Visualizing the morphological and compositional evolution of the interface of InLi-anode|thio-LISION electrolyte in an all-solid-state Li–S cell by <i>in operando</i> synchrotron X-ray tomography and energy dispersive diffraction

Sun, Fu; Dong, Kang; Osenberg, Markus; Hilger, André; Risse, Sebastian; Lü, Yan; Kamm, Paul H.; Klaus, Manuela; Markötter, Henning; García‐Moreno, Francisco; Arlt, Tobias; Manke, Ingo

doi:10.1039/c8ta08821g

Cited by 53 publications

(37 citation statements)

References 41 publications

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“…Figure 1b shows a photographic picture of the beamline setup, while a scheme of it is reported in Figure 1c. [ 29–31 ] Figure S1a in the Supporting Information compares the Al/NG cells voltage profiles obtained using our conventional [ 20,23,24,32 ] and the operando cell setup, showing a good overlap of the curves, thus indicating the validity of the employed configuration. Figure S1b in the Supporting Information demonstrates the long‐term cycling performance of the Al/NG cell obtained using the operando cell setup, evidencing excellent stability for the 50 cycles of the test, i.e., for almost 10 days.…”

Section: Resultsmentioning

confidence: 89%

“…Additionally, the proposed experimental setup can be of interest to investigate other battery technologies, including lithium, sodium, or potassium ion, as shown recently in the literature. [ 31 ]…”

Section: Discussionmentioning

confidence: 99%

“…Each complete measurement took around 90 s. Figure 1b in the Supporting Information shows a photographic picture of the beamline setup, while a schematic is reported in Figure 1c in the Supporting Information. [29][30][31] Strain Evaluation: In order to decouple the contribution of the crystallite size and the inhomogenous strain effect on the ED-XRD peak broadening, the WH plot [55] was used in the reciprocal space for different stages. A Gaussian peak profile was assumed to obtain the WH plot in order to deconvolute the strain contribution from the size one.…”

Section: Methodsmentioning

confidence: 99%

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Simultaneous X‐Ray Diffraction and Tomography Operando Investigation of Aluminum/Graphite Batteries

Elia

Greco

Kamm

et al. 2020

Adv Funct Materials

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Rechargeable graphite dual-ion batteries are extremely appealing for grid-level stationary storage of electricity, thanks to the low-cost and high-performance metrics, such as high-power density, energy efficiency, long cycling life, and good energy density. An in-depth understanding of the anion intercalation mechanism in graphite is fundamental for the design of highly efficient systems. In this work, a comparison is presented between pyrolytic (PG) and natural (NG) graphite as positive electrode materials in rechargeable aluminum batteries, employing an ionic liquid electrolyte. The two systems are characterized by operando synchrotron energy-dispersive X-ray diffraction and time-resolved computed tomography simultaneously, establishing a powerful characterization methodology, which can also be applied more in general to carbon-based energy-related materials. A more in-depth insight into the AlCl 4 − /graphite intercalation mechanism is obtained, evidencing a mixed-staged region in the initial phase and a two-staged region in the second phase. Moreover, strain analysis suggests a correlation between the irreversibility of the PG electrode and the increase of the inhomogenous strain. Finally, the imaging analysis reveals the influence of graphite morphology in the electrode volume expansion upon cycling.

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Section: Resultsmentioning

confidence: 89%

Section: Discussionmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

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Simultaneous X‐Ray Diffraction and Tomography Operando Investigation of Aluminum/Graphite Batteries

Elia

Greco

Kamm

et al. 2020

Adv Funct Materials

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“…Time-resolved tomography for in situ analyses in materials science has become very popular 35–40 . Systems such as rechargeable batteries 41 , solidifying alloys 15,34,42,43 or evolving metallic foams 35,44–46 are of special interest. Time-resolved radioscopy for very short exposure times (down to 100 ps per image) and 1 Mfps repetition rate is possible 47 , but acquisition is limited to very short periods, thus not allowing to follow longer processes continuously.…”

