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使用扫描电化学显微镜对高电阻膜孔进行交流阻抗成像。应用膜电分流器提高测量灵敏度和图像对比度。

Alternating current impedance imaging of high-resistance membrane pores using a scanning electrochemical microscope. Application of membrane electrical shunts to increase measurement sensitivity and image contrast.

作者信息

Ervin Eric Nathan, White Henry S, Baker Lane A, Martin Charles R

机构信息

Department of Chemistry, University of Utah, 315 South 1400 East, Salt Lake City, Utah 84112, USA.

出版信息

Anal Chem. 2006 Sep 15;78(18):6535-41. doi: 10.1021/ac060577k.

Abstract

Whether an individual pore in a porous membrane can be imaged using scanning electrochemical microscopy (SECM), operated in ac impedance mode, is determined by the magnitude of the change in the total impedance of the imaging system as the SECM tip is scanned over the pore. In instances when the SECM tip resistance is small relative to the internal pore resistance, the total impedance changes by a negligible amount, rendering the pore invisible during impedance imaging. A simple solution to this problem is to introduce a low-impedance electrical shunt (i.e., a salt bridge) across the membrane. This principle is demonstrated by imaging polycarbonate membranes (6-12-microm thickness) containing between 1 and 2000 conical-shaped pores (60-nm- and 2.5-microm-diameter openings) using an approximately 1-microm-radius Pt tip. Theory and experiments show that image contrast (the change in ac current measured as the probe is scanned over the pore) is inversely proportional to the total resistance of the membrane and can be increased by a factor of approximately 50x by introducing a low-resistance electrical shunt across the membrane. Remarkably, SECM images of membranes containing a single high-resistance (approximately 1 G Omega) pore can only be imaged by short-circuiting the membrane. Image contrast also becomes independent of membrane resistance when an electrical shunt is used, allowing for more quantitative comparisons of the features in ac impedance images of different membranes.

摘要

在交流阻抗模式下操作的扫描电化学显微镜(SECM)能否对多孔膜中的单个孔进行成像,取决于成像系统的总阻抗变化量,该变化量是在SECM探针扫描过该孔时产生的。当SECM探针电阻相对于孔内电阻较小时,总阻抗变化量可忽略不计,使得该孔在阻抗成像过程中不可见。解决这个问题的一个简单方法是在膜上引入一个低阻抗电分流器(即盐桥)。使用半径约为1微米的铂探针,对含有1至2000个锥形孔(孔径分别为60纳米和2.5微米)的聚碳酸酯膜(厚度为6至12微米)进行成像,证明了这一原理。理论和实验表明,图像对比度(在探针扫描过孔时测量的交流电流变化)与膜的总电阻成反比,通过在膜上引入低电阻电分流器,图像对比度可提高约50倍。值得注意的是,对于含有单个高电阻(约1 GΩ)孔的膜,只有通过使膜短路才能获得SECM图像。当使用电分流器时,图像对比度也与膜电阻无关,这使得不同膜的交流阻抗图像中的特征能够进行更定量的比较。

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