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首页> 外文期刊>Electroanalysis >Voltammetric characterization of micro- and submicrometer-electrode arrays of conical shape for electroanalytical use
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Voltammetric characterization of micro- and submicrometer-electrode arrays of conical shape for electroanalytical use

机译：用于电分析的圆锥形微米级和亚微米级电极阵列的伏安法表征

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摘要

Densely packed micro- and submicrometer electrode arrays of platinum and gold (the nominal number, N, of electrodes in each array varies between 225 and 3600) are fabricated by photolithographic technique and vapor deposition processes of metal films. The electrodes are conical-shaped and only their apexes are exposed to the electrolytic solution. The electrode arrays are characterized electrochemically in Ru(NH3)(6)Cl-3 aqueous solutions by using cyclic voltammetry at low scan rates, to establish the number of electrochemically active electrodes (N-ac) in each array; the geometric characterization is performed by scanning electron microscopy. All the investigated arrays provide steady-state voltammograms, indicating diffusionally independent behavior of each microelectrode. The number of microelectrodes that are active in the fabricated arrays depends on microelectrode density. In particular, for the arrays with N=3600 and N=225, the fraction of active sites is about 45% and 90%, respectively. The analytical performance of some of the Pt version of the arrays is tested in hydrogen peroxide solutions, allowing verifying that linear calibration plots over the concentration range (0.1-20 mM) are obtained. This dynamic range is larger than that typically recorded at smooth polycrystalline platinum electrodes (0.5-5 mM), and the better performance is attributed to both the higher aspect ratio of the cone geometry and the higher mass transport associated to each microelectrode of the array. Reproducibility (within 3.5%, r.s.d.) and long-term stability (within 5%, r.s.d., after 8 h continuous use) of the electrode systems are satisfactory. A low detection limit, based on the signal to noise ratio equal to 3, of 0.05 mM is found, which is adequate for a rapid monitoring of H2O2 in real samples and industrial processes.
机译：通过光刻技术和金属膜的气相沉积工艺制造了铂和金的密集堆积的微米和亚微米级电极阵列（每个阵列中电极的标称数量N在225至3600之间变化）。电极是圆锥形的，只有其顶点暴露在电解液中。通过在低扫描速率下使用循环伏安法在Ru（NH3）（6）Cl-3水溶液中对电极阵列进行电化学表征，以确定每个阵列中的电化学活性电极（N-ac）的数量;几何特征通过扫描电子显微镜进行。所有研究的阵列均提供稳态伏安图，表明每个微电极的扩散独立行为。在所制造的阵列中有效的微电极的数量取决于微电极密度。特别地，对于具有N ＝ 3600和N ＝ 225的阵列，活性位点的比例分别为约45％和90％。在过氧化氢溶液中测试了某些Pt型阵列的分析性能，从而可以验证是否获得了浓度范围（0.1-20 mM）内的线性校准图。该动态范围比通常在光滑的多晶铂电极上记录的动态范围大（0.5-5 mM），更好的性能归因于圆锥几何形状的较高长宽比和与阵列中每个微电极相关的较高质量传输。电极系统的重现性（在3.5％以内，r.s.d.）和长期稳定性（在连续使用8小时后，以r.s.d.在5％以内）是令人满意的。基于等于3的信噪比，发现了一个低检测极限，为0.05 mM，这足以快速监测实际样品和工业过程中的H2O2。

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