The ability to acquire TEM specimens from micrometer sized particles using an innovative FIB LO technique has been previously demonstrated [1-3]. This technique allowed for the preparation of a TEM LO specimen from regions which were smaller than the conventional dimensions of the LO specimen (∼5 μm × 20 μm). This paper shows how the LO technique previously developed for the preparation of micrometer sized particles [3] may be extended and utilized for the preparation of submicrometer sized particles for TEM analysis.

In this study, TiO2 particles on the order of 200 nm in width were investigated. A small portion of the TiO2 particles was dusted onto double stick carbon tape adhered to a sample stud and then sputtered coated with Au-Pd to protect the outer surface from FIB imaging. The sample stud containing the TiO2 particles was placed in an FEI 200TEM FIB workstation. Figure 1 is a FIB image of the Ti02 particles of interest. Gaps around these particles were deposited with Pt using the FIB assisted CVD process as shown in Figure 2. in this procedure, the Pt acts as a “weld” to hold the particles together, and to allow for a larger region to be milled (e.g., >10 μm) for subsequent specimen preparation.