This article reports the development of a robust, one-step electrochemical technique to generate surface-bound conjugated polymers. The electrochemical reduction of arene diazonium salts at the surface of a gold electrode is used to generate tethered bromobenzene monolayers quickly. The oxidative addition of reactive Ni(0) across the aryl halide bond is achieved in situ through a concerted electrochemical reduction of Ni(dppp)Cl-2. This technique limits the diffusion of Ni(0) species away from the surface and overcomes the need for solution deposition techniques which often require multiple steps that result in a loss of surface coverage. With this electrochemical technique, the formation of the reactive monolayer resulted in a surface coverage of 1.29 X 10(14) molecules/cm(2), which is a 6-fold increase over previously reported results using solution deposition techniques.