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Synthesis of Single Lithium-ion Conducting Polymer Electrolyte Membrane for Solid-State Lithium Metal Batteries Guangmei Luo, Bing Yuan, Tianyun Guan, Fangyi Cheng, Wangqing Zhang, and Jun Chen ACS Appl. Energy Mater., Just Accepted Manuscript • DOI: 10.1021/acsaem.9b00440 • Publication Date (Web): 30 Apr 2019 Downloaded from http://pubs.acs.org on May 1, 2019

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is published by the American Chemical Society. 1155 Sixteenth Street N.W., Washington, DC 20036 Published by American Chemical Society. Copyright © American Chemical Society. However, no copyright claim is made to original U.S. Government works, or works produced by employees of any Commonwealth realm Crown government in the course of their duties.

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ACS Applied Energy Materials

Synthesis of Single Lithium-ion Conducting Polymer Electrolyte Membrane for Solid-State Lithium Metal Batteries Guangmei Luo,† Bing Yuan,† Tianyun Guan,† Fangyi Cheng,*‡ Wangqing Zhang,

and

Jun Chen‡ †Key

Laboratory of Functional Polymer Materials of the Ministry of Education, Institute of

Polymer Chemistry, College of Chemistry, Nankai University, Tianjin 300071, China. ‡Key

Laboratory of Advanced Energy Materials Chemistry of the Ministry of Education,

College of Chemistry, Nankai University, Tianjin 300071, China. Collaborative Innovation Center of Chemical Science and Engineering (Tianjin), Nankai University, Tianjin 300071, China. *To

whom correspondence should be addressed. E-mail: [email protected] (F. C.)

and [email protected] (W. Z.), Tel: 86-22-23509794, Fax: 86-22-23503510.

1

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Abstract: Synthesis of single lithium-ion conducting polymer electrolyte membrane (SLIC-PEM)

composed

of

polymerized

lithium

4-styrenesulfonyl(trifluoromethylsulfonyl)imide (PLiSTFSI), poly(ethylene glycol) methyl ether methacrylate (PEGM), poly(ethylene glycol) dimethacrylate (PEGDMA) and ethylene carbonate (EC) is reported. SLIC-PEM combines the advantages of single lithium-ion conducting polymer electrolytes, cross-linked flexible polymer electrolytes and the liquid electrolyte of carbonate. The synthesized SLIC-PEMs have superior thermostability, high ionic conductivity, wide electrochemical window and high lithium ion transference number. The corresponding LiFePO4|SLIC-PEM|Li cell delivers high Coulombic

efficiency,

excellent

discharge

capacity

and

cycling

performance,

demonstrating that SLIC-PEMs will have promising application in next-generation safe lithium metal batteries. Key Words: single lithium-ion conductor, polymer electrolytes, lithium metal batteries, lithium ion transference number, membrane

2


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Recently, lithium ion batteries (LIBs) have been widely used as energy storage and conversion devices in many fields ranging from portable electronics to electric vehicles.1 However, safety issues such as leakage, combustion and explosion deriving from flammable liquid electrolytes have been one of the major bottlenecks. Solid polymer electrolytes (SPEs), composed of a lithium salt associated with a polar polymer matrix,2 have been regarded as promising candidates for replacing liquid electrolytes in LIBs. However, SPEs always suffer from either insufficient room temperature conductivity or low lithium ion transference number,3 which restrains SPEs to be applied to large-scale commercial production. Thus, one strategy to design high-performance SPEs is to synthesize SPEs with high transference number, which is known as single lithium-ion conducting SPEs.4 In single lithium-ion conducting SPEs, anions are immobilized by trapping agents or by anchoring to polymer backbones, leading to lithium ion transference number approaching to unity.5-16 The advantages of single lithium-ion conducting SPEs have been studied theoretically,17,18 such as elimination of concentration polarization and improvements in power and energy densities. Besides, theoretical and experimental studies19-21 suggest that single lithium-ion conducting SPEs can suppress growth of lithium dendrites. Despite aforementioned advantages of single lithium-ion conducting SPEs, most of them suffer from inferior ionic conductivity.4 To improve ionic conductivity of single lithium-ion conducting SPEs, several strategies such as copolymerizing,22-25 blending26-30 and adding plasticizer31-42 have been tried. Among which, adding plasticizer is considered to be the most effective approach,43 yet the mechanical strength is sacrificed. Therefore, preparing single lithium-ion conducting SPEs with high ionic conductivity as well as high 3




