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In the present work, the facile thermal decomposition of raw coconut shells was carried out for the exploitation of the role of inert gas in the carbonization process and its role in determining the morphology, crystallographic parameters, and surface area of biochar before activation. The comparative investigation of mesoporous carbonized products synthesized with the muffle and tube furnace was carried out at a similar temperature and an assessment was made with a commercial carbon. The focus of the work was aimed at the interpretation of surface morphology, elemental identification, phase composition, interplanar spacing, full-width half maximum, crystallite size, lateral size, number of layers, dislocation density, microstrain, packing density, crystallinity index, and the specific surface area of the product obtained from two different approaches. It was revealed that the carbonized coconut shell chars obtained from the tube furnace have better characteristics to be activated further for carbon black synthesis. So, the flow of inert gas in a tube furnace is demonstrated to have a key role in improving the attributes of coconut shell chars.