Cerium-alloyed dendrite-inhibited highly stable anodes for all-solid-state lithium batteries

Abstract

All-solid-state lithium (Li) batteries (ASSLBs) can inhibit the growth of Li dendrites to some extent, whereas Li dendrites are still unavoidable, which decreases the electrochemical performance of ASSLBs. Among the many methods developed for suppressing Li dendrites, the use of Li–In alloy anodes is a common strategy due to its smooth voltage plateau and stable electrochemical performance. However, Li–In dendrites still appear in Li–In anode-based ASSLBs. Herein, a rare earth (RE) element (Ce) was introduced to form Li–In–Ce alloy anodes, which contain micro-sized CeIn₃ particles in a Li–In substrate. Compared with Li–In, the Ce-containing Li–In–Ce anode had better electrochemical properties and greater cycling stability (>10 times, ∼750 cycles) in the ASSLB. The CeIn₃ particles in the Li–In–Ce alloys can limit the deformation of Li–In and promote the even plating of Li, significantly suppressing the growth of Li–In dendrites, which is observed in situ via special solid cells. In addition, this improvement strategy for Li–In alloys is universal for other RE elements (such as Y, La, Pr, Sm, or Yb), and the electrochemical properties can be influenced by the metal bond strength of RE–In in REIn₃. This work can guide the design of high-performance anodes in ASSLBs.

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New concepts

In this work, a rare earth (RE) element Ce was introduced into Li–In alloys to improve the electrochemical properties of all-solid-state lithium batteries (ASSLBs). The obtained Li–In–Ce alloys can obviously suppress the growth of Li–In dendrites according to the in situ observation test, leading to the good cycling stability of the ASSLB (750 cycles). The suppression of Li–In dendrites is associated with the distributed CeIn₃ particles in the Li–In–Ce alloy, which can inhibit the deformation of the Li–In composite and promote the even plating of Li. Moreover, other RE elements can also be selected to improve the Li–In alloys and the electrochemical performances of the Li–In–RE alloys are influenced by the metal bond strength of RE–In. The introduction of RE elements can improve the electrochemical properties and inhibit dendrites of Li–In alloy, which can provide a reference for the design of anodes in ASSLBs.

Introduction

Owing to the application of stable solid electrolytes (SEs), the all-solid-state lithium battery (ASSLB) is an exciting battery system that can achieve better safety than traditional liquid lithium-ion (Li⁺) batteries.^1–7 In addition, ASSLBs are often supposed to reduce Li dendrites because the mechanical strength of SEs is greater than that of liquid electrolytes. However, uncontrolled Li dendrites still appear in ASSLBs and lead to a short circuit, which is harmful to the practical application of ASSLBs.^8–11

The growth of Li dendrites in ASSLBs is rooted in the uneven deposition and dissolution of Li metal at the interface between Li and SE.^12–15 Many strategies involving anodes and electrolytes have been proposed to restrict the uncontrolled growth of Li dendrites.^16–19 The optimization strategies of the Li anode side are important for limiting the production of Li dendrites directly and include alloying,^20–22 3D scaffolds,^23,24 Li powder,²⁵ the interface layer^26–29 and so on. For the alloying method, some metal or semimetal elements (In, Sn, Al, Zn, Si, Ge, etc.) can be introduced into Li metal,^22,30 realizing even Li plating/stripping processes and inhibiting the production of Li dendrites to some extent.

Among the different Li-based alloys, Li–In alloys possess stable lithiation/delithiation processes and good electrochemical stability and have been widely used as anodes for evaluating the electrochemical performance of ASSLBs.^31–36 However, Li–In dendrites may form and lead to a short circuit in the ASSLB during long-term cycling at high current density.³⁷ Owing to the high deformability combined with the volume expansion, the Li–In alloy anodes deform and fill the cracks, pores, and grain boundaries of the SE layer during repeated lithiation/delithiation, leading to the production and spread of Li–In dendrites.³⁷ Rare earth (RE) elements with large atomic radii and low electronegativities^38–43 can form alloys with common alloy-type anodes and buffer volume changes,^44–47 which can further improve the mechanical and electrochemical properties of these anodes. Therefore, RE elements can be adopted to improve the Li–In alloy anodes.

