1. Introduction

Lithium ion batteries (LIBs), first commercialized by Sony in Japan in 1991 [1], have been driving the market for portable electronic devices such as mobile phones, tablets, laptops and MP3 players for more than 30 years, and are becoming increasingly important as industrial technologies such as energy storage systems (ESS), electric vehicles (EVs), personal mobility devices and drones develop. However, current commercially available lithium-ion batteries use flammable organic liquid electrolytes as the medium to deliver lithium ions, which can pose serious safety issues when applied to medium and large power devices such as ESSs and EVs. This safety issue can be fundamentally solved by using an inorganic solid electrolyte instead of an organic liquid electrolyte, and research on all solid-state lithium batteries (ASSLBs) with solid electrolytes is ongoing in academia and industry.

ASSLB is one of the next-generation secondary battery technologies that replaces the separator and organic liquid electrolyte in a conventional commercial LIB, which consists of an anode, cathode, separator, and organic liquid electrolyte, with a solid electrolyte that conducts lithium ions, as shown in Fig. 1. By solidifying the electrolyte, ASSLBs are structurally safe and can achieve approximately 30-60% higher energy density compared to conventional Li-ion batteries [2]. In addition, the package materials and processes can be minimized by adoption of bipolar design which stacked mono cell in series within a single package, leading to reducing the manufacturing cost [3].

Solid electrolytes, the most essential part of ASSLBs, are broadly divided into polymeric and inorganic solid electrolytes based on the type of solid electrolyte, and inorganic solid electrolytes are further classified into oxide and sulfide solid electrolytes (Fig. 2). Polymeric solid electrolytes were first developed by Wright et al. in 1975 using polyethylene oxide (PEO) and alkali salts [6], but their low ionic conductivity of 10⁻⁶ to 10⁻⁸ S/cm at room temperature (RT) and poor thermal and electrochemical stability have left many barriers to overcome before they can be used as solid electrolyte materials for ASSLBs. Inorganic solid electrolytes have been developed in earnest since the development of Li_xPO_yN_z (LiPON) in 1992 [7], and representative oxide solid electrolytes include perovskite type Li_2/3-xLa_3xTiO₃ (LLTO), NASICON-type Li_1+xAl_xTi_2-x(PO₄)₃ (LATP), and garnet-type Li₇La₃Zr₂O₁₂ (LLZO) [8−10]. Oxide-based solid electrolytes have advantages such as relatively high ionic conductivity (10⁻³~10⁻⁴ S/cm) at RT and good thermal and electrochemical stability, but they are difficult to be large-scale due to disadvantages such as high sintering temperatures above 1000°C, brittle properties, and high interfacial and intergranular resistance [11]. Sulfide-based solid electrolytes, such as thio-LISICON type Li₁₀GeP₂S₁₂ (LGPS) and argyrodite type Li₆PS₅X (X = Cl, Br, I), have high ionic conductivity (~10⁻² S/cm) at RT, which is on par with organic liquid electrolytes [12]. In addition, due to its relatively soft mechanical properties, it has excellent contact with the electrode, resulting in low interfacial resistance, and is considered the closest solid electrolyte material to commercialization. However, it is difficult to handle because it reacts with moisture in the air to produce extremely toxic hydrogen sulfide (H₂S).

This review presents a summary of the recent progress for inorganic solid electrolytes among the different types of solid electrolytes for ASSLBs. Section 2 focuses on the challenges and research trends for different types of oxide-based solid electrolytes that are currently being studied in the literature. Section 3 discusses the challenges facing sulfide-based solid electrolytes, including thio-LISICON and argyrodite, and the various research efforts aimed at addressing these challenges. Finally, we discuss emerging issues and prospects of inorganic solid electrolytes for ASSLBs.

