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

The cryo-SEM and FIB method can be used to study solid-liquid interfaces and biological samples while preserving the samples native structure. The main advantage of this technique is that the cryo-SEM allows the user to quickly probe the interface of macroscopic devices like coin cell battery electrodes with tens of nanometers resolution. Begin by installing a cryo-SEM stage and an anticontaminator.

Evacuate the SEM chamber and adjust the gas injection system, GIS, platinum source so that when inserted, the source will sit approximately five millimeters away from the sample surface. Set the GIS temperature to 28 degrees Celsius and open the shutter to vent the system for 30 seconds to clear out any excess material. Then, allow the SEM chamber to evacuate for a minimum of eight hours.