Cryo-analytical STEM of frozen, aqueous dispersions of nanoparticles

In situ characterisation of nanoparticle dispersion and surface coatings is required to further our understanding of the behaviour of nanoparticles in aqueous suspension. Using cryogenic transmission electron microscopy (cryo-TEM) it is possible to analyse a nanoparticle suspension in the frozen, hydrated state; however, this analysis is often limited to imaging alone. This work demonstrates the first use of analytical scanning TEM (STEM) in the examination of nanoparticles captured in a layer of vitreous ice. Imaging and analysis of frozen hydrated suspensions by both STEM energy dispersive X-ray (EDX) spectroscopy and electron energy loss spectroscopy (EELS) under cryogenic conditions demonstrates the identification and separation of CeO₂ , Fe₂ O₃ , ZnO and Ag nanoparticles in suspension. Damage caused by the electron beam was shown to occur at far higher electron fluences in STEM (<2000 e − /Å 2 ) compared to CTEM (