2.Oxide-based solid electrolytes

2.1. Perovskite type solid electrolyte

A perovskite solid electrolyte is a material with an ABO₃ structure, in which the A-site of metal titanate (ATiO₃) is substituted by La³⁺ and Li⁺ [13]. LLTO was first reported in 1987 to exhibit lithium-ion conductivity [14]. In 1993, LLTO bulk crystals were observed to have a high ionic conductivity of 1 × 10⁻³ S/cm at RT [15]. The benefits of LLTO over other solid electrolytes include: i) large ionic transference number (i.e., 0.5~0.9), ii) wide electrochemical window (8 V vs, Li/Li⁺), iii) excellent thermal stability (4~1600 K), iv) environmental friendliness [16]. However, due to high grain boundary resistance (~10⁻⁵ S/cm), the total ionic conductivity was significantly lower at 2 × 10⁻⁵ S/cm [15]. In addition, LLTO suffers from increased electrical conductivity due to Ti⁴⁺ reduction when in direct contact with lithium metal [16]. Up to now, various strategies have been devoted to improving the ionic conductivity and chemical stability of LLTO. For instance, Hu et al. observed that Ge-doped LLTO, containing 5 mol% Ge, exhibited an elevated Li⁺ transference number (nearly closed to 1), enhanced ionic conductivity (1.2 × 10⁻⁵ S/cm at RT), and an expanded electrochemical window (10 V vs. Li/Li⁺) [17]. Liu et al. demonstrated that sandwich structures with PEO/PEO-LLTO/PEO improved ionic conductivity, which was caused by fast and continuous Li⁺ conduction of fibrous LLTO within the polymer matrix [18]. The PEO layer containing LiTFSI also enhanced interfacial stability by impeding the reduction of Ti⁴⁺ due to direct contact between Li metal and LLTO. Tan et al. studied that ionic conductivity of thin film LLTO (~540 nm) with different annealing temperatures [19]. It was established that the annealing of LLTO at 300°C results in the formation of a crystalline amorphous phase. This process yielded the maximum ionic conductivity (9.56 × 10⁻⁵ S/cm at 140°C), while also demonstrating promising potential for application as a solid electrolyte in flexible ASSLBs (Fig. 3). The LTO/LLTO/NCM battery exhibited a capacity of 7.1 μAh at 0.1C and demonstrated excellent stability after bending (length, 12 mm), retaining 89.2% of their original capacity. In another study, MOF-derived LLTO was prepared by impregnation of LLTO into MOF lamellar membrane and in-situ sintering method [20]. The results showed that ionic conductivity of 1.19 × 10⁻⁵ S/cm and ionic conduction of 0.215 S at RT.

2.2. NASICON type solid electrolyte

NASICON-type solid electrolytes typically have a structure of Na_1+xZr₂Si_xP_3-xO₁₂, with various substitutions made to adjust their properties [21]. Several NASICON-type Li-ion conductor, LiM₂(PO₄)₃ (M = Zr, Ge, Ti, Hf), have been developed by replacing Na-ion in NaZr₂(PO₄)₃ by Li-ion [22−25]. In particular, LATP has been obtained by Al substitution with Ti site in LiTi₂(PO₄)₃, leading to a high ionic conductivity of 3 × 10⁻⁴ S/cm at RT [26, 27]. LATP exhibits analogous advantages to those observed in LLTO, including a broad electrochemical window (5 V vs. Li/Li⁺), robust thermal stability, and environmental benignity [28]. Nevertheless, the total ionic conductivity is relatively low (4 × 10⁻⁶ S/cm) due to the high grain boundary resistance (10⁻⁶ S/cm). Furthermore, when LATP is in direct contact with lithium metal, there is an increase in electrical conductivity due to the reduction of Ti³⁺. Recently, various strategies have been developed to improve the interfacial resistance, ionic conductivity, chemical stability, and mechanical strength of LATP. For instance, Yang et al. observed that by using the sticky PEO thin layer as an interfacial adhesive, the interfacial stability of LATP has been enhanced [29]. This method leverages of PEO acceptable Li⁺ conducting capability and its perfect compatibility with the tailored materials to effectively link the compact LATP and electrodes. Lee et al. demonstrated that adding an Ta dopant Ti site in the LATP crystal structure [30]. The applicability of Ta-doped LATP was confirmed in all-solid-state batteries, which showed a high coulombic efficiency and capacity of 98.6% and 0.072 mAh/cm², respectively. These findings suggest a possible way to improve the chemical stability of LATP (Fig. 4). The Max J. Palmer group synthesized a thin film of LATP with a thickness of approximately 25 μm, filled the film with a high-crosslinking polymer electrolyte precursor, and formed a solid composite electrolyte through heat treatment [31]. This method, by forming an interconnected oxide structure, achieved a high oxide content of 77 wt%, resulting in increased ion conductivity (3.5 × 10⁻⁵ S/cm) and exhibited an activation energy of 0.43 eV. There is also a research result where, similar to LLTO, LATP was impregnated into a MOF membrane and subjected to sintering [32]. As a result, it exhibited an ionic conductivity of 9.8 × 10^-5 S/cm at RT and improved mechanical strength.

