New insights into subsurface imaging of carbon nanotubes in polymer composites via scanning electron microscopy.

Despite many studies of subsurface imaging of carbon nanotube (CNT)-polymer composites via scanning electron microscopy (SEM), significant controversy exists concerning the imaging depth and contrast mechanisms. We studied CNT-polyimide composites and, by three-dimensional reconstructions of captured stereo-pair images, determined that the maximum SEM imaging depth was typically hundreds of nanometers. The contrast mechanisms were investigated over a broad range of beam accelerating voltages from 0.3 to 30 kV, and ascribed to modulation by embedded CNTs of the effective secondary electron (SE) emission yield at the polymer surface. This modulation of the SE yield is due to non-uniform surface potential distribution resulting from current flows due to leakage and electron beam induced current. The importance of an external electric field on SEM subsurface imaging was also demonstrated. The insights gained from this study can be generally applied to SEM nondestructive subsurface imaging of conducting nanostructures embedded in dielectric matrices such as graphene-polymer composites, silicon-based single electron transistors, high resolution SEM overlay metrology or e-beam lithography, and have significant implications in nanotechnology.

A quantitative assessment of carbon nanotube dispersion in polymer matrices.

Quantifying the nature and extent of the dispersion of nanomaterials in polymer matrices is the important first step in understanding the relationship between the nanoscale structure and the bulk scale functional performance of nanocomposites. We present here a methodology for using scanning electron microscope images of nanocomposites taken under high accelerating voltages to quantify four parameters that relate to the dispersion of the nanomaterial. This image analysis methodology is general and applicable to images from other microscopes as well. The analysis performed here was done on representative local areas of six samples to determine the effects of processing conditions, matrix chemistry, and carbon nanotube composition on the level of dispersion. Future work will involve expanding this analysis to rapidly cover larger areas and reducing the data in a manner that is similar to the approach of small angle scattering studies.