Master of Science / Department of Mechanical and Nuclear Engineering / Kevin B. Lease / This research was intended to measure the interfacial shear strength between fiber/ matrix systems and to investigate the relation between structure-mechanical properties and performance of fiber/matrix systems. This work conducted a systematic study on model fiber/matrix systems to enhance the fundamental understanding on how variation of polymeric compositions (and hence, different structures), different curing conditions, and fiber surface treatments influence the interactions between the fiber and matrix. In order to measure the interfacial shear strength of fiber/matrix systems, the microdroplet technique was used. In this technique a polymer droplet was deposited on a fiber in the liquid state. Once the droplet was cured a shear force was applied to the droplet in order to detach the droplet from the fiber. The amount of the force needed to de-bond the droplet was directly related to the strength of the bonds formed between the fiber and matrix during the curing process. In addition, the micro-droplet technique was used to evaluate effects of different crosslinker ratio of fiber/ matrix system and also to see if different curing conditions affect the interfacial shear strength of fiber/ matrix system. Surface treatment was also conducted to evaluate its effects on the interfacial shear strength of the fiber/ matrix system using microdroplet technique. The interfacial shear strength of fiber/ matrix system increased along with the increase of crosslinker ratio to a limiting value, and it decreased as long as the crosslinker ratio increased. Curing condition also caused the interfacial shear strength of fiber/ matrix system to increase when it was cured at higher temperature. Fiber surface treatment exhibited a significant effect to the interfacial shear strength as well as the fiber/ matrix contact angle measurement.