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Concentrated electrolytes for rechargeable lithium metal batteries
doi: 10.1088/2752-5724/acac68
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Abstract: Traditional lithium-ion batteries with graphite anodes have gradually been limited by the glass ceiling of energy density. As a result, lithium metal batteries (LMBs), regarded as the ideal alternative, have attracted considerable attention. However, lithium is highly reactive and susceptible to most electrolytes, resulting in poor cycle performance. In addition, lithium grows Li dendrites during charging, adversely affecting the safety of LMBs. Therefore, LMBs are more sensitive to the chemical composition of electrolytes and their relative ratios (concentrations). Recently, concentrated electrolytes have been widely demonstrated to be friendly to lithium metal anodes (LMAs). This review focuses on the progress of concentrated electrolytes in LMBs, including the solvation structure varying with concentration, unique functions in stabilizing the LMA, and their interfacial chemistry with LMA.
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Figure 1. (a) The overview of the available electrolytes. (b) The distribution map of non-aqueous liquid electrolytes with the weight and volume ratios of salt-to-solvent. The A, B and D regions are solvent-in-salt electrolytes, in which the ratio of salt-to-solvent is over 1.0 by volume or weight. The C region is [solvent] > [salt] by weight and volume. (a) and (b) Reproduced from [20], with permission from Springer Nature. (c) Schematic diagram of the solvation structure varied with the salt concentration.
Figure 2. Multiple functions of the concentrated electrolyte in lithium metal batteries. (a) Left: fluctuation diagrams of the LUMO levels of the anode and electrolyte components in LMBs as a function of concentration, where the numbers indicate the reaction order of the lithium anode and electrolyte components. Right: CEI layer formation mechanism in the dilute and concentrated electrolyte. Reproduced from [23]. CC BY 4.0. (b) The Al current collector corrosion in conventional LiPF6-based electrolytes, dilute LiFSI/AN electrolytes, and high concentration LiFSI/AN electrolytes. [30] John Wiley & Sons. [© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim]. (c) The polysulfide dissolution varied with the concentration (LiTFSI in DOL/DME). Reproduced from [20], with permission from Springer Nature. (d) Flame tests of a commercial dilute electrolyte (1.0M LiPF6 in EC/DMC (1:1, v/v)) and the concentrated electrolyte (LiFSI-1.1DMC (in mol)). Reproduced from [31]. CC BY 4.0.
Figure 3. (a), (b) Schematic diagram of corresponding Li growth mechanism in the dilute electrolyte (a) and fluorine-donating concentrated electrolyte (b). Reproduced with permission from [32]. © 2018 National Academy of Science. (c), (d) Calculated electronic structures (projected density of states, pDOS) of dilute (c) and concentrated (d) LiTFSI/AN electrolytes. Reproduced from [33], with permission from Springer Nature. The C 1s (e), F 1s (f), and N 1s (g) XPS spectra of the pristine NMC333 cathode and the NMC333 cathode after 60 cycles in the LiFSI-1.4DME (in mol) electrolyte (2.7-4.3 V voltage window). Reprinted with permission from [34] Copyright (2019) American Chemical Society. (h) Cycling performance of NMC622||Li batteries in 10 M LiFSI EC/DMC and 1 M LiPF6 EC/DMC electrolytes with 2.7-4.6 V cutoff voltage. Reprinted from [35], Copyright (2018), with permission from Elsevier.
Figure 4. (a) Schematic of carbonate-derived (organic-rich) CEI formed on the surface in 1 M electrolyte. (b) Schematic of inorganic-rich CEI formed on the surface in 3 M electrolytes. (c) The amount of transition metal deposited on the different cycled lithium plates in 1 M and 3 M electrolytes at 2 C. (a)-(c) Reproduced from [55]. CC BY 4.0. (d) The color changes of four samples with different salt concentrations containing the same amount of Li2S8 were recorded by the digital camera along with time: 0mol per l solvent, 2#: 2mol per l solvent, 4#: 4mol per l solvent, 7#: 7mol per l solvent. (e) Ultraviolet-visible spectrophotometry. (d) and (e) Reproduced from [20], with permission from Springer Nature.
Figure 5. (a)-(c) Schematic illustrations of the behavior of Al electrodes in (a) conventional LiPF6-based electrolyte, (b) dilute LiFSI/AN electrolyte with a considerable amount of free solvent molecules, and (c) highly concentrated LiFSI/AN electrolyte without free solvent molecules. (a)-(c) [30] John Wiley & Sons. [© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim]. (d) Al corrosion in 1 m FF (1 m LiFSI in FEC) and 7 m HFF (7 m LiFSI in FEC) at the constant current (0.5 mA) charge to 5 V. Optical microscopy images (OMIs) of (d, 1) fresh Al foil, (d, 2) OMIs of Al foil in 1 m FF electrolyte after charging 1 h at 0.5 mA, and (d, 3) OMIs of Al foil in 7 m HFF after charging into 5 V at 0.2 mA. Reproduced with permission from [32]. © 2018 National Academy of Science. (e) LSV of an Al electrode in various concentrations of LiFSI/DMC electrolytes in a three-electrode cell. The scan rate was 1.0mVs-1. The insets are scanning electron microscopy images of the Al surface polarized in the dilute 1:10.8 (in mol, left) and high concentration 1:1.1 (in mol, right) electrolytes. The white scale bar represents 20
m. Reproduced from [31]. CC BY 4.0. 
