Enzymatic fermentation of lignocellulose biomass has shown great potential of hydrogen production but the yield is limited due to the complex structure of cellulose and hemi-celluloses. For the bio-hydrogen production from biomass, the pretreatment of biomass plays a vital role to increase the hydrogen yield. In the present work highly efficient pretreatment by mall milling of corncob biomass has been employed to optimize the thermo-physical and optical properties of corncob powder by employing state of art techniques including scanning electron microscope, x-rays diffractometer, thermogravimetric analysis, and Fourier transform infrared spectroscopy. The morphological observations from microscopic images are consisted with x-ray diffraction results where the broadening in the peaks suggests the smaller particle size (large surface area) after pretreatment. From the decomposition kinetic parameters and apparent activation energy calculation by FWO and DAEM methods, the sample S2 with lowest activation energy, can have highest hydrogen production yield which is consistent with our previous findings. The broadening in the absorption peak near 1046 cm(-1) suggests that C-O stretching vibration (cellulose and hemicellulose)mode has been changed after different ball milling. By tailoring their activation energies through ball milling one can optimize thermo-dynamic characteristics for enhancement of biohydrogen production. (C) 2019 Elsevier Ltd. All rights reserved.