Sustainable Synthesis of High-Surface-Area Graphite Oxide via Dry Ball Milling

A sustainable route to produce graphite oxide (GO) is presented using dry ball milling. The production method was based on pristine graphite flakes in a planetary ball mill. The prepared GO was characterized using UV–vis spectroscopy, BET surface area analysis, thermal analysis, SEM-EDX, TEM, XPS, elemental analysis, and Raman spectroscopy. The degree of graphite oxidation was controllable by the milling time and milling material, and the carbon-based yields ranged from 86 to 97%. The maximum oxygen/carbon ratios of the produced GOs were 0.16 and 0.15 after 24 h of ball milling with steel and zirconia balls, respectively. The BET surface area increased with increasing milling time from 1 m2 g–1 for pristine graphite up to 730 m2 g–1 for the ball-milled samples. Furthermore, the intensity ratios of the D and G bands (ID/IG) from the Raman spectra were 0.84 and 0.77 for GO produced with the steel and zirconia balls, respectively. The in-plane sp2 crystallite sizes (La) of graphite (168 nm) decreased to 20 (steel balls) and 22 nm (zirconia balls). Additionally, the produced GO was tested as an adsorbent for methylene blue dye removal.