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Abstract
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Introduction
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Engineering
Nanotechnology

Advanced electroanalytical chemistry at nanoelectrodes

Profile image of Zhifeng DingZhifeng Ding

2017, Chemical Science

https://doi.org/10.1039/C7SC00433H
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11 pages

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Abstract

In this perspective, we discuss the challenges, advances and opportunities in electroanalytical chemistry at nanoelectrodes, including nanoelectrode fabrication, real-time characterizations, and high-performance electrochemical instrumentation.

Figures (7)
‘State Key Laboratory of Physical Chemistry of Solid Surfaces, Collaborative Innovation Centre of Chemistry for Energy Materials (iChEM), Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, P. R. China
‘State Key Laboratory of Physical Chemistry of Solid Surfaces, Collaborative Innovation Centre of Chemistry for Energy Materials (iChEM), Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, P. R. China
Fig. 2. Characterization of nanoelectrodes. (A) SEM image of a ~110 nm-diameter Pt nanoelectrode;*> (B) TEM image of a 1.5 nm radius Pt nanowire sealed in an SiOz capillary;** (C) TEM image of a 3 nm radius Pt nanoelectrode sealed in an SiOz capillary.1° Noncontact AFM image of a recessed Pt nanoelectrode in air in (D) 3D and (E) 2D. (F) Steady- state voltammogram of 1.2 mM FcCCH2OH. The potential sweep rate was v = 50 mV s_1.” Adapted with permission from ref. 16 Copyright (2009) American Chemical Society. Adapted with permission from ref. 55 Copyright (2013) American Chemical Society. Adapted with permission from ref. 72 Copyright (2012) American Chemical Society.
Fig. 2. Characterization of nanoelectrodes. (A) SEM image of a ~110 nm-diameter Pt nanoelectrode;*> (B) TEM image of a 1.5 nm radius Pt nanowire sealed in an SiOz capillary;** (C) TEM image of a 3 nm radius Pt nanoelectrode sealed in an SiOz capillary.1° Noncontact AFM image of a recessed Pt nanoelectrode in air in (D) 3D and (E) 2D. (F) Steady- state voltammogram of 1.2 mM FcCCH2OH. The potential sweep rate was v = 50 mV s_1.” Adapted with permission from ref. 16 Copyright (2009) American Chemical Society. Adapted with permission from ref. 55 Copyright (2013) American Chemical Society. Adapted with permission from ref. 72 Copyright (2012) American Chemical Society.
Fig. 3 (A) Circuit diagram of a low-current amplifier. During experi- ments, the bias voltage is set by applying a reference voltage to the non-inverting input of the trans-impedance amplifier (TIA). The current signal is transferred to a voltage signal through the TIA. Then, a unity gain differential amplifier is used to deduct the reference voltage from the signal. To lower the noise, a low-pass filter is always used before the signal is transferred to the digital signal by the analog- to-digital convertor (ADC). (B) Chronoamperometric curves of single 4-mercaptobenzene-1,2-diol@AUNP collisions on a carbon-fibre ultramicroelectrode (UME) recorded at a filter frequency of 1 kHz, 2 kHz and 5 kHz, respectively. The experiments were carried out in a15 mM phosphate buffer (pH 7.0) containing 5 mM NADH.” Adapted with permission from ref. 74 Copyright (2016) American Chemical Society. To measure the small and transient current signals accu- rately, high performance electrochemical instrumentation is
Fig. 3 (A) Circuit diagram of a low-current amplifier. During experi- ments, the bias voltage is set by applying a reference voltage to the non-inverting input of the trans-impedance amplifier (TIA). The current signal is transferred to a voltage signal through the TIA. Then, a unity gain differential amplifier is used to deduct the reference voltage from the signal. To lower the noise, a low-pass filter is always used before the signal is transferred to the digital signal by the analog- to-digital convertor (ADC). (B) Chronoamperometric curves of single 4-mercaptobenzene-1,2-diol@AUNP collisions on a carbon-fibre ultramicroelectrode (UME) recorded at a filter frequency of 1 kHz, 2 kHz and 5 kHz, respectively. The experiments were carried out in a15 mM phosphate buffer (pH 7.0) containing 5 mM NADH.” Adapted with permission from ref. 74 Copyright (2016) American Chemical Society. To measure the small and transient current signals accu- rately, high performance electrochemical instrumentation is
