With rapid development of the global economy, increasing environmental pollution and the depletion of fossil fuels, there is a vital need for clean, sustainable and efficient sources of energy as well as new technologies allied with energy conversion and storage (1). Among many application fields, some of the most practical and efficient technologies for electrochemical energy conversion and storage are fuel cells, batteries and electrochemical supercapacitors. In recent years, these devices have attracted significant attention, each with recognized advantages. Driven by this need and the promise of the technology, significant progress in practical and theoretical research and development of these devices has taken place. One of the challenges of developing these electrochemical energy conversion and storage technologies is the use of low cost and readily available materials that possess complex requirements of different applications. To overcome obstacles of high costs of raw materials and avoid usage of depleting sources, bio-based carbon materials are believed to lead the next generation of many industries including aerospace, sports equipment and electrochemical devices due to their abundance, high chemical stability, electrical conductivity, low cost and non-toxicity, high specific surface area and wide operating temperature range (2). The feasibility of the carbon precursors in different electrochemical devices for practical applications including hybrid power sources in electrical vehicles, burst-power generation in electronic devices, back-up power sources, portable and stationary equipment has been demonstrated. Cellulosic fibers in nano and micro scale, the green and most abundant material, have eco-friendly attributes that are economically and technically feasible to replace man-made fibers (3). Carbonization of cellulose yields carbons, including charcoal, activated carbon and graphite fibers. The process comprises of introducing the fibers in an inert atmosphere, preheating and drying the fibers, treating the dried fibers up to a certain temperature at which they carbonize by evolution of a purging gas and finally cooling the carbonized residues (4). The produced carbon materials have been investigated as a potential material in different electrochemical devices and have proved to have prospect as electrode materials for supercapacitors, catalyst supports in fuel cells and membrane separators in lithium-ion batteries. In this project, bio-based cellulosic starting materials have been investigated as a candidate for supercapacitor electrode materials. The produced activated carbon materials upon carbonization of the cellulose fibers have been functionalized and characterized by different techniques to study the effect of the morphology and surface area of the carbonaceous residues on their performance in the electrochemical device. This work has been coupled with a range of electrochemical tests in two and three-electrode systems including cyclic voltammetry, electrochemical impedance spectroscopy and charge-discharge loop tests. The work highlights the importance of relating the different characterization techniques of the raw and produced materials and the effect of each on the performance of the activated carbons as electrode materials in supercapacitors.