Scalable fabrication of nanostructured tin-oxide anodes for high

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Cite This: ACS Appl. Mater. Interfaces 2018, 10, 27019−27029

Scalable Fabrication of Nanostructured Tin Oxide Anodes for HighEnergy Lithium-Ion Batteries Christian Heubner,*,† Tobias Liebmann,‡ Karsten Voigt,‡ Mathias Weiser,‡ Björn Matthey,‡ Nils Junker,† Christoph Lämmel,‡ Michael Schneider,‡ and Alexander Michaelis†,‡ †

Institute of Materials Science, TU Dresden, 01062 Dresden, Germany Fraunhofer IKTS, Fraunhofer Institute for Ceramic Technologies and Systems, 01277 Dresden, Germany

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ABSTRACT: Although tin and tin oxides have been considered very promising anode materials for future highenergy lithium-ion batteries due to high theoretical capacity and low cost, the development of commercial anodes falls short of expectations. This is due to several challenging issues related to a massive volume expansion during operation. Nanostructured electrodes can accommodate the volume expansion but typically suffer from cumbersome synthesis routes and associated problems regarding scalability and cost efficiency, preventing their commercialization. Herein, a facile, easily scalable, and highly cost-efficient fabrication route is proposed based on electroplating and subsequent electrolytic oxidation of tin, resulting in additive-free tin oxide anodes for lithium-ion batteries. The electrodes prepared accordingly exhibit excellent performance in terms of gravimetric and volumetric capacity as well as promising cycle life and rate capability, making them suitable for future high-energy lithium-ion batteries. KEYWORDS: lithium battery, high-energy, anode material, tin oxide, electrode preparation

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INTRODUCTION Over the last two decades, lithium-ion batteries (LIBs) have turned into the leading energy storage devices for portable electronics and are very promising candidates for large-scale applications such as all-electric or hybrid electric vehicles.1−3 Current state-of-the-art anodes for LIBs are porous composites consisting of an active material, a binder, and conductive additives coated on a metallic current collector. The anodes are commonly prepared via the following steps: (1) material synthesis, (2) powder processing, (3) slurry preparation, (4) coating, (5) drying, and (6) calendaring. Afterward, the anode foils are cut and then assembled with separator and cathode foils to form a LIB. Besides the rather limited specific capacities of state-of-the-art anodes, such as graphite with a theoretical capacity of 372 mAh g−1, significant improvement of the conventional electrode fabrication is needed regarding energy efficiency and costs as well as health and environmental aspects. Tin and tin oxides have recently attracted intense attention as possible anode materials for next-generation LIBs because these materials offer both a low electrode potential versus Li/Li+ (0−1 V) and high gravimetric capacities (e.g., Sn ∼1000 mAh g−1).4−6 Furthermore, the materials are highly abundant, inexpensive, and environmentally benign. However, a dramatic volume expansion during the lithiation of tin and tin oxides causes several challenging issues related to mechanical stress and degradation, complicating the practical implementation and commercialization as anode materials in LIBs.7,8 Nevertheless, due to the very promising properties of tin-based active materials, tremendous efforts have been made to tackle these © 2018 American Chemical Society

critical issues. Recent attempts include the nanostructuring of the electrodes and the application of buffer matrices to accommodate the volume expansion.9−15 Tin-based nanomaterials, such as zero-dimensional nanoparticles;16,17 one-dimensional nanowires, nanorods, and nanotubes;6,18,19 and two-dimensional nanosheets, nanobelts, and nanofilms,20−22 have been proven to effectively accommodate the volume changes upon cycling and to improve the effective transport properties by shortening the lithium diffusion pathways.23−25 However, most of these nanomaterials are limited in terms of scalability due to harsh experimental conditions with respect to toxic chemicals, high temperatures, impurities, etc.5,6,26 Moreover, the gravimetric capacity related to the mass of these nanomaterials might be excellent but the energy density at the cell level (including current collectors, separators, electrolytes, and additives) is often insufficient because the mass ratio of the active and inactive materials is quite unfavorable (e.g., area-specific capacities 3 mAh cm−2 lasts approximately 15 min. In our laboratory scale, the costs of such a tin oxide anode are roughly estimated to be $5 m−2 (15 cent Ah−1), including costs of materials, consumables, and energy consumption. Any other costs, such as for equipment and personnel expenses, are not considered in this calculation. By comparison, the laboratory-scale fabrication of a comparable graphite-based anode, with ready-to-use active material and without drying, lasts approximately 4 h, including the mixing of components, ball milling, vacuum mixing, coating, and calendaring. The costs of graphite-based anodes for LIBs, fabricated at an industrial level, amount to approximately $4 m−2 (13 cent Ah−1).63 Thus, in this rough estimate, the costs for the laboratory-scale tin oxide electrodes are almost identical to those of conventional graphite electrodes while providing significantly higher gravimetric and volumetric energy density and improved rate capability due to the nanostructuring. Another advantage of the proposed fabrication route is that both electrodeposition64,65 and electrolytic oxidation66−68 can be carried out continuously wet-on-wet using roll-to-roll processes. Furthermore, the presented fabrication approach is also applicable to three-dimensional structured substrates (e.g., foamlike69−71 or textile-based72 current collectors), which are not suitable for conventional tape-casting processes. Due to the very good electrical conductivity, which is inherent to electrodeposited films, and the mechanical integrity/flexibility of the nanostructured tin oxide, a calendaring of the electrodes is not necessary. Therefore, the proposed fabrication route includes the benefits of nanostructured electrodes (fast kinetics, accommodation of volume changes, mechanical flexibility, etc.) while being potentially more cost-effective (materials and production costs) and environmentally benign (no toxic or environmentally harmful components) than conventional coating processes. However, the most important feature is that, in contrast to the most other synthesis routes for highcapacity nanomaterials, electrodeposition and electrolytic oxidation are easily scalable to high-volume manufacturing. Because the presented fabrication route allows targeted nanoand microstructuring of tin oxide,41 our current work includes the optimization of the plating conditions and the electrolytic oxidation procedure to further improve the cycle life performance. A further important task is to reduce the initial capacity loss, e.g., by prelithiation73 or the formation of an artificial SEI

