Ba2Bi0.572TeO6±δ and SrLa2NiFeNbO9 ceramics were prepared in polycrystalline form by conventional solid-state reaction techniques in air. The crystal structures of the title compounds were determined at room temperature from X-ray powder diffraction (XRPD) data using the Rietveld method. The Ba2Bi0.572TeO6±δ structure crystallizes in a triclinic space group I–1 with unit-cell parameters a = 6.0272(2) Å, b = 6.0367(1) Å, c = 8.5273(3) Å, α = 90.007(7)°, β = 90.061(2)°, and γ = 90.015(4)°. The tilt system of the BiO6 and TeO6 octahedra corresponds to the notation a–b–c–. The crystal structure of the SrLa2NiFeNbO9 compound adopts an orthorhombic Pbnm space group with lattice parameters a = 5.6038(5) Å, b = 5.5988(4) Å, and c = 7.9124(6) Å. The BO6 octahedra (B = Ni/Fe/Nb) sharing the corners in 3D. Along the c-axis, the octahedra are connected by O(1) atoms of (x,y,1/4) positions; while in the ab-plane, they are linked by O(2) atoms of (x,y,z) positions. The bond angle of B–O1–B is 168.7° and that of B–O2–B is 156.3°. The octahedral lattice corresponds to the tilt pattern a–a–c+; it indicates that the octahedra tilt out-of-phase along the a,b-axes and in phase along the c-axis.

It is shown that a xenon plasma focused ion beam (FIB) microscope is an excellent tool for high-quality preparation of functional oxide thin films for atomic resolution electron microscopy. Samples may be prepared rapidly, at least as fast as those prepared using conventional gallium FIB. Moreover, the surface quality after 2 kV final polishing with the Xe beam is exceptional with only about 3 nm of amorphized surface present. The sample quality was of a suitably high quality to allow atomic resolution high-angle annular dark field imaging and integrated differential phase contrast without any further preparation, and the resulting images were good enough for quantitative evaluation of atomic positions to reveal the oxygen octahedral tilt pattern. This suggests that such xenon plasma FIB instruments may find widespread application in transmission electron microscope and scanning transmission electron microscope specimen preparation.