Petroleum coke (petcoke) is a waste material from oil industries and can be applied as an inexpensive material for catalysts. Given the number of components in petcoke, applications for products derived from petcoke are generally limited to “dirty” streams such as upgrading of bitumen. The presence of heavy molecules in bitumen leads to high oil viscosity and transport limitations, and requires the conversion of those molecules, using a catalyst, improves the oil quality. Petcoke requires physicochemical modifications to be used as a catalyst, and high-energy ball milling is one technique for doing these changes mechanically. Ball milling has been applied to modify many carbon materials including biochar, graphene, carbon nanotubes, while its utilisation for functionalising petcoke is an opportunity to be explored. Traditional catalyst preparation methods often include impregnation with an aqueous solution, but as petcoke is hydrophobic, these methods are ineffective. In this project, the ball milling effects on the modification of petcoke were investigated and the materials characterized with a variety of techniques including Scanning Electron Microscopy, Fourier-transform Infrared Spectroscopy and N2 adsorption. Wet ball milling, with heptane or water in different amounts, and dry ball milling were performed with petcoke under the conditions: particle size 45-90 μm, 5 min to 9 h, 300 rpm, zirconia balls Φ5 mm, 1:20 powder to ball mass ratio. The wet procedure resulted in smaller particles (~3 μm versus ~6 μm) and a narrower size distribution than dry ball milling. Heptane or water may provide a better dispersion of the particles and avoid agglomeration while milling. The surface areas were higher when heptane was used in wet ball milling with an increase from ~0.2 m2/g for raw petcoke to 70 m2/g, after 9 h. The surface groups quantified by titration did not show significant acidity increase compared to raw petcoke (0.4 mmol/g) after milling. Petcoke was also ball milled with metal precursors to determine if nickel and molybdenum metals could be loaded on its surface directly. For the chosen conditions, however, metal dispersion was close to zero. More work is required to determine the conditions to prepare catalysts directly with ball milling.