Performance of carbon-carbon composites is known to be influenced by the fibre matrix interactions. The present investigation was undertaken to ascertain the development of microstructure in such composites when carbon fibres possessing different surface energies (T-300, HM-35, P120 and Dialed 1370) and pitch matrices with different characteristics (Coal tar pitch SP110℃ and mesophase pitch SP285℃) are used as precursor materials. These composites were subjected to two different heat treatment temperatures of 1000℃ and 2600℃. Quite interesting changes in the crystalline parameters as well as the matrix microstructure are observed and attempt has been made to correlate these observations with the fibre matrix interactions.