Four fibers from banana-trees (leaf, trunk) and coconut-tree (husk, fabric) were examined before their incorporation in cementitious matrices, in order to prepare insulating material for construction. Their botanical compositions have been determined following a method described previously. Thermal degradation of these fibers were studied between 200 and 700 °C under nitrogen gas flow. Temperature of pyrolysis was the experimental parameter investigated. The solid residues obtained were analyzed by classical elemental analysis, Fourier Transform Infra Red (FTIR) spectroscopy and were observed by Scanning Electron Microscopy (SEM). This study has shown (1) the relation between botanical, chemical composition with both localization of fibers in the tree and type of tree; (2) the rapid and preferential decomposition of banana fibers with increasing temperature of pyrolysis and (3) the rough samples are made of hollow fibers.