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reported by Armand et al.,5 and its high purity was confirmed by 1H NMR (Figure S1). Then by free radical copolymerization in the solvent of EC under mass ratio of [LiSTFSI]0:[PEGM]0:[PEGDMA]0:[EC]0 = 5~20:35~20:10:50 in the Teflon mold under argon atmosphere at 70 °C for 12 h, transparent SLIC-PEM was formed. By changing the ratio of the feeding ingredients, SLIC-PEMs with different chemical compositions as summarized in Table S1 were synthesized. By checking the as-synthesized SLIC-PEM by FTIR (Figure S2), it was found that almost all the monomers were completely polymerized. Herein, the thickness of SLIC-PEM was set at 300 ± 30 Q

which is decided by inner area

in the Teflon mold and the amount of feeding ingredients. SLIC-PEMs can be easily cut into discs and strips, and they can be further bent and knotted without breakage (Figure 1A), indicating that SLIC-PEM is flexible and therefore is suitable for battery fabrication. Also, SLIC-PEM is transparent, the typical SLIC-PEM5 is just slightly inferior to glass slide 7101 (Figure 1B). This possibly indicates all the ingredients are highly compatible and homogeneously distributed in SLIC-PEM. A control experiment of polymerization in absence of the PEGDMA crosslinker is also performed and samples with macro-phase separation are formed (Figure S3). This suggests that there maybe exist microphase separation with a scale less than 0.1 microns in SLIC-PEM, although SLIC-PEM is transparent. The compression test indicates that SLIC-PEM is flexible, and SLIC-PEM5 breaks at 34% compressive strain under 0.513 MPa compressive stress, and the calculated compression modulus is 0.114 MPa for cylindrical sample (Figure 1C). This character of compression resistance affords sufficient contact between electrolytes and electrodes in LIBs, which is very helpful to fabricate LIBs using 6


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SLIC-PEM. Differential scanning calorimeter (DSC) analysis indicates two glass transition temperatures (Tgs) (Figure S4, Table S1) in SLIC-PEMs, and this suggests formation of gradient copolymers due to the different monomer activity. It is thought the lower Tg around -51.0 ~ -36.4 °C is ascribed to the PEGM/PEGDMA-rich phase and the higher Tg around 100.8 ~ 106.3 °C is ascribed to the PLiSTFSI-rich phase. Note: the weight fractions in each phase can be roughly calculated based on equation S1, and the results are summarized in Table S1. Figure 1D displays the thermogravimetric analysis (TGA) of SLIC-PEM5, from which approximately 5% weight loss is observed at about 100 °C and then extends to 50% weight loss at 180 °C. The weight loss before 200 °C is mainly ascribed to EC volatilization. Even so, SLIC-PEM presents sufficient thermal stability under common working temperature below 100 °C. Figure 1E depicts the thermal tolerance of SLIC-PEM5 and a commercial Celgard 2400 separator. After thermal treating of 110 °C for 12 h, SLIC-PEM5 can maintain its initial shape while the Celgard 2400 separator shrinks from the diameter of 16 mm to 14 mm, which demonstrates excellent thermal tolerance of SLIC-PEM. The leakage and volatilization of ethylene carbonate in SLIC-PEM5 was further checked. As shown in Figure 1F, 21 % weight loss of SLIC-PEM5 at 80 °C and 33% weight loss at 100 °C in 90 h are observed due to volatilization of EC under an open environment, and at 30 °C SLIC-PEM5 keeps an almost constant weight for 10 days, suggesting that SLIC-PEM5 exhibits superior solvent retention capacity. In a sealed cell, this volatilization of EC can be greatly depressed. The flexibility, sufficient thermal stability and superior solvent retention capacity of SLIC-PEM5 afford great promise in LIBs, which will be discussed subsequently. 7



