Wei Weng, Dong Zhou, Gaozhan Liu, Lin Shen, Mengqi Li, Xinshuang Chang, Xiayin Yao. Air exposure towards stable Li/Li10GeP2S12 interface for all-solid-state lithium batteries[J]. Materials Futures, 2022, 1(2): 021001. DOI: 10.1088/2752-5724/ac66f5
Citation: Wei Weng, Dong Zhou, Gaozhan Liu, Lin Shen, Mengqi Li, Xinshuang Chang, Xiayin Yao. Air exposure towards stable Li/Li10GeP2S12 interface for all-solid-state lithium batteries[J]. Materials Futures, 2022, 1(2): 021001. DOI: 10.1088/2752-5724/ac66f5
Letter •
OPEN ACCESS

Air exposure towards stable Li/Li10GeP2S12 interface for all-solid-state lithium batteries

© 2022 The Author(s). Published by IOP Publishing Ltd on behalf of the Songshan Lake Materials Laboratory
Materials Futures, Volume 1, Number 2
  • Received Date: March 26, 2022
  • Revised Date: April 08, 2022
  • Accepted Date: April 11, 2022
  • Available Online: April 13, 2022
  • Published Date: April 28, 2022
  • Moist air is a great challenge for manufacturing sulfide-based all-solid-state lithium batteries as the water in air will lead to severe decomposition of sulfide electrolytes and release H2S gas. However, different with direct reaction with water, short-period air exposure of Li10GeP2S12 sulfide electrolyte with controlled humidity can greatly enhance the stability of Li10GeP2S12 against lithium metal, thus realizing stable Li10GeP2S12 based all-solid-state lithium metal batteries. During air exposure, partial hydrolysis reaction occurs on the surface of Li10GeP2S12 pellets, rapidly generating a protective decomposition layer of Li4P2S6, GeS2 and Li2HPO3 in dozens of seconds. This ionically conductive but electronically insulation protecting layer can effectively prevent the severe interface reaction between Li10GeP2S12 and lithium metal during electrochemical cycling. The Li/40s-air-exposed Li10GeP2S12/Li cell shows long cycling stability for 1000 h. And the LiCoO2/40s-air-exposed Li10GeP2S12/Li batteries present good rate capability and long cyclic performances, showing capacity retention of 80% after 100 cycles.
  • Future perspectivesLi10GeP2S12 is a promising solid electrolyte with high ionic conductivity and good lithium dendrite inhibition for application in all-solid-state lithium metal batteries. However, Li10GeP2S12 can be easily reduced by lithium metal with formation of mixed conductive decomposition products including Li2S, Li3P and Ge/Li-Ge alloy, resulting in continuously increased interfacial impedance until cell failure. Interestingly, a stable Li10GeP2S12/Li metal interface can be constructed simply by exposing the Li10GeP2S12 pellet in air for dozens of seconds, and the insight reason comes from the formed ionically conductive but electronically insulated decomposition products from Li10GeP2S12 and water in air, making the fabrication process for Li10GeP2S12 solid electrolyte in the low-dew-point drying room possible in the future. Inspired by the air treatment strategy, further works can focus on the reactions between solid electrolytes and various gas sources to generate stable interface layers with high ionic conductivity, and thus realizing high-performance all-solid-state lithium batteries with excellent rate capability and cycling stability.

    All-solid-state lithium batteries exhibit increased safety due to the employment of nonflammable inorganic solid electrolytes [1-3]. To date, various inorganic solid electrolytes, especially sulfide solid electrolytes, possessing high ionic conductivity have been developed [4-8], potentially achieving high-rate capability of all-solid-state lithium batteries. However, sulfide solid electrolytes exhibit extremely poor air stability and long-time air exposure leads to severe decomposition of sulfide electrolytes with destroyed structure and release of toxic H2S gas [9, 10]. The accumulated decomposition products with poor ionic conductivity deteriorate the bulk and interface ion transfer, and finally resulting in rapid battery decay [10, 11].

