<i>In situ</i> observation of lithiation mechanism of SnO<sub>2</sub> nanoparticles

Xiong Yu-Wei; Yin Kui-Bo; Wen Yi-Feng; Xin Lei; Yao Li-Bing; Zhu Chong-Yang; Sun Li-Tao

doi:10.7498/aps.68.20190431

Abstract

Tin oxide (SnO₂) has attracted a lot of attention among lithium ion battery anode materials due to its rich reserves, high theoretical capacity, and safe potential. However, the mechanism of the SnO₂ nano materials in the lithiation-delithiation reaction, especially whether the first-step conversion reaction is reversible, is still controversial. In this paper, SnO₂ nanoparticles with an average particle size of 4.4 nm are successfully prepared via a simple hydrothermal method. A nanosized lithium ion battery that enables the in situ electrochemical experiments of SnO₂ nanoparticles is constructed to investigate the electrochemical behavior of SnO₂ in lithiation-delithiation process. Briefly, the nanosized electrochemical cell consists of a SnO₂ working electrode, a metal lithium (Li) counter electrode on a sharp tungsten probe, and a solid electrolyte of lithium oxide (Li₂O) layer naturally grown on the surface of metal Li. Then, the whole lithiation-delithiation process of SnO₂ nanocrystals is tracked in real time. When a constant potential of –2 V is applied to the SnO₂ with respect to lithium, lithium ions begin to diffuse from one side of the nanoparticles, which is in contact with the Li/Li₂O layer, and gradually propagate to the other side. Upon the lithiation, a two-step conversion reaction mechanism is revealed: SnO₂ is first converted into intermediate phase of Sn with an average diameter of 4.2 nm which is then further converted into Li₂₂Sn₅. Upon the delithiation, a potential of 2 V is applied and Li₂₂Sn₅ phase can be reconverted into SnO₂ phase when completely delithiated. It is because the interfaces and grain boundaries of nano-sized SnO₂ may impede the Sn diffusing from one grain into another during lithiation/delithiation and then suppress the coarsening of Sn, and enable the Li₂O and Sn to be sufficiently contacted with each other and then converted into SnO₂. This work provides a valuable insight into an understanding of phase evolution in the lithiation-delithiation process of SnO₂ and the results are of great significance for improving the reversible capacity and cycle performance of lithium ion batteries with SnO₂ electrodes.

Keywords:

Authors and contacts

SEU-FEI Nano-Pico Center, Key Laboratory of MEMS of Ministry of Education, Southeast University, Nanjing 210096, China

Corresponding author: Yin Kui-Bo, yinkuibo@seu.edu.cn ; Sun Li-Tao, slt@seu.edu.cn

Funds: Project supported by the National Basic Research Program of China (Grant No. 2017YFA0204800) and the National Natural Science Foundation of China (Grant Nos. 11674052, 11525415, 51420105003).

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References

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Cited By

图 1 基于透射电镜的锂离子电池原型器件原位测试示意图

Figure 1. Schematic diagram of a prototype device for a lithium ion battery in the transmission electron microscope.

DownLoad: Full-Size Img PowerPoint

图 2 SnO₂纳米颗粒的表征　(a) SnO₂纳米颗粒的XRD图谱; (b) 低倍率下的SnO₂纳米颗粒的TEM像, 比例尺为50 nm; (c) SnO₂纳米颗粒的高分辨像, 比例尺为2 nm; (d) SnO₂纳米颗粒的SAED图像; (e) 四方相SnO₂纳米颗粒的晶体结构; (f) SnO₂纳米颗粒粒径尺寸分布

Figure 2. Characterization of SnO₂ nanoparticles: (a) XRD pattern of the as-prepared SnO₂ nanoparticles; (b) TEM image of SnO₂ nanopaticles; (c) HRTEM of SnO₂ nanoparticles; (d) SAED of SnO₂ nanoparticles; (e) crystal structure of the tetracoral SnO₂; (f) distribution of SnO₂ nanoparticles size.

