TEM characterization and microanalysis of the recording media is crucial and complementary to new material system development as well as quality control applications. Due to the type of material generally used for supporting the medium, i.e., a polymer, conventional macro- and microthinning procedures for thin foil preparation are not applicable. Ultramicrotorny (UM) is a viable option and has been employed in previous similar studies. In this work UM has been used for preparation of XTEM samples from a magneto-optical (MO) recording medium in its original production format.The as-received material system consisted of a 4-layer, 2100 Å thick medium including a 300 Å TbFeCo layer enveloped by silicon nitride protective layers supported on a 1.2 mm thick × 135 mm (5.25 in.) diameter polycarbonate disk. Recording tracks had an approximate pitch of 1.6 μm separated by 800 Å deep peripheral grooves. Using a Buehler Isomet low-speed diamond saw, 1 mm wide and 20 mm long strips were cut out of the disk along the recording tracks.