Section: Methodsmentioning

confidence: 99%

Using X-ray tomoscopy to explore the dynamics of foaming metal

et al. 2019

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The complex flow of liquid metal in evolving metallic foams is still poorly understood due to difficulties in studying hot and opaque systems. We apply X-ray tomoscopy –the continuous acquisition of tomographic (3D) images– to clarify key dynamic phenomena in liquid aluminium foam such as nucleation and growth, bubble rearrangements, liquid retraction, coalescence and the rupture of films. Each phenomenon takes place on a typical timescale which we cover by obtaining 208 full tomograms per second over a period of up to one minute. An additional data processing algorithm provides information on the 1 ms scale. Here we show that bubble coalescence is not only caused by gravity-induced drainage, as experiments under weightlessness show, and by stresses caused by foam growth, but also by local pressure peaks caused by the blowing agent. Moreover, details of foam expansion and phenomena such as rupture cascades and film thinning before rupture are quantified. These findings allow us to propose a way to obtain foams with smaller and more equally sized bubbles.

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“…While the mechanisms of crack formation are material-dependent, they have generally been attributed to either lithium dendrite propagation through voids and defects in the SE or to volumetric changes at the electrode/electrolyte interphase due to the electrochemical decomposition of the electrolyte. [21][22][23][24] Regardless of the mechanism, the progressive mechanical failure of SE pellets with cycling results in a sharp decrease in ionic conductivity and allows the facile growth of lithium dendrites through the crack network resulting in subsequent cell shorting. [8] One approach to address the (electro)chemical instabilities of SEs is the application of a coating or interlayer to the SE surface, thereby protecting the electrolyte from the extreme potentials of the electrodes.…”

Section: Introductionmentioning

confidence: 99%

Direct Observation of Interfacial Mechanical Failure in Thiophosphate Solid Electrolytes with Operando X‐Ray Tomography

Madsen

Bassett

et al. 2020

Adv Materials Inter

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at larger scales (electric vehicle or gridscale energy storage) has been hampered by insufficient energy densities, prohibitive material costs, and safety concerns. [2] While significant progress has been made in the development of high energy density battery materials, the implementation of these materials in practical systems without sacrificing cell longevity or safety remains a pressing scientific challenge. One of the best studied approaches to improve the energy density of LIBs is to replace existing graphitic anodes (372 mA h g −1 capacity) with metallic lithium (3860 mA h g −1 capacity). [3] Unfortunately, uneven lithium plating and stripping in conventional organic liquid electrolytes promotes the growth of lithium dendrites, accelerating the formation of internal short-circuits. Additionally, the low thermal stability of electrolyte solvents (often mixtures of cyclic and linear carbonates) incurs exothermic decomposition of the electrolyte in the event of cell failure, often resulting in catastrophic thermal runaway. [4-6] While many approaches have been explored to address these issues, one of the most promising options is the elimination of the liquid electrolyte in favor of a solid electrolyte. [7] Transitioning from conventional liquid electrolytes to Li +conducting solid electrolytes (SEs) presents two primary advantages. The high mechanical rigidity of inorganic SEs may act to suppress the formation of dendrites at lithium anodes, reducing the possibility of internal short circuits. [8] Additionally, the negligible flammability of most SEs dramatically lowers the risk of uncontrolled thermal runaway in the event of cell failure. [9,10] These potential benefits motivate the search for materials with sufficiently high ionic conductivities to serve as replacements for their liquid counterparts. Among the known SE formulations, the thiophosphate class of superionic conductors exhibit exceptionally fast lithium transport at room temperature. [11] Specifically, Li 10 GeP 2 S 12 (LGPS) demonstrates an ionic conductivity of ≈10 mS cm −1 , comparable to conductivities achievable in conventional liquid electrolytes. [12] Despite the favorable ionic conductivity of LGPS, its poor chemical and electrochemical stabilities remain key challenges for practical application. The narrow window of electrochemical stability of LGPS and many other thiophosphate

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Visualizing the morphological and compositional evolution of the interface of InLi-anode|thio-LISION electrolyte in an all-solid-state Li–S cell by in operando synchrotron X-ray tomography and energy dispersive diffraction

Abstract: The interfacial evolution in ASSLSB is reported.

Cited by 53 publications

References 41 publications

Simultaneous X‐Ray Diffraction and Tomography Operando Investigation of Aluminum/Graphite Batteries

Simultaneous X‐Ray Diffraction and Tomography Operando Investigation of Aluminum/Graphite Batteries

Using X-ray tomoscopy to explore the dynamics of foaming metal

Direct Observation of Interfacial Mechanical Failure in Thiophosphate Solid Electrolytes with Operando X‐Ray Tomography

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