Nano‐Structural Observation of in situ Silica in Natural Rubber Matrix by Three Dimensional Transmission Electron Microscopy

Abstract

Summary: Three dimensional (3D) nanostructures of particulate silicas in natural rubber (NR) were observed for the first time by use of 3D transmission electron microscopy (3D‐TEM) combined with electron tomography. The method enabled us to visualize and evaluate structural characteristics in 3D space, such as the size and the volume of in situ silica generated in the NR matrix by the sol‐gel reaction of tetraethoxysilane, at nanometer scale resolution.The reconstructed mass density view of the silica in an in situ silica‐filled natural rubber vulcanizate, as determined by 3D‐TEM.imageThe reconstructed mass density view of the silica in an in situ silica‐filled natural rubber vulcanizate, as determined by 3D‐TEM.

Quantitative mapping of surface elastic moduli in silica-reinforced rubbers and rubber blends across the length scales by AFM

“…Atomic force microscopy (AFM) has been widely used to study the structure and morphology of rubbers and polymers with nanoscale resolution [4][5][6]. It has also been successfully applied to provide insights into surface morphology of composites.…”

“…Tapping mode AFM (TMAFM) is commonly used for probing the topography and composition of rubber surfaces [4]. However, quantitative mechanical mapping is not possible with conventional phase imaging as the phase signal is related to the energy dissipation of the tapping tip which cannot be directly translated into the variation of mechanical moduli [11,12].…”

Microstructural Characterization of Hard Ceramics

“…14 shows silica particles within a polymer/ceramics composite. (Ikeda et al, 2004) While this technique has not been widely applied to ceramics and hard materials, it will clearly be useful for understanding the structure of composites.…”

Machine learning as a tool for classifying electron tomographic reconstructions

“…Tomography is carried out when three-dimensional information is explicitly necessary-for instance, when visualising the distribution of nanoparticles inside a polymer matrix [6,7]. Quantitative 3D information (such as nearest-neighbour distances) can also be extracted from tomograms-something impossible with a twodimensional projection of an irregular structure such as a zeolite or mesoporous catalyst [8][9][10].…”