DOI QR코드

DOI QR Code

Transmission Electron Microscope Specimen Preparation of Si-Based Anode Materials for Li-Ion Battery by Using Focused Ion Beam and Ultramicrotome

  • Chae, Jeong Eun (Testing & Certification Division Materials Characterization Center, Gumi Electronics & Information Technology Research Institute) ;
  • Yang, Jun Mo (Department of Nanostructure Technology, National Nanofab Center) ;
  • Kim, Sung Soo (Graduate School of Energy Science and Technology, Chungnam National University) ;
  • Park, Ju Cheol (Testing & Certification Division Materials Characterization Center, Gumi Electronics & Information Technology Research Institute)
  • 투고 : 2018.04.11
  • 심사 : 2018.04.28
  • 발행 : 2018.06.30

초록

A successful transmission electron microscope (TEM) analysis is closely related to the preparation of the TEM specimen and should be followed by the suitable TEM specimen preparation depending on the purpose of analysis and the subject materials. In the case of the Si-based anode material, lithium atoms of formed Li silicide were removed due to ion beam and electron beam during TEM specimen preparation and TEM observation. To overcome the problem, we proposed a new technique to make a TEM specimen without the ion beam damage. In this study, two types of test specimens from the Si-based anode material of Li-ion battery were prepared by respectively adopting the only focused ion beam (FIB) method and the new FIB-ultramicrotome method. TEM analyses of two samples were conducted to compare the Ga ion damage of the test specimen.

키워드

참고문헌

  1. Chae J E, Yang J M, Park K J, Yoo J H, Park Y C, Sung M S, Yu H J, and Kim S S (2013) Microstructural analysis of Si-Ti-Fe alloy anode materials for Li-ion secondary batteries. Korean J. Met. Mater. 51, 429-436. https://doi.org/10.3365/KJMM.2013.51.6.429
  2. Chan C K, Peng H, Liu G, Mcllwrath K, Zhang X F, Huggins R A, and Cui Y (2008) High-performance lithium battery anodes using silicon nanowires. Nat. Nanotechnol. 3, 31-35. https://doi.org/10.1038/nnano.2007.411
  3. Danet J, Brousse T, Rasim K, Guyomard D, and Moreau P (2010) Valence electron energy-loss spectroscopy of silicon negative electrodes for lithium batteries. Phys. Chem. Chem. Phys. 12, 220-226. https://doi.org/10.1039/B915245H
  4. Jung H, Kim Y U, Sung M S, Hwa Y, Jeong G, Kim G B, and Sohn H J (2011) Si anode embedded in super-elastic nitinol (Ni-Ti) shape memory alloy matrix for Li rechargeable batteries. J. Mater. Chem. 21, 11213-11216. https://doi.org/10.1039/c1jm11020a
  5. Lee H Y and Lee S M (2002) Graphite-FeSi alloy composites as anode materials for rechargeable lithium batteries. J. Power Sources 112, 649-654. https://doi.org/10.1016/S0378-7753(02)00461-5
  6. Mao O, Turner R L, Courtney I A, Fredericksen B D, Buckett M I, Krause L J, and Dahn J R (1999) Active/inactive nanocomposites as anodes for Li-ion batteries. Electrochem. Solid-State Lett. 2, 3-5. https://doi.org/10.1149/1.1390715
  7. Muto S, Sasano Y, Tatsumi K, Sasaki T, Horibuchi K, Takeuchi Y, and Ukyo Y (2009) Capacity-fading mechanisms of $LiNiO_2-based$ lithium-ion batteries(II). J. Electrochem. Soc. 156, 371-377.
  8. Obrovac M N and Christensen L (2004) Structural changes in silicon anodes during lithium insertion/extraction. Electrochem. Solid-State Lett. 7, A93-A96. https://doi.org/10.1149/1.1652421
  9. Park C M, Kim J H, Kim H, and Sohn H J (2010) Li-alloy based anode materials for Li secondary batteries. Chem. Soc. Rev. 39, 3115-3141. https://doi.org/10.1039/b919877f
  10. Raghavan V (2009) Fe-Si-Ti (iron-silicon-titanium). J. Phase Equilibria Diffus. 30, 393-396. https://doi.org/10.1007/s11669-009-9555-5
  11. Sasaki T, Nonaka T, Oka H, Okuda C, Itou Y, Kondo Y, Takeuchi Y, Ukyo Y, Tatsumi K, and Muto S (2009) Capacity-fading mechanisms of $LiNiO_2-based$ lithium-ion batteries(I). J. Electrochem. Soc. 156, 289-293. https://doi.org/10.1149/1.3076136
  12. Weitzer F, Schuster J C, Naka M, Stein F, and Palm M (2008) On the reaction scheme and liquidus surface in the ternary system Fe-Si-Ti. Intermetallics 16, 273-282. https://doi.org/10.1016/j.intermet.2007.10.006
  13. Winter M, Besenhard J O, Spahr M E, and Novak P (1998) Insertion electrode materials for rechargeable lithium batteries. Adv. Mater. 10, 725-763. https://doi.org/10.1002/(SICI)1521-4095(199807)10:10<725::AID-ADMA725>3.0.CO;2-Z