Chemical mechanical polishing is used to polish large area free-standing CVD diamond films with diameters of 66 mm. The influence of polishing plates (iron plate, asphalt plate and soft cushion) and oxidizing agents (K
2S
2O
8 and K
2FeO
4) on polishing results are investigated. Profilometer (tip radius 5 μm), optical microscope and Raman spectroscopy are used to evaluate the polishing effects of the CVD diamond films. Results show that the material removal rate of iron plate is the highest, while the surface polished by soft cushion is the most uniform with roughness of 2 nm. It is also found that the most effective oxidizing agent is K
2FeO
4. In conclusion, the optimum polishing conditions are soft cushion and K
2FeO
4.