pp 1–8 | Cite as

High electrochemical performance of Li4Ti5O12/C synthesized by ball milling and direct flaming of acetylene gas as anode for lithium-ion battery

  • Lukman NoerochimEmail author
  • Amalia Ma’rifatul Maghfiroh
  • Widyastuti
  • Diah Susanti
  • Slamet Priyono
  • Bambang Prihandoko
Original Paper


Li4Ti5O12/C has been successfully synthesized by a solid-state reaction method of Li2CO3 and TiO2 followed by direct flaming of acetylene gas. Li4Ti5O12 with 2-h milling time is indexed as single-phase crystal structure of Li4Ti5O12 (JCPDS 04-0477). The SEM results show particle sizes between 0.192 and 0.360 μm with a spherical shape, but there is agglomeration due to high temperature when the direct flaming of acetylene gas process is applied. The desired carbon content by direct flaming of acetylene gas is still very low at 0.6% for 10 min and 0.9% for 20 min. Li4Ti5O12 with 10 min of direct flaming of acetylene gas has the highest specific discharge capacity of 210.61 mAh/g. This is attributed to the pure single phase and the higher conductivity of the sample. This result shows that Li4Ti5O12/C synthesized by ball milling and direct flaming of acetylene gas could be a good candidate as anode for lithium-ion battery.


Li4Ti5O12/C Ball milling Direct flaming Anode Lithium-ion battery 


Funding information

This work was financially supported by Penelitian Dana Lokal ITS Surabaya (No/PKS/ITS/2019) and partially funded by the Research Grant of National Innovation System Consortium (INSINAS) IRPK-2018-148 Ministry of Research, Technology and Higher Education of the Republic of Indonesia (Kemenristek DIKTI).


