Abstract
Studying liquid phase nanoscale dynamic processes of oxide nanoparticles is of considerable interest to a wide variety of fields. Recently developed liquid phase transmission electron microscopy (LP-TEM) is a promising technique, but destabilization of oxides by solid-liquid-electron interactions remains an important challenge. In this work we present a methodology to assess LP-TEM oxide stability in an aqueous phase, by subjecting several oxides of technological importance to a controlled electron dose in water. We show a correlation based on the Gibbs free energy of oxide hydration that can be used to assess the stability of oxides and demonstrate the existence of several remarkably stable oxides, with no observable structural changes after one hour of electron beam irradiation in LP-TEM. Rationalizing such destabilization phenomena combined with the identification of stable oxides allows for designing LP-TEM experiments free from adverse beam effects and thus investigations of numerous relevant nanoscale processes in water.
Highlights
Since time immemorial, oxides have been incredibly important materials in a wide variety of applications, from ancient pottery to modern superconductors
Before introducing them to liquid phase transmission electron microscopy and studying their stability and behavior, we performed a study of their bulk physicochemical properties
In view of the growing popularity of liquid phase transmission electron microscopy (LP-Transmission electron microscopy (TEM)) in academic and industrial research, in particular for studying metal systems in an aqueous environment, this study represents a critical step towards deepening our understanding of the diverse behaviors of metal oxides in LP-TEM
Summary
Oxides have been incredibly important materials in a wide variety of applications, from ancient pottery to modern superconductors. Industrial applications include heterogeneous catalysts, where nanoparticle oxides are often used as support or catalyst [1,2,3,4], structural and refractory ceramics such as bricks or concrete [5], or semiconductors [6, 7], adsorbents [8], superconductors [9], and protective coatings [10]. Properties and performance of oxides in many of these applications are dictated by nanometer scale structural features. Influence of the catalyst nanoparticle size [11], morphology [12] and nanoparticlesupport interactions [4, 13] on catalyst activity, selectivity and stability, the morphology and nature of nanoscale defects on corrosion [14, 15], or the presence of nanometer-sized defects in oxide boundary layers on semiconductor performance [16] are all important examples of how nanoscale features can influence overall oxide behavior. The development of technologies for in situ heating [20], gas [21,22,23,24,25] and in particular liquid [26,27,28] TEM measurements has expanded the possibilities for characterization of nanomaterials and nanoscale processes dramatically
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