Figure 6. (a), (b) Combustion test of 10 mAh pouch-type cells charged to 4.2 V: 4 M LiFSI in PC/FEC (93:7 v/v) (a) and 4 M LiTFSI in DOL/DME (1:1 v/v) (b) inset shows the result of 1 M LiTFSI in DOL/DME. (c) Capacity retention of 10 mAh pouch-type cells charged to 4.2 V after high-temperature storage test (60 C/24 h). (a)-(c) Reproduced from [65]. CC BY 4.0. (d) Thermogravimetric analysis (TGA) curves of the electrolytes with different salt concentrations. Commercial: 1 M LiPF6 in EC/DEC (1:1, v/v), TMP-1: 1 m LiFSI in TMP, TMP-2: 2 m LiFSI in TMP, TMP-4: 4 m LiFSI in TMP, TMP-6: 6 m LiFSI in TMP. Reprinted with permission from [66]. Copyright (2021) American Chemical Society.
Figure 7. CE of Li||Cu half-cells using different electrolytes. Among them, the abscissa represents solvent types. 1: DME, 2: DOL, 3: DME/DOL, 4: carbonate, 5: phosphate, 6: sulphone, 7: nitrile. Different colored dots represent use of different lithium salts.
Figure 8. Comparison of the properties and performance of concentrated electrolytes and conventional dilute electrolytes.
Table 1. Coulombic efficiency and performances of the concentrated electrolyte in Li ||| Cu cells and Li metal batteries tested under different conditions.
Electrolyte Composition Test Conditions Cycling Performance CE(Li || Cu) CE(LMB cell) References 4 M LiFSI in DME Cu || LiFePO4 (1.6 mAh cm-2) 60% capacity after 50 cycles 99.1% >99.8% [79] LiFSI- 1.4DME (in mol) Li (450 m) || NMC333 (1.5 mAh cm-2) 92% capacity after 500 cycles 99.81% (300 cycles) [46] 2LiFSI-LiTFSI-4.8DME (in mol) Li (150 m) || NMC622 (1.44 mAh cm-2) 88% capacity after 300 cycles 98.2% (200 cycles) 98.6% (54 cycles, AFLMB (Cu || NCM622)) [80] 1 M LiFSI + 2 M LiTFSI in DOL/DME (1:1, v/v) Li|LiFePO4 (6.71 mg cm-2) 95.7% capacity after 100 cycles 98.7% (200 cycles) 99.40% (100 cycles) [81] 1 M LiTFSI + 2 M LiFSI + 3 wt% LiNO3 in DME/DOL (1:1 v/v) Li (600 m,excess 100) || LiFePO4 (5 mg cm-2) 92% capacity after 500 cycles 99.1% (450 cycles, excess Li 4) 99.8% (500 cycles) [47] Li (excess 0.44) || LiFePO4 (5 mg cm-2) 83% capacity after 100 cycles 99.8% (70 cycles) 2 m LiFSI + 2 m LiFTFSI in DOL/DME (1:1 v/v) Li (600 m) || LiFePO4 >92% (200 cycles) >95% [82] 4 m LiFSI in DOL + 3 wt% LiNO3 Li (7 m) || LiFePO4 (2.5 mAh cm-2) (electrolyte 60 l) 78.7% capacity after 120 cycles 99.14% (8.0 mA cm-2, 240 cycles) 99.7% (120 cycles) [83] 2.5 M LiFSI + 0.75 M LiNO3 in DOL Li || LiFePO4 no significant capacity decay within more than 100 cycles 98.8% (400 cyles) [84] 2 M LiFSI + 0.2 M LiNO3 in DME Li (500 m) || LiFePO4 (2 mAh cm-2) (electrolyte 40 l) 80% capacity after 500 cycles [85] 2 M LiFSI + 2 M LiNO3 in DME Cu || LiFePO4 (14 mg cm-2) 52.7% capacity after 100 cycles 98.50% (425 cycles) [86] Cu || NCM622 (12.5 mg cm-2) 47.3% capacity after 100 cycles 3 m LiFNFSI in DOL/DME (1:1, v/v) Li (600 m) || LiFePO4 (9.2 mg cm-2) 98.5% capacity after 200 cycles (First capacity 163 mAh g-1) 97% (180 cycles) 99.8% (200 cycles, ICE = 87.5%) [87] 4M LiFSI in DME Li || Cu (electrolyte 