects of the irradiation conditions. Substantially more data can be harvested from a single test and within a shorter duration by instrumenting irradiation vehicles and measuring desired quantities in situ. This report presents the design and analysis of the MiniFuel INstrumented Irradiation Test Apparatus for Understanding Radiation Effects (MINITAURE)—an instrumented test rig based on the separate-effects MiniFuel concept that aims to capture fission gas release (FGR) and thermal conductivity degradation of fuel specimens during irradiation in the High Flux Isotope Reactor (HFIR). MINITAURE will be integrated with the Materials Irradiation Facility (MIF) located in the HFIR building outside the reactor containment. The MIF will act as the instrumentation and control center for the experiment, enabling real-time feedback from in situ sensors and control of irradiation temperatures via a gas delivery system. Two unique capsule designs were developed to capture each phenomenon: the thermal conductivity capsule, which uses a thermopile method to estimate fuel specimen thermal conductivity, and the fission gas release capsule, which will have continuous flowing gas communication to high-purity germanium detectors that are housed in the MIF for monitoring FGR. This report details the reactor physics and heat transfer modeling activities that were used to inform the experiment design and predict capsule performance. It also describes out-of-pile activities conducted to stand up this new capability and verify the measurement techniques. Modeling efforts to date have demonstrated the feasibility of the in situ measurement techniques and supported the development of the MINITAURE assembly configuration. Out-of-pile testing of the thermal conductivity measurement shows promise in capturing relative changes in thermal conductivity. However, significant errors exist in the measured absolute value, posing a need for further refinement.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Advances in Molecular Beam Epitaxy Growth of Ultra-Wide Bandgap Ga2O3 Based Alloys

Gallium oxide (Ga2O3) is an emerging ultra-wide bandgap semiconductor material that has attracted attention for its potential to outperform existing SiC and GaN based devices operating at high breakdown voltages and high temperature. Isovalent alloying of In and Al in Ga2O3 provides the ability to engineer bandgap energy and strain of the material. Alloying with Al increases the bandgap energy and the theoretically achievable Baliga's figure of merit, a key measure of a material's ultimate performance limits for high power switching devices. Alloying with In introduces compressive strain and can be used to counteract the tensile strain of Al incorporation. The resulting (AlxGa1-x-yIny)2O3 alloy can be lattice-matched to commercially available Ga2O3 wafers and has a tunable bandgap energy greater than that of Ga2O3, 4.76 eV. Such lattice-matched material can be grown arbitrarily thick without the detrimental effects of elastic strain and relaxation, making it suitable for high voltage diodes and transistors. However, efforts to synthesize isovalent alloys are complicated by their tendency to phase separate into corundum Al2O3 or bixbyite In2O3. Literature reports of the quaternary (AlxGa1-x-yIny)2O3 are limited to <1% unintentional indium incorporation in In-catalyzed (AlxGa1-x)2O3. The primary limitation to quaternary growth is the limited incorporation of indium at elevated growth temperatures. This limited incorporation is due to both the volatility of indium oxide and Al and Ga cation exchange reactions which replace indium in In2O3. We report on the development of a novel high-throughput molecular beam epitaxy (MBE) technique to screen the growth conditions for the ternary alloy (InyGa1-y)2O3, and the application of these findings to the first successful synthesis of phase pure monoclinic (AlxGa1-x-yIny)2O3 by MBE. By leveraging the unique sub-oxide chemistry of Ga2O3 and in-situ monitoring of crystal properties by reflection high-energy electron diffraction (RHEED), a cyclical growth and etch-back method is developed and applied to rapidly characterize the (InyGa1-y)2O3 growth space. This cyclical method provides approximately 10x increase in experimental throughput and up to 46x improvement in Ga2O3 substrate utilization. Appropriate growth conditions for monoclinic (InyGa1- y)2O3 are identified by machine learning analysis of RHEED patterns and targeted growths are characterized ex-situ to confirm improved In incorporation. These growth conditions are then combined with established (AlxGa1-x)2O3 growth conditions to grow quaternary (AlxGa1-x-yIny)2O3 with Al mole fractions ranging from 1.4% - 24.4% and In mole fractions ranging from 3.1% to 15.5%. The chemical and optical properties of the alloys are investigated by XRD, XPS, and spectroscopic ellipsometry. A lattice-matched (AlxGa1-x-yIny)2O3 alloy is examined by 4D-STEM and the chemical and physical uniformity of Al and In incorporation are discussed.

alloy↗

DOE OSTI2025

Conceptual Designs for Irradiation Creep Testing of SiC in HFIR

Understanding irradiation creep of nuclear fuel cladding is important to properly size the initial fuel-cladding gap and understand when pellet-cladding contact is expected to occur due to a combination of fuel swelling and cladding creep-down. Irradiation creep also plays a role in relaxing stresses that develop in-pile. Silicon carbide fiber–reinforced silicon carbide matrix (SiC/SiC) composites are the leading long-term accident-tolerant fuel cladding concept for light-water reactors (LWRs). Although some limited data are available regarding irradiation creep of the individual constituents (fibers, matrix), data regarding irradiation creep of SiC/SiC composites are currently insufficient. Additional data regarding irradiation creep compliance and the rupture lifetime (combination of creep and slow crack growth) are needed to understand material limitations. This work describes the design and development of two irradiation vehicles that are being pursued for testing SiC/SiC concepts in the High Flux Isotope Reactor (HFIR). The first is a passive experiment, referred to as the PRECISE experiment, that leverages the constant coolant pressure of HFIR to compress a metallic bellows and provide a well-characterized load to drive creep in a SiC/SiC dog bone specimen. The total creep strain would be quantified post-irradiation by measuring dimensional changes of the specimen length as well as local dimensional changes within the gauge region. Non-stressed specimens would also be irradiated under the same conditions to provide an indication of dimensional changes due to radiation-induced swelling in the absence of creep. A second, more complex experiment, referred to as the INSITE experiment, is being designed in parallel that would use pneumatics to pressurize a metal bellows and linear variable differential transformers (LVDTs) to measure the specimen displacement in situ during irradiation. Such an experiment would provide significantly more data regarding the evolution of the creep compliance as a function of dose and applied stress within a single experiment but would require significantly more development time and cost to execute. The primary concern with the INSITE experiment is the accuracy, reliability, and expected lifetime of the LVDTs during irradiation at elevated temperatures. Efforts are being made to adjust the experiment design and operating procedure to limit LVDT temperatures and mitigate or otherwise compensate for uncertainties due to factors such as temperature fluctuations, creep in the surrounding structural materials, and drift of the LVDTs. This work describes the experiment designs, thermal and structural analysis that were performed to ensure that the desired temperature and stress conditions can be achieved, some initial sensitivity analyses to predict the evolution of the radiation-induced specimen displacements, and potential sources of uncertainty in the measurements. Out-of-pile testing is being performed in parallel to confirm that the test trains achieve the expected stress states in the specimens and do not result in prohibitive stress concentrators (e.g., in the grip regions) that might risk pre-mature failure. The PRECISE experiments are proceeding toward fabrication and assembly with HFIR insertion planned during fiscal year 2026. The INSITE experiment is progressing toward out-of-pile demonstrations, which will provide more conclusive evidence regarding the feasibility of executing these tests in HFIR or whether alternative displacement monitoring techniques may need to be considered.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