2.3. Garnet type solid electrolyte

Garnet-type solid electrolytes have a cubic crystal structure with the formula A₃B₂(XO₄)₃ [33]. In 2003, the Thangadurai et al. first reported the garnet-type solid electrolyte Li₅La₃M₂O₁₂ (M=Nb, Ta) [34]. In 2005, Li₆ALa₂M₂O₁₂ (A = Ca, Sr, Ba; M = Nb, Ta) was reported [35]. However, Li₆BaLa₂Ta₂O₁₂ exhibited a low ionic conductivity of 4 × 10⁻⁵ S/cm at RT, making it unsuitable for all-solid-state battery applications. In 2007, Murugan et al. reported the LLZO, which has a high ionic conductivity of 3 × 10⁻⁴ S/cm at RT [36]. The advantage of LLZO over other solid electrolytes is that it does not contain titanium, allowing it to be used with lithium metal [37, 38]. However, there are some problems with LLZO, such as poor interfacial contact with electrodes, poor wettability with molten lithium [39]. Also, high reactivity with CO₂ and H₂O can lead to the formation of Li₂CO₃, which increases interfacial resistance when exposed to air atmosphere [40]. And LLZO can exist in two different crystal structures: tetragonal and cubic. The cubic structure allows Li-ion migration in all three (x, y, z) directions, whereas the tetragonal structure only allows Li-ion migration in the x-y plane, resulting in lower ionic conductivity [41]. To transform the tetragonal structure of LLZO into the cubic structure, a high heat treatment above 1180°C is required [42]. Therefore, various strategies efforts are underway to address these issues and improve the performance of LLZO solid electrolytes. Abrha et al. investigated that the use of Ga and Nb as dual dopants in LLZO improved the air stability, resulting in the suppression of LLZO decomposition and improvement ionic conductivity (9.28 × 10⁻³ S/cm) [43]. Li et al. establish an efficient approach to transform tetragonal LLZO into cubic LLZO at lower calcination temperatures by using high-energy ball milling, which was caused by the accumulation of Li⁺ vacancies [42]. Jia at el. reported that the LLZO surface was chemically treated with dopamine to form an air-stable shell. This improves electrochemical and cycling stability by inhibiting Li₂CO₃ [44]. Zhang et al. fabricated an all-solid-state lithium metal battery (ASSLMB) using Li_6.55La_2.95Ca_0.05Zr_1.5Ta_0.5O₁₂(LLCZTO), an LLZO-based solid electrolyte [45]. A ZnO coating layer with a thickness of about 200 nm was formed on the surface of LLCZTO pellets using a magnetron sputtering method. This enhanced the Li/LLCZTO interfacial contact, resulting in increased mobility of the lithium ions during the Li plating/stripping process, resulting in excellent cycle efficiency (Fig. 5).

