- Nanoindentation of Phases in Irradiated and Control U-10Zr Fuels

Principal Investigator
Name:
Maria Okuniewski
Email:
[email protected]
Phone:
(208) 526-6918
Team Members:
Name: Institution: Expertise: Status:
Maria Okuniewski Purdue University Irradiation effects, nuclear fuels, and nanoindentation expert Faculty
Daniel Murray Idaho National Laboratory electron microscopy, FIB, SEM, EDS, ebsd, WDS, XPS Other
Xiang Liu Idaho National Laboratory TEM, ODS, nanoindentation, x-ray diffraction, APT, irradiated microstructure, ferritic martensitic steels, advanced alloys Other
Jonova Thomas Purdue University Conduct EM and nanoindentation experiments Graduate Student
Jason Harp Idaho National Laboratory electron microscopy, nuclear fuel fabrication, PIE, tomography, TRISO, uranium compounds, fabrication, mixed oxides, gamma spectrometry Other
Lingfeng He Idaho National Laboratory microstructural characterization, nuclear fuels, TEM, radiation effects, Ceramics Other
Experiment Details:
Experiment Title:
Nanoindentation of Phases in Irradiated and Control U-10Zr Fuels)
Hypothesis:
Fuel failure by fuel cladding mechanical interactions (FCMI) occurs partly due to the formation of brittle, intermetallic phases and fission product precipitate phases at the FCCI regions and cladding. Acquiring both mechanical properties, chemistry and crystal structure of these phases will not only assist in determining which of the phases are brittle/ductile, but can also be used to provide data lacking within fuel performance codes that connects mechanical properties and microstructure.
Work Description:
The work consists of producing multiple in-situ nano-indentation measurements of phases in irradiated and control U-10Zr fuels (1 specimen each) utilizing the Hysitron PI-88 nano-indenter in a plasma-focused ion beam scanning electron microscope (P-FIB SEM) at the Irradiated Materials Characterization Laboratory (IMCL). The goal is to attain hardness measurements via in-situ nano-indentations at regions from where transmission electron microscope (TEM) lamellae were extracted from a previously awarded RTE (2017: 3rd call). The regions of interest for local phase hardness measurements in the irradiated fuel include region the HT-9 cladding, FCCI region, and the 3 concentric phase regions in the irradiated fuel, as well as the cladding and the U-10Zr regions from the un-irradiated control fuel. Local EDS and BSE information are also to be collected along with the indentation measurements. Ideally if time and funds are available, we also propose liftout of 4 addition TEM lamellae to replace previously damaged lamellae from the fuel for analysis in the Titan Chemi TEM at IMCL. However, due to uncertainty of funds, cost structure of equipment usage at IMCL and time intervals available for preparation of the specimens, the number of TEM lamellas prepared can be adjusted as per available options.
Project Summary
A subset of the Mechanistic Fuel Failure-3 (MFF-3) irradiations included U-10wt%Zr (U-10Zr) fuels that were sodium bonded to HT9 cladding with a smear density of 75% and maximum burnup of 13.5 at %. Although early PIE of U-10Zr fuels from EBR-II provided a correlation between the phase transformations and porosity via BSE-SEM imaging, there is a lack of detailed understanding of the crystal structure of phases formed, phase distribution, constituent redistribution, fuel-cladding chemical interaction (FCCI), and mechanical property degradation. Although transmission electron microscope (TEM) and three-dimensional electron backscatter diffraction (3D EBSD) experiments of the irradiated fuel via recently awarded Rapid Turnaround Experiments (18-1243 and 18-1590) will provide a detailed analysis of the phases present at different regions of the fuel, a knowledge gap still persists in understanding the microstructure-mechanical property correlations in these fuels. Additionally, there is a lack of critical assessment on the deviations in microstructure-mechanical properties between the irradiated MFF-3 fuel and unirradiated control fuel to accurately describe the alterations from irradiation. To correlate the microstructural and mechanical property changes occurring at different regions of the irradiated fuel, we propose nanoindentation measurements of major phases at various regions of the irradiated and control fuel, with a specific emphasis on the FCCI and cladding regions. For this work, we propose in-situ nanoindentation measurements using the Hysitron PI-88 nanoindenter in a Plasma Focused Ion Beam (PFIB)-SEM at IMCL along with correlative EDS and BSE information. Correlation between the proposed indentation tests and TEM/3D EBSD assessments of the fuels from recently awarded the RTE’s (18-1243 and 18-1590) will provide an understanding of the mechanical behavior of the specific phases in the FCCI and cladding regions. This can be particularly important when trying to mitigate brittle phase formation during the design of advanced reactors and materials. The proposed indentation experiments should be conducted near regions from where the TEM lamellas were produced from the RTE (18-1243) to provide a one-to-one comparison between the phases observed from the lamella and nanohardness measurements. Nanoindentation measurements on fission products (FPs) precipitates observed at various locations in the fuel is also suggested to identify the potential existence of brittle phases which could lead to fuel cracking, and eventually failure. This proposed work, combined with the synchrotron experiments at ANL, and the recently awarded RTEs for TEM and 3D EBSD/EDS assessment of fuels will also provide the first ever quantitative assessment of microstructural-mechanical property correlations in neutron irradiated U-10Zr fuels. Furthermore, the mechanical properties from these experiments (hardness and elastic moduli) could also be used to enhance the fuel performance codes for irradiated U-10Zr/HT-9 fuels.
Relevance
This proposed research is directly related to the DOE-NE mission by addressing two of the four research initiatives, specifically through the development of technologies and other solutions that can improve the reliability, sustain the safety, and extend the life of current reactors and sustainable fuel cycles. These research initiatives will be addressed by providing a more comprehensive understanding of constituent redistribution, swelling, and fuel-cladding chemical interaction (FCCI), and mechanical property changes, many of which are concerns in a variety of fuels. This research links directly to the Nuclear Technology Research and Development program under the Fuel Cycle Technology initiative, as well as to the Nuclear Reactor Technologies within the Advanced Reactor Technologies, through providing insight into mechanical property changes, swelling, phase evolution, constituent re-distribution, and fuel performance in advanced fuels. Moreover, this research can be extended to establish a better understanding of FCCI and develop mitigation strategies for multiple fuel forms currently being explored within DOE-NE. This work will also provide a direct comparison to unirradiated and irradiated U-10Zr fuels fabricated in the same manner. Information acquired from previously awarded RTE’s (2017 and 2018) with TEM and 3D EBSD/EDS characterization of phases and cavities of U-10Zr fuels that have been irradiated to a moderate burnup (~ 6 at%) coupled with recent SEM and synchrotron results within this fuel will be used to complement this proposal findings. Finally, this research can be used to improve existing fuel performance codes by providing critical mechanical property data currently lacking in various cladding/fuel regions.
Book / Journal Publications

"Nano-mechanical Property Assessment of a Neutron Irradiated HT-9 Steel Cladding and a Fuel-cladding Chemical Interaction Region of a Uranium-10wt.% Zirconium Nuclear Fuel" Maria Okuniewski, MRS Advances 6 2021 1037-1042 Link