Layered-silicate polymer characterization methods

Davis RD, Bur AJ, McBearty M et al. (2004) Dielectric spectroscopy during extrusion processing of polymer nanocomposites a high-throughput processing/characterization method to measure layered silicate content and exfoliation. Polymer 45 6487-6493... 

The dynamic mechanical thermal analyzer (DMTA) is an important tool for studying the structure-property relationships in polymer nanocomposites. DMTA essentially probes the relaxations in polymers, thereby providing a method to understand the mechanical behavior and the molecular structure of these materials under various conditions of stress and temperature. The dynamics of polymer chain relaxation or molecular mobility of polymer main chains and side chains is one of the factors that determine the viscoelastic properties of polymeric macromolecules. The temperature dependence of molecular mobility is characterized by different transitions in which a certain mode of chain motion occurs. A reduction of the tan 8 peak height, a shift of the peak position to higher temperatures, an extra hump or peak in the tan 8 curve above the glass transition temperature (Tg), and a relatively high value of the storage modulus often are reported in support of the dispersion process of the layered silicate. 

Generally, the inorganic materials used to prepare the nanocomposites mainly include layered silicate clay, layered compounds, metal powder, and a variety of inorganic oxides. In our research works, nanosized zinc oxide, iron oxide, silica, and YIG particles were synthesized and used to prepare a variety of polymer nanocomposites, giving the composite materials many new features. This chapter based on our research discusses the methods of preparation and characterization of the polymer-inorganic nanocomposites. 

Even after organic modification of the clays, polypropylene does not wet the surface of clays because it is nonpolar. It is necessary to blend in a functionalized polymer such as maleated polypropylene (PP-g-MA) that wets the modified clay surface more readily and is also miscible with the bulk polymer. Okada and coworkers were the first to produce polypropylene layered silicate nanocomposites by melt compounding the modified elay with PP-g-MA and PP. The progress made since then in preparing and characterizing polypropylene layered silicate nanocomposites is reviewed in this chapter. We discuss advances in formulations, preparation methods and characterization then proceed to effects of the dispersion state (intercalated vs. exfoliated) and of silicate loading on crystallinity, mechanical performance and other properties, and end with a summary of progress to date with these composites. All the results presented in this chapter refer to isotactic polypropylene nanocomposites with layered or smectite clays. 

---