    Compared with commercial lithium-ion batteries, the employment of lithium metal anodes is an essential prerequisite to realize higher energy density all-solid-state batteries [2, 3, 12]. Among sulfide electrolytes, Li10GeP2S12 possesses high ionic conductivity of 12 mS cm-1, which exceeds to that of organic liquid electrolytes [4]. However, the sulfide solid electrolyte Li10GeP2S12 strongly reacts with lithium metal and decomposes to Li15Ge4, Li3P and Li2S [13-15]. The large fraction of metallic Li15Ge4 at the Li/Li10GeP2S12 interface can create electronically conducting pathways, which will continuously consume the bulk Li10GeP2S12 and increase impedance until cell failure. Thus, a passivating layer without electronic conductivity is crucial to suppress the highly reactive Li/Li10GeP2S12 interface. Modification of lithium metal through chemical reaction is an appealing strategy to stabilize the Li/Li10GeP2S12 interface. Zhang et al [16] identified the in-situ formation of the LiH2PO4 by reacting the lithium metal with H3PO4. This LiH2PO4 layer is ionically conducting but electronically insulating, which can prevent the direct contact between Li10GeP2S12 and lithium metal and passivate the interface reaction. A more effective approach is introducing an electronic insulating layer with high interface energy against lithium. Wan et al [17] constructed a bifunctional layer at Li/Li10GeP2S12 interface by reacting the lithium meal with Mg(TFSI)2-LiTFSI-DME liquid electrolyte. The sequential reduction of salts and solvent generates a gradient solid electrolyte interface LixMg/LiF/polymer, resulting in a stabilized interface and demonstrating effective protection for Li10GeP2S12. In addition, using bilayer composite electrolyte can also passivate the Li/Li10GeP2S12 interface [18-20]. The cells employing Li-argyrodites Li5.5PS4.5Cl1.5 or Li10GeP2S12 exhibit distinct failure behavior toward lithium metal due to short circuit by lithium dendrite penetration for Li5.5PS4.5Cl1.5 and increased overpotential by electrolyte decomposition for Li10GeP2S12. The bilayer construction of Li/Li5.5PS4.5Cl1.5/Li10GeP2S12 shows excellent interface stability even at high current density, in which the Li5.5PS4.5Cl1.5 layer as buffer layer is to isolate Li10GeP2S12 from lithium metal and the Li10GeP2S12 can prevent the lithium dendrite penetration [20]. Clearly, designing an artificial passivation interface layer by more convenient method is crucial to stabilize Li/Li10GeP2S12 interface, while the reported approaches generally involve complicated reaction process or electrolyte multilayer structures.

    Considering the severe reaction between sulfide electrolytes and moisture in air, interestingly, it is found that short-period air exposure of sulfide electrolytes with controlled humidity could provide effective passivation against lithium metal. The dramatically improved interface stability between Li10GeP2S12 solid electrolyte and lithium metal is achieved by simply exposing the Li10GeP2S12 pellet into air for dozens of seconds. This air-exposure treatment could rapidly generate a protective layer of Li4P2S6, GeS2 and Li2HPO3 coated on the surface of the Li10GeP2S12 pellets. This protecting layer is ionically conductive but electronically insulation, which can not only physically isolate the contact between Li10GeP2S12 and lithium metal but also effectively suppress the continuous decomposition of Li10GeP2S12 reduced by lithium metal.

    The synthesis of Li10GeP2S12 solid electrolytes can be found elsewhere [21]. The room temperature ionic conductivity of 6.13 10-3 S cm-1 and its X-ray diffraction (XRD) pattern is shown in figure S1 (available online at stacks.iop.org/MF/1/021001/mmedia). The Li10GeP2S12 pellet (10 mm diameter, 1 mm thickness) was prepared by cold pressing 150 mg of Li10GeP2S12 powder under 180 MPa. For the air-exposure treatment of Li10GeP2S12 electrolytes, both side of the Li10GeP2S12 pellet were separately exposed to air in a constant temperature of 30 C and humidity chamber with 45% humidity for different durations. Before one side of the Li10GeP2S12 pellet was exposed to air, the other side was sealed to avoid secondary exposure. Air-exposed Li10GeP2S12 electrolytes with duration of 40 s is labeled as 40 s air-exposed Li10GeP2S12.

