The purpose of this dissertation is to describe a simple and inexpensive method to electrodeposit a composition-spread library of metal alloys (Sn-Zn) onto a lead pattern consisting of 64 individually addressable electrodes. The electrodeposited lead pattern can then be loaded into an electrochemical cell where the 64 unique metal alloy electrodes are tested in parallel for their suitability as advanced negative electrode materials for rechargeable Li-ion batteries. Ninety percent of the Sn- Zn binary composition space is sampled in a single electrodeposition experiment. We show how the power of combinatorial screening techniques can be combined with the simplicity and low cost of masked electrodeposition. (c) 2005 The Electrochemical Society. [DOI: 10.1149/1.1940827] All rights reserved.