75 l, 4mAcm-2) 98.4% (1000 cycles) [88] 1.5 M LiTFSI + 0.2 M LiDFOB in DME/BN (3:1, v/v) + 5 wt% FEC Li (1.8-2.0 mg cm-2) || NCM523 (2.2-2.5 mg cm-2) 88.84% capacity after 150 cycles (-10 C) 99.96% (500 cycles, -10 C) [89] 4 M LiFSI in DME (can also expressed as LiFSI-1.4DME (in mol)) Cu || LiFePO4 (13.9 0.1 mg cm-2) 21.5% capacity after 100 cycles 98.9% (100 cycles) 98.2% (100 cycles) [90] Li (450 m)|FeS2 (4.3 0.1 mg cm-2) 34.4% capacity after 100 cycles 99% (100 cycles) 3 M LiFSI in DME Li (750 m) || S (1 mg cm-2) (60 C) 77% capacity after 1000 cycles 100% [58] 7 m LiTFSI in DME/DOL(1:1, v/v) Li || S 74% capacity after 100 cycles 100% (ICE = 93.7%) [20] 6 m LiFSI in DME (can also expressed as LiFSI-1.45DME (in mol)) Cu || Li1.37Ni0.8Co0.1Mn0.1O2 (31.25 mg cm2) (E/C ratio of 2 g Ah-1) 84% capacity after 100 cycles 93.2% (ICE) >99% (after 10 cycles) [11] 3 M LiTFSI in DOL/DME (1:1, v/v) Li (450 m) || S (1 mg cm-2) (electrolyte 60 l) 71.9% capacity after 200 cycles 96.60% (200 cycles) [91] 2 M LiTFSI + 2 M LiDFOB in DME Li (50 m) || NMC333 (1.7 mAh cm-2) 90% capacity after 300 cycles 94.60% (300 cycles) 99.8% [92] 5.5 mol LiTFSI per kg DOL/DME/TTE (5:5:2, v/v) Li(600 m) || NCM811(5 mg cm-2) (electrolyte 40 l) 100.20% [93] 7 m LiFSI in FEC (can also expressed as LiFSI-1.96FEC (in mol)) Li (10 m) || LiNi0.5Mn1.5O4 (1.43 mAh cm-2; N/P ratio = 1.4) 78% capacity after 130 cycles 97.7% (100 cycles) 99.64% (300-400 cycles) 99.0% [32] LiFSI- 1.1DMC (in mol) Gr || LiNi0.5Mn1.5O4 (electrolyte 160 l) >90% capacity after 100 cycles [31] Li || LiNi0.5Mn1.5O4 (electrolyte 160 l) >95% capacity after 100 cycles 100% 10 M LiFSI in EC/DMC (1:1, v/v) Li || NCM622 (2.5 mAh cm-2, 4.6 V) 86% capacity after 100 cycles 99.3% >99.6% (100 cycles) [35] 8 M LiFTFSI in EC/DMC (1:1, v/v) Li || Cu (0.2 mA cm-2) 98.5% [35] 4 M LiTFSI + 0.5M LiDFOB in FEC/DMC (3:7 v/v) Li (excess 3, full cell) || LiNi0.5Mn1.5O4 (1.8 mAh cm-2) (electrolyte 150 l, 4.9 V) 87.8% capacity after 100 cycles (full cell) 88.5% capacity after 500 cycles (half cell) >98% (900 cycles) 99.6% (500 cycles, half cell) [94] 2.5 mol LiFSI + 0.2 mol LiPF6 per kg FSA Li(60 m) || NCM622 (1.6 mAh cm-2) (electrolyte 40 l,) 89% capacity after 200 cycles 99.03% (400 cycles, ICE 91%) [95] 2.0 M LiDFOB + 1.4 M LiBF4 in FEC/DEC (1:2 v/v) Cu || NMC532 (3.1 mAh cm-2, pouch) 80% capacity after 200 cycles [96] LiFSI- 2TEP (in mol) + 0.05 M LiBOB + 5% FEC (by volume) Gr || LiCoO2 (29.4 mg cm-2) 91% capacity after 100 cycles >99% 99.8% (100 cycles, LIB) [22] Li || LiCoO2 (29.4 mg cm-2) 88% capacity after 350 cycles 99.7% (350 cycles, LMB) 1.5M LiFSI in TMP + 5% FEC Li || LiFePO4 (2 mg cm-2) 93.4% capacity after 100 cycles 95.07% (100 cycles) near 100% [97] LiFSI-3TMS (in mol) Li (50 m) || NCM333(1.5 mAh cm-2) (electrolyte 75 l) 75% capacity after 300 cycles 98.2% (150 cycles) >99.8% (300 cycles) [98] 0.52LiFSI- 1AN- 0.09VC (in mol) Li || NMC333 (1.8 mAh cm-2) 80% capacity after 400 cycles 99.2% [48] 
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