    To identify the composition of interfacial layer of the air-exposed Li10GeP2S12 pellets, XRD measurements were performed on Bruker D8 Advance Diffractometer with Cu K radiation ( = 1.54178 ). The EIS measurements for the symmetric cells were tested using Solartron 1470E electrochemical workstation (Solartron Public Co., Ltd) from 1 MHz to 0.1 Hz under 10 mV at 25 C. Surface and cross-section morphology of Li10GeP2S12 pellet before and after air exposure were investigated by a scanning electron microscope (Regulus-8230, Hitachi).

    The lithium metal foils with thickness of 80 m were used as electrode to assemble the symmetric cells and solid-state lithium metal batteries. To prepare the Li metal symmetric cells, two pieces of metallic lithium foils were attached on both sides of the electrolyte pellet and vacuum sealed in a pouch bag. Then the cells were isostatically pressed under 50 MPa for 5 min. The stainless steel attached with nickel tag was used as current collector. For testing the impedance of the symmetric cells after cycling tests, the galvanostatic Li plating/stripping was performed at 0.1 mA cm-2 and 0.1 mAh cm-2 under 25 C. To fabricate the all-solid-state lithium metal batteries, the composite cathode was prepared by mixing LiNbO3-coated LiCoO2 and Li10GeP2S12 powders with 70:30 weight ratio. The composite cathode (2 mg cm-2) powder was spread on one side of Li10GeP2S12 pellet and pressed at 180 MPa to obtain the integrated cathode-electrolyte pellet. The lithium metal was attached on the other side of electrolyte pellet and sealed in pouch bag. Before assembling the air-exposed Li10GeP2S12 based solid-state batteries, the side of Li10GeP2S12 pellet integrated with cathode powder was sealed to avoid exposing to air. Charge/discharge measurements were conducted between 3.0 and 4.2 V at 25 C using a multichannel battery test system (LAND CT-2001A, Wuhan Rambo Testing Equipment Co., Ltd).

    As shown in figure 1(a), in contrast with the nearly liner increasing Li plating/striping voltage for the symmetric Li/Li10GeP2S12/Li cell without air-exposure treatment, the Li/air-exposed Li10GeP2S12/Li cells show obviously sluggish increasement of the potential. The air-exposure durations were set at 10, 20, 30, 40, and 50 s. In addition, the suppressed increasement of impedance for the Li/air-exposed Li10GeP2S12/Li cells was directly observed during the electrochemical cycling. Figure 1(b) presents the impedance of the Li/Li10GeP2S12 or air-exposed Li10GeP2S12/Li cells for the cycling tests. It can be clearly found that the continuously increasing impedance arising from strong reaction at Li/Li10GeP2S12 interface was dramatically suppressed when the air-exposure treatment for Li10GeP2S12 pellets was employed. Figure 1(c) presents the voltage of the symmetric Li/Li10GeP2S12 or air-exposed Li10GeP2S12/Li cells before and after cycling. The Li/Li10GeP2S12/Li symmetric cell shows much higher polarization voltage than that of air-exposed Li10GeP2S12 based symmetric cells before cycling, which is due to the decomposition reaction occurred once the Li10GeP2S12 solid electrolytes contact with Li metal during assembling the symmetric cells. However, the obviously suppressed increasement of the voltage after cycling was detected after short-time exposure of 10 s. With increased air-exposure durations, such as 40 s and 50 s, the Li plating/striping voltages perform negligible increase even after 400 h cycling, which clearly demonstrates that the air-exposure treatment can effectively stabilize the Li/Li10GeP2S12 interface. Whereas, the impedance of the Li/air-exposed Li10GeP2S12/Li symmetric cells nearly linear increases with the air-exposure durations (figure 1(d)), which implies that the air-exposure treatment introduced a low ionically conducting layer at the interface. Moreover, the difference value of the impedance of the Li/air-exposed Li10GeP2S12/Li cells for cycling tests ( Rt = Rt, (400 h) - Rt, (0 h)) were evaluated. As presented in figure 1(e), the symmetric cells using Li10GeP2S12 with an optimal exposure duration of 40 s exhibit the smallest value of the impedance changes, showing the decreased impedance for the Li/40 s air-exposed LGPS/Li symmetric cell after cycling. Specifically, compared with the impedance of around 660 before cycling, the impedance decreases to around 487 after 400 h cycling (figure 1(f)). The decreased impedance could be attributed to the improved interfacial contact between the decomposition layer and Li metal due to the volume expansion of lithium metal during repeat plating/striping processes [18].

