High-throughput screening of synthesis parameters in the formation of the metal-organic frameworks MOF-5 and HKUST-1

High-throughput methods were employed to study the influence of reaction parameters on the synthesis of the metal-organic frameworks MOF-5 (Zn4O[(OOC)(2) center dot C6H4](3)) and HKUST-1 (Cu-3[(OOC)(3)C6H3](2)(-H2O)(3) center dot xH(2)O). Thus, compositional parameters (metal salt, reagent concentrations, and pH) as well as process parameters (temperature, time) were investigated in order to establish reaction trends and fields of formation. A multiclave reaction block was used to perform the investigation of 24 different solvothermal reactions at a time. Attention was focused on the phase purity and the crystal morphology of the resulting compounds. The characterization of the samples was performed by X-ray powder diffraction and high resolution scanning electron microscopy. The experimental results show that the formation, phase purity. and morphology of MOF-5 and HKUST-1 are extremely sensitive to the synthesis parameters explored in this study. (C) 2008 Elsevier Inc. All rights reserved.