Elucidation of the Formation Mechanism of Metal–Organic Frameworks via in-Situ Raman and FTIR Spectroscopy under Solvothermal Conditions
| Autor: | Wolfgang Peukert, Martin Kriesten, Martin Hartmann, Heidemarie Embrechts, Kilian Hoffmann, Monica Distaso |
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| Rok vydání: | 2018 |
| Předmět: |
Materials science
Formic acid Precipitation (chemistry) Reaction step Nucleation 02 engineering and technology 010402 general chemistry 021001 nanoscience & nanotechnology 01 natural sciences 0104 chemical sciences Surfaces Coatings and Films Electronic Optical and Magnetic Materials chemistry.chemical_compound symbols.namesake General Energy chemistry symbols Molecule Physical chemistry Metal-organic framework Physical and Theoretical Chemistry Fourier transform infrared spectroscopy 0210 nano-technology Raman spectroscopy |
| Zdroj: | The Journal of Physical Chemistry C. 122:12267-12278 |
| ISSN: | 1932-7455 1932-7447 |
| DOI: | 10.1021/acs.jpcc.8b02484 |
| Popis: | The metal–organic framework MIL-53(Al) serves as a model system in this study. Its formation mechanism in N,N-dimethylformamide (DMF) is elucidated through simultaneous FTIR and Raman spectroscopy and turbidity measurements collected under in-situ synthesis conditions in a custom-designed solvothermal reactor coupled with reaction sampling. Different synthesis steps are followed over synthesis time including a prenucleation building unit (PNBU) consisting of one linker molecule and one aluminum atom, the assembly of the PNBUs to MIL-53 nuclei in solution, the decomposition of DMF to formic acid and dimethylammonium, and finally the precipitation of the crystalline MOF phase. The rearrangement of the PNBU to form MIL-53 is identified as the rate-limiting reaction step responsible for the long induction time at low temperatures ( |
| Databáze: | OpenAIRE |
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