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The 30 °C ionic conductivity calculated by equation S2 and static dielectric constants ( s) of the SLIC-PEMs synthesized at different recipes are summarized at Table S1. The ionic conductivity of SLIC-PEM is firmly correlative to the mass ratio of LiSTFSI or the fraction of PLiSTFSI, and it increases with the increasing content of PLiSTFSI to the maximum of ~1.8×10-4 S cm-1 at 15 wt% PLiSTFSI (SLIC-PEM5), and then it decreases when the fraction of PLiSTFSI further increases (Figure S5, Entries 1-7 in Table S1). the SLIC-PEMs follows the similar trend and SLIC-PEM5 has the highest

s

s

of

at 58.7,

indicating the polarizability volumes of the Li-anion ion pairs possibly overlap at the ion content of SLIC-PEM5.44 This phenomenon can be ascribed to the saturation of lithium ion in SLIC-PEM. That is, when the content of PLiSTFSI is lower than 15 wt%, lithium ions tend to dissociate and the dissociation contributes to the increase of ionic conductivity. While with PLiSTFSI content above 15 wt%, formation of ion clusters leads to the decrease of ionic conductivity.45 Besides, EC is also essential for the high ionic conductivity of SLIC-PEM (Entries 8-11 in Table S1), the SLIC-PEM synthesized in absence of EC has poor ionic conductivity as low as 9.85×10-7 S cm-1. It is thought that EC increases Li+ dissociation and therefore improves the ionic conductivity. Besides, EC can act as plasticizer for SLIC-PEM, and it ensures flexibility of SLIC-PEM. However, at the case of EC fraction higher than 50%, e.g., the samples with 60 wt% EC become brittle and those with 70 wt% EC are easily broken, and therefore these SLIC-PEMs are not employed. Furthermore, PEGM and PEGDMA are also essential (Entries 12-14 in Table S1), and the former contains ethylene oxide (EO) brush side-chains46,47 and therefore enhances ion conduction, and the latter forms cross-linking network to improve mechanical strength of 8


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SLIC-PEM, respectively. Besides, the EO segments in the cross-linker can also enhance ion conduction of SLIC-PEM.

(B) 0.5

10 1 2 3 4 5 6 7 11 13 14

1

0.1

0.01 2.9

3.0

3.1

3.2

3.3

3.4

3.5

0.4 0.3 0.2 0.1 0.0 -0.1 -0.2 -0.3 -0.4 -0.5 0

1000/T (K-1)

(C) 40

2

(D)2.0 Initial Steady

160

80 40 0 50

100

150

200

3

4

5

6

7

250

300

0.4

0.1 mA cm-2

1.6

120

Voltage (V)

-Z''(ohm)

1

Potential (V)

200

38 36 34 32 30 28 26 24 22

4.8 V

350

Voltage (V)

2.8

Currnet (mA)

Conductivity (×10-4 S cm-1)

(A)

Current (8A)

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60


1.2

0.2 0.0 -0.2

0.8

-0.4 520

0.4

524

528

532

Time (h)

Z' (ohm)

0.0 -0.4

0

500

1000

1500

2000

0

Time (s)

200

400

600

800

1000

Time (h)

Figure 2. Temperature-dependent ionic conductivity of SLIC-PEMs from 25 to 80 °C (A, in the plots the number x refers to the sample of SLIC-PEMx); LSV curve of SLIC-PEM5 in SS|SLIC-PEM5|Li battery at 30 °C from 0 to 7 V (B, scanning rate: 1.0 mV s-1); DC polarization profile of a Li|SLIC-PEM5|Li cell under 10 mV polarization voltage (C, inset is the EIS spectra before and after polarization, 5 mV AC amplitude, 0.1~106 Hz); lithium plating/stripping curve of SLIC-PEM5 using a Li|SLIC-PEM5|Li cell (D, current density: 0.1 mA cm-2, inset is the enlargement around 520 h). Figure 2A depicts the temperature-dependent ionic conductivity of SLIC-PEMs at temperature range from 25 to 80 °C at intervals of 5 °C. It is found that a linear dependence between the logarithmic conductivity and reciprocal temperature in SLIC-PEMs, which can be perfectly fitted by the Arrhenius equation, and the calculated activation energy of the