In this work, Ce metal with a low melting point, low cost and good processability was introduced into Li–In to form Li–In–Ce alloys via melting and cold-pressing methods. In the Li–In–Ce alloys, Ce is present as micro-sized particles (CeIn₃), which can limit the deformation of Li–In alloys and suppress Li–In dendrites during cycling. Thus, the Li–In–Ce anode can realize significantly better electrochemical performance than the Li–In anode in ASSLBs on the basis of the RE halide SE Li₃YBr₆ (LYB). In addition, other RE elements (Y, La, Pr, Sm, or Yb) were also used to prepare Li–In–RE alloys, and the relationships between the electrochemical properties and the metal bond strength (RE–In) were analyzed. The introduction of RE can improve the performance of the Li–In anode, which can serve as a reference for the design of Li–metal-based anodes in ASSLBs.

Results and discussion

The Li–In and Li–In–Ce materials were obtained via a cold-pressing method combined with a heating process. The Li–In sample contains In (PDF#04-010-6206) and LiIn (PDF#04-001-3138) phases, and the Li–In–Ce sample contains In (PDF#04-010-6206), LiIn (PDF#04-001-3138) and CeIn₃ (PDF#04-006-4230) phases, which are judged by X-ray diffraction (XRD) and Rietveld refinement results (Fig. 1a and Fig. S1, ESI†). Thus, Ce is present as CeIn₃ alloys in the Li–In–Ce sample. Compared with the flat surface of the Li–In sample, there are additional evenly distributed micro-sized particles in the Li–In–Ce material according to the scanning electron microscopy (SEM) images, and the isolated particles can be confirmed as CeIn₃ alloys by energy dispersive spectroscopy (EDS) mapping results (Fig. 1b and c and Fig. S2, ESI†).

Fig. 1 (a) XRD Rietveld refinement result of the Li–In–Ce material. (b) and (c) SEM images of the prepared Li–In and Li–In–Ce materials. EIS spectra of pristine, rested (20 h), and cycled (10th) symmetrical cells with (d) Li–In or (e) Li–In–Ce electrodes. (f) Average voltage polarization values of Li–In- and Li–In–Ce-based symmetrical solid cells during the cycling process.

To evaluate the compatibility between the synthesized purified SE (LYB) (Fig. S3, ESI†) and the prepared alloys (Li–In and Li–In–Ce), symmetrical solid cells based on LYB were assembled and tested at room temperature (RT). According to the electrochemical impedance spectroscopy (EIS) plots, the interface impedance (R_int) values of the Li–In-based symmetrical cells at different states (assembled, rested, and cycled) obviously changed to 3.1 Ω, 5.0 Ω, and 7.8 Ω, respectively (Fig. 1d and Fig. S4a, ESI†). In comparison, the symmetrical cells with different Li–In–Ce alloys presented smaller and stable R_int values, and the Li–In–Ce electrode (molar ratio of Ce–In : 10–90)-based cells presented the lowest R_int values, which were 1.5 Ω, 1.2 Ω, and 1.5 Ω (Fig. 1e and Fig. S4b, ESI†). In addition, the voltage polarization of the Li–In–Ce-based symmetrical battery was small and half that of the Li–In-based cell (Fig. 1f and Fig. S5, ESI†).

These Li–In- and Li–In–Ce-based symmetrical solid cells were cycled (0.5 mA cm⁻²) to evaluate their stability. After 5 cycles, the Li–In–Ce-based symmetrical solid battery shows a much smaller R_int value (3.8 Ω) than the Li–In-based cell (18.3 Ω) (Fig. 2a). Compared with the stable voltage polarization of the Li–In–Ce-based symmetrical cell, the voltage polarization of the Li–In-based symmetrical battery was greater and increased rapidly after cycling for 250 h (Fig. 2b). Owing to the stable and small R_int of the symmetrical cell with Li–In–Ce, this battery can further achieve good cycling stability for 1000 h, and its voltage polarization can maintain a low value of less than 0.07 V (Fig. 2b and c). In addition, the assembled Li–In–Ce/LYB/Li₄Ti₅O₁₂ (LTO) battery has much better cycling stability (∼750 cycles) than the Li–In/LYB/LTO battery (∼50 cycles) (Fig. 2d and e). Thus, compared with Li–In alloys, the prepared Li–In–Ce alloys are more compatible with the LYB SE and can help the ASSLB achieve stable cycling performance.

