Preparation and Electrochemical Response of 1-3 nm Pt Disk Electrodes

Preparation and Electrochemical Response of 1-3 nm Pt Disk Electrodes
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DOI:
10.1021/ac900777n
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发表时间:
2009-07-01
影响因子:
7.4
通讯作者:
Zhang, Bo
Zhang, Bo
中科院分区:
化学1区
文献类型:
--
作者:
Li, Yongxin;Bergman, David;Zhang, Bo

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报道了半径为1 ~ 3 nm的Pt纳米电极的制备和表征。一个铂微丝密封到一个双层石英毛细管和拉成ultrasharp铂纳米线密封在二氧化硅尖端使用激光辅助拉过程。然后将超尖锐尖端密封到一块玻璃管中,手动抛光以暴露Pt。透射电子显微镜和稳态伏安法被用来表征纳米电极。结果表明,Pt纳米电极的最小尺寸取决于Pt微丝的尺寸和提拉过程中使用的参数。用Mirkin和Bard的方法从稳态伏安法测定了二茂铁、二茂铁甲醇和六氯铱酸钾(III)氧化的非均相电子转移速率常数,并发现对于二茂铁,k度= 7.6 +/- 3.4 cm/s和α = 0.85 +/- 0.06,对于二茂铁甲醇,k度= 7.4 +/- 6.9 cm/s和α = 0.78 +/- 0.16,对于IrCl 63-,k度= 6.0 +/- 4.2 cm/s和α = 0.72 +/- 0.15。
The preparation and characterization of Pt nanoelectrodes in the range of 1 to 3 nm in radii are reported. A Pt microwire is sealed into a bilayer quartz capillary and pulled into an ultrasharp Pt nanowire sealed in a silica tip using a laser-assisted pulling process. The ultrasharp tip is then sealed into a piece of glass tubing, which is manually polished to expose the Pt. Transmission electron microscopy and steady-state voltammetry are utilized to characterize the nanoelectrodes. The results show that the minimum size of the Pt nanoelectrode is determined by the size of the Pt microwire and parameters used in the pulling process. The heterogeneous electron transfer rate constant for the oxidation of ferrocene, ferrocenemethanol, and potassium hexachloroiridate (III) are determined from steady-state voltammetry using the method of Mirkin and Bard and are found to be k degrees = 7.6 +/- 3.4 cm/s and alpha = 0.85 +/- 0.06 for ferrocene, k degrees = 7.4 +/- 6.9 cm/s and alpha = 0.78 +/- 0.16 for ferrocenemethanol, and k degrees = 6.0 +/- 4.2 cm/s and alpha = 0.72 +/- 0.15 for IrCl63-.