Fig.4 (A) TEM image of a single Au nanoparticle immobilized on a Pt nanoelectrode.*8 (B) Cyclic voltammetry of a bare 7 nm diameter Pt nanoelectrode (black), a 14 nm Au single nanoparticle immobilized Pt nanoelectrode (SNPE), an 18 nm Au SNPE (green) and a 24 nm Au SNPE (blue) in an oxygen-saturated 0.10 M KOH solution.4® TEM images of (C) a carbon nanopipette electrode and (D) a carbon nanopipette electrode with a 20 nm AuNP attached to its tip.°* (E) The current transients of 80 nm collisions of individual AgNPs with a nominal diameter on the Au UME (diameter of UME: 12.5 um) at an applied potential of +0.6 V vs. Ag/AgCl QRE.”; (i) i-t transients response; (ii and iii) close-ups of the representative spike clusters shown by crosses with different colours. (iv) Enlarged sections of the red and blue transient in (iii). Adapted with permission from ref. 48 Copyright (2010) American Chemical Society. Reproduced from ref. 93 with permission from the Royal Society of Chemistry. Adapted with permission from ref. 73. Electrochemical monitoring of single nanoparticle collisions provides detailed information about the nanoparticles including their size, concentration, shapes and diffusion coefficients.***” The electrochemical measurements of single nanoparticles were performed in both immobilization and nanocollision strategies.**°* For example, single Pt nano- particles were electrodeposited on carbon nanoelectrodes to readily study the effect of an ultra-high mass-transfer rate for the reduction of oxygen.” As shown in Fig. 4A, a ~15 nm Au nanoparticle was immobilized on a ~10 nm Pt nanoelectrode, which was used to study the size-dependent electrocatalytic activity at the single-nanoparticle level.** The results show that the steady-state limiting current increased with the size of the Au nanoparticle ranging from 14, 18 and 24 nm, while
Fig.4 (A) TEM image of a single Au nanoparticle immobilized on a Pt nanoelectrode.*8 (B) Cyclic voltammetry of a bare 7 nm diameter Pt nanoelectrode (black), a 14 nm Au single nanoparticle immobilized Pt nanoelectrode (SNPE), an 18 nm Au SNPE (green) and a 24 nm Au SNPE (blue) in an oxygen-saturated 0.10 M KOH solution.4® TEM images of (C) a carbon nanopipette electrode and (D) a carbon nanopipette electrode with a 20 nm AuNP attached to its tip.°* (E) The current transients of 80 nm collisions of individual AgNPs with a nominal diameter on the Au UME (diameter of UME: 12.5 um) at an applied potential of +0.6 V vs. Ag/AgCl QRE.”; (i) i-t transients response; (ii and iii) close-ups of the representative spike clusters shown by crosses with different colours. (iv) Enlarged sections of the red and blue transient in (iii). Adapted with permission from ref. 48 Copyright (2010) American Chemical Society. Reproduced from ref. 93 with permission from the Royal Society of Chemistry. Adapted with permission from ref. 73. Electrochemical monitoring of single nanoparticle collisions provides detailed information about the nanoparticles including their size, concentration, shapes and diffusion coefficients.***” The electrochemical measurements of single nanoparticles were performed in both immobilization and nanocollision strategies.**°* For example, single Pt nano- particles were electrodeposited on carbon nanoelectrodes to readily study the effect of an ultra-high mass-transfer rate for the reduction of oxygen.” As shown in Fig. 4A, a ~15 nm Au nanoparticle was immobilized on a ~10 nm Pt nanoelectrode, which was used to study the size-dependent electrocatalytic activity at the single-nanoparticle level.** The results show that the steady-state limiting current increased with the size of the Au nanoparticle ranging from 14, 18 and 24 nm, while
Fig. 5 Studying the single HRP with a BLM-Au nanoelectrode.® (A) Cyclic voltammograms of the BLM-Au nanoelectrode (1) and HRP- embedded BLM-Au nanoelectrode (2) in a solution of 20 mM H2O. and PBS buffer (pH: 7.4). (B) Chronoamperometric response of HRP collision into the BLM-Au electrode.® Reproduced by permission of ref. 6 from The Royal Society of Chemistry.
Fig. 5 Studying the single HRP with a BLM-Au nanoelectrode.® (A) Cyclic voltammograms of the BLM-Au nanoelectrode (1) and HRP- embedded BLM-Au nanoelectrode (2) in a solution of 20 mM H2O. and PBS buffer (pH: 7.4). (B) Chronoamperometric response of HRP collision into the BLM-Au electrode.® Reproduced by permission of ref. 6 from The Royal Society of Chemistry.
Fig. 6 (A) Current responses from a carbon fibre nanotip electrode pushed against a PC12 cell are shown (i) without breaking into the cytoplasm and (ii) inserted into a PC12 cell.%° (B) A schematic of the nanoelectrode incorporated nanokit for single cell analysis.*® (C) Bright-field image of a nanokit electrode inserted into the cell.*® (D) Charges of the nanokit electrode before (a) and after (b) being inserted into the cell1® Reproduced by permission of ref. 18 from Copyright (2016) National Academy of Sciences. Reproduced by permission of ref. 95 from John Wiley and Sons.
Fig. 6 (A) Current responses from a carbon fibre nanotip electrode pushed against a PC12 cell are shown (i) without breaking into the cytoplasm and (ii) inserted into a PC12 cell.%° (B) A schematic of the nanoelectrode incorporated nanokit for single cell analysis.*® (C) Bright-field image of a nanokit electrode inserted into the cell.*® (D) Charges of the nanokit electrode before (a) and after (b) being inserted into the cell1® Reproduced by permission of ref. 18 from Copyright (2016) National Academy of Sciences. Reproduced by permission of ref. 95 from John Wiley and Sons.

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