  1. 1.
    Kuribayashi I, Yokoyama M, Yamashita M (1995) Battery characteristics with various carbonaceous materials. J Power Sources 54(1):1–5CrossRefGoogle Scholar
  2. 2.
    Qu X, Huang G, Xing B, Si D, Xu B, Chen Z, Zhang C, Cao Y (2019) Core-shell carbon composite material as anode materials for lithium-ion batteries. J Alloys Compd 772:814–822CrossRefGoogle Scholar
  3. 3.
    Ohzuku T, Matoba N, Sawai K (2001) Direct evidence on anomalous expansion of graphite-negative electrodes on first charge by dilatometry. J Power Sources 97–98:73–77CrossRefGoogle Scholar
  4. 4.
    Sawai K, Iwakoshi Y, Ohzuku T (1994) Carbon materials for lithium-ion (shuttlecock) cells. Solid State Ionics 69(3):273–283CrossRefGoogle Scholar
  5. 5.
    Chen Z, Liu Y, Zhang Y, Shen F, Yang G, Wang L, Zhang X, He Y, Luo L, Deng S (2018) Ultrafine layered graphite as an anode material for lithium ion batteries. Mater Lett 229:134–137CrossRefGoogle Scholar
  6. 6.
    Ohta N, Nagaoka K, Hoshi K, Bitoh S, Inagaki M (2009) Carbon-coated graphite for anode of lithium ion rechargeable batteries: graphite substrates for carbon coating. J Power Sources 194(2):985–990CrossRefGoogle Scholar
  7. 7.
    Mu T, Zuo P, Lou S, Pan Q, Zhang H, Du C, Gao Y, Cheng X, Ma Y, Huo H, Yin G (2019) A three-dimensional silicon/nitrogen-doped graphitized carbon composite as high-performance anode material for lithium ion batteries. J Alloys Compd 777:190–197Google Scholar
  8. 8.
    Miao F, Miao R, Wu W, Cong W, Zang Y, Tao B (2018) A stable hybrid anode of graphene/silicon nanowires array for high performance lithium-ion battery. Mater Lett 228:262–265CrossRefGoogle Scholar
  9. 9.
    Yi T-F, Jiang L-J, Shu J, Yue C-B, Zhu R-S, Qiao H-B (2010) Recent development and application of Li4Ti5O12 as anode material of lithium ion battery. J Phys Chem Solids 71(9):1236–1242CrossRefGoogle Scholar
  10. 10.
    Ohzuku T, Ueda A, Yamamoto N (1995) Zero-strain insertion material of Li[Li1/3Ti5/3]O4 for rechargeable lithium cells. J Electrochem Soc 142(5):1431–1435CrossRefGoogle Scholar
  11. 11.
    Shang Y (2018) Outstanding lithium-storage performance of carbon-free Li4Ti5O12 anode material for rechargeable lithium-ion batteries. Solid State Ionics 322:39–43CrossRefGoogle Scholar
  12. 12.
    Lim J-E, Kim J, Kim Y, Kim J-K (2018) Binder-free hybrid Li4Ti5O12 anode for high performance lithium-ion batteries. Electrochim Acta 282:270–275CrossRefGoogle Scholar
  13. 13.
    Seo I, Lee C-R, Kim J-K (2017) Zr doping effect with low-cost solid-state reaction method to synthesize submicron Li4Ti5O12 anode material. J Phys Chem Solids 108:25–29CrossRefGoogle Scholar
  14. 14.
    Yang Z, Huang Q, Li S, Mao J (2018) High-temperature effect on electrochemical performance of Li4Ti5O12 based anode material for Li-ion batteries. J Alloys Compd 753:192–202CrossRefGoogle Scholar
  15. 15.
    Haridas AK, Sharma CS, Hebalkar NY, Rao TN (2017) Nano-grained SnO2/Li4Ti5O12 composite hollow fibers via sol-gel/ electrospinning as anode material for Li- ion batteries. Mater Today Energy 4:14–24CrossRefGoogle Scholar
  16. 16.
    Liu G, Zhang R, Bao K, Xie H, Zheng S, Guo J, Liu G (2016) Synthesis of nano-Li4Ti5O12 anode material for lithium ion batteries by a biphasic interfacial reaction route. Ceram Int 42(9):11468–11472CrossRefGoogle Scholar
  17. 17.
    Bian M, Yang Y, Tian L (2018) Carbon-free Li4Ti5O12 porous nanofibers as high-rate and ultralong-life anode materials for lithium-ion batteries. J Phys Chem Solids 113:11–16CrossRefGoogle Scholar
  18. 18.
    Chang-Jian C-W, Ho BC, Chung CK, Chou JA, Chung CL, Huang JH, Huang JH, Hsiao YS (2018) Doping and surface modification enhance the applicability of Li4Ti5O12 microspheres as high-rate anode materials for lithium ion batteries. Ceram Int 44(18):23063–23072CrossRefGoogle Scholar
  19. 19.
    Fang W, Cheng X, Zuo P, Ma Y, Yin G (2013) A facile strategy to prepare nano-crystalline Li4Ti5O12/C anode material via polyvinyl alcohol as carbon source for high-rate rechargeable Li-ion batteries. Electrochim Acta 93:173–178CrossRefGoogle Scholar
  20. 20.
    Jugović D, Mitrić M, Cvjetićanin N, Jančar B, Mentus S, Uskoković D (2008) Synthesis and characterization of LiFePO4/C composite obtained by sonochemical method. Solid State Ionics 179(11):415–419CrossRefGoogle Scholar
  21. 21.
    Wang Y, Wang Y, Hosono E, Wang K, Zhou H (Sep. 2008) The design of a LiFePO4/carbon nanocomposite with a core–shell structure and its synthesis by an in situ polymerization restriction method. Angew Chemie Int Ed 47(39):7461–7465CrossRefGoogle Scholar
  22. 22.
    Kim J-K, Cheruvally G, Ahn J-H (2008) Electrochemical properties of LiFePO4/C synthesized by mechanical activation using sucrose as carbon source. J Solid State Electrochem 12(7):799–805CrossRefGoogle Scholar
  23. 23.
    Oh SW, Myung ST, Oh SM, Oh KH, Amine K, Scrosati B, Sun YK (Jul. 2010) Double carbon coating of LiFePO4 as high rate electrode for rechargeable lithium batteries. Adv Mater 22(43):4842–4845CrossRefGoogle Scholar
  24. 24.
