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Solvothermal synthesis is the most common método for producing high-quality, crystalline Metal-Organic Frameworks. The process involves heating a solution of the metal salt and organic linker in a sealed vessel, such as a Teflon-lined autoclave. The elevated temperature and pressão facilitate the dissolution of precursors and promote the crystallization of the thermodynamically stable MOF product over several hours or days.
Solvothermal synthesis is a subset of hydrothermal synthesis where the solvent is not necessarily water. For MOFs, high-boiling point organic solvents like N,N-dimethylformamide (DMF), N,N-diethylformamide (DEF), or N-methyl-2-pyrrolidone (NMP) are frequently used. The reaction is carried out in a sealed container, which allows the temperature to be raised above the solvent’s boiling point at atmospheric pressure, creating autogenous pressure inside the vessel.
The key advantages of this method are manifold. The increased temperature enhances the solubility of the reactants, ensuring a homogeneous reaction medium. It also provides the necessary activation energy for the formation of the metal-ligand coordination bonds and the subsequent nucleation and growth of the crystalline framework. The slow cooling process that often follows the heating period allows for the growth of large, well-defined single crystals, which are essential for determining the MOF’s structure via X-ray crystallography. Furthermore, the solvent molecules can act as templates or structure-directing agents, influencing which crystalline phase is formed. Modulators, such as monocarboxylic acids (e.g., acetic acid or formic acid), are often added to the reaction mixture to compete with the linker for coordination sites on the metal cluster, thereby slowing down the crystallization rate and improving the quality and size of the resulting crystals.
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Síntese solvotérmica de MOFs
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