In Situ Deformation and Breakage of Silica Particles Inside a SEM

Mechanical properties and particle breakage behavior in the submicron size range are of fundamental importance for many particle related processes and applications. Although many (in situ) studies have been dedicated to materials’ size dependent mechanical characterization, particles as free standing structures have been omitted widely. An important, yet open question is the structure property relationship at small scales. Within this account, the application of a custom built manipulator for particle compression inside a scanning electron microscope (SEM) is presented: Stöber-Fink-Bohn (SFB) particles with mean diameters of 500 nm and 1000 nm are subjected to heat treatments and their mechanical properties are directly correlated to the internal structure. The as-synthesized SFB particles exhibit a complex and size dependent internal structure. Mechanical properties undermatching the values of fused silica are found and only plastic cracking at large strains is observed: cracks are formed at the surface and propagate in radial direction towards the particle center. Heat treatment leads to densification. The degree of changes is controlled by temperature and treatment time. Starting from initially low values, Young's modulus and hardness are increasing with treatment temperature. Properties of fused silica are approached or even exceeded after a treatment at 1000 °C. A significant level of plasticity and high sustained deformations are still found. Whereas small particle show ductile cracking, the heat treated micron sized particles show a brittle behavior. A brittle to ductile transition in the size range of 500 nm to 1000 nm is thus identified.