X-ray diffraction line profile analysis of nanocrystalline graphite

The structure evolution to nanocrystalline graphite produced by ball milling in n-dodecane has been studied by Fourier analysis of broadened X-ray diffraction line profiles according to double-Voigt method. The Fourier analysis gave size and strain distributions of the coherently diffracting domains (X-ray crystallite size) and root-mean-square-strain (rmss) and their average values. The precursor graphite was defined by average crystal sizes of about hundreds of nanometers, measured along the in-plane and out-of-plane directions, and low rmss value of 0.38 × 10⁻³. During milling, the average crystallite sizes of graphite decreased to about 6 and 43 nm along the out-of-plane and in-plane directions, respectively. Correspondingly, the rmss of milled graphite increased to 6.54 × 10⁻³. Analysis of the out-of-plane to in-plane crystallite size ratios showed that the crystallites became progressively thinner and flatter. A linear relationship between rmss and reciprocal crystallite size along the stacking axis revealed that size of disordered boundary regions gradually increased at the expense of ordered crystalline regions. A model describing crystalline–nanocrystalline transformation of graphite along different crystallographic axis was formulated and used to discuss the experimental data. It was concluded that a distortion-controlled process is responsible for the crystalline–nanocrystalline transformation of graphite milled in n-dodecane.