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Impact of Synthesis Parameters on the Formation of Defects in HKUST‐1
Author(s) -
Zhang Wenhua,
Kauer Max,
Guo Penghu,
Kunze Sebastian,
Cwik Stefan,
Muhler Martin,
Wang Yuemin,
Epp Konstantin,
Kieslich Gregor,
Fischer Roland A.
Publication year - 2017
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201601239
Subject(s) - chemistry , thermogravimetric analysis , x ray photoelectron spectroscopy , sorption , copper , infrared spectroscopy , metal organic framework , adsorption , linker , ion , metal , spectroscopy , nuclear magnetic resonance spectroscopy , nuclear chemistry , crystallography , inorganic chemistry , stereochemistry , chemical engineering , organic chemistry , physics , quantum mechanics , computer science , engineering , operating system
By employing various synthetic conditions, such as Cu(NO 3 ) 2 · 3H 2 O and Cu(BF 4 ) 2 · 6H 2 O as copper ion sources and different solvents, defect‐engineered analogues of metal–organic framework (MOF) [Cu 3 (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 N 2 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(BF 4 ) 2 · 6H 2 O 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.