Department of Physics, Faculty of Science, Huaykaew, Sutep, Muang, Chiang Mai University, Chiang Mai 50200, Thailand.
Micron. 2010 Jul;41(5):423-9. doi: 10.1016/j.micron.2010.02.009. Epub 2010 Feb 25.
In this work, a method to determine the atomic ratio of Mo and C within complex metal carbides using EELS in the TEM has been developed. The method is based on the determination of k-factors for given experimental conditions from the EEL spectra of Mo(2)C and MoO(3) standards, which had been independently checked by XRD and EPMA. Factors affecting the k(Mo/C) value of the Mo(2)C standard were also investigated and the value was shown to be insensitive to background subtraction window width but sensitive to prolonged irradiation and specimen thicknesses above a critical value. The method and k-factor obtained from the Mo(2)C standard was applied to spectra from a complex metal carbide precipitate formed during furnace cooling of a cast duplex stainless steel. Using EELS and EDS in the TEM, the composition was estimated to be (Cr(1.52)Fe(2.33)Mo(1.25)Ni(0.17)Si(0.46))C, which is close to M(6)C stoichiometry, and the structure was confirmed by electron diffraction.
在这项工作中,开发了一种使用 TEM 中的 EELS 确定复杂金属碳化物中 Mo 和 C 原子比的方法。该方法基于从 Mo(2)C 和 MoO(3)标准的 EEL 光谱确定给定实验条件下的 k 因子,这些标准已经通过 XRD 和 EPMA 独立检查。还研究了影响 Mo(2)C 标准 k(Mo/C)值的因素,结果表明该值对背景扣除窗口宽度不敏感,但对长时间辐照和超过临界厚度的样品敏感。从 Mo(2)C 标准获得的方法和 k 因子应用于在铸造双相不锈钢炉冷过程中形成的复杂金属碳化物析出物的光谱。使用 TEM 中的 EELS 和 EDS,估计组成接近 M(6)C 化学计量,结构通过电子衍射得到确认。