Electrochemical atomic layer deposition (E-ALD) has been used to deposit PbSe/PbTe superlattices, both with equal (4:4) and unequal (3:15) periods. The periods were formed from the repeated application of a PbTe E-ALD cycle four times, followed by a PbSe E-ALD cycle four times to complete one (4:4) period. The period was repeated as many times as desired to form a superlattice of a particular thickness. The deposition potentials used to form atomic layers of Pb, Se, and Te, for the growth of PbSe/PbTe superlattices, were approximated by first developing E-ALD cycles for the binary compounds PbSe and PbTe. Cyclic voltammetry (CV) for the individual elements are presented, as are coverages, as a function of the cycle number and period for PbSe and PbTe. Coverages were based on the charges for the deposition of the individual elements. In each case, coverages were found to average very close to one monolayer per cycle. Deposits were stoichiometric, from electron probe microanalysis, and the relative elemental coverages were consistent with the ratio of PbSe to PbTe cycles in the period. Scanning tunneling microscopy revealed the formation of conformal hexagonal mesas, with 240 nm wide atomically flat terraces on the gold on glass substrates. (C) 2010 The Electrochemical Society. [DOI: 10.1149/1.3521463] All rights reserved.