Fiber-optic evanescent wave FTIR spectroscopy was combined with phase imaging AFM to examine two thermosetting polymer matrix composite systems. The epoxy/NMA system data from the fiber-optic, evanescent wave FTIR analysis showed incomplete curing (similar to75% complete) in the region near the fiber, but essentially complete (similar to95% complete) curing in the bulk. Conversely, the unsaturated polyester system exhibited essentially complete curing (similar to95% complete) both near the fiber and in the bulk material. For the same samples, phase imaging AFM indicated that the epoxy/NMA system had an similar to2.5 micron thick interphase, while the unsaturated polyester system showed no interphase between the fiber and the matrix. Therefore, the presence of the interphase in the epoxy/NMA system can be attributed to the incomplete curing next to the fiber. In addition, the systems chosen allowed the reactivity of adsorbed gamma-APS coupling agent to be assessed simultaneously with polymer curing. For the epoxy/NMA system, the amine band decreased about 54% during curing. For the polyester system, the amine band decreased 43% during curing.