Cellulose fibrils of microscale and nanoscale sizes have great strength and hence furnish the possibility of reinforcing polymers. Fibrils can be isolated from natural cellulose fibers by chemical or mechanical methods. However, the existing procedures either produce low yields or severely degrade the cellulose and, moreover, are not environment friendly or energy efficient. The purpose of this study was to develop a novel process that uses high-intensity ultrasonication (HIUS) to isolate fibrils from several cellulose resources. Six factors that may affect the efficiency of fibrillation, including power, temperature, time, concentration, size, and distance, have been considered and discussed. HIUS treatment can produce very strong mechanical oscillating power; therefore, the separation of cellulose fibrils from its biomass is possible by the action of hydrodynamic forces of the ultrasound. Water-retention value and volume change were used to evaluate and optimize the process parameters. The degree of fibrillation of the cellulose fibers treated by HIUS was significantly increased. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 113: 1270-1275, 2009