The X-ray Debye temperatures, q M , of spinel ferrite composition Ni 0.5 Zn 0.5 Fe 2 O 4, mechanically milled upto 9 hrs, were determined from integrated intensities of selected Bragg reflections. The q M was found to increase with milling time. The results are explained in the light of milling induced grain orientation and surface effect. The values of q M were found to be lower as compared to the Debye temperatures obtained from infrared spectral data analysis. The difference can be explained on the basis of increase in an excess free volume in the form of vacancies and vacancy clusters associated with grain boundaries.