Friction and adhesion tests were conducted to investigate tribological characteristics of materials for MEMS/NEMS using atomic force microscope (AFM). AFM Si tips were chemically modified with a self-assembled monolayer (SAM) derived from trichlorosilane like octadecyltrichlorosilane (OTS) and (1H, 1H, 2H, 2H-perfluorooctyl) trichlorosilane (FOTS), and various materials, such as Si, Al, Au, Cu, Ti and PMMA films, were prepared for the tests. SAMs were coated on Si wafer by dipping method prior to AFM tip to determine a proper dipping time. The proper dipping time was determined from the measurements of contact angle, surface energy and thickness of the SAMs. AFM tips were then coated with SAMs by using the same coating condition. Friction and adhesion forces between the AFM Si tip modified with SAM and MEMS/NEMS materials were measured. These forces were compared to those when AFM tip was uncoated. According to the results, after coating OTS and FOTS, the friction and adhesion forces on all materials used in the tests decreased; however, the effect of SAM on the reduction of friction and adhesion forces could be changed according to counterpart materials. OTS was the most effective to reduce the friction and adhesion forces when counterpart material was Cu film. In case of FOTS, friction and adhesion forces decreased the most effectively on Au films.