The agricultural wastes from harvesting corn, viz. corn husks and corn cobs were used as raw materials for the preparation of microcrystalline cellulose. From chemical composition analysis, holocellulose, -cellulose, hemicellulose, extractive and ash contents found in the corn husk were higher than those in the corn cob except for lignin. The study found that these corn residues could potentially be used for microcrystalline cellulose preparation. The properties of the microcrystalline cellulose obtained from these corn residues were examined in comparison with the commercial microcrystalline cellulose, Avicel PH101. Their crystal feature was in cellulose I form which showed the crystal reflections at 2s around 15 o, 17 o and 22o, being the same as that of Avicel PH101. Whilst their crystallinity was lower and the crystal size was smaller than Avicel PH101. The crystal size of the microcrystalline cellulose from the corn residues was around 3 nm whereas that of Avicel PH101 was about 4 nm. In addition, the thermal stability of the prepared microcrystalline cellulose was slightly lower than that of Avicel PH101. Corn husks provided more thermally stable microcrystalline cellulose than corn cobs.