Combining Electrodeposition and Optical Microscopy for Probing Size‐Dependent Single‐Nanoparticle Electrochemistry

Lemineur, Jean‐François; Noël, Jean‐Marc; Ausserré, Dominique; Combellas, Catherine; Kanoufi, Frédéric

doi:10.1002/anie.201807003

Cited by 58 publications

(67 citation statements)

References 35 publications

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“…This OPT microscopy technique is thus sensitive to local refractive index variations and is able to image a broad range of nanomaterials, from dielectric to noble metal NPs. 48,52,53 Opto-electrochemical analyses are performed using the gold AR layer as a working electrode. Briefly, the homemade 3-electrode electrochemical cell, with a diameter of 300 µm, was machined in house from plastic and stuck onto the gold AR surface in order to host a drop of electrolytic solution.…”

Section: Opto-electrochemical Set-upmentioning

confidence: 99%

Optical monitoring of the electrochemical nucleation and growth of silver nanoparticles on electrode: From single to ensemble nanoparticles inspection

Lemineur

Noël

Combellas

et al. 2020

Journal of Electroanalytical Chemistry

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The electrochemical nucleation and growth of nanoparticles (NPs) on an electrode surface at a constant potential is traditionally followed by recording the resulting current density during the experiment. The obtained chronoamperometric transients are average measurements, making it difficult to separate individual NP behaviors and to study their cross-talks. Herein, the recently developed Backside Absorbing Layer Microscopy (BALM) is employed to monitor optically in situ and operando the electrodeposition of silver NPs. This latter technique exploits a pseudo-antireflective and metallic contrast layer and allows both subnanometer vertical and sub-micrometer spatial resolutions. The information from the recorded movies is readily exploited to study the NP electrodeposition at the single entity level. The image sequences allow quantifying the local electrodeposition of nanomaterials onto the electrode surface, probing the NP dynamics through the extraction of single optical NP growth transients, and analyzing the effect of the neighboring nuclei on the growth of individual NPs.

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Section: Opto-electrochemical Set-upmentioning

confidence: 99%

Optical monitoring of the electrochemical nucleation and growth of silver nanoparticles on electrode: From single to ensemble nanoparticles inspection

Lemineur

Noël

Combellas

et al. 2020

Journal of Electroanalytical Chemistry

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“…[31] Herein, we expand this technique to the w|IL one, where the Galvani potential difference across the interface, − IL = ∆ IL , is controlled by electrodes immersed in either phase, allowing control and quantification of charge transfer across the LLI. Transmission electron microscopy (TEM) and stochastic impacts were used to provide NC sizing, while optical microscopies (back absorbing layer, BALM [42,43], and darkfield [28,[44][45][46]) provided in situ visualisation of the reactivity of such NCs in solution. The latter have emerged as powerful techniques for imaging objects in situ below the diffraction limit of classical bright-field optical microscopies (<500nm) and have been used effectively for NP sizing as well as for monitoring the transport, electrochemical transformation or growth of NPs at nano/microelectrodes or pipettes [28,42,[47][48][49][50][51].…”

Section: Introductionmentioning

confidence: 99%

Single LiBH4 nanocrystal stochastic impacts at a micro water|ionic liquid interface

Stockmann

Lemineur

Liu

et al. 2019

Electrochimica Acta

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LiBH4 is often employed as a reducing agent for metal nanoparticle (NP) preparation but is inherently a solid-state H2 hydrogen storage agent. Herein it is shown, through a combination of electron/optical microscopies and single entity electrochemical study, that LiBH4 is stored in the solid state within an ionic liquid (IL) as nanocrystals (NCs). The electrochemical monitoring of an immiscible water|IL (w|IL) micro-liquid|liquid interface (LLI) shows interfacial charge exchange associated with the stochastic impacts of single NCs. Meanwhile, in situ optical monitoring of a w|metal or w|IL interface shows that such impacts are associated with the development of a H2-in-IL micro/nano-foam related to the poor solubility of H2. Both the presence of solid NCs and the latter H2-in-IL foam suggest that H2 release from LiBH4-in-IL is a slow, but likely controlled process. The rate of H2 production at a macroscopic LLI is further confirmed by gas chromatographic measurements, in very good agreement with microscopic observations. The electrochemical LLI provides unique investigative access to LiBH4 NCs and offers insight into H2 storage in ILs, or for direct borohydride fuel cells, as well as NP synthesis. Highlights:1. Single entity electrochemical detection of LiBH4 nanocrystals at a water|ionic liquid interface.2. Single H2 bubble generated from LiBH4 nanocrystals inside an ionic liquid.3. LiBH4 induced H2-in-ionic liquid foam at water|ionic liquid interface.

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“…This thickness depends on the nature of the top medium (air, water, other solvent) and is typically close to 7 nm of gold for the glass/gold/air system and of 2-3 nm of gold for the glass/gold/water one. This configuration allows many types of observations with exceptional contrast 25,26,28,29 in particular for 2D materials. 26 Most importantly, the reverse geometry provides a full half space available for different techniques so that BALM can be easily coupled with other techniques such as electrochemistry.…”

Section: Introductionmentioning

confidence: 99%

“…26 Most importantly, the reverse geometry provides a full half space available for different techniques so that BALM can be easily coupled with other techniques such as electrochemistry. 25,26,28,29 However, when implemented in this way (i.e. using a single few-nm thick metallic layer as ARA material), BALM can be further improved.…”

Section: Introductionmentioning

confidence: 99%

Ideal optical contrast for 2D material observation using bi-layer antireflection absorbing substrates

et al. 2019

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The capability to observe 2D materials with optical microscopy techniques is of central importance in the development of the field and is a driving force for the assembly and study of 2D material van der Waals heterostructures. Such observation of ultrathin materials usually benefits from antireflection conditions associated with the choice of particular substrate geometry. The most common configuration uses a transparent oxide layer with a thickness minimizing light reflection at the air/substrate interface when light travels from air to substrate. Backside Absorbing Layer Microscopy (BALM) is a newly proposed configuration in which light travels from glass to air (or another medium such as water or a solvent) and the antireflection layer is a light-absorbing material (typically a metal). We recently showed that this technique produces images of 2D materials with unprecedented contrast and can be ideally coupled to chemical and electrochemical experiments. Here, we show that contrast can be optimal using double-layer antireflection coatings. By following in situ and with sub-nm precision the controlled deposition of molecules, we notably establish precisely the ideal observation conditions for graphene oxide monolayers which represents one of the most challenging 2D material cases in terms of transparency and thickness. We also provide guidelines for the selection of antireflection coatings applicable to a large variety of nanomaterials. This work strengthens the potential of BALM as a generic, powerful and versatile technique for the study of molecular-scale materials and phenomena.

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Combining Electrodeposition and Optical Microscopy for Probing Size‐Dependent Single‐Nanoparticle Electrochemistry

Cited by 58 publications

References 35 publications

Optical monitoring of the electrochemical nucleation and growth of silver nanoparticles on electrode: From single to ensemble nanoparticles inspection

Optical monitoring of the electrochemical nucleation and growth of silver nanoparticles on electrode: From single to ensemble nanoparticles inspection

Single LiBH4 nanocrystal stochastic impacts at a micro water|ionic liquid interface

Ideal optical contrast for 2D material observation using bi-layer antireflection absorbing substrates

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