In this work, we demonstrate a facile approach to develop mixed-valence vanadium oxides (VOx nanoparticle) and their derived nanostructured materials, which can be used as electrode materials for supercapacitor applications and capacitive deionization (CDI) applications. Our work starts on the development of suitable synthetic and characterization methods for the fabrication of VOx nanostructures with controlled properties. In the first part of this work, a continuous aerosol-based synthetic route with in-situ mobility size characterization is developed to fabricate VOx nanoparticles (NPs). Differential mobility analysis, X-ray diffractometry, X-ray photoelectron spectroscopy, and field emission scanning electron microscopy were employed complementarily for material characterization. Cyclic voltammetry and galvanostatic charge-discharge tests are used to evaluate the specific capacitance and charge-discharge stability of the synthesized VOx NPs. Particle size and mean valence of VOx NPs are controllable by adjusting the gas-phase synthetic conditions (atmosphere, temperature, gas flow rate). The specific capacitance of VOx NPs is shown to be proportional to the average valence of V, and the maximum specific capacitance (147.8 F/g) is achievable at an average oxidation state of 4.79 for vanadium.
In the second part of this work, we aim to develop vanadium oxide hybrid nanoparticles and study the interfacial phenomena of the hybrid nanostructured materials. Firstly, an aerosol-based synthetic approach is demonstrated for the development of vanadium oxide-carbon hybrid nanoparticles, which is used as electrode material for capacitive deionization technology. X-ray diffractometry, differential mobility analysis and field emission scanning electron microscopy along with elemental EDS analysis are employed complementarily for material characterization. Hybrid CDI cells are formed by combining vanadium oxide-carbon hybrid nanoparticles as the positive electrode and silver-carbon nanoparticle clusters as the negative electrode. The ions are stored through the charge transfer reaction between the two electrodes, which contributes to a large amount of deionization capacity and improves electrochemical stability. A remarkably high salt adsorption capacity up to 27.5 mg/g is achievable. Furthermore, the electrodes are modified by an electrochemical polymerization process of polypyrrole (PPy) to provide a protective layer for the structure of VOx-C NPC. The electrodes are successfully modified to yield salt adsorption capacity up to 49.3 mg/g and salt adsorption capacity retention is as high as 92%. This work provides a concept of using the aerosol-based synthesis with the support of complementary material characterization for the development of VOx-C NPC with high CDI performance.
In summary, this work demonstrates a prototype study of fast and continuous production of VOx NPs and their derived nanostructured materials with controlled material properties, showing promise in the tuning of cluster size, pore size and valence for the optimization of the corresponding electrochemistry performance. In addition, this work also provides an understanding of interfacial phenomena relevant to the formation of hybrid nanostructured materials and the performance in applications.

Abstract I
Table of Contents III
List of Figures V
List of Tables VIII
Chapter 1: Introduction 1
1.1 Overview of current development in electrical energy storage technologies and desalination technologies 1
1.2 Supercapacitor and capacitive deionization 3
1.2.1 Energy storage mechanism of supercapacitors [13] 3
1.2.2 Capacitive deionization 5
1.3 Vanadium oxides (VOx) nanomaterials 8
1.4 VOx Hybrid nanostructure is useful as electrode material 10
1.5 Aerosol-based synthesis and characterization 11
1.6 Scope and research objective 16
Chapter 2: Experimental Methods 20
2.1 Material 20
2.2 Material Characterization 21
2.2.1 X-Ray Diffraction (XRD) 21
2.2.2 Scanning electron microscope (SEM) 21
2.2.3 Differential Mobility Analyzer (DMA) 21
2.2.4 Specific Surface Area and Pore Volume Analyses 22
2.2.5 X-Ray Photoelectron Spectroscopy (XPS) 23
2.3 Experimental procedure 24
2.3.1 Aerosol-based synthesis of VOx nanoparticles 24
2.3.2 Aerosol-based synthesis of VOx-C nanoparticles and Ag-C-NPC 24
2.3.3 Electrode preparation for supercapacitor application 25
2.3.4 Electrochemical performance evolution 26
2.3.5 Electrode preparation for CDI application 27
2.3.6 CDI performance test 28
2.3.7 Preparation of PPy-coated electrodes 29
Chapter 3: Results and Discussions 33
3.1. Development of nanostructured mixed-valence vanadium oxides (VOx) as electrode materials for supercapacitor applications 33
3.1.1 Determination of the calcination temperature 33
3.1.2 Morphologies, crystalline and particle sizes 37
3.1.3 Analyses of the valence of the vanadium in VOx nanoparticle 42
3.1.4 Electrochemical analyses of VOx nanoparticle 53
3.2 Development of Vanadium oxide-carbon hybrid nanoparticles as electrode materials for inverted-capacitive deionization applications 58
3.2.1 Characterization of the VOx-C-NPC 58
3.2.2 Determination of potential window via electrochemical tests 64
3.2.3 Determination of the time for the charge/discharge cycles 68
3.2.4 Effect of carbon at the positive electrode on i-CDI performance 71
3.2.5 Effect of AgNP at negative electrode on i-CDI 74
3.2.6 Effect of surface passivation of VOx-C-NPC by PPy 76
3.2.7 Analyses of Salt Removal rate 85
Chapter 4: Conclusions 90
Chapter 5: Future Work 92
Chapter 6: References 96

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