Fig. 2 (a) EIS spectra of symmetrical solid cells based on Li–In or Li–In–Ce after 5 cycles. (b) Voltage–time curves of Li–In- and Li–In–Ce-based symmetrical solid cells based on cycling. (c) Cycling performance of the Li–In–Ce-based symmetrical cell. Cycling properties of the assembled (d) Li–In/LYB/LTO and (e) Li–In–Ce/LYB/LTO batteries.

To analyze the mechanism of improving the cycling performance of Li–In–Ce-based ASSLBs, the symmetrical solid cells (electrode: Li–In or Li–In–Ce; electrolyte: LYB) with a small fabricated pressure (100 MPa) of electrodes were tested for 5 cycles. The Li–In–Ce-based symmetrical cell has a smooth and stable voltage–time curve, indicating the reversible lithiation/delithiation process of the Li–In–Ce alloys (Fig. S6a, ESI†). In contrast, the Li–In-based symmetrical cell has an unstable charge–discharge process with uncontrollable voltage polarization (Fig. S6b, ESI†). To further analyze the electrode/electrolyte interface, the electrodes were peeled off carefully, and the LYB layers were observed (Fig. S6a and b, ESI†). For the Li–In–Ce-based symmetrical cell, the surface of LYB layer did not obviously change, indicating excellent compatibility between LYB and Li–In–Ce. For the Li–In-based symmetrical cell, there is a black layer on the LYB electrolyte, which may cause unstable battery performance. After that, the surface morphologies and components of the cycled LYB layers were further analyzed via SEM/EDS (Fig. S6c and d, ESI†). After peeling off the Li–In–Ce electrode, the cycled LYB layer has a flat and clean surface with negligible In and Ce. In contrast, there is a large rough area on the cycled LYB layer of the Li–In-based symmetrical cell, which is enriched in In.

On the basis of the X-ray photoelectron spectroscopy (XPS) spectra, the signals of nonvalent Li and In were detected from the black layer on the surface of the LYB layer in the Li–In-based symmetrical cell, which can be confirmed as Li–In alloys (Fig. 3a). In contrast, there are no obvious signals of nonvalent Li or In on the cycled LYB layer in the Li–In–Ce-based symmetrical cell, indicating negligible Li–In dendrites and good stability between the Li–In–Ce and LYB layer (Fig. 3b). The black layer possesses a porous and spreading morphology (thickness: ∼10 μm) and a concentrated distribution of In, as observed by the cross-sectional SEM/EDS mapping images, which can be regarded as growing Li–In dendrites during the cycling process (Fig. 3c). Conversely, the cycled LYB layer of the Li–In–Ce-based cell has no black layer completely; thus, the Li–In–Ce electrode can clearly inhibit the production of Li–In dendrites in ASSLB. To explore the reason for the inhibited dendrite growth, a Brinell hardness (HB) test (Video. S1, ESI†) of Li–In-based electrodes was conducted, and the Li–In–Ce sample had a higher HB value (5.618) than the Li–In material (3.923) (Fig. 3d). A higher hardness can suppress the deformation of the Li–In component in the Li–In–Ce alloys; thus, the Li–In dendrites were inhibited. The electrode/electrolyte interfaces were also analyzed via cross-sectional SEM. The cycled Li–In/LYB interface had cracks, which were attributed to the deformation of the Li–In alloys (Fig. S7, ESI†), and the cycled Li–In–Ce/LYB interface remained stable, indicating the inhibited deformation of the Li–In–Ce alloys (Fig. S8, ESI†). Furthermore, the discharge–charge processes of Li–In- and Li–In–Ce-based cells were analyzed by in situ EIS and the distribution of relaxation times (DRT). The Li–In–Ce/LYB interface clearly showed better stability than the Li–In/LYB interface (Fig. S9, ESI†).

