本文結合自組裝奈米球微影及光輔助電化學蝕刻兩項技術，用以製作出趨近完美排列之奈米柱狀陣列結構，以應用於直接甲醇燃料電池電極之開發，藉由電極接觸表面積之大量增加，提高觸媒催化反應效率。實驗結果證實使用薄光阻格狀結構搭配震盪塗佈法，可於 2 × 2 cm2 的試片上獲得趨近完美排列的單層奈米球。使用光輔助電化學蝕刻可製作出柱體高度為 1.56 μ m、直徑為 250 nm－300 nm、柱體深寬比可達6.2:1－5.2:1 之奈米柱狀陣列。在燃料電池電極性能測試中，平板電極之開路電壓、極限電流密度、最大功率密度分別為 105 mV、0.319 mA/cm2、9.3 μ W/cm2，而奈米柱狀電極最大開路電壓、極限電流密度、最大功率密度分別為 280 mV、1.044 mA/cm2、58.4 μ W/cm2，分別為平板電極的 1.98、3.27 與 6.3 倍，顯示奈米結構可提升觸媒與燃料接觸之接觸面積，使電池性能也隨之獲得有效提升。

This research will integrate self-assembled nanosphere lithography (SANL) and photo-assisted electrochemical etching (PAECE) techniques for fabricating perfect and high regular arrangement of the nanopillars array structure. In addition, we fabricate the electrodes applied in the direct methanol fuel cell by means of these techniques. Experimental results show that the nanosphere array with a nearly perfect arrangement can be obtained in the sample area of 2 × 2 cm2 by integrating thin photoresist and vibration method. Nanopillar array can be regularly arranged, and the array dimensions of width and height are 250 nm－300 nm and 1.56 μ m (aspect ratio, 6.2:1－5.2:1, respectively). The current density of 1.044 mA/cm2 is found from nanopillar electrode which is three times larger than that from the planar electrode at electrode potential of 1V. The current density from planar electrode is 0.319 mA/cm2 under the same potential. We found the nanopillar electrode DMFC of 58.4 μ W/cm2 power density showed maximum 6.3 times higher than the planar electrode DMFC of 9.3 μ W/cm2 power density in fuel cell test.