Ultra-fast supercritically solvothermal polymerization for large single-crystalline covalent organic frameworks

Xuejun Wang, Yunqi Liu, Dacheng Wei, Jiang Sun, Qiankun Wang, Lan Peng

Published: 2023-11-24 DOI: 10.1038/s41596-023-00915-7

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Introduction
Materials
Procedure
Troubleshooting
Timing
Anticipated results
Acknowledgements
Extended Data Fig. 1 Growth of sc-COFTP-Py in sc-CO2 with different concentrations of n-BuOH.
Extended Data Fig. 2 Morphologies of the as-synthesized os-COFs.
Extended Data Fig. 3 FT-IR spectra of the samples.
Extended Data Fig. 4 N2 adsorption isotherms of the samples.
Extended Data Fig. 5 13C solid-state NMR spectra.
Extended Data Fig. 6 PXRD characterization of sc-COFs and os-COFs.
Extended Data Fig. 7 TEM images of sc-COFTB-BA.
Extended Data Fig. 8 TEM images of a sc-COFTP-Py single crystal.
Extended Data Fig. 9 OM images and cross-polarized OM images of sc-COFs.
Extended Data Fig. 10 Comparison with different polymerization methods.

Figure 1
Fig. 1: Schematic illustration of the crystal growth process.
Figure 2
Fig. 2: Single-crystal polymerization mechanism of COFs in sc-CO2.
Figure 3
Fig. 3: Workflow of the preparation of monomer dispersion.
Figure 4
Fig. 3: Workflow of the preparation of monomer dispersion.
Figure 5
Fig. 4: Workflow of polymerization in sc-CO2.
Figure 6
Fig. 4: Workflow of polymerization in sc-CO2.
Figure 7
Fig. 5: Workflow of purifying and drying the product.
Figure 8
Fig. 5: Workflow of purifying and drying the product.
Figure 9
Fig. 6: The polymerization reactions for producing COFs in sc-CO2.
Figure 10
Fig. 6: The polymerization reactions for producing COFs in sc-CO2.
Figure 11
Fig. 7: Ultra-fast crystal growth of sc-COFs.
Figure 12
Fig. 7: Ultra-fast crystal growth of sc-COFs.
Figure 13
Fig. 8: Equipment setup for supercritically solvothermal synthesis.
Figure 14
Fig. 8: Equipment setup for supercritically solvothermal synthesis.
Figure 15
Fig. 9: Stainless steel reactor.
Figure 16
Fig. 9: Stainless steel reactor.
Figure 17
Fig. 10: Workflow of optical microscope characterization.
Figure 18
Fig. 10: Workflow of optical microscope characterization.
Figure 19
Fig. 11: Morphologies of the as-synthesized sc-COFs.
Figure 20
Fig. 11: Morphologies of the as-synthesized sc-COFs.
Figure 21
Fig. 12: PXRD characterization of sc-COFs and os-COFs.
Figure 22
Fig. 12: PXRD characterization of sc-COFs and os-COFs.
Figure 23
Fig. 13: HR-TEM images and SAED patterns of 2D sc-COFs.
Figure 24
Fig. 13: HR-TEM images and SAED patterns of 2D sc-COFs.
Figure 25
Fig. 14: HR-TEM images and SAED patterns of 3D sc-COFs.
Figure 26
Fig. 14: HR-TEM images and SAED patterns of 3D sc-COFs.
Figure 27
Fig. 15: Characterization of the sc-COFTP–Py single crystals.
Figure 28
Fig. 15: Characterization of the sc-COFTP–Py single crystals.
Figure 29
Fig. 16: Polarized PL and SHG results of sc-COFs.
Figure 30
Fig. 16: Polarized PL and SHG results of sc-COFs.

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Ultra-fast supercritically solvothermal polymerization for large single-crystalline covalent organic frameworks

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