DownLoad: Full-Size Img PowerPoint

图 3 SnO₂纳米颗粒第一次嵌锂前后的变化　(a) SnO₂嵌锂前的形貌, 比例尺为15 nm; (b) SnO₂第一次嵌锂后的形貌, 比例尺为15 nm; (c) SnO₂嵌锂一段时间后的HRTEM像, 比例尺为1 nm; (d) SnO₂嵌锂一段时间后的SAED图; (e) SnO₂第一次嵌锂结束后的HRTEM图, 比例尺为5 nm; (f) SnO₂第一次嵌锂结束后的SAED图; (g)−(k) SnO₂纳米颗粒第一次锂化过程, 比例尺为10 nm

Figure 3. Changes of SnO₂ nanoparticles during the first lithiation: (a) Morphology of SnO₂ before lithiation; (b) morphology of SnO₂ after first lithiation; (c) HRTEM image of SnO₂ after a moment; (d) SAED pattern of SnO₂ after a moment; (e) HRTEM image of SnO₂ after first completely lithiated; (f) SAED pattern of SnO₂ after first completely lithiated; (g)−(k) SnO₂ nanoparticle first lithiation process.

DownLoad: Full-Size Img PowerPoint

图 4 SnO₂纳米颗粒脱锂前后的变化　(a) SnO₂第一次脱锂前的形貌, 比例尺为40 nm; (b) SnO₂第一次脱锂后的形貌, 比例尺为40 nm; (c) SnO₂第一次脱锂结束后的HRTEM图, 比例尺为1 nm; (d) SnO₂第一次脱锂结束后的SAED图; (e)—(l) SnO₂纳米颗粒第一次脱锂过程, 比例尺为40 nm; (m) SnO₂纳米颗粒第二次嵌锂后的HRTEM图, 比例尺为1 nm; (n) SnO₂纳米颗粒第二次嵌锂后的SAED图; (o) SnO₂纳米颗粒第二次脱锂后的HRTEM图, 比例尺为1 nm; (p) SnO₂纳米颗粒第二次脱锂后的SAED图

Figure 4. Changes of SnO₂ nanoparticles during the delithiation: (a) Morphology of SnO₂ before delithiation; (b) morphology of SnO₂ after first delithiated; (c) HRTEM image of SnO₂ after completely first delithiated; (d) SAED pattern of SnO₂ after first completely delithiated; (e)–(l) SnO₂ nanoparticle first delithiation process; (m) HRTEM image of SnO₂ after second lithiated; (n) SAED pattern of SnO₂ after second lithiated; (o) HRTEM image of SnO₂ after second delithiated; (p) SAED pattern of SnO₂ after second delithiated.

