Ordered two-dimension macroporous gold array (MGA) was prepared for application in spectroelectrochemistry by electrochemical depositing method with colloid crystal as template. It was mounted to optical transparent thin-layer electrode using to measure E°' and n of o-tolidine. AFM and SEM were used to characterize the monolayer gold void. The absorption spectra of macroporous gold array were measured. Results show that gold hole is just about half-sphere shape and arranged to closed-hexagonal array when electrodepositing at -0. 8 V for 300 s, and the transmission of MGA was about 20％. E°' was measured to be 0. 660 V by thin-layer cyclic Voltammetry. The change of absorbance in thin layer was monitored at different potentials according to which E°' and n o-tolidine redox system were calculated to be 0. 659 V and 1. 7 in spectroelectrochemistry. The results were agreed with literature, which showed electrochemical and spectroelectrochemical properties of MGA were good%为研究多孔材料的光谱电化学应用,以模板-电沉积法制备了导向性的二维大孔金阵列,将其制成光透薄层电极,测定3,3'-二甲基联苯胺的E°'和n.采用原子力显微镜和扫描电子显微镜对其进行表征.测定了不同厚度的大孔金膜的吸收光谱.结果表明,在-0.8 V电沉积约300 s,得到大面积的厚度为292 nm的大孔金膜,透光率达20%;薄层循环伏安法测得E°'=0.660 V,光谱电化学法测得E°'=0.659 V,n=1.7,与文献一致,表明大孔金阵列的电化学和光谱电化学性能较好.
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