This three part research project to study the details of chemical vapor deposition processes is supported in the Analytical and Surface Chemistry Program. It is carried out in the laboratory of Professor Nuzzo at the University of Illinois-Urbana Champaign. New methods are developed for the direct deposition of sub-micron structures, using a combination of sol-gel chemistry, patterned metallization, and patterned catalyzed polymerization. Molecular beam deposition coupled with surface spectroscopic characterization of adsorbed intermediates is used to characterize the details of the CVD growth process. Phase behavior in self assembled organic thin films forms the focus of the third part of this project. The results of this research are applicable to the developing technologies of nanoscale fabrication and electronic device preparation. Understanding the details of the synthesis and growth of thin films of electronically interesting materials is the focus of this research project. Self assembled organic overlayers, sol-gel chemistry, and detailed kinetic studies of chemical vapor deposition combine to provide the knowledge base essential to apply new thin layer growth methods to the preparation of material microstructures. Electronic device processing technologies are impacted by this work.