    Figure  1.  Evaluation of the Li/Li10GeP2S12 interface stability through Li plating/striping experiments and evolution of impedance for the symmetric Li/Li10GeP2S12 or air-exposed Li10GeP2S12/Li cells. (a) Cyclic performance of the Li/Li10GeP2S12 or air-exposed Li10GeP2S12/Li cells at 0.1 mA cm-2 and 0.1 mAh cm-2. (b) EIS plots of the symmetric Li/Li10GeP2S12 or air-exposed Li10GeP2S12/Li cells before cycling and after different cycling time. (c) Li plating/striping voltages of the Li/Li10GeP2S12 or air-exposed Li10GeP2S12/Li cells before and after cycling. (d) Total impedance (Rt) of the Li/air-exposed Li10GeP2S12/Li cells before cycling. (e) Difference value of the total impedance of the Li/air-exposed Li10GeP2S12/Li cells for cycling tests ( Rt = Rt (400 h) - Rt (0 h)). (f) Evolution of the total impedance (Rt) of the Li/40 s air-exposed Li10GeP2S12/Li cells for cycling tests.

    Figure 2(a) shows the galvanostatic Li plating/striping of the Li/40 s air-exposed Li10GeP2S12/Li and the Li/Li10GeP2S12/Li cells. The Li/Li10GeP2S12/Li cell shows a rapid increase in polarization voltage due to the continuous and deteriorative Li/Li10GeP2S12 interface reaction. In contrast, the Li/40 s air-exposed Li10GeP2S12/Li cell presents improved interface stability with small polarization voltage of 26 mV after 1000 h cycling. Moreover, the rate capability of the Li/40 s air-exposed Li10GeP2S12/Li cell was evaluated in figure 2(b). When the current densities are set at 0.2 or 0.4 mA cm-2, the polarization voltage is steady. However, gradual rise of polarization voltage was observed with increasing of current density to 0.6 and 0.8 mA cm-2. Nevertheless, the Li/40 s air-exposed Li10GeP2S12/Li cell can still stably cycle for 300 h at 0.2 mA cm-2 under an areal capacity of 0.5 mAh cm-2 (figure 2(c)).

    Figure  2.  Galvanostatic Li plating/striping of the Li/40 s air-exposed Li10GeP2S12/Li cells. (a) Cyclic performance of the Li/40 s air-exposed Li10GeP2S12/Li cell at 0.1 mA cm-2 and 0.1 mAh cm-2. The Li/Li10GeP2S12/Li cell is also shown for comparison. (b) Rate capability at different current density and (c) cyclic performance at 0.2 mA cm-2 and 0.5 mAh cm-2 of the Li/40 s air-exposed Li10GeP2S12/Li cell.

