TSEM-based contour analysis as a tool for the quantification of the profile roughness of silica shells on polystyrene core particles

Abstract

Core-shell (CS) particles with a polymeric core and a silica shell play an important role in the materials and (bio)analytical sciences. Besides the establishment of reliable synthesis procedures, comprehensive particle characterization is essential for batch-to-batch reproducibility and objective performance assessment across architectures, protocols, and laboratories. Particle characterization with respect to size, size distribution, shell thickness and texture, surface area and roughness or materials composition is commonly conducted with different analytical methods, often on different samples. Our approach uses a dual-mode TSEM/SEM set-up with an EDX detector to obtain a complementary data set with sufficient statistical confidence of one and the same sample on a single instrument. Our protocol reveals information about size, size distribution and shell thickness of the various particles employed from overview images, while an increased field of view (FOV) and high-resolution EDX analysis yields detailed information on shell texture and elemental composition. An image analysis tool was developed to derive and quantify the profile roughness of CS particles from individual beads. Comparison with surface roughness data from AFM showed a similar trend in roughness across the series of particles. Reliable classification into smooth and rough is proposed and roughness changes within different particle batches were tracked systematically.