Synthesis and Characterization of Nanostructured Metal Oxides and Metal-Organic Frameworks

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Synthesis and Characterization of Nanostructured Metal Oxides and Metal-Organic Frameworks

Abstract

The field of metal oxides is as large as it is fascinating. Whereas the amount of metal oxides in
the world are finite, their potential applications are seemingly endless. This thesis aims to
explore the synthesis of metal oxides using two different approaches: Electrochemical
deposition of a metal oxide as a method for the indirect electrosynthesis of a metal-organic
frameworkand thermal oxidation of templated novel metal oxide structures.

Metal-organic frameworks (MOFs) are a versatile class of porous materials. A high surface area,
remarkable stability and seemingly endless tunability has led to various synthesis methods as
well as a vast number of applications. Chapter 1 presents a literature review into the
electrosynthesis of MOFs through direct as well as indirect means. It provides an introduction
into the field of MOFs and an explanation of the most important concepts.

Chapter 2 discusses the indirect electrosynthesis of the well-known ZIF-8. By using a new
method that relies on zinc oxide as a nucleation site as well as a reactant source, the formation
of a nanostructured hybrid material was achieved in a fast and simple manner. First, the
electrodeposition of zinc oxide nanorods on FTO glass was optimized in order to obtain a welldefined,
homogenous nanorod arrays. A thin layer of linker was then deposited onto these rods
and heated. The result is the formation of a ZIF-8 thin film. The effect of synthesis conditions
were investigated for both zinc oxide synthesis as well as thin film formation using XRD and
SEM.

Finally, chapter 3 discusses the use of polymers of intrinsic microporosity (PIMs) as templating
materials for the synthesis of praseodymium and cerium oxides through thermal oxidation.
These metal oxides were formed using two different PIMs (PIM-EA-TB and PIM-1). Each PIM
yields a pure oxide with a novel, unique porous structure. The composition, oxidation state and
the electrochemical properties of these oxides were studied using CV, SEM, XPS and Raman
spectroscopy.

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