One application of octadecyltrichlorosilane (OTS) self-assembled monolayers (SAMs) is its use as thin film resists. In this work, we demonstrated that OTS SAMs can be reliable resists for organo-metallic chemical vapor deposition (OMCVD) grown gold nanoparticles (Au NPs). In optical sensing applications based on Au NPs, one candidate system consists of patterned OTS SAMs and precisely grown OMCVD Au NPs for achieving a high sensitivity. As an initial step, the OTS SAMs need to perfectly resist the OMCVD Au NP growth. Hence the optimized formation of the OTS SAMs affected by different assembly times and baking temperatures was studied by contact angle, ellipsometry, XPS, SEM, and atomic force microscopy (AFM). To demonstrate the ability of the OTS SAMs to resist OMCVD Au NP growth, the OMCVD process was carried out on two sets of samples: OTS SAMs fabricated under optimized conditions on one set and the other set without OTS SAMs. High-resolution XPS, RBS, SEM, and ultraviolet-visible (UV-Vis) spectroscopy were applied to study the growth of Au NPs on the samples with and without OTS SAM resists.