Facile synthesis and electrochemical properties of Na-rich anti-perovskite solid electrolytes

Peng Lin-Feng; Zeng Zi-Qi; Sun Yu-Long; Jia Huan-Huan; Xie Jia

doi:10.7498/aps.69.20201227

Abstract

All-solid-state sodium batteries are promising candidates in energy storage applications due to their high safety and low cost. A suitable solid electrolyte is a key component for high-performance all-solid-state sodium battery. Current inorganic solid electrolytes mainly include oxide- and sulfide-based electrolytes. However, the oxide-based electrolytes require to be sinetred above 1000 ℃ for high ionic conductivity, and most sulfide-based electrolytes can react with H₂O torelease toxic H₂S gas. These features will hinder the practical application of all-solid-state sodium batteries. In recent years, novel sodium ionic conductors have appeared successively. Among them, anti-perovskite type of Li/Na ionic conductor has received a lot of attention because of its high ionic conductivity and flexible structure design. Nevertheless, the synthesis of Na-rich anti-perovskite Na₃OBr_xI_1–x(0 < x < 1) is complex, the ionic conductivity at room temperature is relatively low, and its electrochemical properties remain unknown. Here in this work, the phase-pure Na-rich anti-perovskite Na₃OBr_xI_1–x is synthesized by a facile synthesis way. The X-ray diffraction patterns show that the anti-perovskite structure without any impurity phase is obtained. Alternating-current (AC) impedance spectrum is used for measuring ionic conductivity of electrolyte pellets after thermally being treated at around 100 ℃. The Na₃OBr_0.3I_0.7 exhibits an ionic conductivity of 1.47 × 10^–3 S/cm at 100 ℃. Unfortunately, the ionic conductivity experiences a sharp drop with the decrease of temperature, which may be related to the change of structural symmetry and Na sites in the structure revealed by solid state ²³Na NMR. In particular, the ionic conductivities of Na₃OBr_xI_1–x demonstrate the potential applications at medium temperature (40－80 ℃ in which the ionic conductivity of Na₃OBr_xI_1–x is close to or higher than 10^–4 S/cm) for all-solid-state sodium battery. Therefore, the compatibility against Na metal and the electrochemical performance in all-solid-state batteries have been evaluated. Since Na₃OBr_xI_1–x is not “Na-philic”, the resistance in impedance of the Na/Na₃OBr_0.5I_0.5/Na is very high. However, after modifying the interface by ionic liquid, the Na₃OBr_0.5I_0.5 exhibits good compatibility against Na metal and tiny ionic liquid also leads to high initial discharge specific capacity of 190 mAh/g and excellent cycling stability (around 127 mAh/g after 10 cycles) in the TiS₂/Na₃OBr_0.5I_0.5/Na-Sn solid-state battery. The capacity decay maybe results from the inferior interfacial contact between the solid electrolyte and the electrode materials because the electrode materials in this system experience large volume change during cycling. The successful operation in solid-state sodium batteries indicates that the Na₃OBr_xI_1–x is feasible to be used as a sodium solid electrolyte, which is of great importance for practical application of Na-rich anti-perovskite solid electrolytes.

Keywords:

Authors and contacts

1.
Hubei Electric Power Security and High Efficiency Key Laboratory, State Key Laboratory of Advanced Electromagnetic Engineering and Technology, School of Electrical and Electronic Engineering, Huazhong University of Science and Technology, Wuhan 430074, China
2.
School of Physics, Huazhong University of Science and Technology, Wuhan 430074, China
3.
School of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074, China

Corresponding author: Xie Jia, xiejia@hust.edu.cn

Funds: Project supported by the Program of Joint Funds of the National Natural Science Foundation of China (Grant No. U1966214), the Young Scientists Fund of the National Natural Science Foundation of China (Grant No. 51902116), and the China Postdoctoral Science Foundation (Grant No. 2019M652634)

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References

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[2]	Service R F 2019 Science 366 292 Google Scholar
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Cited By

图 1 (a)合成的反钙钛矿Na₃OBr_xI_1–x (x = 0.3, 0.5, 0.7)样品的XRD图谱; (b)图(a)的局部放大图

Figure 1. (a) The X-ray diffraction (XRD) patterns of synthezied anti-perovskites Na₃OBr_xI_1–x (x = 0.3, 0.5, 0.7); (b) local zoom of Fig. (a).

DownLoad: Full-Size Img PowerPoint

图 2 通过(a)冷压和(b)热压方法制备得到的Na₃OBr_0.5I_0.5电解质片的SEM图; (c)不同温度下测得的热压Na₃OBr_0.5I_0.5片的Nyquist曲线; (d) Na₃OBr_xI_1–x (x = 0.3, 0.5, 0.7)的logσ与1000/T对应曲线

Figure 2. SEM images of (a) cold-pressed and (b) hot-pressed Na₃OBr_0.5I_0.5 solid electrolyte pellets; (c) Nyquist plots of hot-pressed Na₃OBr_0.5I_0.5 measured at different temperatures; (d) logσ versus 1000/T plots for Na₃OBr_xI_1–x (x = 0.3, 0.5, 0.7).