DownLoad: Full-Size Img PowerPoint

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[3]	Nitta N, Yushin G 2014 Part. Part. Syst. Charact. 31 317 Google Scholar
[4]	Armand M, Tarascon J M 2008 Nature 451 652 Google Scholar
[5]	Shao-Horn Y, Croguennec L, Delmas C, Nelson E C, O'Keefe M A 2003 Nat. Mater. 2 464 Google Scholar
[6]	季怡汝, 张庆华, 谷林 2018 电子显微学报 37 532 Google Scholar Ji Y R, Zhang Q H, Gu L 2018 J. Chin. Electron Microsc. Soc. 37 532 Google Scholar
[7]	侯贤华, 余洪文, 胡社军 2010 物理学报 59 8226 Google Scholar Hou X H, Yu H W, Hu S J 2010 Acta Phys. Sin. 59 8226 Google Scholar
[8]	侯贤华, 胡社军, 石璐 2009 物理学报 59 2109 Google Scholar Hou X H, Hu S J, Shi L 2009 Acta Phys. Sin. 59 2109 Google Scholar
[9]	Wu F, Li X, Wang Z, Guo H J, He Z J, Zhang Q, Xiong X H, Yue P 2012 J. Power Sources 202 374 Google Scholar
[10]	Wu F, Li X, Wang Z, Guo H J 2013 Nanoscale 5 6936 Google Scholar
[11]	Sun L, Gao Y M, Xiao B, Li Y F, Wang G L 2013 J. Alloy. Compd. 579 457 Google Scholar
[12]	Tian Q H, Tian Y, Zhang Z X, Yang L, Hirano S I 2014 J. Power Sources 269 479 Google Scholar
[13]	Guo X W, Fang X P, Sun Y, Shen L Y, Wang Z X, Chen L Q 2013 J. Power Sources 226 75 Google Scholar
[14]	Chen L, Wu P, Wang H, Ye Y, Xu B, Cao G P, Zhou Y M, Lu T H, Yang Y S 2014 J. Power Sources 247 178 Google Scholar
[15]	Han Q Y, Zai J T, Xiao Y L, Li B, Xu M, Qian X F 2013 RSC Adv. 3 20573 Google Scholar
[16]	Chen J S, Lou X W 2013 Small 9 1877 Google Scholar
[17]	Ye H J, Li H Q, Jiang F Q, Yin J, Zhu H 2018 Electrochim. Acta 266 170 Google Scholar
[18]	刘美梅, 钱翔英 2018 电子显微学报 37 15 Google Scholar Xiu M M, Qian X Y 2018 J. Chin. Electron Microsc. Soc. 37 15 Google Scholar
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[21]	Thackeray M M, Johnson C S, Kahaian A J, Kepler K D, Vaughey J T, Shao-Horn Y, Hackney S A 1999 J. Power Sources 81-82 60 Google Scholar
[22]	Idota Y, Kubota T, Matsufuji A, Maekawa Y, Miyasaka T 1997 Science 276 1395 Google Scholar
[23]	Hu R Z, Sun W, Liu H, Zeng M Q, Zhu M 2013 Nanoscale 5 11971 Google Scholar
[24]	Brousse T, Retoux R, Herterich U, Schleich D M 1998 J. Electrochem. Soc. 145 1 Google Scholar
[25]	Retoux R, Brousse T, Schleich D M 1999 J. Electrochem. Soc. 146 2472 Google Scholar
[26]	Lou X W, Li C M, Archer L A 2009 Adv. Mat. 21 2536 Google Scholar
[27]	Holmberg V C, Panthani M G, Korgel B A 2009 Science 326 405 Google Scholar
[28]	Zheng H M, Smith R K, Jun Y W, Kisielowski C, Dahmen U, Alivisatos A P 2009 Science 324 1309 Google Scholar
[29]	Huang J Y, Zhong L, Wang C M, Sullivan J P, Xu W, Zhang L Q, Mao Scott X, Hudak N S, Liu X H, Subramanian A, Fan H Y, Qi L, Kushima A, Li J 2010 Science 330 1515 Google Scholar
[30]	Hu R Z, Zhang H P, Lu Z C, Liu J, Zeng M Q, Yang L C, Yuan B, Zhu M 2018 Nano Energy 45 255 Google Scholar
[31]	Hu R Z, Chen D C, Waller G, Ouyang Y P, Chen Y, Zhao B, Rainwater B, Yang C H, Zhu M, Liu M L 2016 Energy Environ. Sci. 9 595 Google Scholar
[32]	Li B S, Feng J K, Qian Y T, Xiong S L 2015 J. Mater. Chem. A 3 10336 Google Scholar
[33]	Wang C M, Xu W, Liu J, Zhang J G, Saraf L V, Arey B W, Choi D, Yang Z G, Xiao J, Thevuthasan S, Baer D R 2011 Nano Lett. 11 1874 Google Scholar
[34]	Meduri P, Clark E, Dayalan E, Sumanasekera G U, Sunkara M K 2011 Energy Environ. Sci. 4 1695 Google Scholar
[35]	Meduri P, Pendyala C, Kumar V, Sumanasekera G U, Sunkara M K 2009 Nano Lett. 9 612 Google Scholar
[36]	Haines J, Leger J M 1997 Phys. Rev. B 55 11144 Google Scholar
[37]	Liu L G 1978 Science 199 422 Google Scholar
[38]	Chen Z W, Lai J K L, Shek C H 2006 Appl. Phys. Lett. 89 231902 Google Scholar
[39]	Carvalho M H, Pereira E C, de Oliveira A J A 2018 RSC Adv. 8 3958 Google Scholar

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In situ observation of lithiation mechanism of SnO₂ nanoparticles

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Corresponding author: Yin Kui-Bo, yinkuibo@seu.edu.cn ; Sun Li-Tao, slt@seu.edu.cn

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In situ observation of lithiation mechanism of SnO2 nanoparticles

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Corresponding author: Yin Kui-Bo, yinkuibo@seu.edu.cn ; Sun Li-Tao, slt@seu.edu.cn

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In situ observation of lithiation mechanism of SnO₂ nanoparticles