Three-dimensional operando optical imaging of single particle and electrolyte heterogeneities inside Li-ion batteries

Pandya, Raj; Valzania, Lorenzo; Dorchies, Florian; Xia, Fei; Hugh, Jeffrey Mc; Mathieson, A. R.; Tan, Jien Hwee; Parton, Thomas G.; Volder, Michaël De; Tarascon, Jean‐Marie; Gigan, Sylvain; Aguiar, Hilton B. de; Grimaud, Alexis

doi:10.48550/arxiv.2207.13073

Cited by 5 publications

(10 citation statements)

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“…3D mapping is also possible through confocal imaging (under pseudo-steady-state electrochemical conditions), − illustrated recently from the 3D diffusion layer build-up during enzymatic reactions . The instruments are sufficiently mature to tackle the transport of active species in real energy storage or conversion systems, such as porous electrodes for electrolyzers or batteries − under operation.…”

Section: Optical Microscopies In Electrochemistrymentioning

confidence: 99%

“…These differences are discussed based on the difference in conductivities in each state of the particle, which is then manifested locally . The method was extended to imaging in the presence of the usual electrode components (polymer binder and carbon paste) and developed to enable 3D probing inside the particles using confocal visualization . Complemented with 2-photon fluorescence excitation, the local distribution of the LiPF 6 electrolyte could be imaged around the particles, revealing inhomogeneous electrolyte diffusion as a result of the geometry and porosity of the carbon/binder matrix surrounding the particles.…”

Section: Optical Microscopies In Electrochemistrymentioning

confidence: 99%

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The New Era of High-Throughput Nanoelectrochemistry

Valavanis

Ciocci

et al. 2023

Anal. Chem.

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Section: Optical Microscopies In Electrochemistrymentioning

confidence: 99%

Section: Optical Microscopies In Electrochemistrymentioning

confidence: 99%

The New Era of High-Throughput Nanoelectrochemistry

Valavanis

Ciocci

et al. 2023

Anal. Chem.

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“…3D mapping is also possible through confocal imaging (under pseudo steady-state electrochemical conditions) [378][379][380] , illustrated recently from the 3D diffusion layer build-up during enzymatic reactions. 381 The instruments are sufficiently mature to tackle the transport of active species in real energy storage or conversion systems, such as porous electrodes 382 for electrolysers or batteries [383][384][385] under operation.…”

Section: Probing Concentration Profilesmentioning

confidence: 99%

“…383 The method was extended to imaging in the presence of the usual electrode components (polymer binder and carbon paste) and developed to enable 3D probing inside the particles using confocal visualization. 385 Complemented with 2-photon fluorescence excitation, the local distribution of the LiPF6 electrolyte could be imaged around the particles, revealing inhomogeneous electrolyte diffusion as a result of the geometry and porosity of the carbon/binder matrix surrounding the particles.…”

Section: Probing Concentration Profilesmentioning

confidence: 99%

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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“…As such, we expect this approach will be a valuable label-free probe for ionic transport in a wide range of physical, chemical, and biological contexts, including product formation and collection in (photo)electrochemical energy conversion, , water splitting, phototriggered ion transport, ion transport in soft matter, aqueous battery function, dissolution dynamics after proper calibration of the refractive index near saturation, microfluidic ion flow, bioelectronic device function, or even label-free electrophysiology dynamics . It could also be readily combined with established strategies to optically detect oxygen and hydrogen evolution, especially since the sensitivity required to see gaseous products is orders of magnitude lesser than what we have demonstrated for solution-phase species, and to potentially probe three-dimensional ion transport in such contexts. , Second, the MSE analysis used here could serve as a general approach to reveal nondiffusive behavior or spatially dependent transport parameters. Specifically, similar to the case for carrier transport probed by spatiotemporal methods, , deviations from diffusive transport manifest as nonlinear MSE curves that would be readily discerned.…”

mentioning

confidence: 99%

Operando Label-Free Optical Imaging of Solution-Phase Ion Transport and Electrochemistry

et al. 2023

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Ion transport is a fundamental process in many physical, chemical, and biological phenomena, and especially in electrochemical energy conversion and storage. Despite its immense importance, demonstrations of label-free, spatially and temporally resolved ion imaging in the solution phase under operando conditions are not widespread. Here we spatiotemporally map ion concentration gradient evolution in solution and yield ion transport parameters by refining interferometric reflection microscopy, obviating the need for absorptive or fluorescent labels. As an example, we use an electrochemical cell with planar electrodes to drive concentration gradients in a ferricyanide-based aqueous redox electrolyte, and we observe the lateral spatiotemporal evolution of ions via concentration-dependent changes to the refractive index. Analysis of an evolving spatiotemporal ion distribution directly yields the diffusivity of the redox-active species. The simplicity of this approach makes it amenable to probing local ion transport behavior in a wide range of electrochemical, bioelectronic, and electrophysiological systems.

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Three-dimensional operando optical imaging of single particle and electrolyte heterogeneities inside Li-ion batteries

Cited by 5 publications

References 0 publications

The New Era of High-Throughput Nanoelectrochemistry

The New Era of High-Throughput Nanoelectrochemistry

The new era of high throughput nanoelectrochemistry

Operando Label-Free Optical Imaging of Solution-Phase Ion Transport and Electrochemistry

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