Sequential ion-electron irradiation of zirconium carbide ceramics: Microstructural analysis

Abstract

Zirconium Carbide (ZrCx) was irradiated with 10 MeV Au3+ ions to a dose of 10 displacements per atoms (dpa) and subsequently with 100 and 300 keV electrons in a transmission electron microscope (TEM). After ion irradiation, dislocation loops were observed in the microstructure and an increase in the number of carbon vacancies was revealed by Raman spectroscopy. Grazing incidence X-ray diffraction (GIXRD) analysis showed that neither amorphization nor oxidation occurred during ion irradiation of the specimen. Subsequent electron irradiation of the pre-implanted ZrCx foil led to formation of nanosized tetragonal ZrO2 precipitates (5−10 nm diameter) on the surface of the TEM lamella. The formation of the new oxide phase was not related to the electron beam-induced heating of the specimen, but to electron stimulated oxidation caused by the residual oxygen inside the transmission electron microscope. Changes in size and density of ZrO2 crystallites were observed between the pristine and ion irradiated ZrCx regions following electron irradiation, suggesting that the initial microstructure of the ZrCx substrate played a key role in the nucleation and growth of the oxide islands. The obtained results provide insights into the microstructural response of ZrCx to different types of radiation and the inadvertent effects of the electron beam during TEM analysis of in-situ and ex-situ ion irradiated ZrCx. Additionally, the findings of this work suggest a method to prepare local ZrO2 nanoprecipitates within ZrCx grains by selective electron beam irradiation.