Name: nanoscale characterization of liquid-solid interfaces by coupling cryo-focused ion beam milling with scanning electron microscopy and spectroscopy
Uploaded: 2022-07-14T12:30:00
Description: Watch this Scientific Journal Video about Nanoscale Characterization of Liquid-Solid Interfaces by Coupling Cryo-Focused Ion Beam Milling with Scanning Electron Microscopy and Spectroscopy at JoVE.com

We greatly acknowledge the contributions by Shuang-Yan Lang and H&#233;ctor D. Abru&#241;a who provided samples for our research. This work was supported by the National Science Foundation (NSF) (DMR-1654596) and made use of the Cornell Center for Materials Research Facilities supported by the NSF under Award Number DMR-1719875.

1. Prepare the sample and transfer into the SEM chamber
<ol>
	<li>Set up the microscope
	<ol>
		<li>For systems that convert between room temperature and cryogenic equipment, install the cryo-SEM stage and anticontaminator according to the equipment manufacturer&#8217;s instructions and evacuate the SEM chamber.</li>
		<li>Adjust the gas injection system (GIS) platinum source so that when inserted it sits approximately 5 mm further away from the sample surface compared to typical room temperature experiments. This posi...

<ol>
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The cryogenic preparation method described here is important and must be done correctly for the chemistry and morphology to be preserved8. The foremost concern is freezing the sample quickly since this is what allows the liquid to be vitrified8. If the sample cools too slowly, liquids may crystalize resulting in a change in morphology6. To prevent crystallization, slush nitrogen is used in this procedure, as it reduces the Leidenfrost effect and acce...

Interfaces between solids and liquids play a vital role in the function of energy materials such as batteries, fuel cells, and supercapacitors1,2,3. While characterizing the chemistry and morphology of these interfaces could play a central role in improving functional devices, doing so has presented a substantial challenge1,3,4. Liquids are incompatible with the high vacuum environments needed for many common characterization techniques, such as x-ray photoemission spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy2. Historically, the solution has been to remove the liquid from the device, but this comes at the expense of potentially damaging delicate structures at the interface2,4 or modifying morphology3. In the case of batteries, especially those which employ highly reactive alkali metals, this physical damage is compounded by chemical degradation upon exposure to air5.
This paper describes cryo-SEM and focused ion beam (FIB) as a method for preserving and characterizing solid-liquid interfaces. Similar methods have been shown to preserve the structure of cells in biological samples6,7,8, energy devices5,9,10,11,12 and nanoscale corrosion reactions13,14,15. The crux of the technique is to vitrify the sample via plunge freezing in slush nitrogen prior to transfer into the microscope where it is placed onto a cryogenically cooled stage. Vitrification stabilizes the liquid in the vacuum of the microscope while avoiding the structural deformations associated with crystallization6,8. Once in the microscope, a dual beam system allows nanoscale imaging with the electron beam, and preparation of cross-sections with the focused ion beam. Lastly, chemical characterization is enabled via Energy Dispersive X-ray (EDX) mapping. Altogether, cryo-SEM/FIB can preserve the native structure of a solid-liquid interface, create cross-sections, and provide both chemical and morphological characterization.
In addition to providing a general workflow for cryo-SEM and EDX mapping, this paper will describe a number of methods to mitigate artifacts from milling and imaging. Often vitrified liquids are delicate and insulating, making them prone to charging as well as beam damage8. While a number of techniques have been established to reduce these unwanted effects in specimens at room-temperature16,17,18, several have been modified for cryogenic applications. In particular, this procedure details application of conductive coatings, first a gold-palladium alloy, followed by a thicker platinum layer. Additionally, instructions are provided to help users identify charging when it occurs and adjust the electron beam conditions to mitigate the accumulation of charge. Lastly, although beam damage has many characteristics in common with charging, the two can occur independent of one another16, and guidelines are provided for minimizing beam damage during the steps where it is most likely.
While dual-beam SEM/FIB is not the only electron microscopy tool to have been adapted for cryogenic operation, it is particularly well-suited for this work. Often realistic devices like a battery are on the scale of several centimeters in size, while many of the features of interest are on the order of microns to nanometers, and the most meaningful information can be contained in the cross-section of the interface4,5,19. Although techniques like Scanning Transmission Electron Microscopy (STEM) combined with Electron Energy Loss Spectroscopy (EELS) enable imaging and chemical mapping down to the atomic scale, they require extensive preparation to make the sample sufficiently thin to be electron transparent, dramatically limiting throughput3,4,19,20,21,22. Cryo-SEM, by contrast, allows for the rapid probing of interfaces in macroscopic devices, such as the anode of a lithium metal battery coin cell, albeit at a lower resolution of tens of nanometers. Ideally, a combined approach that leverages the advantages of both techniques is applied. Here, we focus on higher throughput cryogenic FIB/SEM techniques.
Lithium metal batteries were used as the primary test case for this work, and they demonstrate the broad utility of cryo-SEM techniques: they feature delicate structures of scientific interest4,5,9,10,11,12, have broadly varying chemistry to be revealed via EDX2, and cryogenic techniques are required to preserve the reactive lithium5,21. In particular, the uneven lithium deposits known as dendrites, as well as the interfaces with the liquid electrolyte are preserved and can be imaged and mapped with EDX4,5,12. Additionally, lithium typically would oxidize during preparation and form an alloy with gallium during milling, but the preserved electrolyte prevents oxidation and cryogenic temperatures mitigate reactions with gallium5. Many other systems (energy devices especially) feature similarly delicate structures, complex chemistries and reactive materials, so the success of cryo-SEM on the study of lithium metal batteries can be considered a promising indication that it is suitable for other materials as well.
The protocol uses a dual-beam FIB/SEM system fitted with a cryogenic stage, a cryogenic preparation chamber and a cryogenic transfer system, as detailed in the&#160;Table of Materials. For preparing the cryo-immobilized samples there is a workstation with a &#34;slush pot,&#34; which is a foam insulated pot that sits in a vacuum chamber in the station. The foam insulated dual pot slusher contains a primary nitrogen chamber and a secondary chamber which surrounds the former and reduces boiling in the main part of the pot. Once filled with nitrogen, a lid is placed over the pot and the whole system can be evacuated to form slush nitrogen. A transfer system featuring a small vacuum chamber is used to transfer the sample under vacuum to the preparation or &#34;prep&#34; chamber of the microscope. In the prep chamber the sample can be kept at -175 &#176;C and sputter coated with a conductive layer, such as a gold-palladium alloy. Both the prep chamber and the SEM chamber feature a cryogenically cooled stage for holding the sample, and an anticontaminator to adsorb contaminants and to prevent ice buildup on the specimen. The whole system is cooled with nitrogen gas that flows through a heat exchanger submerged in liquid nitrogen, and then through the two cryo-stages and two anticontaminators of the system.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>INCA EDS</td>
			<td>Oxford instruments</td>
			<td></td>
			<td>Control software for X-max 80</td>
		</tr>
		<tr>
			<td>PP3010T Cryo-preparation system</td>
			<td>Quorum Technologies, Inc.</td>
			<td></td>
			<td>FIB/SEM cryogenic preparation system. Includes pumping station, transfer rod system, preparation (prep) chamber, cryogenic stages, sample shuttles&#160;</td>
		</tr>
		<tr>
			<td>Strata 400 DualBeam System&#160;</td>
			<td>FEI Co. (now Thermo Fisher Scientific)</td>
			<td></td>
			<td>Dual beam FIB/SEM</td>
		</tr>
		<tr>
			<td>X-Max 80</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td>80mm2 EDX detector</td>
		</tr>
		<tr>
			<td>xT Microscope Control</td>
			<td>FEI Co. (now Thermo Fisher Scientific)</td>
			<td></td>
			<td>Software for controlling FEI Strata&#160;</td>
		</tr>
	</tbody>
</table>

