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Diamond, renowned for its exceptional semiconducting properties, stands out as a promising material for high-performance power electronics, optics, quantum, and biosensing technologies. This study methodically investigates the optimization of polycrystalline diamond (PCD) substrate surfaces through Inductively Coupled Plasma Reactive Ion Etching (ICP-RIE). Various parameters, including gaseous species, flow rate, coil power, and bias power were tuned to understand their impact on surface morphology and chemistry. A thorough characterization, encompassing chemical, spectroscopic, and microscopic methods, shed light on the effects of different ICP-RIE conditions on surface properties. CF 4 /O 2 plasma emerged as a viable treatment for achieving smooth PCD surfaces with minimal etch pit formation. Most notably, surface fluorination, a critical aspect of increasing chemical and thermal stability, was successfully accomplished using CF 4 , SF 6 , and other F-containing plasmas. The fluorine concentration and surface chemistry variations were studied, with high resolution X-ray Photoelectron Spectroscopy unveiling differences amongst the sp2 C phase, sp3 C phase, C–O, C O, and C–F bonds. Time-of-flight secondary Ion Mass Spectrometry (ToF-SIMS) and depth-profile analysis unveiled a consistent surface fluorination pattern with CF 4 /O 2 treatment. Furthermore, contact angle measurements showcased heightened hydrophobicity. This study provides valuable insights into precise diamond surface engineering, important for the development of future diamond-based semiconductor technologies. [Display omitted] [ABSTRACT FROM AUTHOR]