Three-Dimensional Visualization of Conductive Domains in Battery Electrodes with Contrast-Enhancing Nanoparticles

Morelly, Samantha L.; Gelb, Jeff; Iacoviello, Francesco; Shearing, Paul R.; Harris, Stephen J.; Alvarez, Nicolas J.; Tang, Maureen H.

doi:10.1021/acsaem.8b01184

Cited by 24 publications

(28 citation statements)

References 29 publications

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“…Although challenging, reports of successful mappings of the CBD are rising: Daemi et al demonstrated methods to directly characterise the CBD using lab-based X-ray nano-CT to estimate the ensemble tortuosity factor for LIB positive electrodes [67]; alternatively, Morelly et al have shown that the use of contrast-enhancing agents such as carbon-coated iron nanoparticles may also prove useful in resolving the CBD [68]; and, Müller et al have shown that the detachment of the CBD from the active material can be visualised and quantified in order to examine such phenomena with cycling [69].…”

Section: X-ray Characterisation Of Libsmentioning

confidence: 99%

Developments in X-ray tomography characterization for electrochemical devices

et al. 2019

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Over the last century, X-ray imaging instruments and their accompanying tomographic reconstruction algorithms have developed considerably. With improved tomogram quality and resolution, voxel sizes down to tens of nanometres can now be achieved. Moreover, recent advancements in readily accessible lab-based X-ray computed tomography (X-ray CT) instruments have produced spatial resolutions comparable to specialist synchrotron facilities. Electrochemical energy conversion devices, such as fuel cells and batteries, have inherently complex electrode microstructures to achieve competitive power delivery for consideration as replacements for conventional sources. With resolution capabilities spanning tens of microns to tens of nanometres, X-ray CT has become widely employed in the three-dimensional (3D) characterisation of electrochemical materials. The ability to perform multiscale imaging has enabled characterisation from system-down to particle-level, with the ability to resolve critical features within device microstructures. X-ray characterisation presents a favourable alternative to other 3D methods such as focused ion beam scanning electron microscopy, due to its non-destructive nature, which allows four-dimensional (4D) studies, three spatial dimensions plus time, linking structural dynamics to device performance and lifetime. X-ray CT has accelerated research from fundamental understanding of the links between cell structure and performance, to the improvement in manufacturing and scale-up of full electrochemical cells. Furthermore, this has aided in the mitigation of degradation and celllevel failures such as thermal runaway. This review presents recent developments in the use of X-ray CT as a characterisation method and its role in the advancement of electrochemical materials engineering.

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Section: X-ray Characterisation Of Libsmentioning

confidence: 99%

Developments in X-ray tomography characterization for electrochemical devices

et al. 2019

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“…Recent experiments have indicated that carbon black nanoparticles and polymeric binder aggregate during electrode manufacturing into a nanoporous carbon binder domain (CBD) phase with a typical length scale of 100nm. [8][9][10][11] The industrial battery manufacturing process involves mixing AM particles, carbon black nanoparticles, and polymeric binder into a nonaqueous solvent (such as N-methyl pyrrolidone) to form a slurry, which is then coated onto a current collector, dried to remove the solvent, and calendered into high density electrodes, which are eventually filled with a liquid electrolyte. 12 The slurry-based manufacturing process is low-cost and highly scalable; as a result, it is the method of choice for large-scale industrial battery manufacturing.…”

Section: Introductionmentioning

confidence: 99%

Controlling Binder Adhesion to Impact Electrode Mesostructures and Transport

Srivastava

Bolintineanu

Lechman

et al. 2020

ACS Appl. Mater. Interfaces

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The complex three-phase composition of lithium-ion battery electrodes-containing an ion-conducting pore phase, a nanoporous electron-conducting carbon binder domain (CBD) phase, and an active material (AM) phase-provides several avenues of mesostructural engineering to enhance battery performance. We demonstrate a promising strategy for engineering electrode mesostructures by controlling the strength of adhesion between the AM and CBD phases. Using high-fidelity, physics-based colloidal and granular dynamics simulations, we predict that this strategy can provide significant control over electrochemical transport-relevant properties such as ionic conductivity, electronic conductivity, and available AM surface area. Importantly, the proposed strategy could be experimentally realized through surface functionalization of the AM and CBD phases and would be compatible with traditional electrode manufacturing methods.

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“…Typically, 3D structures where the active particles, the conductive additives, binder, and the pore-space are present are investigated using correlative measurement techniques, [13,14] computer-generated material phases, [15] or (partial) substitution of the low-contrast carbonblack binder domain with more detectable substances. [16,17] Indeed, the high-resolution 3D reconstructions of battery electrodes typically suffer from one of two drawbacks: either (1) individual particles are recorded without the surrounding electrode structure, [18] or (2) the pore space of the sample is infilled with epoxy during sample preparation, which may destroy the fine features. [19,20] Here, we show how these challenges can be overcome with advanced sample preparation and multimodal imaging.…”

Section: Introductionmentioning

confidence: 99%

Multimodal Nanoscale Tomographic Imaging for Battery Electrodes

Müller

Lippuner

Verezhak

et al. 2020

Advanced Energy Materials

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Accurate representations of the 3D structure within a lithium-ion battery are key to understanding performance limitations. However, obtaining exact reconstructions of electrodes, where the active particles, the carbon black and polymeric binder domain, and the pore space are visualized is challenging. Here, we show that multi-modal imaging can be used to overcome this challenge. We combine high-resolution ptychographic x-ray computed tomography with lower resolution but higher contrast transmission x-ray tomographic microscopy to obtain 3D reconstructions of pristine and cycled graphite-silicon composite electrodes. This cross-correlation enables quantitative analysis of the surface of active particles, including the heterogeneity of carbon-black and binder domain and solid-electrolyte interphase coverage. Capturing the active particles as well as the carbon-black binder domain allows using these segmented structures for electrochemical simulations to highlight the influence of the particle embedding on local state of charge heterogeneities.

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Three-Dimensional Visualization of Conductive Domains in Battery Electrodes with Contrast-Enhancing Nanoparticles

Cited by 24 publications

References 29 publications

Developments in X-ray tomography characterization for electrochemical devices

Developments in X-ray tomography characterization for electrochemical devices

Controlling Binder Adhesion to Impact Electrode Mesostructures and Transport

Multimodal Nanoscale Tomographic Imaging for Battery Electrodes

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