Electrochemical copolymerizations of thiophene (Th) and 3,4-ethylenedioxythiophene (EDOT) was performed in this study. Incorporation of Th with EDOT units have accelerated deposition rate in relative to the simple polymerization behavior of EDOT. The electrochemical properties of poly(thiophene-co-3,4-ethylenedioxythiophene) (PTh-EDOT) are different from the homopolymers of polythiophene (PTh) and poly(3,4-ethylenedioxythiophene) (PEDOT). PTh-EDOT were then served as cathode materials of lithium-ion (Li-ion) batteries to test their capability to transfer lithium ion in 1.0 M LiPF6/ethylene carbonate/dimethyl carbonate solution. PTh-EDOT copolymer prepared from the monomer ratio of 1/1 (Th/EDOT) shows better stability than PEDOT and PTh homopolymers, polymer property enhancement by copolymerization is thus demonstrated. A composite electrode material PEDOT/LiCoO2 was prepared from the electrochemical polymerization of EDOT on LiCoO2 electrode was primarily prepared to inspect the influence of PEDOT on the electrochemical features of LiCoO2. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) show the successful deposition of PEDOT over LiCoO2 particles. Compared to the simple LiCoO2 electrode, PEDOT/LiCoO2 composite cathode shows enhanced properties including rate capability and cycle stability for potential Li-ion battery application. Nevertheless, differential scanning calorimetry (DSC) scans on the fully charged cathodes imply that PEDOT may reduce the thermal stability of LiCoO2. Two carbon materials, vapor grown carbon fibers (VGCF) and nano-scaled Ketjen black EC (KB), were implemented into LiCoO2 electrode. The influence of different carbon additive and their content on the performance of LiCoO2 such as rate capability and cycle ability has been evaluated. KB shows more positive effects than VGCF even in the case of a low 1 wt% content. Furthermore, incorporation of PEDOT was made by electrochemical deposition of EDOT on the preformed LiCoO2-VGCF and LiCoO2-KB composite electrodes. The influence of the carbon additives and the conductive PEDOT polymer on LiCoO2 was then investigated. Compared to the electrodes without PEDOT coating, PEDOT-incorporated composite electrodes show larger capacity, better transfer rate of lithium ions in electrolytes, and enhanced cycle ability. The electrochemical deposition of PEDOT on the LiCoO2/nano-carbon cathodes provides a new approach to implement the conducting polymers in Li-ion batteries.

The experimental data and results demonstrated here illustrate the preparation and application of mesoporous metal oxides in energy storage, adsorption, and catalysis. First, a new method of controlling the pore size and wall thickness of mesoporous silica was developed by controlling the calcination temperature. A series of such silica were used as hard templates to prepare the mesoporous metal oxide Co₃O₄. Using other methods, such as varying the silica template hydrothermal treatment temperature, using colloid silica, varying the materials ratio etc., a series of mesoporous β-MnO₂ with different pore size and wall thickness were prepared. By using these materials it has been possible to explore the influence of pore size and wall thickness on the rate of lithium intercalation into mesoporous electrode. There is intense interest in lithium intercalation into titanates due to their potential advantages (safety, rate) replacing graphite for new generation Li-ion battery. After the preparation of an ordered 3D mesoporous anatase the lithium intercalation as anode material has been investigated. To the best of our knowledge, there are no reports of ordered crystalline mesoporous metal oxides with microporous walls. Here, for the first time, the preparation and characterization of three dimensional ordered crystalline mesoporous α-MnO₂ with microporous wall was described, in which K+ and KIT-6 mesoporous silica act to template the micropores and mesopores, respectively. It was used as a cathode material for Li-ion battery. Its adsorption behavior and magnetic property was also surveyed. Following this we described the preparation and characterization of mesoporous CuO and reduced Cu[subscript(x)]O, and demonstrated their application in NO adsorption and delivery. Finally a series of crystalline mesoporous metal oxides were prepared and evaluated as catalysts for the CO oxidation.

Transition metal oxide coupling with carbon is an effective method for improving electrical conductivity of battery electrodes and avoiding the degradation of their lithium storage capability due to large volume expansion/contraction and severe particle aggregation during the lithium insertion and desertion process. In our present work, we develop an effective approach to fabricate the nanocomposites of porous rod-shaped Fe₃O₄ anchored on reduced graphene oxide (Fe₃O₄/rGO) by controlling the in situ nucleation and growth of β-FeOOH onto the graphene oxide (β-FeOOH/GO) and followed by dielectric barrier discharge (DBD) hydrogen plasma treatment. Such well-designed hierarchical nanostructures are beneficial for maximum utilization of electrochemically active matter in lithium ion batteries and display superior Li uptake with high reversible capacity, good rate capability, and excellent stability, maintaining 890 mA h g⁻¹ capacity over 100 cycles at a current density of 500 mA g⁻¹.

This doctoral thesis deals with synthesis and characterisation of electroactive electrode materials for li-ion batteries and accumulators. The work is divided into two main parts. One deals with LiFePO4 based cathode composite electroactive material and in the second is described the synthesis and utilization of monoclinic TiO2(B) as an anode for li-ion cell. The main aim of the work is to relate the synthesis procedure and structural properties of both materials to its electrochemical preformance.