Conclusions¶

By combining UPL with SEM/PFIB, Laser PFIB enables large 2D area and 3D volume analysis of complex multiphase materials systems with nanoscale resolution at cryo temperatures. Here, we describe in detail the benefits and drawbacks of a variety of laser parameters and their utility for revealing and differentiating different classes of materials. The methodologies described here were tailored for coin cells, but would require minimal adaption for other multiphase systems, including systems that combine beam sensitive materials, hard metals, and composites, where cryogenic operation may or may not be necessary. The tunability of this method makes it particularly desirable for the characterization and advancement of clean energy materials, including solar panels, membranes for water purification, and wind turbine blade materials.

Future Outlook¶

Given advancements in microscopy technology, there are new accessible improvements that can be made to the original Laser PFIB methodology, allowing for even better resolution and more advanced analysis. The workflow was originally demonstrated on a prototype system with limited rotation, tilt, and sample transfer capabilities, but there are now commercial Laser PFIB systems available with compatible cryo-transfer, air-free transfer, and 360° cryo stages, enabling improved PFIB polishing. With fewer instrument limitations, Laser PFIB workflows could be used to target a specific ROI with cryo-PFIB lift out for cryo-TEM analysis. Additionally, the integration of EDS and ESBD to the automated 3D slice-and-view routines allows for 3D chemical mapping of beam sensitive or multiphase materials systems, a powerful tool for understanding key structure-property relationships.