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The formation of a self-assembled monolayer (SAM) on a gold electrode, a procedure called direct electrical self-assembly (DESA), requires the use of a neutral, alkanethiol monolayer that provides the electrical "bonding" between the surface and the electrode. To date, the best monolayer for DESA is a mixed SAM containing a phosphonic acid terminal group (PA-SAM). This SAM is made by treating a self-assembled monolayer of alkanethiol with phosphoric acid at low temperature, in an attempt to chemically "tether" the alkanethiols to the electrode. However, this procedure has been plagued by poor reproducibility. This paper describes the preparation of PA-SAMs on electrodes, using a controlled, two-step exposure procedure. 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