3. Sulfide-based solid electrolytes

3.1. Thio-LISICON type solid electrolyte

Thio-LISICON, such as β-Li₃PS₄, was introduced in 2000 and is an analogue created by substituting sulfur for oxygen in LISICON [46]. It is crystallized in the γ-Li₃PO₄ structure of LISICON [47]. Kanno reported in 2001 that Li_3.25Ge_0.25P_0.75S₄ (Thio-LISCON), a solid electrolyte, exhibits high ion conductivity of approximately 2.2 × 10⁻³ S/cm at RT [48]. This result is significant as it represents the first crystalline lithium-ion conductor with the highest ionic conductivity at the time. However, the use of Ge presents challenges such as high material costs, issues related to Ge reduction at low potentials, and instability when exposed to air. Various strategies have been devoted to improving ionic conductivity, reduce costs, improve stability, and other related challenges. At first, Kamaya et al. developed Li₁₀GeP₂S₁₂ (LGPS) with a new three-dimensional framework structure through heterogeneous element substitution, achieving higher ionic conductivity (1.2 × 10⁻² S/cm at RT) [49]. Based on this Kato et al. improved the ionic conductivity (2.5 × 10⁻² S/cm) and reduced costs by using Si instead of Ge [50]. Also, they synthesized the Li_9.6P₃S₁₂ electrolyte, which overcame the issues of transition metal reduction in low voltage regions. Zhang et al. fabricated a LiH₂PO₄ protective layer between the LGPS electrolyte and Li anode, synthesized in situ through controlled reactions of Li metal and H₃PO₄ in THF solvent [51] (Fig. 6). As a result, the stability of LGPS including lithium metal increased, and cycling of symmetric Li/Li cells remained relatively stable for over 950 hours, maintaining polarization voltages within ±0.05 V and current densities of 0.1 mA/cm². James A et al. show how reducing the size of LGPS crystallites to the nanoscale results in a substantial enhancement in Li-ion conductivity [52]. In addition, Li et al. conducted research contributing to the design and fabrication of sulfide-based polymer/ceramic composite electrolytes for implementing high-performance lithium metal batteries [53].

3.2. Argyrodite type solid electrolyte

An argyrodite solid electrolyte is a material with a cubic crystal structure and is generally composed of compounds such as Li₆PS₅X (X = Cl, Br, I). The structure of argyrodite was first reported in the form of Ag₈GeS₆ [54]. Subsequently, sulfide-based solid electrolytes Li₆PS₅X (X = Cl, Br, I) synthesized by halogen substitution of Li₇PS₆ were also reported. In 2005, the Li-ion conductivity of argyrodite solid electrolytes was observed to be approximately 10⁻³ S/cm at RT, which is a very high level compared to existing solid electrolyte materials [55]. The advantages of Li6PSCl (LPSC) compared to other solid electrolytes are as follows: i) Long cycle performance (maintains a high discharge capacity of about 535 mAh/g at a current density of 56 mA/g even after 650 cycles) ii) Ease of manufacturing iii) Relatively high ionic conductivity (approximately 10⁻⁴ S/cm at RT) [55,56]. When the current density exceeds the critical threshold during cycling with the lithium anode, argyrodite SSEs can form dendritic lithium deposits, leading to short circuits [57]. Additionally, Li₆PS₅X can decompose at the interface due to strong reduction of lithium. Furthermore, Li₆PS₅I has low ionic conductivity (10⁻⁷ S/cm) due to the ordering of I^-/S^2- sites within its structure. Various strategies have been researched to improve the ionic conductivity and chemical stability of Li₆PS₅X. For example, Zhang et al. observed that doping Li₆PS₅I with silicon improved both ionic conductivity and interface compatibility [58]. Silicon doping significantly enhanced the conductivity within the Li_6+xP_1-xSi_xS₅I structure to 1.1 × 10⁻³ S/cm and reduced the activation energy to 0.19 eV. Jiang et al. demonstrated that the adsorption of CO₂ chemically onto the active sulfur (S^2-) sites on the surface of LPSC forms S–C bonds, thereby enhancing the interfacial stability between lithium and LPSC [59]. This results in reduced cell resistance. Li|CO₂@LPSC|LTO demonstrated a capacity retention of 62% after 1000 cycles and achieved an ultra-high Coulombic efficiency of 99.91% over 1000 cycles. Su et al. studied that in symmetric cells with an introduced lithium phosphate oxynitride (LiPON) interlayer, the interfacial resistance was significantly reduced to 1.3 Ω cm² [60]. These symmetric cells with the LiPON interlayer demonstrated stable lithium plating/stripping cycles for over 1000 hours at a current density of 0.5 mA/cm². They also achieved a critical current density of 4.1 mA/cm² at 30°C, showing stable performance even at high current densities. In another study, Sun et al. showed that oxygen-doped Li₆PS_4.75ClO_0.25 (LPSCO_0.25) exhibited the highest ionic conductivity of 4.7 × 10^-3 S/cm, which is higher than the 4.2 × 10^-3 S/cm of undoped LPSC [61]. Oxygen doping improved stability with lithium metal, as confirmed by periodic voltage measurements and powder X-ray diffraction tests (Fig. 7).