9



optimized SLIC-PEM5 is 0.257 eV, indicating easy movement of lithium ions in SLIC-PEM5.48,49 The ionic conductivity of SLIC-PEM5, 1.56×10-4 S cm-1 at 25 °C and 1.83×10-4 S cm-1 at 30 °C, is calculated according to the impedance plots, which is almost satisfactory for practical LIBs operation. Another vital property for electrolytes applied in LIBs is the electrochemical stability. The electrochemical stability window of SLIC-PEMs was tested by linear sweep voltammetry (LSV) using SS|SLIC-PEM|Li battery, in which SS represents stainless steel. As shown in Figure 2B, there is no obvious anodic current peak until 4.8 V for SLIC-PEM5, indicating excellent electrochemical stability of SLIC-PEM5 at high voltage. The chemical composition exerts slight influence on electrochemical stability of SLIC-PEMs, and those synthesized in absence of EC generally have high electrochemical stability (Table S1). As reported previously,50 the electrochemical stability window of electrolytes is mainly related to decomposition of anions in cathode. In SLIC-PEM, anions covalently anchored on polymer network can hardly migrate in a long distance, which avoids decomposition of most anions on cathode surface and therefore ensures electrochemical stability. Lithium ion transference number (tLi+) plays an important role in charging and discharging of LIBs, and a large tLi+ can reduce concentration polarization and suppress undesirable side reactions of anions on electrodes and thus enhances battery performance in practical application.51 Herein, the lithium ion transference number (tLi+) is evaluated according to the method proposed by Abraham et al,52 which is a slight revision of the classical method developed by Peter Bruce,53 by combining potentiostatic DC polarization and electrochemical impedance spectroscopy. All SLIC-PEMs have relatively high tLi+ 10


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exceeding 0.80 (Table S1). Figure 2C shows the DC polarization profile of a Li|SLIC-PEM5|Li cell. According to equation S3, the calculated tLi+ of SLIC-PEM5 is 0.91 (Table S2), exhibiting superior single lithium-ion conducting behavior. The high tLi+ value of SLIC-PEMs is ascribed to immobilization of anions in the polymer network. Figure 2D shows the time-dependent plating/stripping profile of the cell with SLIC-PEM5 as electrolyte over 1000 h at a constant current density of 0.1 mA cm-2 and at 30 °C. Noticeably, a stable overpotential of 0.18 V demonstrates that reversible lithium plating/stripping performance can be achieved in Li|SLIC-PEM5|Li cell, and no short circuit is observed. By checking fresh Li foil and Li electrode after cycling 1000 h with scanning electron microscope (SEM), a little bit dim but a uniform surface of Li electrode after cycling is observed (Figure S6), indicating no obvious dendrites growth, and therefore it is concluded that SLIC-PEM5 can suppress the dendrites growth effectively. The EIS spectra of Li|SLIC-PEM5|Li cell as function of the storage time is depicted in Figure S7. After the storage time of 10 days, the interfacial resistance remains changeless, and a relatively low interfacial resistance of 180 V for SLIC-PEM5 is obtained. This low interfacial resistance toward lithium electrode ensures superior interface compatibility, which is quite attractive in LIBs with lithium anode. The overall electrochemical properties of SLIC-PEMs are competitive in comparison with mostly single lithium-ion conducting polymer electrolytes reported previously (Table S3).

11



80 150

60 100

40

0.2 C, 26 °C 0.3 C, 26 °C

50

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0 0

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0 100

280

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0.2 C, 50 °C 0.5 C, 50 °C

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Numbers of cycles

40

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0 100

Coulombic efficiency (%)

100

200

(B) Discharge capacity (mAh g-1)

120

250

Coulombic efficiency(%)

Discharge capacity (mAh g-1)

(A)

Numbers of cycles

(C)

(D) T=26 °C

3.6 3.2 0.2 C, 50th cycle 0.3 C, 50th cycle

2.8

T=50 °C

4.0

Voltage (V)

4.0

Voltage (V)

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

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3.6 3.2 0.2 C, 50th cycle 0.5 C, 50th cycle

2.8

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2.4 0

20

40

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80 100 120 140 160

0

20

Capacity (mAh g-1)

40

60

80 100 120 140 160

Capacity (mAh g-1)

