Summary: Laser‐induced fluorescence spectroscopy of the optical probe Nile Blue A in polymer clay nanocomposites is described. Concentration quenching of the fluorescence dominates the probe behavior until the clay platelets are physically separated by polymer intercalation. Further separation into an exfoliated structure results in an intense increase in probe fluorescence. Preliminary results indicate the ability to discriminate between intercalated and exfoliated structures in nanocomposites formed by melt processing.
