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| Title: | TRANSMISSION ELECTRON MICROSCOPY AND FLOW FIELD-FLOW FRACTIONATION: EXPLORATION OF THE NANOSCOPIC COMPONENTS IN PARTIALLY REDUCED POLYOXOMOLYBDATES BY KINETIC PRECIPITATION WITH DE NOVO ORGANIC MOLECULES |
| Authors: | Zhu, Yan |
| Keywords: | Molecular recognition
Nanostructure
Polyoxomolybdate
Electron microscopy
Field flow fractionation |
| Date Created: | 2003 |
| Publisher: | University of Kentucky |
| Abstract: | Although molybdenum blue solutions have been known for more than two
centuries, an understanding of their chemical nature is only beginning to emerge.
This dissertation aimed at elucidating the structural nature of the polydisperse,
nanoscopic components in the solution phases and the solid states of partially
reduced polyoxomolybdate (Mo-POM). The study offered at least four
contributions to the area: (1) a rational protocol for the molecular recognition of
Mo-POM with de novo organic hosts. (2) demonstration of kinetic precipitation of
a dynamic mixture of polyoxomolybdates and application of the technique to the
study of the dynamic mixture by TEM (3) characterization of the Mo-POM
nanostructures by an unusual combination of complementary analytical
techniques. (4) a general approach for the synthesis of crown-ethers-containing
tripodal molecules.
The molecular recognition of Mo-POM with designer tripodal hexaminetris-
crown ethers opened a window to the solution phase structures of Mo-POM
nanoscopic components. Studies with a series of structurally analogous hosts
probed the relationship between the structure of the molecular host and the
formation of nanostructures.
An unusual combination of complementary analytical protocols: flow fieldflow
fractionation, electron microscopy (transmission and scanning), and
inductively coupled plasma – emission spectroscopy, was used to monitor the
solution-phase evolution of Mo-POM nanostructures. The crystallization – driven
formation of keplerate Mo-POM and solution-phase evolution of structurally
related nanoscopic species were apparent in the self-assembling process of
partially reduced Mo-POM. |
| URI: | http://hdl.handle.net/10225/155 |
| Appears in Collections: | Electronic Theses and Dissertations
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| YanZhuPHDthesis.pdf | | 12215Kb | Adobe PDF | View/Open |
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