DownLoad: Full-Size Img PowerPoint

图 3 Na₃OBr_0.3I_0.7在不同温度下的　(a)固态核磁图谱; (b)XRD图谱

Figure 3. (a) Solid state ²³Na NMR spectra and (b) XRD patterns of Na₃OBr_0.3I_0.7 at different temperature.

DownLoad: Full-Size Img PowerPoint

图 4 (a) Na/Na₃OBr_0.5I_0.5/Na对称电池的电化学阻抗谱; (b) 添加了离子液体的Na/IL/Na₃OBr_0.5I_0.5/IL/Na对称电池的电化学阻抗谱; (c) Na/IL/Na₃OBr_0.5I_0.5/IL/Na对称电池在不同电流密度下的充放电曲线; (d) TiS₂/IL/Na₃OBr_0.5I_0.5/IL/Na-Sn在50 ℃, 0.1 C条件下充放电曲线

Figure 4. (a) Electrochemical impedance plot of Na/Na₃OBr_0.5I_0.5/Na symmetrical cell; (b) electrochemical impedance plot of Na/IL/Na₃OBr_0.5I_0.5/IL/Na symmetrical cell with ionic liquid; (c) charge-discharge curves of Na/IL/Na₃OBr_0.5I_0.5/IL/Na symmetrical cell at different current density; (d) charge-discharge curves of TiS₂/IL/Na₃OBr_0.5I_0.5/IL/Na-Sn operated at 50°C, 0.1 C.

DownLoad: Full-Size Img PowerPoint

表 1 Na₃OBr_0.5I_0.5在冷压和热压下的密度

Table 1. Density of hot- and cold-pressed Na₃OBr_0.5I_0.5

	密度/ g·cm^–3	致密度
冷压	2.11	69%
热压	2.55	83%
真实密度*	3.06	—
*真实密度基于XRD谱得到的晶格参数计算, 晶格参数计算基于简单的立方相^[26], 忽略结构对称性破坏引起的细微变化.

DownLoad: CSV

表 2 Na₃OBr_xI_1–x (x = 0.3, 0.5, 0.7)离子电导率

Table 2. Ionic conductivity of Na₃OBr_xI_1–x (x = 0.3, 0.5, 0.7).

温度/℃	离子电导率/ S·cm^–1
温度/℃	Na₃OBr_0.7I_0.3	Na₃OBr_0.5I_0.5	Na₃OBr_0.3I_0.7
130	1.67 × 10^–3	—	—
110	8.96 × 10^–4	1.32 × 10^–3	5.55 × 10^–3
100	4.50 × 10^–4	6.56 × 10^–4	1.47 × 10^–3
80	9.73 × 10^–5	2.01 × 10^–4	3.93 × 10^–4
60	1.22 × 10^–5	6.78 × 10^–5	2.05 × 10^–4
40	—	1.06 × 10^–5	—

