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

Published online by Cambridge University Press:  21 November 2016

Michael J. Zachman ,
Emily Asenath-Smith ,
Lara A. Estroff  and
Lena F. Kourkoutis
Michael J. Zachman
Affiliation:
School of Applied and Engineering Physics, Cornell University, Ithaca, NY 14853, USA Kavli Institute at Cornell for Nanoscale Science, Cornell University, Ithaca, NY 14853, USA
Emily Asenath-Smith
Affiliation:
Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA
Lara A. Estroff
Affiliation:
Kavli Institute at Cornell for Nanoscale Science, Cornell University, Ithaca, NY 14853, USA Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA
Lena F. Kourkoutis*
Affiliation:
School of Applied and Engineering Physics, Cornell University, Ithaca, NY 14853, USA Kavli Institute at Cornell for Nanoscale Science, Cornell University, Ithaca, NY 14853, USA
*
*Corresponding author.lena.f.kourkoutis@cornell.edu
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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-free in situ method 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.

Keywords

cryo-scanning transmission electron microscopycryo-focused ion beam lift-outsolid–liquid interfacesspatially resolved electron energy loss spectroscopy
Type
Instrumentation and Software Techniques
Information
Microscopy and Microanalysis , Volume 22 , Issue 6 , December 2016 , pp. 1338 - 1349
Copyright
© Microscopy Society of America 2016 

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Footnotes

†

B90 Physical Sciences Building, Cornell University, 245 East Avenue, Ithaca, NY 14853, USA.

‡

US Army Engineer Research & Development Center (ERDC), Cold Regions Research & Engineering Laboratory (CRREL), 72 Lyme Road, Hanover, NH 03755, USA.

§

329 Bard Hall, Cornell University, Ithaca, NY 14853, USA.

‖

235 Clark Hall, Cornell University, Ithaca, NY 14853, USA.

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