Direct Imaging of Tunable Crystal Surface Structures of MOF MIL-101 Using High-Resolution Electron Microscopy,Journal of the American Chemical Society

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Direct Imaging of Tunable Crystal Surface Structures of MOF MIL-101 Using High-Resolution Electron Microscopy
Journal of the American Chemical Society ( IF 14.4 ) Pub Date : 2019-07-19 , DOI: 10.1021/jacs.9b04896
Xinghua Li ₁ , Jianjian Wang ₂ , Xin Liu ₃ , Lingmei Liu ₁ , Dongkyu Cha ₄ , Xinliang Zheng ₅ , Ali A. Yousef ₄ , Kepeng Song ₁ , Yihan Zhu ₆ , Daliang Zhang ₂ , Yu Han ₁

Affiliation

Metal-organic frameworks (MOFs) are often synthesized using various additives to modulate the crystallization. Here, we report the direct imaging of the crystal surface of MOF MIL-101 synthesized with different additives, using low-dose high-resolution transmission electron microscopy (HRTEM), and identify three distinct surface structures, at subunit cell resolution. We find that the mesoporous cages at the outermost surface of MIL-101 can be opened up by vacuum heating treatment at different temperatures, depending on the MIL-101 samples. We monitor the structural evolution of MIL-101 upon vacuum heating, using in situ X-ray diffraction, and find the results to be in good agreement with HRTEM observations, which leads us to speculate that additives have an influence not only on the surface structure but also on the stability of framework. In addition, we observe solid-solid phase transformation from MIL-101 to MIL-53 taking place in the sample synthesized with hydrofluoric acid.

中文翻译：

使用高分辨率电子显微镜对 MOF MIL-101 的可调谐晶体表面结构进行直接成像

金属有机骨架 (MOF) 通常使用各种添加剂合成以调节结晶。在这里，我们报告了用不同添加剂合成的 MOF MIL-101 晶体表面的直接成像，使用低剂量高分辨率透射电子显微镜 (HRTEM)，并以亚单位细胞分辨率识别三种不同的表面结构。我们发现 MIL-101 最外表面的介孔笼可以通过在不同温度下的真空加热处理打开，具体取决于 MIL-101 样品。我们使用原位 X 射线衍射监测真空加热时 MIL-101 的结构演变，发现结果与 HRTEM 观察结果非常一致，这使我们推测添加剂不仅对表面结构有影响还要看框架的稳定性。

更新日期：2019-07-19

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