Precious metals are choice materials for a myriad of applications due their high electrical conductivity, resistance to corrosion, and ligand binding specificity. Indispensable in modern electronics fabrication, precious metals also enjoy widespread use as catalysts, support substrates, and sensor elements. Recent progress towards metallization on diminishing size regimes has imposed increasingly stringent demands upon thin film preparation methodologies. Metallization techniques employed in ultra large scale integration (ULSI) device fabrication, nanoelectromechanical systems (NEMS), and arrayed nanosensors will require unparalleled control of surface morphology, deposition rate, and substrate adhesion without sacrificing throughput or cost effectiveness. Furthermore, precious metal films of this type are essential for fundamental investigations aimed at elucidating the intricate nature of interfacial topics ranging from self-assembled monolayers (SAMs) to heterogeneous catalysis. In contrast to complex and expensive vacuum methods of metallization, research in our laboratory has focused on the preparation of precious metal thin films on semiconductor substrates via electroless deposition. Thin and thick films of gold, platinum, and palladium nanoparticles have been prepared as a result of the immersion of germanium and gallium arsenide substrates into dilute, aqueous solutions of tetrachloraurate (III), tetrachloroplatinate (II), and tetrachloropalladate (II), respectively. This methodology yields nanostructured precious metal films with control over surface morphology and deposition rate. Moreover, metal films prepared in this manner exhibit excellent adhesion to the underlying semiconductor substrate. The resultant films were characterized utilizing scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and scanning probe microscopy (SPM). This method provides for the facile interfacing of metal nanostructures with group (IV) and III-IV compound semiconductor surfaces.