Hybrid carbon fiber reinforced composites are a new breed of materials that are currently being explored and characterized for next generation aerospace applications. Through the introduction of secondary reinforcements, such as alumina nanoparticles, hybrid properties including improved mechanical properties and stress sensing capabilities can be achieved. In order to maximize these properties, it is necessary to achieve a homogeneous dispersion of particulate filler. Utilizing the photoluminescent properties of alumina, it is possible to compare local levels of particle concentration through emission intensities as a way to determine the effectiveness of the tested manufacturing parameters in increasing material homogeneity. Parameters of these photoluminescence emissions have been established to be stress dependent, which allows for in situ residual stress measurements. It is shown here that the application of silane coupling agents as particle surface treatments improves particle dispersion when compared to untreated samples. Reactive silane coupling agent (RSCA) treatments were found to provide for greater dispersion improvements when compared to non-reactive silane coupling agents (NRSCA). Higher resolution investigations into these samples found that treatment with a reactive coupling agent altered the stress state of particles concentrated around the fiber from a tensile stress state to a compressive stress state. This is proposed to result from bonding of the reactive groups on the coupling agent to the organic groups on the carbon fibers which adjusts the stress state of the particle. Future mechanical tests will verify the effects of the particle surface functionalization treatments on mechanical properties of the composites.