4.8 Article

Rapid Generation of Metal-Organic Framework Phase Diagrams by High-Throughput Transmission Electron Microscopy

Journal

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
Volume 144, Issue 15, Pages 6674-6680

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/jacs.2c01095

Keywords

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Funding

  1. Army Research Office [W911NF-15-1-0189]
  2. Northwestern University Ryan Fellowship
  3. International Institute of Nanotechnology
  4. Graduate School at Northwestern University
  5. Human Frontier Science Program [LT000869/2018-C]

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Metal-organic frameworks (MOFs) constructed from Zr-6 nodes and tetratopic carboxylate linkers exhibit high structural diversity and complexity. By utilizing high-throughput transmission electron microscopy (TEM), phase diagrams for Zr-6-MOFs with 1,4-dibromo-2,3,5,6-tetrakis(4-carboxyphenyl)benzene linkers can be rapidly generated, providing valuable insights into the correlation between MOF topologies and experimental parameters.
Metal-organic frameworks (MOFs) constructed from Zr-6 nodes and tetratopic carboxylate linkers display high structural diversity and complexity in which various crystal topologies can result from identical building units. To determine correlations between MOF topologies and experimental parameters, such as solvent choice or modulator identity and concentration, we demonstrate the rapid generation of phase diagrams for Zr-6-MOFs with 1,4-dibromo-2,3,5,6-tetrakis(4-carboxyphenyl)benzene linkers under a variety of conditions. We have developed a full set of methods for high-throughput transmission electron microscopy (TEM), including automated sample preparation and data acquisition, to accelerate MOF characterization. The use of acetic acid as a modulator yields amorphous, NU-906, NU-600, and mixed-phase structures depending on the ratio of N,N-dimethylformamide to NN-diethylformamide solvent and the quantity of the modulator. Notably, the use of formic acid as a modulator enables direct control of crystal growth along the c direction through variation of the modulator quantity, thus realizing aspect ratio control of NU-1008 crystals with different catalytic hydrolysis performance toward a nerve agent simulant.

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