Semiconducting Nanoparticles: Single Entity Electrochemistry and Photoelectrochemistry

Mathuri, S.; Zhu, Yuanhang; Margoni, Mudaliar Mahesh; Li, Xiuting

doi:10.3389/fchem.2021.688320

Cited by 7 publications

(5 citation statements)

References 63 publications

(133 reference statements)

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“…) ,, and nanoconfinement techniques (ultramicroelectrodes, nanoelectrodes, single NP collision, nanopores, nanochannels, etc. ). ,, In addition, there is SECCM that permits obtaining the region-specific electrochemical signal, correlating structure/function in the nanoscale in situ/operando. , Nanoconfinement experiments and SECCM excel at electrochemical activity, but they do not provide information about the structure of the particles. In this context, BCDI is a potentially powerful technique to explore electrocatalysts, as it can be performed in situ with the right experimental setup, providing the necessary complementary information.…”

Section: Experimental Results Obtained With the Developed Electrochem...mentioning

confidence: 99%

“…36,53,54 and nanoconfinement techniques (ultramicroelectrodes, nanoelectrodes, single NP collision, nanopores, nanochannels, etc.). 36,55,56 In addition, there is SECCM that permits obtaining the region-specific electrochemical signal, correlating structure/function in the nanoscale in situ/operando. 57,58 Nanoconfinement experi- ments and SECCM excel at electrochemical activity, but they do not provide information about the structure of the particles.…”

Section: Developed Electrochemical Cellsmentioning

confidence: 99%

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Development of Electrochemical Cells and Their Application for Spatially Resolved Analysis Using a Multitechnique Approach: From Conventional Experiments to X-Ray Nanoprobe Beamlines

Vicente,

Raju,

Gomes

et al. 2023

Anal. Chem.

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Real (electro)catalysts are often heterogeneous, and their activity and selectivity depend on the properties of specific active sites. Therefore, unveiling the so-called structure−activity relationship is essential for a rational search for better materials and, consequently, for the development of the field of (electro-)catalysis. Thus, spatially resolved techniques are powerful tools as they allow us to characterize and/or measure the activity and selectivity of different regions of heterogeneous catalysts. To take full advantage of that, we have developed spectroelectrochemical cells to perform spatially resolved analysis using X-ray nanoprobe synchrotron beamlines and conventional pieces of equipment. Here, we describe the techniques available at the Carnauba beamline at the Sirius-LNLS storage ring, and then we show how our cells enable obtaining X-ray (XRF, XRD, XAS, etc.) and vibrational spectroscopy (FTIR and Raman) contrast images. Through some proof-of-concept experiments, we demonstrate how using a multi-technique approach could render a complete and detailed analysis of an (electro)catalyst overall performance.

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Section: Experimental Results Obtained With the Developed Electrochem...mentioning

confidence: 99%

Section: Developed Electrochemical Cellsmentioning

confidence: 99%

Development of Electrochemical Cells and Their Application for Spatially Resolved Analysis Using a Multitechnique Approach: From Conventional Experiments to X-Ray Nanoprobe Beamlines

Vicente,

Raju,

Gomes

et al. 2023

Anal. Chem.

View full text Add to dashboard Cite

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“…There are also reports that have shown nano-impact events through the collisions of "soft" particles (micelles) with an UME and an applied electrochemical potential. [28][29][30][46][47][48][49][50] There are several reviews on the subject, [51][52][53][54][55][56][57][58][59][60] but in this paper, we focus on introducing critical concepts and techniques related to nanoparticles or other entities colliding with a working UME. Other modes that are not addressed in depth here, are based on scanning probes techniques and instrumentation, such as such scanning electrochemical microscopy, SECM, [23,24] and scanning electrochemical cell microscopy, SECCM.…”

