Using a multi-target pulsed laser deposition (PLD) process we synthesized superlattices in the (La0.8Ba0.2CuO2.6±x)m(AECuO2)
system, where AE = Ca or Sr, and m and n were varied. Owing to the sequential deposition process, two-dimensional order is obtained on the perovskite A-sites in the superlattice structures, as evidenced by X-ray diffraction for the materials where AE = Sr. However, when AE = Ca, the films were unstable. Structural units of CaCuO2 could be incorporated into the superlattices by containing them between layers of SrCuO2: (SrCuO2)l(CaCuO2)m(SrCuO2)l(La0.8Ba0.2CuO2.6±x)n. The stability and structural characteristics of particular stacking sequences are discussed with respect to their chemical preferences and are compared to bulk materials of similar stoichiometries, i.e., the (La,AE)CuO3-x system. The latter materials do not exhibit two-dimensional cation-order. Resistance measurements of as-synthesized and post-annealed materials are also discussed.