A multi-electrolyte-step (MES) anodic aluminum oxide (AAO) method was used to achieve nanochannel arrays with good circularity and periodic structure. The nano-channel array fabrication process included immersion in a phosphoric acid solution with a 120-150 bias voltage. Bowl-shaped structures were then formed by removing the walls of the nano-channel arrays. The nano-channel arrays were grown from the bottom of the bowl structure in an oxalic solution using a 50 V bias voltage. A comparison of this new MES process with the one-step and five-step AAO process showed a 50% improvement in the circularity over the one-step process. The standard deviation of the average period in the MES array was 25 nm which is less than that of one-step process. This MES method also took 1/4 of the growing time of the five-step process. The orderliness of the nano-channel arrays for the five-step and MES process was similar. Finally, Cu nanoparticle arrays with a 200 nm period were grown using an electroplating process inside the MES nano-channel arrays on fluorine doped tin oxide glass. Stronger surface plasmon resonance absorption from 550 nm to 750 nm was achieved with the MES process than was possible with the one-step process.