Airtight container for the transfer of atmosphere-sensitive materials into vacuum-operated characterization instruments

Gaumé, Romain; Joubert, Lydia‐Marie

doi:10.1063/1.3669784

Cited by 8 publications

(4 citation statements)

References 19 publications

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“…Samples were transferred directly from an argon filled glove box without any air exposure by means of a homemade transfer chamber following the procedure described by Gaume et al 18 The SEI formed on Na and Li metal anodes was analyzed by IR spectroscopy on a Vertex 70 FT-IR Spectrometer using a praying mantis diffuse reflectance accessory (HARRICK) in order to prevent any air exposure.…”

Section: Methodsmentioning

confidence: 99%

On the Comparative Stability of Li and Na Metal Anode Interfaces in Conventional Alkyl Carbonate Electrolytes

Iermakova

Dugas

Palacín

et al. 2015

J. Electrochem. Soc.

268

275

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A comparative study of the electrode/electrolyte interface was carried out for lithium and sodium metal anodes in electrolytes consisting in 1 M LiPF 6 in EC 0.5 :DMC 0.5 (LP30) and 1 M NaPF 6 in both EC 0.5 :DMC 0.5 and EC 0.45 PC 0.45 DMC 0.1 . Symmetric Li/Li cells exhibited low polarization and smooth charge discharge curves with current densities of 0.1 and 1 mA/cm 2 . In contrast, large overpotentials were observed even at 0.1 mA/cm 2 for Na/Na cells. Such differences cannot be related to ionic conductivity of the electrolytes but are rather due to an enhanced interfacial resistance (R ct + R SEI ) as deduced from impedance measurements. The composition of the SEI layer was investigated by FTIR and found to be stable for Li electrodes but to evolve upon cycling for Na electrodes which is also in agreement with differences in surface morphology detected by SEM. A lower stability (partial solubility) of the SEI would also enable to understand the differences in the impedance of identical hard carbon (HC) electrodes in cells with either Li or Na counterelectrodes. These results cast some concerns on the reliability of the so termed half cell characterization and call for caution when interpreting the results of potential electrode materials for sodium ion batteries. The use of metallic anodes has attracted large attention in the battery field due to their high capacity and low operation potential. Nonetheless, almost all commercialized technologies are either primary cell (e.g. alkaline Zn/MnO 2 ), operating through chemical reaction mechanisms (e.g. Ni/Cd in which Cd oxidizes to Cd(OH) 2 , using liquid metal anodes (Na/S cells) or polymer 1 electrolytes, thus avoiding many of the problems of metal reversible plating/stripping in liquid electrolytes. Indeed, the formation of metal dendrites upon cycling was early identified as bottleneck for the development of safe Li metal anode batteries which lead to the commercialization of Li-ion batteries (LIB) to the expense of a severe penalty in energy density. Even so, lithium metal anodes are widely used as counter (or also reference) electrodes in the so termed half cell tests, performed mostly at laboratory scale within the battery research community. These are mostly intended to assess the electrochemical performance of a given compound as either positive or negative electrode material for LIB in a simple way, avoiding the assembly of full cells in which electrode balancing can severely affect performance. Their outcomes are typically the electrochemical capacity and operation potential values at different rates. The reliability of extrapolating such half cell testing results to potential performance in full cells relies on the stability of the Solid Electrolyte Interphase (SEI) typically formed on the surface of lithium metal anodes as a result of electrolyte degradation reactions. 2The development of a room temperature sodium (solid) metal anode battery technology, using conventional liquid electrolytes does not seem to have been seriously considered in the pa...

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Section: Methodsmentioning

confidence: 99%

On the Comparative Stability of Li and Na Metal Anode Interfaces in Conventional Alkyl Carbonate Electrolytes

Iermakova

Dugas

Palacín

et al. 2015

J. Electrochem. Soc.

268

275

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“…Thus, an airtight container similar to the one used in Ref. [42] was used to transfer the sensitive samples from the argon atmosphere in the glovebox into the SEM. The transfer container was made up from an aluminum base with a cover, separated by a sealing ring and a latex rubber membrane (Figure S21).…”

Section: Morphological Characterizationsmentioning

confidence: 99%

Thermal Structural Behavior of ElectrochemicallyLithiated Graphite (Li_xC₆) Anodes in Li‐ion Batteries

Hölderle,

Monchak,

Baran

et al. 2024

Batteries & Supercaps

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A full series of variously lithiated graphite anodes material LixC6 (0<x<1) corresponding to a different state‐of‐charge (SOC) between 0% and 100% was collected from 18650‐type cylinder Li‐ion batteries, and the thermal structural behavior of these electrodes was mapped using ex situ high‐resolution X‐ray and neutron diffraction. Their structural behavior was analyzed over a broad temperature range. At high temperatures, a non‐reversible decomposition of the lithiated graphite anodes takes place, accompanied by a loss of intercalated lithium ions, forming novel phases such as LiF and Li2O strongly coupled to the degradation of the solid electrolyte interface (SEI). Complementary calorimetric measurements showed the strongly exothermic chemical reactions during the decomposition matching well to the collected diffraction data. Post mortem analysis applying scanning electron microscopy revealed various morphological features supplementing the treatment of battery anodes and highlighted the importance of the SEI layer during the cycling of the cell and its thermal degradation.

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“…4. Evaluation of devices, where control of chamber pressure coupled with non-conductive EM imaging, enables atmosphere sensitive surfaces to be visualized [6]. We inserted atmosphere sensitive ceramics (SrI 2 ) into an airtight chamber covered by a latex membrane that, upon inflation under lower pressure, was pierced by a needle, thereby exposing the surface to the electron beam for imaging without the need for sputter-coating of sample surface (Fig.3).…”

mentioning

confidence: 99%

Variable-Pressure Scanning Electron Microscopy: Dark Horse of SEM imaging

Joubert

2012

Microsc Microanal

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Airtight container for the transfer of atmosphere-sensitive materials into vacuum-operated characterization instruments

Cited by 8 publications

References 19 publications

On the Comparative Stability of Li and Na Metal Anode Interfaces in Conventional Alkyl Carbonate Electrolytes

On the Comparative Stability of Li and Na Metal Anode Interfaces in Conventional Alkyl Carbonate Electrolytes

Thermal Structural Behavior of ElectrochemicallyLithiated Graphite (Li_xC₆) Anodes in Li‐ion Batteries

Variable-Pressure Scanning Electron Microscopy: Dark Horse of SEM imaging

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Airtight container for the transfer of atmosphere-sensitive materials into vacuum-operated characterization instruments

Cited by 8 publications

References 19 publications

On the Comparative Stability of Li and Na Metal Anode Interfaces in Conventional Alkyl Carbonate Electrolytes

On the Comparative Stability of Li and Na Metal Anode Interfaces in Conventional Alkyl Carbonate Electrolytes

Thermal Structural Behavior of ElectrochemicallyLithiated Graphite (LixC6) Anodes in Li‐ion Batteries

Variable-Pressure Scanning Electron Microscopy: Dark Horse of SEM imaging

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Product

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Thermal Structural Behavior of ElectrochemicallyLithiated Graphite (Li_xC₆) Anodes in Li‐ion Batteries