Microscopic measurement of the degree of mixing for nanoparticles in polymer nanocomposites by TEM images

Abstract

For polymer nanocomposites, the small size of the fillers makes it difficult to analyze the degree of mixing quantitatively and often requires direct assessment via transmission electron microscopy (TEM). To date, qualitative comparisons and indirect measurements of the degree of mixing by measurement of certain properties are the most common methods. Better methods to quantitatively characterize the degree of mixing in nanocomposites would aid in studies investigating the effect of process conditions on the mixing behavior. Alumina/PET nanocomposites of identical composition, but with different degrees of mixing were prepared using a batch mixer. For evaluation of the degree of mixing with respect to both dispersion and distribution, three different techniques were applied and compared. TEM particle density was useful for dispersion, but did not adequately characterize distribution, while the Morisita's index gave poor results due to a wide range of effective particle sizes. Both methods ranked the samples differently compared to direct visual observation. In contrast, the skewness calculated by the quadrat method produced results consistent with visual rankings, and was found to be most effective in comparing and quantifying the degree of mixing. Although the quadrat method requires proper selection of quadrat size for a particular particle concentration, the skewness from the quadrat method was found to be most suitable as a standard index for the degree of mixing in nanocomposites. The usefulness of the quadrat method was verified using a second set of nanocomposites prepared by a twin screw extruder showing the potential for application of this technique for process development and quality control in commercial nanomanufacturing processes.