Impact of Synthesis Parameters on the Formation of Defects in HKUST-1

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• 作者：Wenhua Zhang ; Max Kauer ; Penghu Guo ; Sebastian Kunze ; Stefan Cwik ; Martin Muhler ; Yuemin Wang ; Konstantin Epp ; Gregor Kieslich and Roland A. Fischer
• 刊名：European Journal of Inorganic Chemistry
• 出版年：2017
• 出版时间：February 03, 2017
• 年：2017
• 卷：2017
• 期：5
• 页码：925-931
• 全文大小：1626K
• ISSN：1099-0682c

文摘

By employing various synthetic conditions, such as Cu(NO₃)₂·3H₂O and Cu(BF₄)₂·6H₂O as copper ion sources and different solvents, defect-engineered analogues of metal–organic framework (MOF) [Cu₃(BTC)₂] (HKUST-1; BTC = 1,3,5-benzenetricarboxylate) with isophthalate (IP) incorporation (DEMOFs) were synthesised and characterised by powder XRD, SEM, IR spectroscopy, thermogravimetric analysis, NMR spectroscopy and N₂ sorption. The results show that the choice of counter ions impacts the properties of the samples especially at high concentrations of IP. The combination of DMF and Cu(BF₄)₂·6H₂O turns out to be superior for DEMOFs with IP incorporation up to 25 %. Ultrahigh-vacuum IR spectra recorded upon CO adsorption together with the results of X-ray photoelectron spectroscopic studies show the generation of coordinatively unsaturated Cu⁺ sites. The results suggest the presence of two different defect types, that is, missing-linker defects and missing paddlewheels for high concentrations of IP.