Graphite Microstructural Characterization Using Time-Domain and Correlation-Based Ultrasonics

Abstract

Among techniques that have been used to determine elastic modulus in nuclear graphites, ultrasonic methods have enjoyed wide use and standards using contacting piezoelectric tranducers have been developed to ensure repeatability of these types of measurements. However, the use of couplants and the pressures used to effectively couple transducers to samples can bias measurements and produce results that are not wholly related to the properties of the graphite itself. In this work, we have investigated the use of laser ultrasonic methods for making elastic modulus measurements in nuclear graphites. These methods use laser-based transmitters and receivers to gather data and do not require use of ultrasonic couplants or mechanical contact with the sample. As a result, information directly related to the elastic responses of graphite can be gathered even if the graphite is porous, brittle and compliant. In particular, we have demonstrated the use of laser ultrasonics for the determination of both Young’s modulus and shear modulus in a range of nuclear graphites including those that are being considered for use in future nuclear reactors. These results have been analyzed to assess the contributions of porosity and microcracking to the elastic responses of these graphites. Laser-based methods have also been used to assess the moduli of NBG-18 and IG-110 where samples of each grade were oxidized to produce specific changes in porosity. These data were used to develop new models for the elastic responses of nuclear graphites and these models have been used to infer specific changes in graphite microstructure that occur during oxidation that affect elastic modulus. Specifically, we show how ultrasonic measurements in oxidized graphites are consistent with nano/microscale oxidation processes where basal plane edges react more readily than basal plane surfaces. We have also shown the use of laser-based methods to perform shear-wave birefringence measurements and have shown how these measurements can be used to assess elastic anisotropy in nuclear graphites. Using models developed in this program, ultrasonic data were interpreted to extract orientation distribution coefficients that could be used to represent anisotropy in these materials. This demonstration showed the use of ultrasonic methods to quantify anisotropy and how these methods provide more detailed information than do measurements of thermal expansion – a technique commonly used for assessing anisotropy in nuclear graphites. Finally, we have employed laser-based, ultrasonic-correlation techniques in attempts to quantify aspects of graphite microstructure such as pore size and distribution. Results of these measurements indicate that additional work must be performed to make this ultrasonic approach viable for quantitative microstructural characterization.