Experimental procedures to mitigate electron beam induced artifacts during in situ fluid imaging of nanomaterials

Abstract

Scanning transmission electron microscopy of various fluid and hydrated nanomaterial samples has revealed multiple imaging artifacts and electron beam-fluid interactions. These phenomena include growth of crystals on the fluid stage windows, repulsion of particles from the irradiated area, bubble formation, and the loss of atomic information during prolonged imaging of individual nanoparticles. Here we provide a comprehensive review of these fluid stage artifacts, and we present new experimental evidence that sheds light on their origins in terms of experimental apparatus issues and indirect electron beam sample interactions with the fluid layer. A key finding is that many artifacts are a result of indirect electron beam interactions, such as production of reactive radicals in the water by radiolysis, and the associated crystal growth. The results presented here will provide a methodology for minimizing fluid stage imaging artifacts and acquiring quantitative in situ observations of nanomaterial behavior in a liquid environment.