Functional Group Mapping by Electron Beam Vibrational Spectroscopy from Nanoscale Volumes.,Nano Letters

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Functional Group Mapping by Electron Beam Vibrational Spectroscopy from Nanoscale Volumes.
Nano Letters ( IF 9.6 ) Pub Date : 2020-01-21 , DOI: 10.1021/acs.nanolett.9b04732
Sean M Collins ₁ , Demie M Kepaptsoglou _{2,

3} , Jingwei Hou ₁ , Christopher W Ashling ₁ , Guillaume Radtke ₄ , Thomas D Bennett ₁ , Paul A Midgley ₁ , Quentin M Ramasse _{2,

5}

Affiliation

Vibrational spectroscopies directly record details of bonding in materials, but spatially resolved methods have been limited to surface techniques for mapping functional groups at the nanoscale. Electron energy loss spectroscopy (EELS) in the scanning transmission electron microscope presents a route to functional group analysis from nanoscale volumes using transmitted subnanometer electron probes. Here, we now use vibrational EELS to map distinct carboxylate and imidazolate linkers in a metal-organic framework (MOF) crystal-glass composite material. Domains <100 nm in size are observed using vibrational EELS, with recorded spatial resolution <15 nm at interfaces in the composite. This nanoscale functional group mapping is confirmed by correlated EELS at core ionization edges as well as X-ray energy dispersive spectroscopy for elemental mapping of the metal centers of the two constituent MOFs. These results present a complete nanoscale analysis of the building blocks of the MOF composite and establish spatially resolved functional group analysis using electron beam spectroscopy for crystalline and amorphous organic and metal-organic solids.

中文翻译：

通过电子束振动光谱从纳米级体积进行官能团映射。

振动光谱法直接记录了材料中键合的细节，但是空间分辨方法仅限于用于绘制纳米级官能团的表面技术。扫描透射电子显微镜中的电子能量损失谱（EELS）提出了使用透射亚纳米电子探针从纳米级体积进行官能团分析的途径。在这里，我们现在使用振动EELS在金属-有机骨架（MOF）晶体玻璃复合材料中绘制不同的羧酸盐和咪唑盐连接子。使用振动EELS观察到尺寸小于100 nm的畴，在复合材料的界面处记录的空间分辨率小于15 nm。通过在核心电离边缘处的相关EELS以及用于对两个组成MOF的金属中心进行元素映射的X射线能量色散光谱学，证实了这种纳米级官能团映射。这些结果提供了对MOF复合材料结构单元的完整纳米级分析，并使用电子束光谱技术对晶体和非晶有机和金属有机固体进行了空间分辨的官能团分析。

更新日期：2020-01-22

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