4. Summary and outlook

ASSLBs are attracting attention as a potential next generation secondary battery technology that can reduce the risk of commercial lithium-ion batteries. In this review, we have comprehensively examined the previous literature on inorganic solid electrolytes for ASSLBs. In particular, this review highlights the contributions of existing studies to the development of inorganic solid electrolytes with high ionic conductivity and demonstrates their impact on the advancement of the field. Key findings include recent research advances that have significantly overcome the challenges faced with oxide and sulfide-based solid electrolytes. Despite these contributions, there are still important questions and issues, such as interfacial resistance, chemical/electrochemical stability and fabrication process, that need to be addressed in future research. Thus, future work should focus on electrode/electrolyte interface comparability, using novel methodologies and approaches to explore these unresolved issues.

Article information

Conflict of Interest Declaration

The authors declare no competing financial interests or personal relationships.

Author Information and Contribution

S.K.C. : Ph.D. candidate, writing-original draft & editing, J.H.H. : MS candidate, writing-original draft, G.J.K. : undergraduate student, writing-original draft, Y.H.K. : undergraduate student, writing-original draft, J.C.: Professor, supervision, writing-review & editing, M.H.Y. : Professor, conceptualization, writing-original draft, funding acquisition, supervision.

Acknowledgements

This work was supported by the National Research Foundation of Korea(NRF) grant funded by the Korea government(MSIT) (2022R1C1C1006536 and RS-2023-00221237).

Fig. 1.

Schematic diagram of a conventional lithium-ion battery (LIB) and an all-solid-state lithium battery (ASSLB).

Fig. 2.

Comparison of the (a-c) performance [4] Copyright 2017 Springer Nature and (d) conductivity of various solid-state electrolytes (ASR: area-specific resistance, black: polymers, green and blue: oxides, red: sulfides) [5] Copyright 2019 The Royal Society of Chemistry.

Fig. 3.

(a, c) Schematic images of flexible LTO/LLTO/NCM-based all-solid-state lithium batteries (ASSLBs). (b, d) Cross-sectional scanning electron microscopy (SEM) images of LTO/LLTO/NCM-based ASSLBs. (e-g) Top-view SEM images of NCM, LTO, LLTO, respectively [19]. Copyright 2021 The Royal Society of Chemistry.

Fig. 4.

Schematic images of the Ti reduction–mitigating mechanism though Ta doping in Li_1+xAl_xTi_2-x(PO₄)₃ solid electrolyte [30]. Copyright 2023 Elsevier.

Fig. 5.

(a) Schematic illustration of the method of ZnO coating on LLCZTO. (b) Schematic illustration of the evolution of Li/LLCZTO interfacial contact and Li metal growth through LLCZTO with different ZnO thicknesses during the Li plating/stripping process. Nyquist plots of Li−LLCZTO−Li and Li−ZnO−LLCZTO−ZnO−Li cells with different thicknesses (c) before cycling and (d) after several cycles. (e) Change rule of the corresponding interfacial area specific resistance (IASR). (f) Cycling performance of the Li−30mZnO−Li and Li−90mZnO−Li cells at current densities of 50, 100, and 200 μA/cm² [45]. Copyright 2020 American Chemical Society.

Fig. 6.

(a) Schematic of the LCO/LGPS/LiH₂PO₄–Li all-solid-state lithium battery (ASSLB) with an optimized structure. (b) Preparation process of in situ LiH₂PO₄ protective layer. (c) Long cycle performance of a LCO/LGPS/80%-Li cell [51]. Copyright 2018 American Chemical Society.

Fig. 7.

(a) Li⁺ migration barrier between the Li₆S cages of LPSC and LPSCO_0.25 by a density functional theory (DFT) calculation with the climbing image nudged elastic band (CI-NEB) method (blue atoms represent the popping trajectory of Li⁺). (b) cycling performance of all the LCO/LPSCO_x cells for 100 cycles at 0.3 C rate at 25°C [61]. Copyright 2021 American Chemical Society.

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