Macroscale and Nanoscale Photoelectrochemical Behavior of p-Type Si(111) Covered by a Single Layer of Graphene or Hexagonal Boron Nitride

Thompson, Annelise C.; Simpson, Burton H.; Lewis, Nathan S.

doi:10.1021/acsami.9b21134

Cited by 13 publications

(12 citation statements)

References 40 publications

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“…Benefiting from unique structures and electronic properties, two-dimensional (2D) materials, including transition metal dichalcogenides (TMDCs, e.g., WS2, MoS2 and WSe2), 229,[280][281][282][283][284] graphene and graphene derivatives, 223,285,286 hexagonal boron nitride (h-BN) etc., 287 have generated great interest in catalysis applications, especially in the area of photocatalysis and electrocatalysis. SECCM is ideally suited for studying the electrochemistry of such materials, as small flakes or regions of a 2D material can be targeted directly and the properties of those regions can be deduced by a range of co-located complementary techniques, e.g., Raman microscopy, AFM etc.…”

Section: Two-dimensional Materialsmentioning

confidence: 99%

“…Heterojunctions between 2D MoS2 and 3D Cu2O nanorods have also been probed. 302 2D materials can serve as coatings for semiconductor surfaces, and other work 287 examined p-Si/graphene and p-Si/h-BN interfaces. SECCM was used to determine the open-circuit voltage at the photoelectrodes, revealing the local electronic states of the material.…”

Section: Photoelectrochemistrymentioning

confidence: 99%

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The new era of high throughput nanoelectrochemistry

Valavanis

Ciocci

et al. 2022

Preprint

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Scanning electrochemical probe microscopies (SEPMs) have played a key role in advancing small-scale electrochemistry. SEPMs use an electrochemical probe (micro/nanoelectrode or pipet) to quantify and map local interfacial fluxes of electroactive species and have found increasingly wide applications. Our contribution to the Fundamental and Applied Reviews in Analytical Chemistry 2019 discussed how advances in SEPMs converged towards nanoscale electrochemical mapping. This inflection in experimental capability has opened up myriad opportunities for SEPMs in many types of systems, from material and energy sciences to the life sciences. The enhancement in the spatial resolution of imaging techniques, and instrumental developments, have resulted in significant increases in the size of electrochemical datasets from a typical experiment and served to speed up measurement throughput. Next generation nanoelectrochemistry will thus see an emphasis on “big data”, its analysis, storage and curation, high throughput analysis and parallelization, “intelligent” instruments and experiments, active control of nanoscale systems, and the integration of nanoelectrochemistry and nanoscale micro(spectro)scopy. For this review article, we focus on recent advances in frontier nanoscale electrochemistry, analysis and imaging techniques that are already addressing some of these key targets, and are well-placed to embrace other aspects in the near future. Our goal is to provide an overview of the present state-of-the-art in high throughput nanoelectrochemistry and imaging, and signpost promising new avenues for nanoscale electrochemical methods.

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Section: Two-dimensional Materialsmentioning

confidence: 99%

Section: Photoelectrochemistrymentioning

confidence: 99%

The new era of high throughput nanoelectrochemistry

Valavanis

Ciocci

et al. 2022

Preprint

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“…The topographical and electrochemical activity image acquisition is conducted through a programmed contact motion sequence between the meniscus droplet and the substrate electrode. , The most prominent advantage of SECCM is that it does not need to immerse the sample in solution, which completely avoids possible sample damage that could be caused by electrolyte and excludes any signal interference from the nonmeasured area . After more than 10 years of development, SECCM has been successfully applied to studies of two-dimensional semiconductor materials (such as WSe 2 ,, and MoS 2 − ), nanoparticles (NPs) ,− and nanoclusters, carbon-based materials, − energy storage materials, − and nanofabrication. − Recently, SECCM was used to probe single-entity electrochemistry nanoscopically, such as iridium oxide particles, Pt NPs , and Pt nanoclusters, Au nanorods, Au NPs , and Au (111) nanocrystals, single ZIF-derived nanocomposite particles, Sn deposited on reduced graphene oxide (rGO), and single-crystal boron-doped diamond particles . Although some works have demonstrated the capability of electrochemical activity imaging on the scale of less than 100 nm, most of them could not record in situ topography but only correlate with other ex situ approaches, such as SEM. , Hill et al presented state-of-the-art SECCM images that synchronously map topography and photoelectrochemical properties of p-type WSe 2 nanosheets with a probe ∼200 to 300 nm diameter.…”

mentioning

confidence: 99%

Topography Mapping with Scanning Electrochemical Cell Microscopy

Liu

Hao

et al. 2022

Anal. Chem.

