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A Method for FIB Liftout of Particles in Epoxy Resin

Preparation of electron transparent samples from small particles can be extremely challenging, even when using the Focused Ion Beam (FIB). In particular, when the dimensions of the particles are less than a typical liftout (<10um) and are loosely packed, a uniform thin area of several particles can be difficult to achieve. One way to overcome this is to use the carbon deposition available in the FIB to encapsulate particles. However, in our case, this caused a variety of problems because the C did not penetrate into all of the pores between particles. This caused severe “curtaining” (fig. 1c) and redeposition of material on the particle surfaces. Epoxy resin is a good alternate because the voids between the particles can be removed through proper vacuum encapsulation procedures, but the differential milling rates of the powder and resin material can cause additional problems. Presently there are several small particle TEM preparation techniques described in the literature, for example reference [2]. Here, we investigate how to minimize Ga-induced beam damage and prepare a site-specific specimen of a particle cluster or individual particle in a cold setting epoxy resin we had on hand.