Abstract

The structure and mechanism of formation of a novel hexagonal mesostructured vanadium oxide−surfactant composite (HMVO), synthesized by acid-catalyzed hydrolysis of ethanolic cetyltrimethylammonium vanadate (CTAV) solution, has been studied by a variety of spectroscopic techniques. The poorly crystalline CTAV precursor used in the synthesis has been characterized and is shown to consist of pyrovanadate-like anions in which one oxygen atom is shared between vanadate tetrahedra. The HMVO formed from this precursor appears to feature a distorted octahedral vanadium coordination similar to that found in extended structures such as the two-dimensional vanadium pentoxide gel network. Information on the solution speciation during the synthesis is monitored by 51V NMR spectroscopy. Prior to acid addition, the ethanolic solution of CTAV shows a single narrow resonance at −556.7 ppm, assigned to a tetrahedral diester anion [VO2(OEt)2]-, undergoing fast reorientational averaging of the quadrupole interaction in solu...

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