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Review
. 2024 Apr 26;6(23):14124-14132.
doi: 10.1021/acsapm.4c00473. eCollection 2024 Dec 13.

In Situ Hybrid Solid-State Electrolytes for Lithium Battery Applications

Natalia Stankiewicz  1 , Miryam Criado-Gonzalez  1 , Jorge L Olmedo-Martínez  1 , Eider Matxinandiarena  1 , Pedro López-Aranguren  2 , Francisco Bonilla  2 , Grazia Accardo  2 , Damien Saurel  2 , Didier Devaux  3 , Irune Villaluenga  1   4
Affiliations
Review

In Situ Hybrid Solid-State Electrolytes for Lithium Battery Applications

Natalia Stankiewicz et al. ACS Appl Polym Mater. .

Abstract

The translation of inorganic-polymer hybrid battery materials from laboratory-scale to industry-relevant battery manufacturing processes is difficult due to their complexity, scalability, and cost and the limited fundamental knowledge that is available. Herein, we introduce a unique and compelling approach for the preparation of hybrid solid electrolytes based on an in situ synthesized halide electrolyte (Li3InCl6) in the presence of a non-conducting polymer (styrene-ethylene-butylene-styrene block copolymer). This innovative in situ approach delivers flexible self-standing membranes with good ionic conductivity (0.7 × 10-4 S/cm at 30 °C) and low activation energy (0.25 eV). This study suggests that the total conductivity is dominated by the inorganic-polymer interfaces and the microstructure of the hybrids affects the energy barriers to ion transport. This work opens a promising sustainable and cost-efficient route that can be easily implemented in current battery manufacturing lines.

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Conflict of interest statement

The authors declare the following competing financial interest(s): The authors declare a provisional patent application (EP23306871.7) owned by the Basque Center for Macromolecular Design and Engineering, POLYMAT Fundazioa, UPV/EHU, Institut Polytechnique de Grenoble, Universite Grenoble Alpes, Centre National de la Recherche Scientifique, and Universite Savoie Mont Blanc that discloses the in situ approach to obtaining hybrid electrolytes.

Figures

Figure 1
Figure 1
(a) Schematic presentation of two approaches [in situ synthesis and conventional physical mixture (blend)] for HSEs preparation and (b) ionic conductivity of the blend HSE as a function of the processing temperature.
Figure 2
Figure 2
(a) XRD patterns for SEBS, pure LIC, blend HSE, and in situ HSE. The collected data are shown as colored circles, the results of the refinement are given as black solid lines, the vertical green bars show the Bragg peaks’ positions for the refined phase C12/m1, and the differences between the data and refinement results are shown as blue solid lines. Inset: χ2 values for the refinements. (b) 1H NMR spectra for pure SEBS, blend HSE, and in situ HSE.
Figure 3
Figure 3
(a) TGA curves, (b) DSC thermograms, (c) HRR diagram of the microcalorimetry tests for SEBS, LIC, blend HSE, and in situ HSE, and (d) pHRR and THR values of SEBS, blend HSE, and in situ HSE.
Figure 4
Figure 4
(a) SAXS profiles at RT of the SEBS block copolymer and blend and in situ HSEs. Cross-sectional SEM images of (b) blend and (c) in situ HSEs. Clusters of inorganic particles are indicated by arrows.
Figure 5
Figure 5
Top-view SEM images of (a) blend and (e) in situ HSEs and EDX mappings for (b and f) C, (c and g) Cl, and (d and h) In for blend and in situ HSEs, respectively. Scale bars: 5 μm.
Figure 6
Figure 6
(a) Nyquist plot for HSEs at 50 °C (inset: equivalent circuit used for the fittings), (b) ionic conductivity as a function of the temperature for LIC at 360 MPa (blue ▲), LIC at 150 MPa (light-blue ▼), blend HSE at 150 MPa (■), and in situ HSE at 150 MPa (purple ●).
Figure 7
Figure 7
σn plotted against the temperature for HSEs.
Figure 8
Figure 8
(a) G′ and G″ moduli as a function of ω at 40 °C and (b) oscillation stress dependence on G′ and G′′ at 40 °C for HSEs.
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