Influence of TEM specimen preparation on chemical composition of Pb(Mg1/3Nb2/3)O3–PbTiO3 single crystals

• Improvement of TEM sample preparation of lead-containing perovskite ceramics.
• PMN–PT single crystals prepared by tripod polishing and ion milling.
• Cooling the samples during ion milling reduces preparation-induced sample damage.

The influences of different transmission electron microscopy (TEM) specimen preparation techniques on the chemical composition of Pb(Mg1/3Nb2/3)O3–PbTiO3 (PMN–PT) single crystals was studied. Ion-milled samples where no cooling with liquid nitrogen (L-N2) was applied show permanently changed composition also deep inside the bulk material. When the PMN–PT samples were cooled to L-N2 temperature during the ion-milling process and in addition lower accelerating voltages were used, the chemical composition was altered only in the thinnest parts close to the specimen edge. Samples prepared using only tripod polishing technique show compositional irregularities close to the specimen edge. For the preparation of lead-containing samples, such as PMN–PT single crystals, a combination of tripod polishing and short Ar-ion-milling at low accelerating voltages while cooling the samples to liquid nitrogen temperature proved to be the most suitable to obtain artefact-free electron-transparent TEM lamellae.