Applications of focused ion beam for preparation of specimens of ancient ceramic for electron microscopy and synchrotron X-ray studies

In this paper the capabilities of FIB systems as a tool for TEM studies of ancient pottery are explored, especially when the amount of available material is very limited and when, for instance, there is stringent demand for very accurate location of the electron-transparent area as is the case for investigation of outer surface layers, such as slips and patinas. The advantages of the two main FIB milling techniques (H-bar and Lift-out) are discussed in detail and illustrated through the study of metallic lustre decorations and a particular type of Roman Terra Sigillata coating. The H-bar technique is ideal for investigations where the features of interest are near the edges of a ceramic fragment. A significantly large area of surface decoration can be studied without any restriction on the size and the shape of fragment. On the other hand, the Lift-out technique is very powerful for extracting TEM membranes far from the edges. An added advantage of this technique is that the thickness of the foil is very uniform and that allows large tilts and makes it possible to obtain electron diffraction patterns of several zones axes from the same crystal, making crystallographic phase identification easier and precise, and identification of complex structures possible. We also show that the FIB system can be used to deposit very precise registration marks, allowing an experimenter to correlate results from TEM measurements with other complementary techniques, such as synchrotron based microdiffraction and μXANES. Combination of these complementary techniques is becoming a very powerful approach to probe the chemical and morphological microstructure of heterogeneous and complex material from the nanometre to millimetre scale.