AbstractLightweight lignocellulosic composites are potentially contributing to sustainable development. However, lignocellulosic fillers are not always fully compatible with an inorganic matrix, which causes a variety of adverse outcomes such as the coherence and mechanical properties of composites. Therefore, experiments are made with natural fiber surface treatment. Experiments were conducted to further development of natural fibers - hemp shives of another application to lightweight composites. Untreated and chemically treated hemp shives surfaces by NaOH, Ca(OH)2 and EDTA were characterized by FTIR and TG. Changes in the FTIR spectra at 1730, 1625 and cm-1 indicated that hemicellulose and lignin from natural fiber surfaces were removed by alkaline treatment. Thermal stability of hemp shives was studied using thermal gravimetric and DSC method.