Journal Highlights
Techniques and Instrumentation Development
Site-Specifi c Preparation of Intact Solid-Liquid Interfaces by Label-Free In Situ Localization and Cryo-Focused Ion Beam Liſt -Out by MJ Zachman, E Asenath-Smith, LA Estroff , and LF Kourkoutis. Microsc Microanal 22(6) (2016) 1338–49
Interfaces between solids and liquids play a key role in a range of processes. For example, in hydrogel-based crystal growth the crystal- hydrogel interface dictates the fi nal crystal morphology and properties, and in batteries the electrode-electrolyte interfaces play a pivotal role in device performance and safety. High-resolution characterization of such complex interfaces with the liquids intact is, however, oſt en lacking. In this paper, we describe a method for preparing liquid/solid interfaces for high-resolution analytical cryo-scanning transmission electron microscopy (cryo-STEM). Access to buried structures inside cryo-immobilized specimens is achieved by cryo-focused ion beam (cryo-FIB) liſt -out, which involves site-specifi c ion milling to produce a cross section of the target interface, extracting the cross section from the larger sample, and thinning it to electron transparency, all near liquid nitrogen temperature to preserve the liquids. To guide the milling process, we introduce a label-free in situ method of localizing subsurface structures directly in the cryo-FIB by EDX mapping. Aſt er transfer of the sample to the cryo-STEM, the structure, elemental distribution, and local bonding environment of intact liquid/solid interfaces can be determined at the nanometer scale.
Iron oxide nanocrystals in an intact hydrogel imaged by annular dark fi eld cryo-STEM. The sample was prepared by cryo-FIB lift-out and subsequently transferred to the cryo-STEM for analysis.
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