DownLoad: CSV

[1]	Li M, Lu J, Chen Z, Amine K 2018 Adv. Mater. 30 e1800561 Google Scholar
[2]	Service R F 2019 Science 366 292 Google Scholar
[3]	Yabuuchi N, Kubota K, Dahbi M, Komaba S 2014 Chem. Rev. 114 11636 Google Scholar
[4]	Lee J M, Singh G, Cha W, Kim S, Yi J, Hwang S J, Vinu A 2020 ACS Energy Lett. 5 1939 Google Scholar
[5]	Yang C, Xin S, Mai L, You Y 2020 Adv. Energy Mater. 10.1002/aenm.202000974 Google Scholar
[6]	Rajagopalan R, Tang Y, Jia C, Ji X, Wang H 2020 Energy Environ. Sci. 13 1568 Google Scholar
[7]	Xiao Y H, Wang Y, Bo S H, Kim J C, Miara L J, Ceder G 2020 Nat. Rev. Mater. 5 105 Google Scholar
[8]	Feng X, Ren D, He X, Ouyang M 2020 Joule 4 743 Google Scholar
[9]	Chen R, Li Q, Yu X, Chen L, Li H 2019 Chem. Rev. 120 6820 Google Scholar
[10]	Xu L, Li J, Deng W, Shuai H, Li S, Xu Z, Li J, Hou H, Peng H, Zou G, Ji X 2020 Adv. Energy Mater. 10.1002/aenm. 202000648 Google Scholar
[11]	Lu Y, Li L, Zhang Q, Niu Z, Chen J 2018 Joule 2 1747 Google Scholar
[12]	Kamaya N, Homma K, Yamakawa Y, Hirayama M, Kanno R, Yonemura M, Kamiyama T, Kato Y, Hama S, Kawamoto K, Mitsui A 2011 Nat. Mater. 10 682 Google Scholar
[13]	Kato Y, Hori S, Saito T, Suzuki K, Hirayama M, Mitsui A, Yonemura M, Iba H, Kanno R 2016 Nat. Energy 1 16030 Google Scholar
[14]	Zhang Z, Sun Y, Duan X, Peng L, Jia H, Zhang Y, Shan B, Xie J 2019 J. Mater. Chem. A 7 2717 Google Scholar
[15]	Zhou L, Assoud A, Zhang Q, Wu X, Nazar L F 2019 J. Am. Chem. Soc. 141 19002 Google Scholar
[16]	Wang C, Fu K, Kammampata S P, McOwen D W, Samson A J, Zhang L, Hitz G T, Nolan A M, Wachsman E D, Mo Y, Thangadurai V, Hu L 2020 Chem. Rev. 120 4257 Google Scholar
[17]	Zhang Z, Zhang J, Jia H, Peng L, An T, Xie J 2020 J. Power Sources 450Google Scholar
[18]	Fuchs T, Culver S P, Till P, Zeier W G 2019 ACS Energy Lett. 5 146 Google Scholar
[19]	Jia H, Sun Y, Zhang Z, Peng L, An T, Xie J 2019 Energy Storage Mater. 23 508 Google Scholar
[20]	Hayashi A, Masuzawa N, Yubuchi S, Tsuji F, Hotehama C, Sakuda A, Tatsumisago M 2019 Nat. Commun. 10 5266 Google Scholar
[21]	Jia H, Liang X, An T, Peng L, Feng J, Xie J 2020 Chem. Mater. 32 4065 Google Scholar
[22]	Zheng F, Kotobuki M, Song S, Lai M O, Lu L 2018 J. Power Sources 389 198 Google Scholar
[23]	Jia H, Peng L, Zhang Z, An T, Xie J 2020 J. Energy Chem. 48 102 Google Scholar
[24]	Narayanan S, Reid S, Butler S, Thangadurai V 2019 Solid State Ionics 331 22 Google Scholar
[25]	Zhao Y S, Daemen L L 2012 J. Am. Chem. Soc. 134 15042 Google Scholar
[26]	Wang Y, Wang Q, Liu Z, Zhou Z, Li S, Zhu J, Zou R, Wang Y, Lin J, Zhao Y 2015 J. Power Sources 293 735 Google Scholar
[27]	Fan S S, Lei M, Wu H, Hu J, Yin C L, Liang T X, Li C L 2020 Energy Storage Mater. 31 87 Google Scholar
[28]	Yang Q F, Li C L 2018 Energy Storage Mater. 14 100 Google Scholar
[29]	Nguyen H, Hy S, Wu E, Deng Z, Samiee M, Yersak T, Luo J, Ong S P, Meng Y S 2016 J. Electrochem. Soc. 163 A2165 Google Scholar
[30]	Braga M H, Ferreira J A, Murchison A J, Goodenough J B 2016 J. Electrochem. Soc. 164 A207 Google Scholar
[31]	Braga M H, Murchison A J, Ferreira J A, Singh P, Goodenough J B 2016 Energy Environ. Sci. 9 948 Google Scholar
[32]	Sun Y, Wang Y, Liang X, Xia Y, Peng L, Jia H, Li H, Bai L, Feng J, Jiang H, Xie J 2019 J. Am. Chem. Soc. 141 5640 Google Scholar
[33]	Wang Y, Wen T, Park C, Kenney B C, Pravica M, Yang W, Zhao Y 2016 J. Appl. Phys. 119 025901 Google Scholar
[34]	Zhu J, Wang Y, Li S, Howard J W, Neuefeind J, Ren Y, Wang H, Liang C, Yang W, Zou R, Jin C, Zhao Y 2016 Inorg. Chem. 55 5993 Google Scholar
[35]	Lv Z L, Cui H L, Wang H, Li X H, Ji G F 2017 Phys. Status Solidi B) 254 1700089 Google Scholar
[36]	Dawson J A, Chen H, Islam M S 2018 J. Phys. Chem. C 122 23978 Google Scholar
[37]	Pham T L, Samad A, Kim H J, Shin Y H 2018 J. Appl. Phys. 124 164106 Google Scholar
[38]	Wan T H, Lu Z, Ciucci F 2018 J. Power Sources 390 61 Google Scholar
[39]	Fang H, Jena P 2019 ACS Appl. Mater. Interfaces 11 963 Google Scholar
[40]	Yu Y, Wang Z, Shao G 2019 J. Mater. Chem. A 7 21985 Google Scholar
[41]	Hippler K, Sitta S, Vogt P, Sabrowsky H 1990 Acta Cryst. C 46 736
[42]	Hu J L, Yao Z G, Chen K Y, Li C L 2020 Energy Storage Mater. 28 37 Google Scholar

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