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Abstract
Many unique adsorption properties of metal-organic frameworks (MOFs) have been revealed by diffraction crystallography, visualizing their vacant/guest-loaded crystal structures at the molecular scale. However, it has been challenging to see the spatial distribution of the adsorption behaviors throughout a single MOF particle in a transient equilibrium state. Here, we report three-dimensional (3D) visualization of molecular adsorption behaviors in a single crystalline particle of a MOF by operando X-ray absorption fine structure spectroscopy combined with computed tomography for the first time. The 3D maps of water-coordinated Co sites in a 100-µm-scale MOF-74-Co crystal were obtained with 1 µm spatial resolution under sever-al water vapor pressures. Through the visualization of the water vapor adsorption process, the 3D spectroimaging revealed the mechanism and spatial heterogeneity of guest adsorption inside a single particle of a crystalline MOF.
Supplementary materials
Title
SI_3D XAFS-CT on H2O Adsorption of MOF-74
Description
Details of the sample preparation, characterization, and procedures of XAFS-CT measurements, and analyses of image datasets, microbeam X-ray diffraction, and the 3D parameter maps of the other particles.
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