We propose a precise diamond micromachining method based on ultraviolet femtosecond laser direct writing and a mixed acid heating chemical treatment. The chemical composition of the attached clusters generated during laser ablation and their effects on morphologies were investigated in experiments. The averaged roughness of pristine and processed regions reduced to 0.64 nm and 9.4 nm from 20.5 nm and 37.4 nm, respectively. With this method, spiral zone plates (SZPs) were inscribed on a high-pressure high-temperature diamond surface as micro-optical vortex generators. The optical performances of the diamond SZPs were characterized in both experiments and simulations, which were very consistent with each other. This chemical auxiliary processing method will contribute greatly to the wide application of integration and miniaturization of diamond surface optical components.