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Kurley, J. Matthew

Publications and source records attributed to Kurley, J. Matthew.

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Raman spectroscopy of uranium nitride kernels

Uranium nitride is an advanced fuel candidate for a wide variety of advanced nuclear reactors. This work summarizes the first characterization of UN kernels by Raman spectroscopy. First-principles density functional theory calculations were performed to predict the Raman spectra of uranium sesquinitride (U 2 N 3 ), uranium dinitride (UN 2 ), uranium mononitride (UN), uranium monocarbide (UC), as well as U-N-C (UN 1-x C x ) and a U-N-C-O mixture. Further, a core–shell structure was identified by scanning electron microscopy and Raman spectroscopy imaging. A signal at ~500 cm -1 was identified on the periphery of the core-shell structure, possibly corresponding to U 2 N 3 and/or UN 2 . This signal broadens and shifts to 470 cm -1 because of the formation of UNC, UNCO or U 2 N 3+x structures. The culmination of this work demonstrates the feasibility of using Raman spectroscopy to identify variations in composition and phases in UN kernels.

36 MATERIALS SCIENCE↗

The effect of powder feedstock and heat treatment on the thermal and mechanical properties of binder jet printed ZrC

In this study, zirconium carbide (ZrC) disks were fabricated using binder jet printing to study the effect of powder feedstock, print parameters, and heat treatment on flowability and final materials properties. A median volumetric particle size smaller than 10 μm was shown to cause the powder to stop flowing during printing. Disks were printed using ZrC with suitable flowability and then heat-treated at temperatures between 1800°C and 2200°C for 1 or 5h. The density, part shrinkage, thermal diffusivity, and fracture strength all increased with increasing temperature and time. The heat-treated disks were then heated to 2200°C for 5h and the properties converged for disks of the same particle size, indicating the hottest temperature and longest time of exposure dictates the final properties. Lastly, it was shown that larger particles produce lower density materials with worse thermal diffusivity, most likely because of poor connectivity between particles after heat treatment.

36 MATERIALS SCIENCE↗

Rapid Quenching of Molten Salts as an Approach for the Coordination Characterization of Corrosion Products

A new apparatus was built to rapidly cool molten salts in liquid argon to prevent contamination during quenching and enable new insight into the structure in the liquid state. To test the applicability of the apparatus, several industrially relevant chloride salt compositions were first melted, rapidly solidified, and then characterized. The design proved applicable for the rapid quenching of molten salt. Furthermore, the structure of the apparatus prevented exposure of the rapidly quenched salt to impurities (humidity, oxygen, etc.). X-ray diffraction of salt specimens cooled with and without liquid argon showed differences including a structure further from the expected stoichiometric equilibrium with rapid cooling. Of particular interest is the chemical state of metallic impurities, and this may be probed using electron paramagnetic resonance.

36 MATERIALS SCIENCE↗

Synthesis of U 3 O 8 and UO 2 microspheres using microfluidics

Uranium-bearing microspheres below 50µm with a narrow size distribution allows for a wider variety of fuel forms. To accommodate the smaller size, gel microspheres with a composition of UO 3 ∙nH 2 O∙mNH 3 were synthesized using microfluidics and subsequently converted to U 3 O 8 and UO 2 . To accommodate the slower flow rates required by microfluidics, a more stable broth was established. Additionally, the gelation studies resulted in a broth that was stable for more than two days at 0°C and for close to 3 h at room temperature while still gelling within 25 s. Synthesis of gel microspheres with a narrow size distribution lasted for 5 h and produced ~0.5 g of air-dried material. The gelled microspheres were converted to U 3 O 8 and UO 2 and with sizes of 50 and 40 µm in diameter, respectively.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Validating modern methods for impurity analysis in fluoride salts

Salt impurities directly affect degradation of structural materials in molten salt environments, so impurity quantification and analysis of salts is important for the deployment of next generation molten salt nuclear reactors. Despite the importance of moisture and other oxygen containing impurities, reliable methods of measuring these impurities are not well qualified or commonly used. Herein, we present two methods for analysis of oxygen content and one method for analysis of hydrogen content in fluoride salts demonstrated on two batches of LiF-NaF-KF (FLiNaK) salt with differing purity levels. The intentional addition of varying amounts of oxygen and hydrogen to the FLiNaK salt as internal standards produced a linear response using a commercial combustion analysis instrument, and measured amounts were consistent with the standards. Overall, these results indicate the technique is a valid method for measuring oxygen and hydrogen content in fluoride salts. Corrosion studies of 316H in FLiNaK revealed 5 times more mass loss in the salt containing more impurities including hydrogen and transition metals.

36 MATERIALS SCIENCE↗