Forming a complete understanding of the physical mechanisms that govern friction on the nanometer and atomic scales is an ongoing endeavor for scientists from various disciplines. While atomic force microscopy (AFM) has proven to be invaluable for the detailed study of nano-scale frictional properties associated with various surfaces, issues related to the precise characterization of the contact formed by the probe tip and the sample surface remain largely unsolved. In recent years, an alternative approach to nanotribology experiments has involved the lateral manipulation of well-characterized nanoparticles on sample surfaces via AFM and the measurement of associated frictional forces. In line with this idea, ambient-condition structural/nanotribological characterization and nano-manipulation experiments involving gold nanoparticles (AuNP) thermally deposited on highly oriented pyrolytic graphite (HOPG) are presented in this thesis. The effect of deposition amount on thin film morphology is discussed and post- deposition annealing procedure in terms of different annealing temperatures and times are tackled in order to characterize AuNP formation on HOPG. The morphology and distribution of AuNPs on HOPG are studied via scanning electron microscopy (SEM) while the confirmation of AuNP crystallinity via transmission electron microscopy (TEM) is also described. Topographical characterization of the resulting AuNP/HOPG material system performed via contact-mode AFM is demonstrated. Lateral force measurements are also presented, in terms of the dependence of friction force on normal load as well as the dependence of friction force increase at AuNP edges on normal load and particle height. Subsequent to comprehensive structural and frictional characterization, the results of nano-manipulation experiments performed on AuNPs on the HOPG substrate are reported and it is observed that AuNPs experience remarkably low frictional forces during sliding. A detailed study of friction with respect to contact area firmly confirms the occurrence of structurally lubric sliding under ambient conditions for this material system. This result constitutes the first observation of structurally lubric sliding under ambient conditions between different materials in the scientific literature.