Site-Specific Preparation of Intact Solid–Liquid Interfaces by Label-Free In Situ Localization and Cryo-Focused Ion Beam Lift-Out

Zachman, Michael J.; Asenath-Smith, Emily; Estroff, Lara A.; Kourkoutis, Lena F.

doi:10.1017/s1431927616011892

Site-Specific Preparation of Intact Solid–Liquid Interfaces by Label-Free In Situ Localization and Cryo-Focused Ion Beam Lift-Out

Journal Article · Sun Nov 20 23:00:00 EST 2016 · Microscopy and Microanalysis

DOI:https://doi.org/10.1017/s1431927616011892· OSTI ID:1397228

Zachman, Michael J.; Asenath-Smith, Emily; Estroff, Lara A.; Kourkoutis, Lena F.

Abstract

Scanning transmission electron microscopy (STEM) allows atomic scale characterization of solid–solid interfaces, but has seen limited applications to solid–liquid interfaces due to the volatility of liquids in the microscope vacuum. Although cryo-electron microscopy is routinely used to characterize hydrated samples stabilized by rapid freezing, sample thinning is required to access the internal interfaces of thicker specimens. Here, we adapt cryo-focused ion beam (FIB) “lift-out,” a technique recently developed for biological specimens, to prepare intact internal solid–liquid interfaces for high-resolution structural and chemical analysis by cryo-STEM. To guide the milling process we introduce a label-freein situmethod of localizing subsurface structures in suitable materials by energy dispersive X-ray spectroscopy (EDX). Monte Carlo simulations are performed to evaluate the depth-probing capability of the technique, and show good qualitative agreement with experiment. We also detail procedures to produce homogeneously thin lamellae, which enable nanoscale structural, elemental, and chemical analysis of intact solid–liquid interfaces by analytical cryo-STEM. This work demonstrates the potential of cryo-FIB lift-out and cryo-STEM for understanding physical and chemical processes at solid–liquid interfaces.

Research Organization:: Energy Frontier Research Centers (EFRC) (United States). Energy Materials Center at Cornell (EMC2)

Sponsoring Organization:: USDOE SC Office of Basic Energy Sciences (SC-22)

DOE Contract Number:: SC0001086

OSTI ID:: 1397228

Journal Information:: Microscopy and Microanalysis, Journal Name: Microscopy and Microanalysis Journal Issue: 06 Vol. 22; ISSN 1431-9276; ISSN applab

Publisher:: Microscopy Society of America (MSA)

Country of Publication:: United States

Language:: English

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