Preparation of nanoscale cellulose materials with different morphologies by mechanical treatments and their characterization

Rod-like cellulose nanowhiskers and spherical cellulose nanoparticles were prepared from wood-pulp-derived cellulose powder by mechanical refining processes such as high-pressure homogenization (HPH) and ball-milling (BM). The nanowhiskers obtained by the HPH method were found to be 200–500 nm long and 11–16 nm wide. The diameters of the nanoparticles were in the range 40–200 nm, depending on the BM time, and were reduced to 25–50 nm after extra HPH. By adjusting the BM time, cellulose nanoparticles having different polymorphs with similar morphologies were prepared. The X-ray diffraction patterns revealed the recrystallization of cellulose I (1 h of BM time) or cellulose II (4–8 h of BM time) in ball-milled nanoparticles after water washing and solvent exchange treatments. The nanowhisker widths derived from the specific surface areas (SSA) by adsorption methods such as Congo red dye, nitrogen, and water vapor, sorptions were in agreement with those obtained from transmission electron microscopy and atomic force microscopy images. Similar SSA values were obtained for micro- and nano-scale cellulose materials using water vapor adsorption methods, and the SSAs of nanoparticles obtained by different adsorption methods are also discussed.