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Recent process and reliability issues in state-of-the-art copper on-chip interconnects systems have spurred an interest in finding new materials to augment, or in some cases, replace copper as an interconnect material for future technology nodes. Carbon nanofiber (CNF) is one such candidate material for on-chip interconnect integration. Three main aspects of our research are discussed, controllable CNF synthesis, CNF-metal interface characterization, and development of new test structures and methods. We present fundamental electrical measurements of vertically-aligned CNF arrays for use as vias and on-chip interconnect wiring. CNF arrays are synthesized using plasma enhanced chemical vapor deposition (PECVD). The synthesis process is discussed as it relates to device architecture and electrical characterization.