An X-ray powder profile analysis in vanadium pentoxide powder milled in a high energy vibrational ball-mill for different lengths of time (0–250 h), is presented. The strain and size induced broadening of the Bragg reflection for two different crystallographic directions ([001] and [100]) was determined by Warren–Averbach analysis using a pattern-decomposition method assuming a Pseudo–Voigt function. The deformation process caused a decrease in the crystallite size and a saturation of crystallite size of ∼ 10 nm was reached after severe milling. The initial stages of milling indicated a propensity of size-broadening due to fracture of the powder particles caused by repeated ball-to-powder impact whereas with increasing milling time microstrain broadening was predominant. WA analysis indicated significant plastic strain along with spatial confinement of the internal strain fields in the crystallite interfaces. Significant strain anisotropy was noticed in the different crystallographic directions. A near-isotropy in the crystallite size value was noticed for materials milled for 200 h and beyond. The column-length distribution function obtained from the size Fourier coefficients progressively narrowed down with the milling time.

A comprehensive analysis of size and strain broadened profile shapes in X-ray diffraction line broadening analysis is presented. Both size and strain broadened profiles were assumed to be Voigtian and the derived microstructural parameters (size and strain) were found to be in close agreement with those calculated from model independent Warren–Averbach method. The method is applied to three different alumina samples viz. micron size 𝛼-alumina (𝛼-Al₂O₃) prepared by the combustion of aluminium nitrate and urea mixture, annealed samples and commercial 𝛼-Al₂O₃ sample. It is likely from the present analysis that a significant Gaussian size contribution is related to narrow size distribution observed from the analysis. It has been concluded that present Voigtian analysis is more reliable and may largely replace the earlier simplified integral breadth methods of analysis often used in line broadening analysis.