    Xu D, Chu X, He YB, Ding Z, Li B, Han W, du H, Kang F (2015) Enhanced performance of interconnected LiFePO4/C microspheres with excellent multiple conductive network and subtle mesoporous structure. Electrochim Acta 152:398–407CrossRefGoogle Scholar
  25. 25.
    Kellerman DG, Gorshkov VS, Shalaeva EV, Tsaryev BA, Vovkotrub EG (2012) Structure peculiarities of carbon-coated lithium titanate: Raman spectroscopy and electron microscopic study. Solid State Sci 14(1):72–79CrossRefGoogle Scholar
  26. 26.
    Saroha R, Panwar AK (2017) Effect of in situ pyrolysis of acetylene (C 2 H 2 ) gas as a carbon source on the electrochemical performance of LiFePO 4 for rechargeable lithium-ion batteries. J Phys D Appl Phys 50(25):255501CrossRefGoogle Scholar
  27. 27.
    Ding Y, Li GR, Xiao CW, Gao XP (2013) Insight into effects of graphene in Li4Ti5O12/carbon composite with high rate capability as anode materials for lithium ion batteries. Electrochim Acta 102:282–289CrossRefGoogle Scholar
  28. 28.
    Tenorio Gonzalez FN, Barajas Rosales IR, Vera Serna P, Sánchez de Jesus F, Bolarin Miró AM, Garrido Hernández A, Kusý M (2019) Reducing the crystallite and particle size of SrFe12O19 with PVA by high energy ball milling. J Alloys Compd 771:464–470CrossRefGoogle Scholar
  29. 29.
    Cabeza M, Feijoo I, Merino P, Pena G, Pérez MC, Cruz S, Rey P (2017) Effect of high energy ball milling on the morphology, microstructure and properties of nano-sized TiC particle-reinforced 6005A aluminium alloy matrix composite. Powder Technol 321:31–43CrossRefGoogle Scholar
  30. 30.
    Li K, Zhang Y, Sun Y, Xu Y, Zhang H, Ye P, Zheng M, Zhou N, Wang D (2018) Template-free synthesis of biomass-derived carbon coated Li4Ti5O12 microspheres as high performance anodes for lithium-ion batteries. Appl Surf Sci 459:572–582CrossRefGoogle Scholar
  31. 31.
    Noerochim L, Yurwendra AO, Susanti D (2016) Effect of carbon coating on the electrochemical performance of LiFePO4/C as cathode materials for aqueous electrolyte lithium-ion battery. Ionics (Kiel) 22(3):341–346CrossRefGoogle Scholar
  32. 32.
    Shi Y, Wen L, Li F, Cheng H-M (2011) Nanosized Li4Ti5O12/graphene hybrid materials with low polarization for high rate lithium ion batteries. J Power Sources 196(20):8610–8617CrossRefGoogle Scholar
  33. 33.
    Chen Y, Zhang H, Li Y, Chen Y, Luo T (2017) Electrochemical performance of Li4Ti5O12/carbon nanotubes/graphene composite as an anode material in lithium-ion batteries. Int J Hydrog Energy 42(10):7195–7201CrossRefGoogle Scholar
  34. 34.
    Shen L, Zhang X, Uchaker E, Yuan C, Cao G (Apr. 2012) Li4Ti5O12 nanoparticles embedded in a mesoporous carbon matrix as a superior anode material for high rate lithium ion batteries. Adv Energy Mater 2(6):691–698CrossRefGoogle Scholar
  35. 35.
    Eom J-Y, Cho Y-H, Kim S-I, Han D, Sohn D (2017) Improvements in the electrochemical performance of Li4Ti5O12-coated graphite anode materials for lithium-ion batteries by simple ball-milling. J Alloys Compd 723:456–461CrossRefGoogle Scholar
  36. 36.
    Li F, Chen P, Wu H, Zhang Y (2015) Cooperative enhancement of electrochemical properties in double carbon-decorated Li4Ti5O12/C composite as anode for Li-ion batteries. J Alloys Compd 633:443–447CrossRefGoogle Scholar
  37. 37.
    Shu H, Wang X, Wu Q, Hu B, Yang X, Wei Q, Liang Q, Bai Y, Zhou M, Wu C, Chen M, Wang A, Jiang L (2013) Improved electrochemical performance of LiFePO4/C cathode via Ni and Mn co-doping for lithium-ion batteries. J Power Sources 237:149–155CrossRefGoogle Scholar
  38. 38.
    Yang X, Hu Z, Liang J (2015) Effects of sodium and vanadium co-doping on the structure and electrochemical performance of LiFePO4/C cathode material for lithium-ion batteries. Ceram Int 41(2, Part B):2863–2868CrossRefGoogle Scholar
  39. 39.
    Shu H, Wang X, Wu Q, Ju B, Liu L, Yang X, Wang Y, Bai Y, Yang S (Jan. 2011) Ammonia assisted hydrothermal synthesis of monodisperse LiFePO4/C microspheres as cathode material for lithium ion batteries. J Electrochem Soc 158(12):A1448–A1454CrossRefGoogle Scholar
  40. 40.
    Shu H, Wang X, Wu Q, Liu L, Liang Q, Yang S, Ju B, Yang X, Zhang X, Wang Y, Wei Q, Hu B, Liao Y, Jiang H (2012) The effect of ammonia concentration on the morphology and electrochemical properties of LiFePO4 synthesized by ammonia assisted hydrothermal route. Electrochim Acta 76:120–129CrossRefGoogle Scholar
  41. 41.
    Cui Y, Zhao X, Guo R (2010) High rate electrochemical performances of nanosized ZnO and carbon co-coated LiFePO4 cathode. Mater Res Bull 45(7):844–849CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  • Lukman Noerochim
    • 1
    Email author
  • Amalia Ma’rifatul Maghfiroh
    • 1
  • Widyastuti
    • 1
  • Diah Susanti
    • 1
  • Slamet Priyono
    • 2
  • Bambang Prihandoko
    • 2
  1. 1.Department of Materials and Metallurgical EngineeringSepuluh Nopember Institute of TechnologySurabayaIndonesia
  2. 2.Research Center of PhysicsIndonesian Institute of ScienceSerpongIndonesia

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