Abstract: This study compared the properties of nano structure extraction from walnut shell using mechanical and chemical methods. Walnut shell is an agro- waste with source of lignin and cellulose. Mechanical method including using ball mill with different time and in present of additive and without additives and for chemical method hydrolysis acid were used. This study highlights the particle size and morphology and efficiency these methods in nano structure extraction. The result showed mechanical method is unable to extract nanoparticle and just reshape the walnut shell. Milling time were also found important in morphology of fiber extracted. FE-SEM images represented that structure mean diameter of using ball mill was 1± 5 μm while hydrolysis acid method extract nano particle with mean diameter of 40± 20 nm.