Analysis of small-angle scattering of suspensions of organically modified montmorillonite: Implications to phase behavior of polymer nanocomposites

A generalized model for scattering from a collection of independent (isolated) stacks of layers enabled predictions of and parameterized fits to small-angle X-ray scattering from layered silicate dispersions. From this fundamental development, example investigations that use small-angle scattering to examine the structure of organically modified montmorillonite dispersions in toluene and toluene–acetone blends provided detailed information on the distribution of the stacks (relative concentrations, K and fraction of individual layers, χ) and characteristics of the intercalated crystallite (mean number of layers per stack, 〈N〉; layer repeat distance, D; and fractional stack disorder, δ). The analysis initially supported correlations with discotic phase behavior, which provides concise definitions for various morphologies (exfoliated, intercalated, and mixed). Finally, examination of the deviations between the scattering model and the experiment provided insights for improved experimental technique, more complete utilization of the scattering data, a sound basis for real-time observations, insight into inconsistencies between scattering and microscopy, and minimization of incorrect or overinterpretation of data. © 2003 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 41: 3214–3236, 2003