Fig. 3 Li 1s and In 3d XPS spectra of cycled LYB layers of (a) Li–In- and (b) Li–In–Ce-based symmetrical cells (inset: photos of cycled LYB layers). (c) Cross-sectional SEM image and EDS mapping of the cycled LYB layer of the Li–In-based cell. (d) SEM images of Li–In and Li–In–Ce samples containing indentations after the Brinell hardness test.

In addition, for a more intuitive view of Li–In dendrites, special solid cells were assembled and cycled at 2.0 mA cm⁻² (Fig. 4a). In this special cell, one circular electrode was cut into two semicircles, which were cold pressed on one side of the LYB pellet (gap between electrodes: ∼1.0 mm). The growth process of Li–In dendrites was observed by in situ video (Fig. 4b and Video S2, ESI†) and SEM/mapping (Fig. 4c–h) through the gap between semicircular Li–In-based electrodes. During the cycling process, the Li–In dendrites grew rapidly in the special cells with Li–In electrodes, and the Li–In–Ce-based special cells maintained good stability with no dendrite growth. The situations of Li–In dendrite growth in Li–In- and Li–In–Ce-based solid cells are shown graphically in schematic diagrams (Fig. 5a, b and Video S3, ESI†). To further study the mechanism of Li–In dendrite suppression by the Li–In–Ce electrode, the detailed structures of the phases in the Li–In and Li–In–Ce alloys were obtained by XRD Rietveld refinements (Fig. 1a, Fig. S1b and Tables S1, S2, ESI†). The Li adsorption energies of different phases in Li–In-based alloys were subsequently calculated via density functional theory by the Vienna ab initio simulation package (Fig. 5c and d). The Li adsorption energies of the In (100) and LiIn (220) crystal planes increase significantly after the introduction of Ce into the Li–In alloys (Li–In–Ce). Notably, the Li adsorption energy gap between In (100) and LiIn (220) decreases significantly with the introduction of Ce (Li–In: ∼2.1 eV; Li–In–Ce: ∼1.0 eV). Therefore, the inhibited Li–In dendrites of the Li–In–Ce electrode can be attributed to the high hardness of Li–In–Ce and the small gap in the Li adsorption energies of In (100) and LiIn (220).

Fig. 4 (a) Diagram and (b) photos for in situ observations of the cycled special solid cells based on Li–In and Li–In–Ce. SEM and mapping results of the cycled special solid cells based on (c)–(e) Li–In and (f)–(h) Li–In–Ce (inset: photos of the special solid cells).

Fig. 5 Schematic diagrams of Li–In dendrite growth in (a) Li–In- and (b) Li–In–Ce-based solid cells. The calculated adsorption models (Li atoms) with charge densities and Li adsorption energies of the In (110) and LiIn (220) phases in (c) Li–In and (d) Li–In–Ce alloys. (e) Interface impedances after 5 cycles and (f) voltage polarizations of symmetrical solid cells based on Li–In–RE (RE elements: Y, La, Ce, Pr, Sm, or Yb) alloys (0.5 mA cm⁻²). (g) The calculated EN/D values of RE–In metal bonds.

To expand the improvement methods for Li–In electrodes, other low-cost RE elements (Y, La, Pr, Sm, or Yb) have been introduced. Like Li–In–Ce alloys, the prepared Li–In–RE materials possess In, LiIn and REIn₃ phases, and the REIn₃ particles are distributed in the Li–In substrate according to the XRD Rietveld refinements (Fig. S10 and Tables S3–S7, ESI†) and SEM results (Fig. S11, ESI†). In addition, symmetrical Li–In–RE/LYB/Li–In–RE cells were fabricated and evaluated. The R_int values of the pristine and cycled symmetrical Li–In–RE-based cells are all smaller than those of the Li–In-based symmetrical cells (Fig. 5e and Fig S4, S12, ESI†). Moreover, Li–In–RE/LYB/Li–In–RE cells can realize low voltage polarization and stable cycling stability, in addition to Li–In–Yb-based cells. The trend of the voltage polarization of Li–In–RE-based cells is Li–In–Ce < Li–In–Pr ∼ Li–In–Sm ∼ Li–In–La < Li–In–Y < Li–In–Yb (Fig. 5f and Fig. S13, ESI†). Among the Li–In–RE-based cells, the Li–In–Ce-based symmetrical battery exhibited the lowest R_int value and the smallest voltage polarization.