Figure 8. Comparison of tin oxide electrodes prepared by electrolytic oxidation and commercial graphite anodes with similar area-specific capacity: (a) impedance and (b) thickness dependence of the areal capacity.

sites within a relatively mobile tin layer. (3) The ICL grows, controlled by the mutual diffusion of tin and copper through the vacancy-rich ICL. (4) The successive deposition of tin occurs at the surface of the ICL. Surprisingly, the thickness of the ICL varies between 100 and 500 nm (cf. Figures 3 and 6). Thereby, the ICL is thickest close to the grain boundaries of the deposited tin layer, indicating fast grain boundary diffusion of Cu. Consequently, the microstructure of the deposited tin layer is crucial for the formation and growth of the ICL. The formation of tin oxide is accompanied with a vigorous oxygen evolution during electrolytic oxidation, especially enhanced under high voltages, which disturbs the stable growth of tin oxide.60,61 Lee et al. suggested that the current efficiency ratio of oxygen evolution to tin oxide formation is the key factor responsible for internal crack development.61 However, a certain macroporosity might be desirable to avoid significant electrolyte depletion during fast discharging62 because it can ensure improved electrolyte transport through the nanostructured oxide film. Consequently, the adjustment of the electrolytic oxidation conditions (electrolyte composition, current−voltage regime) is a key factor to achieve optimal electrochemical properties of the resulting tin oxide electrode. In comparison with the previous reports,50,51 the lower voltage (7.0 vs 10.0 V) used in this study during the electrolytic oxidation should result in reduced oxygen evolution. This might lead to a more favorable electrode structure (e.g., ratio of macro- to nanoporosity) with respect to the electrochemical properties and 27026

DOI: 10.1021/acsami.8b07981 ACS Appl. Mater. Interfaces 2018, 10, 27019−27029

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ACS Applied Materials & Interfaces film after the electrolytic oxidation process.74 Another interesting attempt is to explore suitable nanostructures that enable a high reversibility of the conversion reaction to expand the usable potential window and to obtain even higher specific capacity.

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CONCLUSIONS Nanostructured tin oxide electrodes prepared by electrodeposition and subsequent electrolytic oxidation of tin clearly show superior performance in comparison to that of state-ofthe-art anodes for LIBs. The excellent performance results from the large surface area, the short lithium diffusion pathways, and the mechanical integrity (flexibility) as well as from the redundancy of binder and conductive additives in the tin oxide nanostructures formed by the electrolytic oxidation process. Moreover, the proposed fabrication route is potentially very cost-effective (materials and production costs), environmentally benign (no toxic or environmentally harmful components), and easily scalable to high-volume manufacturing.

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AUTHOR INFORMATION

Corresponding Author

*E-mail: [email protected]. Phone: +49 351 2553-7324. ORCID

Christian Heubner: 0000-0003-2581-6180 Notes

The authors declare no competing financial interest.

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ACKNOWLEDGMENTS The authors are grateful to Maria Striegler and Mathias Herrmann (Fraunhofer IKTS Dresden) for the EDX measurements and fruitful discussions.

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DOI: 10.1021/acsami.8b07981 ACS Appl. Mater. Interfaces 2018, 10, 27019−27029