Figure 3. Cycling performance of LiFePO4|SLIC-PEM5|Li cell at 0.2 and 0.3 C at 26 °C (A); cycling performance of LiFePO4|SLIC-PEM5|Li cell at 0.2 and 0.5 C at 50 °C (B); charge-discharge curves of LiFePO4|SLIC-PEM5|Li cell at 0.2 and 0.3 C at 26 °C (C); charge-discharge curves of LiFePO4|SLIC-PEM5|Li cell at 0.2 and 0.5 C at 50 °C (D). To further confirm feasibility of SLIC-PEM in practical application, coin-type cells (CR 2032) were assembled using metallic Li anode and LiFePO4 cathode and their cycling performances were tested. Figure 3A reveals the charge-discharge profiles of the LiFePO4|SLIC-PEM5|Li cell obtained at a current rate of 0.2 C and 0.3 C (1 C = 170 mA g-1) with the cut-off voltage between 2.5 and 4.2 V at 26 °C. The initial discharge capacities are 153 mAh g-1 at 0.2 C and 130 mAh g-1 at 0.3 C, respectively. After 100 cycles, the capacity maintains ~141 mAh g-1 at 0.2 C and 120 mAh g-1 at 0.3 C with same capacity retention of 92%, and the Coulombic efficiencies at different current rates are virtually invariant above 99%, which demonstrates that SLIC-PEM5 delivers excellent cycling 12


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performance at room temperature around 26 °C. Besides, the cycling performance of LiFePO4|SLIC-PEM5|Li cell at a higher temperature of 50 °C was evaluated in the same way. As depicted in Figure 3B, the initial capacity is about 156.5 mAh g-1 at 0.2 C and 126.6 mAh g-1 at 0.5 C, respectively. After 100 cycles, the discharge capacity maintains 137.5 mAh g-1 at 0.2 C with the capacity retention of 88% and 126.3 mAh g-1 at 0.5 C with the capacity retention almost 100%, and the Coulombic efficiencies at both current rates are virtually invariant above 99%, which further confirms that SLIC-PEM5 is potential in practical application in lithium metal battery. Furthermore, discharge capacity of Li|SLIC-PEM5|LiFePO4 cell at different discharge rate at 26 °C and 50 °C was shown in Figure S8. At higher current rate of 1.0 C, the discharge capacity of 97 mAh g-1 at 50 °C is relatively high, which is definitely attractive for SLIC-PEM. In addition, as shown in Figure 3C and Figure 3D, the overpotential of SLIC-PEM5 is found to be 0.15 V at 0.2 C and 0.2 V at 0.3 C at 26 °C, and 0.1 V at 0.2 C and 0.15 V at 0.5 C at 50 °C, respectively, which indicates reduced polarization in SLIC-PEM. In short, the cell assemblied with SLIC-PEM presents considerable cycling performance, which is due to excellent ionic conductivity, high transference number and lower interfacial resistance of SLIC-PEM. In conclusion, synthesis of cross-linked SLIC-PEM via free radical polymerization is proposed. The cross-linked SLIC-PEM combines the advantages of single-ion conducting SPEs, cross-linked polymer electrolytes and carbonate, such as achieving high lithium ion transference number, high ionic conductivity and sufficient flexibility. The synthesized SLIC-PEM possesses considerable thermal stability and interfacial compatibility with lithium anode. Moreover, SLIC-PEM presents a decent ionic conductivity of ~1.8×10-4 S 13



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cm-1 at 30 °C, an excellent lithium ion transference number of 0.91 and a superior electrochemical

stability

window

up

to

4.8

V

vs.

Li+/Li.

The

fabricated

LiFePO4|SLIC-PEM|Li cell exhibits remarkable cycling performance with discharge capacity of 141 mAh g-1 at 0.2 C after 100 cycles and Coulombic efficiency over 99% at 26 °C. Besides, the cell delivers discharge capacity of ~126 mAh g-1 at 0.5 C after 100 cycles at 50 °C with the Coulombic efficiency of 99.7%. This SLIC-PEM is believed to have promising application in next-generation safe LIBs.

ASSOCIATED CONTENT Supporting Information. The experimental details and supplementary Figures can be found in the Supporting Information. AUTHOR INFORMATION Corresponding Authors *E-mail: [email protected] (F. C.) and [email protected] (W. Z.). Notes The authors declare no competing financial interest. ACKNOWLEDGMENTS The financial support by the National Science Foundation for Distinguished Young Scholars (No. 21525419), the Ministry of Science and Technology of the People's Republic of China (2016YFA0202503) and the Science and Technology Commission Foundation of Tianjin (No. 15JCZDJC40800) is gratefully acknowledged. REFERENCES 1.

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Synthesis of Single Lithium-Ion Conducting ... - ACS Publications

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