Journal of Sol-Gel Science and Technology

, Volume 89, Issue 1, pp 225–233 | Cite as

Impact of the synthesis parameters on the microstructure of nano-structured LTO prepared by glycothermal routes and 7Li NMR structural investigations

  • Mateusz OdziomekEmail author
  • Frederic ChaputEmail author
  • Frederic Lerouge
  • Anna Rutkowska
  • Konrad Świerczek
  • Dany Carlier
  • Maciej Sitarz
  • Stephane Parola
Original Paper: Nano-structured materials (particles, fibers, colloids, composites, etc.)


The efficient materials for Li-ion battery electrodes require suitable composition, high-crystallinity and appropriate structuration. The last one is important to assure an efficient exchange of Li ions between the anode and electrolyte, thus enhancing the kinetics of electrochemical reactions. Therefore, the synthesis of well-crystallized nano-sized electrode materials exhibiting high surface area is of great interest. Herein, we explore the influence of the glycothermal synthesis variations on the structure and porosity of Li4Ti5O12. The utilized precursors and their concentration have a minor influence on crystallites size, but they could be used to control the porosity of assembled particles. The prepared Li-ion battery anode could be charged at low and high rate reaching the theoretical capacity of Li4Ti5O12. The material retains its peculiar porous structuration even after 1000 cycles at charging/discharging rate of 50C which contributes to the lack of capacity fading. Additionally, 7Li NMR is performed on one of synthesized nano-structured Li4Ti5O12 and compared with commercially available nanosized Li4Ti5O12 to understand the excellent electrochemical performance.

Glycothermal synthesis of lithium titanate, in 1,4-butanediol leads to crystalline NPs of 4-5 nm assembled into highly porous microstructures. Such structuration assures well-developed contact area between the electrode and an electrolyte in Li-ion batteries, which facilitates exchange of Li-ions. Therefore, the material shows excellent electrochemical performances. LTO characterized by different nanostructuration is obtained by varying the synthesis conditions (precursors type and concentration, temperature and co-solvent).


  • Pure nanostructure Li4Ti5O12 was synthesized in varying glycothermal conditions using 1,4-butanediol as the solvent.

  • Simple adjustment of precursors and their concentration tuned the microstructure of the material without affecting the size of crystallites which oscillated around 4 nm.

  • Nano-scaling and proper microstructuration is an effective way to improve kinetics of electrochemical reactions due to the efficient exchange of Li ions between electrodes and electrolytes.

  • 7Li NMR was performed on synthesized material and commercial one in order to understand the peculiar electrochemical properties of the material.


Li-ion batteries Lithium titanate Nanoparticles Glycothermal synthesis Polyols 



MO was supported primarily by the French Minister of Research through Ecole Normale Superieure and by the LABEX IMUST funding for PhD project.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

10971_2018_4844_MOESM1_ESM.docx (84 kb)
Supplementary Information


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Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2018

Authors and Affiliations

  • Mateusz Odziomek
    • 1
    • 2
    Email author
  • Frederic Chaput
    • 1
    Email author
  • Frederic Lerouge
    • 1
  • Anna Rutkowska
    • 3
  • Konrad Świerczek
    • 3
  • Dany Carlier
    • 4
  • Maciej Sitarz
    • 2
  • Stephane Parola
    • 1
  1. 1.Université de Lyon, Ecole Normale Supérieure de Lyon, CNRS UMR 5182, Université Lyon 1, Laboratoire de ChimieLyonFrance
  2. 2.Department of Chemistry of Silicates and MacromoleculesAGH University of Science and Technology, Faculty of Materials Science and CeramicsKrakowPoland
  3. 3.Department of Hydrogen EnergyAGH University of Science and Technology, Faculty of Energy and FuelsKrakowPoland
  4. 4.CNRSUniv. Bordeaux, Bordeaux INP, ICMCB UMR 5026PessacFrance

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