The key for a successful gate-first process is when subsequent processing steps cannot degrade the semiconductor, the dielectric, or the oxidesemiconductor interfaces. For silicon, the only commercial ALD high-k fabrication process, which avoids processing induced damage, is a replacement gate process (a type of gate-last process). While preparing silicon for gate-last processing is straightforward, the key to a gate-last process for III -V semiconductors is the order and cleanliness of the III- V channel prior to dielectric deposition. Aggressive oxide thickness reduction (equivalent oxide thickness, or EOT, scaling) is needed to fabricate small gate length devices with small subthreshold swings. Furthermore, aggressive EOT scaling requires a very high uniform ALD nucleation density, with no pinholes due to surface contaminants. The key barrier to solving a very practical problem is a surface chemistry challenge: develop a chemical process which removes nearly all air induced defects and contaminants and leaves the III-V surface flat and electrically active for high nucleation density ALD gate oxide deposition, which unpins the Fermi level. The following study uses scanning tunneling microscopy (STM) and scanning tunneling spectroscopy (STS) to observe the removal of the oxide layer and restoration of the clean InGaAs surface reconstruction with atomic hydrogen cleaning, allowing for a gate-last or replacement-gate process. Along with surface cleaning STM and STS was used to characterize the initial passivation of InGaAs surfaces via ALD of trimethyl aluminum (TMA). The substrate temperature and initial surface reconstruction was critical to forming an unpinned passivation layer with a high nucleation density. A method was developed to use Kelvin probe force microscopy (KPFM) as a tool for insightful feedback on the electrostatics of scaled MOSFET devices. KPFM is a unique technique for providing two- dimensional potential profiles inside a working device. A procedure is described to obtain high-resolution KPFM results on ultra-high vacuum (UHV) cleaved III-V MOSCAPs