This study reports on an electrochemical capacitive properties of nickel tetraaminophthalocyanine (NiTAPc), nickel tetraaminophthalocyanine incorporated with Nickel oxide (NiTAPc-NiO) and nickel oxide incorporated with multi-walled carbon nanotubes (NiO-MWCNT), using three different techniques known as successive ionic layer adsorption reaction (SILAR), electrodeposition and dip-dry. This study also reports on the effect of undoped polymer of poly-pyrrole on NiTAPc. The physical properties of the synthesised materials were investigated using SEM and EDX and the electrochemical properties were investigated using cyclic voltammetry (CV), charge-discharge (CD) and electrochemical impedance spectroscopy (EIS). The supercapacitive properties of NiTAPc film on nickel foam showed a maximum specific capacitance of 416.0 Fg-1, a maximum power density of 15.50x103 WKg-1 and a maximum specific energy of 66.0 WhKg-1. The NiO-MWCNT film on nickel foam gave a maximum specific capacitance of 1034.0 Fg-1, a maximum power density of 10.41x103 WKg-1 and a maximum specific energy of 132.0 WhKg-1. The NiTAPc-NiOE film on nickel foam was found to possess a maximum specific capacitance of 1117.0 Fg-1, a maximum power density of 20.48x103 WKg-1 and a maximum specific energy of 119.0 WhKg-1. The NiTAPc-NiOE-S film on nickel foam gave a maximum specific capacitance of 1279.0 Fg-1, a maximum power density of 26.96x103 WKg-1 and a maximum specific energy of 114.0 WhKg-1. Finally, the NiO mixed with an oxidant (NiOS-ox) film on nickel foam gave a maximum specific capacitance of 1403.0 Fg-1, power density of 14.44x103 WKg-1 and a maximum specific energy of 147.0 WhKg<sdup>-1. In addition, the electrodes were found to be very stable even after repetitive cycling. These electrodes have clearly proved that they may be suitable for use as potential supercapacitors. Further research is necessary to fully explore their supercapacitive behaviour in single cell (2-electrode)systems. Copyright / Dissertation (MSc)--University of Pretoria, 2012. / Chemistry / unrestricted