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Sequential ion-electron irradiation of zirconium carbide ceramics: Microstructural analysis
Journal of the European Ceramic Society ( IF 5.7 ) Pub Date : 2021-09-09 , DOI: 10.1016/j.jeurceramsoc.2021.09.017
Raul Florez 1 , Miguel L. Crespillo 2 , Xiaoqing He 3, 4 , Tommi A. White 3, 5 , Gregory Hilmas 6 , William G. Fahrenholtz 6 , Joseph Graham 1, 6
Affiliation  

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.



中文翻译:

碳化锆陶瓷的顺序离子-电子辐照:显微结构分析

在透射电子显微镜 (TEM)中用 10 MeV Au 3+离子照射碳化锆 (ZrC x )至每原子 10 个位移 (dpa) 的剂量,然后用 100 和 300 keV 电子照射。离子照射后,在微观结构中观察到位错环,拉曼光谱显示碳空位数量增加。掠入射X射线衍射(GIXRD)分析表明,样品在离子辐照过程中既没有发生非晶化也没有发生氧化。随后对预先植入的 ZrC x箔进行电子照射导致形成纳米尺寸的四方 ZrO 2在 TEM 薄片表面沉淀(5-10 nm 直径)。新氧化物相的形成与样品的电子束诱导加热无关,而是与透射电子显微镜内残留氧引起的电子刺激氧化有关。在电子照射后,在原始和离子照射的 ZrC x区域之间观察到ZrO 2微晶的尺寸和密度的变化,表明 ZrC x衬底的初始微观结构在氧化物岛的成核和生长中起关键作用。获得的结果提供了对 ZrC x微观结构响应的见解不同类型的辐射和电子束在原位异位离子辐照 ZrC x 的TEM 分析过程中的无意影响。此外,这项工作的发现提出了一种通过选择性电子束照射在 ZrC x晶粒内制备局部 ZrO 2纳米沉淀物的方法。

更新日期:2021-10-19
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