To further explore the inherent law of Li–In–RE alloys, the metal bond strengths of RE–In in REIn₃ were analyzed by the ratio of electronegativity difference (EN) and interatomic distance (D, obtained from XRD Rietveld refinement results) between RE and In. The metal bond strengths are positively correlated with EN and negatively correlated with D; thus, the value of EN/D (Y–In < Sm–In < Pr–In < Ce–In < La–In < Yb–In) can represent the strength of the metal bond to some extent (Fig. 5g). Combining the trends of cycling performance (Li–In–RE-based cells) and EN/D values (RE–In), the proper EN/D values can correspond to the good electrochemical performance of Li–In–RE-based cells. A too large EN/D value (such as Yb–In) may lead to large and uneven REIn₃ particles with high strength, which may be bad for physical contact between the Li–In–RE electrode and the LYB layer. A too small EN/D value (such as Y–In) may lead to easily deformed REIn₃ particles with low strength, which may be weak in inhibiting the deformation of the Li–In component and suppressing Li–In dendrites.

Conclusions

A new improvement method for Li–In anodes has been developed to restrict the growth of Li–In dendrites in this work. The Ce element was introduced into the Li–In alloys by melting and cold pressing processes, forming the Li–In–Ce alloys, which possess micro-sized particles (CeIn₃) in the Li–In substrate. Compared with Li–In-based symmetrical cells, the prepared Li–In–Ce-based symmetrical cells can realize lower interface impedance, smaller voltage polarization and higher cycling stability (∼1000 h). Moreover, the Li–In–Ce-based ASSLB possesses better cycling stability (∼750 cycles) than the Li–In-based ASSLB (∼50 cycles). The Li–In dendrites of the ASSLBs were analyzed via SEM, EDS, mapping and in situ observation tests. The Li–In–Ce alloys clearly suppress the production of Li–In dendrites, which may be due to the influence of CeIn₃ particles, which restrict the deformation of Li–In and facilitate the even plating of Li. Other RE elements (Y, La, Pr, Sm, or Yb) were also selected to prepare Li–In–RE alloys, which improved the electrochemical properties of the Li–In electrode. Moreover, a correlation exists between the performance of Li–In–RE and the bond strength (EN/D) of RE–In; that is, the good electrochemical performance of the Li–In–RE alloys corresponds to the appropriate EN/D value of RE–In. In summary, the introduction of RE elements can improve the electrochemical properties and inhibit dendrites of Li–In alloy anodes, which has an important driving effect on the development and practical application of anode materials in ASSLBs.

Author contributions

X. S.: investigation and writing of the original draft. Z. Z.: conceptualization, supervision, investigation, writing – review & editing, formal analysis, funding acquisition. C. Li and W. Z: review & editing. Y. D.: supervision, conceptualization, review & editing, resources, funding acquisition. All the authors discussed the results and the manuscript. All the authors have agreed to the publication of this manuscript.

Data availability

The data supporting this article have been included as part of the ESI.†

Conflicts of interest

There are no conflicts to declare.

Acknowledgements

We gratefully acknowledge the support from the National Science Foundation for Distinguished Young Scholars of China (22425503), Natural Science Foundation of China (22371131, 22305129), 111 Project (No. B18030) from China, Tianjin Natural Science Foundation (24JCQNJC01980), the China Postdoctoral Science Foundation (BX20220157, 2022M721698, 2023M741812), Rare Earth Advanced Materials Technology Innovation Center, Haihe Laboratory of Sustainable Chemical Transformations, and the Key Laboratory of Rare Earths, Chinese Academy of Sciences.

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Footnote

† Electronic supplementary information (ESI) available. See DOI: https://doi.org/10.1039/d5mh00466g

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