Imaging of a Thin Oxide Film Formation from the Combination of Surface Reflectivity and Electrochemical Methods

Chakri, Sara; Patel, Anisha N.; Frateur, Isabelle; Kanoufi, Frédéric; Sutter, Éliane; Tran, Mai T.T.; Tribollet, Bernard; Vivier, Vincent

doi:10.1021/acs.analchem.6b04921

Cited by 32 publications

(53 citation statements)

References 50 publications

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“…The capacitance of the oxide film can be extracted from the impedance data by using the complexcapacitance representation [58,59] and then, the oxide film thickness can be calculated. It was shown that this methodology allows an easy determination of the oxide film thickness that agrees well with the results obtained with other techniques, such as XPS [38] or reflectometry [41]. A similar methodology has been recently used to investigate the stability of the oxides film formed on a Mg alloy containing rare-earth elements [42].…”

Section: Interfacial Capacitance: Graphical Analysis and Power-law Modelsupporting

confidence: 70%

On the corrosion mechanism of Mg investigated by electrochemical impedance spectroscopy

Gomes

Costa

Pébère

et al. 2019

Electrochimica Acta

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196

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This work reported a detailed analysis of the electrochemical impedance spectra obtained for the Mg electrode during immersion in a sodium sulfate solution. A model was proposed which took into account the presence of: (i) a thin oxide film (MgO) which progressively covered the Mg electrode surface, (ii) film-free areas where the Mg dissolution occurs in two consecutive steps, (iii) a thick layer of corrosion products (Mg(OH) 2), (iv) an adsorbed intermediate ðMg þ ads Þ which is responsible for the chemical reaction allowing the negative difference effect to be explained. From the impedance data analysis, various parameters were extracted such as the thin oxide film thickness, the resistivity at the metal/oxide film interface and at the oxide film/electrolyte interface, the active surface area as a function of the exposure time to the electrolyte, the thickness of the thick Mg(OH) 2 layer and the kinetic constants of the electrochemical reaction.

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Section: Interfacial Capacitance: Graphical Analysis and Power-law Modelsupporting

confidence: 70%

On the corrosion mechanism of Mg investigated by electrochemical impedance spectroscopy

Gomes

Costa

Pébère

et al. 2019

Electrochimica Acta

Self Cite

196

View full text Add to dashboard Cite

show abstract

“…Comparing the signal recorded at each pixel I(x,y,t) to that recorded on the first image I(x,y,t = 0) allows monitoring of the local relative variation in reflectivity, ∆R(x,y,t)/R, from, Under the λ = 490 nm blue light illumination used herein, an ideal reflecting Au substrate ( ñ M . = 1.1 + 1.83i) immersed in water (n A = 1.33) is expected to reflect toward the CCD camera 37% of the incident light, and our setup was shown to detect local variation of reflectivity down to ∆R/R = 0.002 [16][17][18], meaning variation in collected signal down to 0.2%.…”

Section: Principle Of the Reflectivity Measurementmentioning

confidence: 80%

“…As a perspective of this work, reflectance microscopy is a simple yet powerful tool that has allowed monitoring electrochemical processes [15][16][17][18]63]. It does not require a transparent electrode unlike methods relying on darkfield illuminations, it is not restricted to Au electrodes, but to many reflecting surfaces [18], and can be performed at standard glass-insulated microelectrodes [16], or be coupled to local probing such as STM [63]. Based on these reported results, we expect that the technique could be applied to imaging the electrochemical reactivity of a wide range of NPs at the single entity level.…”

Section: Resultsmentioning

confidence: 99%

“…The detection of individual NPs freely moving in solution or adsorbed on an Au-coated Si wafer (Aldrich) was investigated in real time by light reflectivity microscopy. It was performed, as previously described [16][17][18], with an in-house developed setup consisting of a standard microscope (Olympus) equipped with a water-immersion objective (Olympus LUMP-LFLN 40XW, 40 ×, NA 0.8), and a CCD camera (Photon-Focus MV-D1024E-160-CL). A light halogen source, filtered at 490 nm with an interference filter (spectral bandwidth of 20 nm), was used to illuminate, from the top solution and via the objective, the Au substrate.…”

