Nanostructured materials have emerged as a key research field in order to confer materials with unique or enhanced properties. The performance of nanocomposites depends on a number of parameters, but the suitable dispersion of nanoparticles remains the key in order to obtain the full nanocomposites’ potential in terms of, e.g., flame retardance, mechanical, barrier, thermal properties, etc. Likewise, the performance of nanocoatings to obtain, for example, tailored surface affinity with selected liquids (e.g., for self-cleaning ability or anti-fog properties), protective effects against flame propagation, ultra violet (UV) radiation or gas permeation, is highly dependent on the nanocoating’s thickness and homogeneity. In terms of recent advances in the monitoring of nanocomposites and nanocoatings, this review discusses commonly-used offline characterization approaches, as well as promising inline systems. All in all, having good control over both the dispersion and thickness of these materials would help with reaching optimal and consistent properties to allow nanocomposites to extend their use.