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Direct Synthesis of ZIF‐8 on Transmission Electron Microscopy Grids Allows Structure Analysis and 3D Reconstruction
Particle & Particle Systems Characterization ( IF 2.7 ) Pub Date : 2020-09-28 , DOI: 10.1002/ppsc.202000209
Milena Hugenschmidt 1, 2 , Ksenia Kutonova 2, 3 , Elvia P. Valadez Sánchez 4 , Sarah Moulai 4 , Hartmut Gliemann 4 , Stefan Bräse 2, 3, 5 , Christof Wöll 4 , Dagmar Gerthsen 1, 2
Affiliation  

The first example of layer‐by‐layer growth of a metal–organic framework (MOF) directly on transmission electron microscopy (TEM) grids is described. ZIF‐8 is deposited on thin amorphous carbon films and subjected to a structure analysis by (scanning) TEM ((S)TEM). This method serves as a two‐in‐one synthesis and TEM sample‐preparation technique and allows straightforward analysis of ZIF‐8 crystallites. Artifacts resulting from sample preparation are completely avoided by this approach. The morphological properties, crystal structure, and the chemical composition of the material are investigated with high spatial resolution by a variety of methods of (analytical) electron microscopy. Furthermore, the incorporation of metallic nanoparticles in ZIF‐8 by integrating a corresponding step into the layer‐by‐layer deposition process is examined. The formation of ZIF‐8 crystals on the film proceeds as under the absence of nanoparticle‐forming synthesis steps. However, the nanoparticles rather cover the supporting amorphous carbon film than being incorporated in the ZIF‐8 material. This information cannot be obtained from standard characterization techniques but requires the application of analytical (S)TEM techniques.

中文翻译:

ZIF-8 在透射电子显微镜网格上的直接合成允许结构分析和 3D 重建

描述了直接在透射电子显微镜 (TEM) 网格上逐层生长金属有机框架 (MOF) 的第一个例子。ZIF-8 沉积在非晶碳薄膜上,并通过(扫描)TEM((S)TEM)进行结构分析。该方法可作为一种二合一的合成和 TEM 样品制备技术,可以直接分析 ZIF-8 微晶。这种方法完全避免了因样品制备而产生的伪影。通过各种(分析)电子显微镜方法以高空间分辨率研究材料的形态特性、晶体结构和化学成分。此外,通过将相应的步骤集成到逐层沉积过程中,研究了将金属纳米粒子掺入 ZIF-8 中。在没有纳米颗粒形成合成步骤的情况下,ZIF-8 晶体在薄膜上的形成过程。然而,纳米粒子更倾向于覆盖支撑的无定形碳膜,而不是包含在 ZIF-8 材料中。此信息无法通过标准表征技术获得,但需要应用分析 (S)TEM 技术。
更新日期:2020-09-28
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