    To understand the mechanism of the protective layer for improving the Li/Li10GeP2S12 interface stability, the composition of the formed protective layer through air-exposure treatment was identified. Generally, most sulfide solid electrolytes are not stable to moisture because they easily react with H2O by release of toxic H2S gas [10, 22, 23]. Calpa et al [24] reported their DFT calculation results that the hydrolysis of Li3PS4 would decompose into Li3PO4 and H2S. Ohtomo et al [9] experimentally detected the Li3PO4 phase after the 75Li2S·25P2S5 electrolytes reacting with water. However, the reaction products of Li10GeP2S12 and water are unclear. Through dissolving the Li10GeP2S12 powder into water followed by vacuum drying at 150 C for 3 h, the reaction products are determined to be Li3PO4 and Li4GeO4, as shown in figure S2. Noticeably, the Li3PO4 and Li4GeO4 were not observed on the surface of the air-exposed Li10GeP2S12 pellet, indicating a different reaction process occur during the air-exposure treatment. As shown in figure 3(a), for the Li10GeP2S12 pellet after 40 s air exposure, most of diffraction peaks can be indexed to Li10GeP2S12 phase [25, 26]. Only three diffraction peaks at 12.58, 14.60 and 17.56 belongs to Li10GeP2S12 phase disappear and two new diffraction peaks at 16.07 and 16.99 were detected. After 30 min air exposure, large amounts of new diffraction peaks were observed, indicating new phases formed on the surface of Li10GeP2S12 pellet. The diffraction peaks at 16.94, 27.08, 29.24, 32.04, 32.46, 34.32, 40.62 can be indexed to Li4P2S6 (PDF#01-076-0992), while 15.48, 16.94, 26.42, 28.82, 31.38 belong to GeS2 (PDF#00-030-0597) and 13.04, 26.42, 40.62 correspond to Li2HPO3 (PDF#00-035-0172). The XRD results suggest that a partial hydrolysis reaction occurs on the surface of the Li10GeP2S12 pellet after air exposure with formation of the mixed phases of Li4P2S6, GeS2 and Li2HPO3, where the Li4P2S6 is main phase as majority of diffraction peaks belong to it. The compound, Li4P2S6, have been reported to exhibit considerable ionic conductivity and good interface stability towards lithium metal [27-30], making it desirable for interface protection for Li10GeP2S12. Besides, both LiH2PO4 and Li3PO4 have been proven to be efficient protective layers for Li/solid electrolyte interface [16, 31-34], indicating phosphide, such as Li2HPO3, can stabilize the Li/Li10GeP2S12 interface. Figures S3 and S4 presents the surface and cross-section morphology of Li10GeP2S12 pellets before and after air exposure, showing the obvious decomposition layer coated on the surface of Li10GeP2S12 pellet. Figure 3(b) presents schematic illustrations of the mechanism of the protective layer formed by air exposure for stabilizing the Li/Li10GeP2S12 interface. For the Li/Li10GeP2S12 interface, a mixed conductive interface is formed when Li10GeP2S12 attaches with lithium metal, leading to continuously consume inner Li10GeP2S12 and increase the cell impedance. After exposing Li10GeP2S12 pellet in air, a passivating layer rapidly generated. On one hand, this layer can physically isolate the Li10GeP2S12 from lithium metal. On the other hand, this layer comprising of the Li4P2S6, GeS2 and Li2HPO3 is lithium-ion permeable but electronic obstructed, which can effectively suppress the decomposition of Li10GeP2S12 during the Li metal plating/striping.

    Figure  3.  Improvement of the interface stability between Li10GeP2S12 solid electrolytes and lithium metal through introducing a protective layer by air-exposure treatment. (a) XRD patterns of the Li10GeP2S12 pellets before and after 40 s and 30 min air exposure. (b) Schematic illustrations of the mechanism of the protective layer formed by air exposure for stabilizing the Li/Li10GeP2S12 interface.

