Department of Chemistry-Ångström, Uppsala University, Box 538, S-751 21 Uppsala, Sweden.
Department of Chemistry-Ångström, Uppsala University, Box 538, S-751 21 Uppsala, Sweden and Department of Physics & Astronomy, University College London, London WC1E 6BT, United Kingdom.
Phys Rev Lett. 2014 Apr 18;112(15):156102. doi: 10.1103/PhysRevLett.112.156102. Epub 2014 Apr 17.
We propose a resolution to the puzzle presented by the surface defects observed with STM at the (111) surface facet of CeO 2 single crystals. In the seminal paper of Esch et al. [Science 309, 752 (2005)] they were identified with oxygen vacancies, but the observed behavior of these defects is inconsistent with the results of density functional theory (DFT) studies of oxygen vacancies in the literature. We resolve these inconsistencies via DFT calculations of the properties of both oxygen vacancies and fluorine impurities at CeO2(111), the latter having recently been shown to exist in high concentrations in single crystals from a widely used commercial source of such samples. We find that the simulated filled-state STM images of surface-layer oxygen vacancies and fluorine impurities are essentially identical, which would render problematic their experimental distinction by such images alone. However, we find that our theoretical results for the most stable location, mobility, and tendency to cluster, of fluorine impurities are consistent with experimental observations, in contrast to those for oxygen vacancies. Based on these results, we propose that the surface defects observed in STM experiments on CeO2 single crystals reported heretofore were not oxygen vacancies, but fluorine impurities. Since the similarity of the simulated STM images of the two defects is due primarily to the relative energies of the 2p states of oxygen and fluorine ions, this confusion might also occur for other oxides which have been either doped or contaminated with fluorine.
我们提出了解决 CeO2 单晶 (111) 表面面元的 STM 观测到的表面缺陷这一难题的方案。在 Esch 等人的开创性论文[Science 309, 752 (2005)]中,这些缺陷被认为是氧空位,但这些缺陷的观测行为与文献中氧空位的密度泛函理论(DFT)研究结果不一致。我们通过 DFT 计算 CeO2(111)上的氧空位和氟杂质的性质来解决这些不一致性,最近的研究表明,在广泛使用的此类样品商业来源的单晶中,氟杂质的浓度很高。我们发现,模拟的表面层氧空位和氟杂质的填充态 STM 图像基本相同,这使得仅凭这些图像难以区分它们。然而,我们发现,我们对氟杂质最稳定位置、迁移率和聚集倾向的理论结果与实验观察结果一致,而氧空位的结果则不一致。基于这些结果,我们提出,迄今为止在 CeO2 单晶的 STM 实验中观察到的表面缺陷不是氧空位,而是氟杂质。由于两种缺陷的模拟 STM 图像的相似性主要归因于氧离子和氟离子的 2p 态的相对能量,因此这种混淆也可能发生在其他已经掺杂或被氟污染的氧化物中。