Effect of synthesis conditions on formation pathways of metal organic framework (MOF-5) Crystals

McKinstry, Colin and Cussen, Eddie and Fletcher, Ashleigh and Patwardhan, Siddharth and Sefcik, Jan (2013) Effect of synthesis conditions on formation pathways of metal organic framework (MOF-5) Crystals. Crystal Growth and Design, 13. pp. 5481-5489. ISSN 1528-7483

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    Abstract

    Metal Organic Frameworks (MOFs) represent a class of nanoporous crystalline materials with far reaching potential in gas storage, catalysis, and medical devices. We investigated the effects of synthesis process parameters on production of MOF-5 from terephthalic acid and zinc nitrate in diethylformamide. Under favorable synthesis conditions, we systematically mapped a solid formation diagram in terms of time and temperature for both stirred and unstirred conditions. The synthesis of MOF-5 has been previously reported as a straightforward reaction progressing from precursor compounds in solution directly to the final MOF-5 solid phase product. However, we show that the solid phase formation process is far more complex, invariably transferring through metastable intermediate crystalline phases before the final MOF-5 phase is reached, providing new insights into the formation pathways of MOFs. We also identify process parameters suitable for scale-up and continuous manufacturing of high purity MOF-5.