    To further demonstrate the effect of the protective layer on stabilizing the Li/Li10GeP2S12 interface, the LiCoO2 based all-solid-state lithium metal batteries were fabricated by using both Li10GeP2S12 and 40 s air-exposed Li10GeP2S12 pellets as solid electrolyte. Figure 4(a) shows charge and discharge curves of the LiCoO2/Li10GeP2S12/Li battery, showing a rapid decay in specific capacity and large polarization after 5 cycles. In contrast, for the LiCoO2/40 s air-exposed Li10GeP2S12/Li battery, high reversible specific capacity and low degree of polarization are delivered (figure 4(b)). The LiCoO2/40 s air-exposed Li10GeP2S12/Li battery shows an initial charge specific capacity of 127 mA h g-1 with high initial Columbic efficiency of 92% and delivered long cyclic stability for 100 cycles with capacity retention of 80%, as shown in figure 4(c). The good rate performances of the LiCoO2/40 s air-exposed Li10GeP2S12/Li battery were also presented (figures 4(d) and (e)), exhibiting the discharge capacities of 113, 87, 66, 46 mAh g-1 at 0.1, 0.2, 0.5 and 1 C, respectively. The high reversible specific capacity and long cyclic stability strongly support the rapid generated protective layer by simple air-exposure treatment can effectively stabilize the Li/Li10GeP2S12 interface.

    Figure  4.  Electrochemical performances of all-solid-state lithium batteries. Charge and discharge curves of (a) the LiCoO2/Li10GeP2S12/Li battery and (b) the LiCoO2/40 s air-exposed Li10GeP2S12/Li battery at 0.1 C (1 C = 120 mA g-1) under 25 C. (c) Cyclic performances of the LiCoO2/Li10GeP2S12/Li and LiCoO2/40 s-air-exposed Li10GeP2S12/Li batteries at 0.1 C under 25 C. (d) Charge and discharge curves and (e) cyclic performances of the LiCoO2/40 s-air-exposed Li10GeP2S12/Li battery at different rates.

    In summary, the strong reactive Li/Li10GeP2S12 interface was effectively passivated via a rapid formed protective layer through simply exposing the Li10GeP2S12 pellet to air for dozens of seconds. The protective layer coated on the surface of the Li10GeP2S12 pellets is derived from the partial hydrolysis reaction of Li10GeP2S12 in air, generating the decomposition products of Li4P2S6, GeS2 and Li2HPO3. This lithium-ion permeable but electronic obstructed layer can both separate the contact and effectively suppress the decomposition reaction between Li10GeP2S12 and lithium metal during electrochemical cycling. After optimal air-exposure duration of 40 s, the Li/40 s air-exposed Li10GeP2S12/Li symmetric cell presents long cyclic stability for 1000 h with small polarization voltage of 26 mV at 0.1 mA cm-2. Compared with the LiCoO2/Li10GeP2S12/Li battery with rapid capacity decay after 10 cycles, the all-solid-state LiCoO2/40 s air-exposed Li10GeP2S12/Li battery shows long cyclic performances for 100 cycles with capacity retention of 80%, and good rate capabilities of discharge capacity of 113, 87, 66, 46 mAh g-1 at 0.1, 0.2, 0.5 and 1 C, respectively.

    The work was supported by the National Key R&D Program of China (Grant No. 2018YFB0905400), the National Natural Science Foundation of China (Grant Nos. U1964205, 51872303, 51902321 and 52172253), Zhejiang Provincial Key R&D Program of China (Grant No. 2022C01072), Ningbo S&T Innovation 2025 Major Special Programme (Grant Nos. 2019B10044 and 2021Z122) and Youth Innovation Promotion Association CAS (Y2021080).

    Conflict of interest

    The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

    Authors contributions

    Wei Weng: investigation, methodology, formal analysis, data curation, visualization, writing-original draft. Dong Zhou: visualization, validation. Gaozhan Liu, Lin Shen: methodology, visualization. Mengqi Li, Xinshuang Chang: validation. Xiayin Yao: conceptualization, supervision, project administration, funding acquisition, resources, writing-review and editing.

    Author to whom any correspondence should be addressed.

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