Direct imaging of correlated defect nanodomains in a metal-organic framework,Journal of the American Chemical Society

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Direct imaging of correlated defect nanodomains in a metal-organic framework
Journal of the American Chemical Society ( IF 14.4 ) Pub Date : 2020-07-04 , DOI: 10.1021/jacs.0c04468
Duncan N Johnstone ₁ , Francesca C N Firth ₂ , Clare P Grey ₂ , Paul A Midgley ₁ , Matthew J Cliffe ₃ , Sean M Collins _{1,

4}

Affiliation

Defect engineering can enhance key properties of metal–organic frameworks (MOFs). Tailoring the distribution of defects, for example in correlated nanodomains, requires characterization across length scales. However, a critical nanoscale characterization gap has emerged between the bulk diffraction techniques used to detect defect nanodomains and the subnanometer imaging used to observe individual defects. Here, we demonstrate that the emerging technique of scanning electron diffraction (SED) can bridge this gap uniquely enabling both nanoscale crystallographic analysis and the low-dose formation of multiple diffraction contrast images for defect analysis in MOFs. We directly image defect nanodomains in the MOF UiO-66(Hf) over an area of ca. 1000 nm and with a spatial resolution ca. 5 nm to reveal domain morphology and distribution. Based on these observations, we suggest possible crystal growth processes underpinning synthetic control of defect nanodomains. We also identify likely dislocations and small angle grain boundaries, illustrating that SED could be a key technique in developing the potential for engineering the distribution of defects, or “microstructure”, in functional MOF design.

中文翻译：

金属有机框架中相关缺陷纳米域的直接成像

缺陷工程可以增强金属有机框架（MOF）的关键性能。定制缺陷的分布（例如相关纳米域中的缺陷分布）需要跨长度尺度的表征。然而，用于检测缺陷纳米域的体衍射技术和用于观察单个缺陷的亚纳米成像之间出现了关键的纳米级表征差距。在这里，我们证明了新兴的扫描电子衍射（SED）技术可以弥合这一差距，以独特的方式实现纳米级晶体分析和低剂量形成用于 MOF 缺陷分析的多重衍射对比图像。我们直接对 MOF UiO-66(Hf) 中面积约 100 微米的缺陷纳米域进行成像。 1000 nm，空间分辨率约为 1000 nm。 5 nm 揭示域形态和分布。基于这些观察，我们提出了可能的晶体生长过程，以支持缺陷纳米域的合成控制。我们还确定了可能的位错和小角度晶界，这表明 SED 可能是开发功能 MOF 设计中缺陷分布或“微观结构”工程潜力的关键技术。

更新日期：2020-07-04

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