Section: Single Entity Electrochemistry Modesmentioning

confidence: 99%

Why Measure Particle-by-Particle Electrochemistry? A Tutorial and Perspective

Alpuche Aviles,

Gutierrez-Portocarrero

2023

J. Mex. Chem. Soc.

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Single-particle electrochemistry has become an important area of research with the potential to determine the rules of electrochemical reactivity at the nanoscale. These techniques involve addressing one entity at the time, as opposed to the conventional electrochemical experiment where a large number of molecules interact with an electrode surface. These experiments have been made feasible through the utilization of ultramicroelectrode (UMEs), i.e., electrodes with at least one dimension, e.g., diameter of 30 μm or less. This paper provides a theoretical and practical introduction to single entity electrochemistry (SEE), with emphasis on collision experiments between suspended NPs and UMEs to introduce concepts and techniques that are used in several SEE experimental modes. We discuss the intrinsically small currents, below 1 nA, that result from the electroactive area of single entities in the nanometer scale. Individual nanoparticles can be detected using the difference in electrochemical reactivity between a substrate and a nanoparticle (NP). These experiments show steady-state behavior of single NPs that result in discrete current changes or steps. Likewise, the NP can have transient interactions with the substrate electrode that result in current blips. We review the effect of diffusion, the main mass transport process that limits NP/electrode interactions. Also, we pointed out the implications of aggregation and tunneling in the experiments. Finally, we provid a perspective on the possible applications of single-element electrochemistry of electrocatalyst. Resumen. La electroquímica de partículas individuales se ha convertido en un área importante de investigación con el potencial de facilitar la comprensión de las reglas de reactividad electroquímica en la escala de nanómetros. Estas técnicas implican abordar una entidad a la vez, en contraste con el experimento electroquímico convencional en el que un gran número de moléculas interactúa con la superficie de un electrodo. Estos experimentos se han vuelto posibles gracias al uso de ultramicroelectrodos (UME, por sus siglas en inglés), es decir, electrodos con al menos una dimensión, como, por ejemplo, el diámetro de 30 μm o menos. Este artículo proporciona una introducción teórica y práctica a la electroquímica de entidad única (SEE, por sus siglas en inglés), con énfasis en los experimentos de colisión entre nanopartículas (NPs) suspendidas y UME para introducir conceptos y técnicas utilizadas en varios modos experimentales de SEE. Discutimos las corrientes intrínsecamente pequeñas, por debajo de 1 nA, que resultan de la superficie electroactiva de entidades únicas en la escala de nanómetros. Las nanopartículas individuales pueden detectarse mediante la diferencia en reactividad electroquímica entre el sustrato y las nanopartículas. Estos experimentos muestran el comportamiento en estado estacionario de NPs individuales que resulta en cambios discretos de corriente o escalones. De manera similar, la NP puede tener interacciones transitorias con el electrodo de sustrato que dan lugar a picos de corriente. Revisamos el efecto de la difusión, el principal proceso de transporte de masa que limita las interacciones NP/electrodo. Además, señalamos las implicaciones de la agregación y del efecto túnel cuántico en los experimentos. Finalmente, ofrecemos una perspectiva sobre las posibles aplicaciones de la electroquímica de entidad única en electrocatálisis.

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“…[44,86,87] and nanoconfinement techniques (ultramicroelectrodes, nanoelectrodes, single NP collision, nanopores, nanochannels, etc.). [44,88,89] Besides the aforementioned techniques, an appealing technique for single NP analysis, especially for (electro-)catalysis is the Scanning Electrochemical Cell Microscopy (SECCM), which permits correlating structure/function in the nanoscale in situ/operando. [90][91][92] At last, we can also mention Scanning Tunneling Microscopy (STM), Atomic Force Microscopy (AFM), and High-resolution Transmission Electron Microscopy (HR-TEM), which can also provide nanoscale, or even atomic, resolution.…”

Section: Bcdi Of Shape-controlled Platinum Npsmentioning

confidence: 99%

Development of electrochemical cells for spatially resolved analysis using a multi-technique approach: from conventional experiments to X-ray nanoprobe beamlines

Vicente

Raju

Gomes

et al. 2023

Preprint

View full text Add to dashboard Cite

Real (electro-)catalysts are often heterogeneous, and their activity and selectivity depend on the properties of specific active sites. Therefore, unveiling the so-called structure-activity relationship is essential for a rational search for better materials and, consequently, for the development of the field of (electro-)catalysts. Thus, spatially resolved techniques are powerful tools as they allow us to characterize and/or measure the activity and selectivity of different regions of heterogeneous catalysts. To take full advantage of that, we have developed spectroelectrochemical cells (SEC) to perform spatially resolved analysis using X-ray nanoprobe synchrotron beamlines, and conventional pieces of equipment. Here, we describe the techniques available at the Carnaúba beamline at Sirius-LNLS storage ring, then we show how our SECs enable obtaining X-ray (XRF, XRD, XAS, etc.) and vibrational spectroscopy (FTIR and Raman) contrast images. Through some proof-of-concept experiments, we demonstrate how using a multi-technique approach could render a complete and detailed analysis of an (electro-)catalyst overall performance.

show abstract

Semiconducting Nanoparticles: Single Entity Electrochemistry and Photoelectrochemistry

Cited by 7 publications

References 63 publications

Development of Electrochemical Cells and Their Application for Spatially Resolved Analysis Using a Multitechnique Approach: From Conventional Experiments to X-Ray Nanoprobe Beamlines

Development of Electrochemical Cells and Their Application for Spatially Resolved Analysis Using a Multitechnique Approach: From Conventional Experiments to X-Ray Nanoprobe Beamlines

Why Measure Particle-by-Particle Electrochemistry? A Tutorial and Perspective

Development of electrochemical cells for spatially resolved analysis using a multi-technique approach: from conventional experiments to X-ray nanoprobe beamlines

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