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Spatially resolved detection of a nanometer-scale gap by scanning electrochemical microscopy.

ABSTRACT: Nanowires with nanometer-scale gaps are an emerging class of nanomaterials with potential applications in electronics and optics. Here, we demonstrate that the feedback mode of scanning electrochemical microscopy (SECM) allows for spatially resolved detection of a nanogap on the basis of its electrical conductivity. A gapped nanoband is used as a model system to describe a mechanism of a unique feedback effect from a nanogap. Interestingly, both experiments and numerical simulations confirm that a peak current response is obtained when an SECM tip is laterally scanned above an insulating nanogap formed in an unbiased nanoband. On the other hand, no peak current response is expected for a highly conductive nanogap, which must be extremely narrow or filled with highly conductive molecules for efficient electron transport.

SUBMITTER: Kim E

PROVIDER: S-EPMC2702147 | biostudies-literature | 2009 Jun

REPOSITORIES: biostudies-literature

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Spatially resolved detection of a nanometer-scale gap by scanning electrochemical microscopy.

Kim Eunkyoung E Kim Jiyeon J Amemiya Shigeru S

Analytical chemistry 20090601 12

Nanowires with nanometer-scale gaps are an emerging class of nanomaterials with potential applications in electronics and optics. Here, we demonstrate that the feedback mode of scanning electrochemical microscopy (SECM) allows for spatially resolved detection of a nanogap on the basis of its electrical conductivity. A gapped nanoband is used as a model system to describe a mechanism of a unique feedback effect from a nanogap. Interestingly, both experiments and numerical simulations confirm that ...[more]

PMID: 19518142

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Project description:The electrochemical reduction of CO2 is widely studied as a sustainable alternative for the production of fuels and chemicals. The electrolyte's bulk pH and composition play an important role in the reaction activity and selectivity and can affect the extent of the buildup of pH gradients between the electrode surface and the bulk of the electrolyte. Quantifying the local pH and how it is affected by the solution species is desirable to gain a better understanding of the CO2 reduction reaction. Local pH measurements can be realized using Scanning Electrochemical Microscopy (SECM); however, finding a pH probe that is stable and selective under CO2 reduction reaction conditions is challenging. Here, we have used our recently developed voltammetric pH sensor to perform pH measurements in the diffusion layer during CO2 reduction using SECM, with high time resolution. Using a 4-hydroxylaminothiophenol (4-HATP)/4-nitrosothiophenol (4-NSTP) functionalized gold ultramicroelectrode, we compare the local pH developed above a gold substrate in an argon atmosphere, when only hydrogen evolution is taking place, to the pH developed in a CO2 atmosphere. The pH is monitored at a fixed distance from the surface, and the sample potential is varied in time. In argon, we observe a gradual increase of pH, while a plateau region is present in CO2 atmosphere due to the formation of HCO3 - buffering the reaction interface. By analyzing the diffusion layer dynamics once the sample reaction is turned "off", we gain insightful information on the time scale of the homogeneous reactions happening in solution and on the time required for the diffusion layer to fully recover to the initial bulk concentration of species. In order to account for the effect of the presence of the SECM tip on the measured pH, we performed finite element method simulations of the fluid and reaction dynamics. The results show the significant localized diffusion hindrance caused by the tip, so that in its absence, the pH values are more acidic than when the tip is present. Nonetheless, through the simulation, we can account for this effect and estimate the real local pH values across the diffusion layer.

Dataset Information

Spatially resolved detection of a nanometer-scale gap by scanning electrochemical microscopy.

Publications

Spatially resolved detection of a nanometer-scale gap by scanning electrochemical microscopy.

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