We have developed an improved vapor-phase deposition method and an apparatus for the wafer-scale coating of monolayer films typically used in anti-stiction applications. The method consists of a surface preparation step using an O-2 plasma followed by the tunable deposition of a monolayer film in the same reactor. This process has been successfully applied to MEMS test structures and has demonstrated superior anti-stiction performance. The deposition process allows tuning of the film properties by the precise metering of the precursor and a catalyst as part of the process control scheme. The anti-stiction monolayer film deposited from dimethyldichlorosilane (DDMS), tridecafluoro-1,1,2,2-tetrahydrooctyltrichlorosilane (FOTS), and heptadecafluoro-1.1,2,2-tetrahydrodecyltrichlorosilane (FDTS) were characterized using contact angle analysis, atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS). The coefficient of static friction was measured using a sidewall test device and the work of adhesion using a cantilever beam array. The results showed that excellent quality, uniformity, and reproducibility could be achieved across a whole wafer using this method and equipment.