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Abstract Electrochemical energy storage devices have promoted considerable revolution to the state-of- the-art energy storage technologies because of the commercialization of portable electronics and the potential for widespread implementation on plug-in hybrid electric vehicles. To advance such technologies, it is of great importance to develop electrode materials with high electrochemical activity. As a result, developing and improving the performance of these active materials is critical to improving the performance of these types of energy devices. Nanostructured materials have a lot of promise as an effective electrode material for high- performance supercapacitor applications. In my thesis, I show how to produce nanostructured materials from transition metal oxides and sulfides in a simple and efficient sol–gel auto- combustion and hydrothermal method for Li-ion batteries and supercapacitor applications. In this respect, the fundamental elements of supercapacitors in terms of charge storage methods, as well as recent advancements in the design and manufacture of electrode materials, as well as energy-related performance, were discussed. In Chapter 3: Spinel Li2 Co 1-x Cu xTi3 O8 nanopowders (x = 0, 0.25, 0.5 molar ratios) have been fabricated using a sol–gel auto-combustion method. The synthesis conditions such as annealing temperature, Cu2+ ion substituted on the crystal structure, microstructure and chemical composition were investigated using X-ray diffraction, scanning electron microscopy and X- rays photoelectron spectroscopy, respectively. Furthermore, the electrochemical properties of have been inspected via cyclic voltammetry (CV), galvanostatic charge-discharge, and electrochemical impedance spectroscopy (EIS). The Li2 Co 0.75 Cu 0.25 Ti3 O8 electrode exhibited high similarity to Li2 CoTi3 O 8 with a good reversible charge-discharge capacity and excellent cycling stability. Li2 Co 0.75 Cu 0.25Ti3 O8 exhibited initial discharge capacity of 527 mAh g−1 , and superlong stability performance of 98.75% coulombic efficiency. In Chapter 4: The ability to prepare two-dimensional (2D) metal chalcogenide nanoflakes is of great importance for the further exploration of their properties. In the light of this, my aim in this thesis is to synthesize 2D metal chalcogenide nanoflakes and then explore their potential applications in Li-ion batteries and supercapacitor |