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High-resolution scanning electrochemical cell microscopy (SECCM), synchronously visualizing the topography and electrochemical activity, could be used to directly correlate the structure and activity of materials nanoscopically. However, its topographical measurement is largely restricted by the size and stability of the meniscus droplet formed at the end of the nanopipette. In this paper, we report a scheme that could reliably gain several tens nanometer resolution (≥65 nm) of SECCM using homemade ∼50 nm inner diameter probes. Furthermore, the topography and hydrogen evolution reaction (HER) activity of ∼45 nm self-assembled Au nanoparticles monolayer were simultaneously recorded successfully. This scheme could make mapping of both topologic and chemical properties of samples in the nanometer regime with SECCM routinely, which potentially can largely expand the field of SECCM applications.

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“…An example from this class of QREs are polypyrrole (PPy) quasi-references (PPyQRE). A detailed investigation into these QREs was reported by Ghilane et al, and since then, the PPyQRE has been used in several electroanalytical measurements involving electrodeposition, scanning electrochemical microscopy, among others. − The poising reaction for such polypyrrole QREs is based on the doping reaction of PPy as shown in eq , with A – being the counterion …”

mentioning

confidence: 99%

Pt/Polypyrrole Quasi-References Revisited: Robustness and Application in Electrochemical Energy Storage Research

2021

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Choosing reference electrodes for nonaqueous electrochemical measurements, especially in energy storage research, is challenging due to lengthy experiments (>1 day), the lack of alternatives to the commonly used Ag/Ag + reference electrode (RE), the introduction of junction potentials, and the possibility of sample contamination. Often, quasi-reference electrodes (QREs) such as Ag wires and Li metal strips are used. However, small changes in electrolyte composition can cause large potential drifts, and their surfaces may be reactive to the solution. Here, we propose an alternative QRE based on polypyrrole electrodeposited on Pt wire (PPyQRE) encased in a glass tube with the open end sealed with commercial frits. While freestanding PPyQRE wires have been reported in the literature, simple encasing of the PPyQRE overcomes the above-mentioned drawbacks of QREs while providing a reliable reference potential that is closer to the performance of an RE. During cyclic voltammetric and bulk electrolysis testing of a redox mediator in solution, the encased PPyQRE exhibited stable reference potentials over multiple charge/discharge cycles with minimal drift (∼5 mV) after ∼2.25 days of operation. We also tested the reliability of our reference during the testing of multilayer graphene Li-ion anodes, which often involve cycling samples at highly reducing potentials (<−3 V vs Fc/Fc + ) over long durations (>1 day). In the same testing conditions, the Ag/Ag + electrode led to observable Ag deposits on the graphene and large potential drifts (∼50 mV), while the PPyQRE exhibited no measurable drift and revealed changes in voltammetric features that were obscured by reference drift when using Ag/Ag + . Minor reference drifts of ∼30 mV over long usage of the PPyQRE (∼2 months) can be addressed by calibration with a ferrocene couple at the end of experiments. These results highlight the advantages of using an encased PPyQRE as a simple and practical reference electrode for electrochemical measurements in the field of nonaqueous energy storage research.

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Macroscale and Nanoscale Photoelectrochemical Behavior of p-Type Si(111) Covered by a Single Layer of Graphene or Hexagonal Boron Nitride

Cited by 13 publications

References 40 publications

The new era of high throughput nanoelectrochemistry

The new era of high throughput nanoelectrochemistry

Topography Mapping with Scanning Electrochemical Cell Microscopy

Pt/Polypyrrole Quasi-References Revisited: Robustness and Application in Electrochemical Energy Storage Research

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