The mechanical performance of composite materials depends not only on the matrix and the reinforcing fiber, but also to a great extent on the fiber/matrix interfacial adhesion. The focus of this work was to study carbon fiber surface chemical and physical properties and their effects on fiber/matrix adhesion. Untreated, commercially surface treated and oxygen plasma treated PAN based carbon fibers were used for study. XPS was used to determine fiber surface chemistry. A two-liquid tensiometric method was conducted to determine fiber surface energy and its dispersion and polar components. SEM was used to examine the fiber surface topography. Commercial surface treatment increased the carbon fiber surface oxygen content and fiber surface energy primarily in the polar component. An even higher level of fiber surface oxygen functionality and polar surface energy were achieved by oxygen plasma treatment. Oxygen plasma treatment also resulted in etching and pitting of AU-4 carbon fiber surface. Carbon fibers with varying surface properties were incorporated into epoxy matrices. Single fiber fragmentation tests were carried out to evaluate the strength as well as the temperature dependence and humidity durability of interfacial adhesion. Commercially treated carbon fibers which having a higher surface oxygen content and higher surface energy clearly produced superior interfacial adhesion, relative to untreated fibers. An even greater level of adhesion was achieved with oxygen plasma treated fibers. Fiber surface roughness improved durability under elevated temperature and relative humidity conditions. The presence of sodium on the fiber surface dramatically decreased durability at high relative humidity. / Master of Science