nanoscale characterization of liquid-solid interfaces by coupling cryo-focused ion beam milling with scanning electron microscopy and spectroscopy

Physical and chemical processes at solid-liquid interfaces play a crucial role in many natural and technological phenomena, including catalysis, solar energy and fuel generation, and electrochemical energy storage. Nanoscale characterization of such interfaces has recently been achieved using cryogenic electron microscopy, thereby providing a new path to advancing our fundamental understanding of interface processes.
This contribution provides a practical guide to mapping the structure and chemistry of solid-liquid interfaces in materials and devices using an integrated cryogenic electron microscopy approach. In this approach, we pair cryogenic sample preparation which allows stabilization of solid-liquid interfaces with cryogenic focused ion beam (cryo-FIB) milling to create cross-sections through these complex buried structures. Cryogenic scanning electron microscopy (cryo-SEM) techniques performed in a dual-beam FIB/SEM enable direct imaging as well as chemical mapping at the nanoscale. We discuss practical challenges, strategies to overcome them, as well as protocols for obtaining optimal results. While we focus in our discussion on interfaces in energy storage devices, the methods outlined are broadly applicable to a range of fields where solid-liquid interface play a key role.

This method has been developed on a dual FIB/SEM system equipped with a commercially available cryogenic stage, anticontaminator, and preparation chamber. For details, see the table of materials. We have primarily tested this method on lithium metal batteries with a number of different electrolytes, but the method is applicable to any solid-liquid interface that will endure the amount of dose applied during EDX mapping.
Figure 1&#160;illustrates the various compon...

Watch this Scientific Journal Video about Nanoscale Characterization of Liquid-Solid Interfaces by Coupling Cryo-Focused Ion Beam Milling with Scanning Electron Microscopy and Spectroscopy at JoVE.com

Nanoscale Characterization of Liquid-Solid Interfaces by Coupling Cryo-Focused Ion Beam Milling with Scanning Electron Microscopy and Spectroscopy

Cryogenic Focused Ion Beam (FIB) and Scanning Electron Microscopy (SEM) techniques can provide key insights into the chemistry and morphology of intact solid-liquid interfaces. Methods for preparing high quality Energy Dispersive X-ray (EDX) spectroscopic maps of such interfaces are detailed, with a focus on energy storage devices.

Physical and chemical processes at solid-liquid interfaces play a crucial role in many natural and technological phenomena, including catalysis, solar ...

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