Evolution of graphite during low-energy ball milling.

To study the microstructural evolution of graphite and its allotropes under milling, graphite powder was processed using horizontal stainless-steel ball mills. A Ball-to-Powder Volume Ratio (BPVR) of 90 was maintained. Milling durations of 8, 16, 32, and 64 hours were investigated.
This dataset comprises raw laser diffraction particle size analysis results. For the analysis, samples were dispersed in a 0.2% sodium hexametaphosphate solution (pH 10) and subjected to 5 minutes of ultrasonic bath treatment to ensure complete particle deagglomeration. The data reveal the dominant stages of graphite exfoliation and fracture, as well as the formation of micrometric aggregates after 64 hours.
Additionally, X-ray diffraction (XRD) data are included. Measurements were performed using an Inel EQUINOX 2000 X-ray diffractometer configured with: A curved position-sensitive detector, CoKα₁ radiation (λ = 1.78901 Å), and a germanium monochromator. The acquired data were post-processed to convert results to CuKα₁ radiation (λ = 1.5406 Å) for consistency with standard references. 2θ peak positions were calibrated using a high-purity graphite standard (99.99%, Aldrich). Thanks to this analysis, it was possible to detect changes in the intensity of the main peak, shifts in the 2θ peaks, and their broadening. From these results, the variation in the lattice parameters "a" and "c" was calculated, which proved crucial for understanding the microstructural changes caused by lattice expansión.