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tert ‐Butyl( tert ‐butoxy)zinc Hydroxides: Hybrid Models for Single‐Source Precursors of ZnO Nanocrystals
Author(s) -
Sokołowski Kamil,
Justyniak Iwona,
Bury Wojciech,
Grzonka Justyna,
Kaszkur Zbigniew,
Mąkolski Łukasz,
Dutkiewicz Michał,
Lewalska Agnieszka,
Krajewska Elżbieta,
Kubicki Dominik,
Wójcik Katarzyna,
Kurzydłowski Krzysztof J.,
Lewiński Janusz
Publication year - 2015
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201406245
Subject(s) - zinc , thermogravimetric analysis , thermal decomposition , crystallography , powder diffraction , chemistry , nanocrystal , yield (engineering) , single crystal , molar ratio , infrared spectroscopy , crystal structure , nuclear chemistry , inorganic chemistry , materials science , catalysis , organic chemistry , nanotechnology , metallurgy
Alkylzinc alkoxides, [RZnOR′] 4 , have received much attention as efficient precursors of ZnO nanocrystals (NCs), and their “Zn 4 O 4 ” heterocubane core has been regarded as a “preorganized ZnO”. A comprehensive investigation of the synthesis and characterization of a new family of tert ‐butyl( tert ‐butoxy)zinc hydroxides, [( t Bu) 4 Zn 4 (μ 3 ‐O t Bu) x (μ 3 ‐OH) 4− x ], as model single‐source precursors of ZnO NCs is reported. The direct reaction between well‐defined [ t BuZnOH] 6 ( 1 6 ) and [ t BuZnO t Bu] 4 ( 2 4 ) in various molar ratios allows the isolation of new mixed cubane aggregates as crystalline solids in a high yield: [( t Bu) 4 Zn 4 (μ 3 ‐O t Bu) 3 (μ 3 ‐OH)] ( 3 ), [( t Bu) 4 Zn 4 (μ 3 ‐O t Bu) 2 (μ 3 ‐OH) 2 ] ( 4 ), [( t Bu) 4 Zn 4 (μ 3 ‐O t Bu)(μ 3 ‐OH) 3 ] ( 5 ). The resulting products were characterized in solution by 1 H NMR and IR spectroscopy, and in the solid state by single‐crystal X‐ray diffraction. The thermal transformations of 2 – 5 were monitored by in situ variable‐temperature powder X‐ray diffraction and thermogravimetric measurements. The investigation showed that the ZnOH groups appeared to be a desirable feature for the solid‐state synthesis of ZnO NCs that significantly decreased the decomposition temperature of crystalline precursors 3 – 5 .