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Nucleation and Crystal Growth of a {V 14 Sb 8 O 42 } Cluster from a {V 15 Sb 6 O 42 } Polyoxovanadate: In Situ XRD Studies
Author(s) -
Wendt Michael,
Mahnke Lisa K.,
Heidenreich Niclas,
Bensch Wolfgang
Publication year - 2016
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.201601025
Subject(s) - chemistry , nucleation , crystallography , crystal growth , cluster (spacecraft) , dissolution , kinetics , limiting , crystal (programming language) , ethylenediamine , hydrothermal circulation , activation energy , chemical kinetics , inorganic chemistry , chemical engineering , mechanical engineering , physics , organic chemistry , quantum mechanics , computer science , engineering , programming language
The hydrothermal transformation of the heteroatom polyoxovanadate compound {Ni(en) 3 } 3 [V 15 Sb 6 O 42 (H 2 O)] · ≈15H 2 O (en = ethylenediamine) in water into [{Ni(en) 2 } 2 V 14 Sb 8 O 42 ] · 5.5H 2 O was investigated by in situ XRD experiments at different temperatures. First, the precursor undergoes very fast amorphization or dissolution, and an induction period is observed that depends on the reaction temperature. Crystal growth of the product is completed within 3 h, while higher temperatures lead to accelerated reaction progress. Evaluation of the kinetics showed that heterogeneous nucleation is the rate‐limiting step of the reaction. The activation energies for nucleation and crystal growth are very low compared to data reported in the literature for several other chemical systems.