Section: Methodsmentioning

confidence: 99%

“…Simpler and yet quantitative strategies consist in analyzing images collected by a standard microscope operating in the reflection mode. Indeed, our group showed that the analysis of the light reflected by a reflecting surface illuminated under normal incidence [16][17][18], allowed quantifying and mapping heterogeneous electrochemical processes with sub-monolayer formation or deposition sensitivity. Particularly, we demonstrated the versatility of the strategy to the in situ imaging, using water-immersion objectives, of various electrode systems such as microfabricated Au-coated Si wafer [17], the standard glass-shielded microelectrodes [16], or various electrode materials, such as iron [18], for operando corrosion studies.…”

Section: Introductionmentioning

confidence: 99%

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Optical Nanoimpacts of Dielectric and Metallic Nanoparticles on Gold Surface by Reflectance Microscopy: Adsorption or Bouncing?

et al. 2019

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Optical modeling coupled to experiments show that a microscope operating in reflection mode allows imaging, through solutions or even a microfluidic cover, various kinds of nanoparticles, NPs, over a (reflecting) sensing surface, here a gold (Au) surface. Optical modeling suggests that this configuration enables the interferometric imaging of single NPs which can be characterized individually from local change in the surface reflectivity. The interferometric detection improves the optical limit of detection compared to classical configurations exploiting only the light scattered by the NPs. The method is then tested experimentally, to monitor in situ and in real time, the collision of single Brownian NPs, or optical nanoimpacts, with an Au-sensing surface. First, mimicking a microfluidic biosensor platform, the capture of 300 nm FeOx maghemite NPs from a convective flow by a surface-functionalized Au surface is dynamically monitored. Then, the adsorption or bouncing of individual dielectric (100 nm polystyrene) or metallic (40 and 60 nm silver) NPs is observed directly through the solution. The influence of the electrolyte on the ability of NPs to repetitively bounce or irreversibly adsorb onto the Au surface is evidenced. Exploiting such visualization mode of single-NP optical nanoimpacts is insightful for comprehending single-NP electrochemical studies relying on NP collision on an electrode (electrochemical nanoimpacts).

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Electrochemistry and Optical Microscopy

Kanoufi

2021

Encyclopedia of Electrochemistry

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Electrochemistry exploits local current heterogeneities at various scales ranging from the micrometer to the nanometer. The last decade has witnessed unprecedented progress in the development of a wide range of electroanalytical techniques allowing to reveal and quantify such heterogeneity through multiscale and multifonctionnal operando probing of electrochemical processes. However most of these advanced electrochemical imaging techniques, employing scanning probes, suffer from either low imaging throughput or limited imaging size. In parallel, optical microscopies, which can image a wide field of view in a single snapshot, have made considerable progress in terms of sensitivity, resolution and implementation of detection modes. Optical microscopies are then mature enough to propose, with basic bench equipment, to probe in a non destructive way a wide range of optical (and therefore structural) properties of a material in situ, in real time: under operating conditions. They offer promising alternative strategies for quantitative high-resolution imaging of electrochemistry. The first sections recall the optical properties of materials and how they can be probed optically. They discuss fluorescence, Raman, surface plasmon resonance, scattering or refractive index. Then the different optical microscopes used to image electrochemical processes are examined along with some strategies to extract quantitative electrochemical information from optical images. Finally the last section reviews some examples of in situ imaging, at micro-to nanometer resolution, and quantification of electrochemical processes ranging from solution diffusion to the conversion of molecular interfaces or solids.]

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Imaging of a Thin Oxide Film Formation from the Combination of Surface Reflectivity and Electrochemical Methods

Cited by 32 publications

References 50 publications

On the corrosion mechanism of Mg investigated by electrochemical impedance spectroscopy

On the corrosion mechanism of Mg investigated by electrochemical impedance spectroscopy

Optical Nanoimpacts of Dielectric and Metallic Nanoparticles on Gold Surface by Reflectance Microscopy: Adsorption or Bouncing?

Electrochemistry and Optical Microscopy

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