Li4Ti5O12 Synthesis with High Specific Surface Area and Single Phase
Affiliation(s)
Department of Mechanical Systems Engineering, Faculty of Engineering, Aich University of Technology, Gamagori, Japan.
Department of Mechanical Systems Engineering, Faculty of Engineering, Aich University of Technology, Gamagori, Japan.
ABSTRACT
We have investigated a novel Li4Ti5O12 synthesis with high specific surface area, high crystallization and single phase and its mechanism. The method was performed with a solid phase synthesis by using CH3COOLi·2H2O and anatase TiO2 via Li2TiO3 as an intermediate in pre-sintering at 500°C and sintering at 750°C. This result showed specific surface area of 12 m2/g and single phase- Li4Ti5O12 by applying the high specific surface anatase TiO2 as a precursor.
We have investigated a novel Li4Ti5O12 synthesis with high specific surface area, high crystallization and single phase and its mechanism. The method was performed with a solid phase synthesis by using CH3COOLi·2H2O and anatase TiO2 via Li2TiO3 as an intermediate in pre-sintering at 500°C and sintering at 750°C. This result showed specific surface area of 12 m2/g and single phase- Li4Ti5O12 by applying the high specific surface anatase TiO2 as a precursor.
Cite this paper
Ohtake, T. and Iijima, K. (2015) Li4Ti5O12 Synthesis with High Specific Surface Area and Single Phase. Journal of Materials Science and Chemical Engineering, 3, 68-73. doi: 10.4236/msce.2015.39009.
Ohtake, T. and Iijima, K. (2015) Li4Ti5O12 Synthesis with High Specific Surface Area and Single Phase. Journal of Materials Science and Chemical Engineering, 3, 68-73. doi: 10.4236/msce.2015.39009.
References
[1] Tsutomu, O., Atsushi, U. and Norihiro, Y. (2005) Zero-Strain Insertion Material Insertion Material of Li[Lil/3Ti5/3]O4 for Rechargeable Lithium Cells. Journal of the Electrochemical Society, 142, 1431-1435. [2] Masataka, W. (2001) Recent Developments in Lithium Ion Batteries. Materials Science and Engineering: R: Reports, 33, 109-134.
http://dx.doi.org/10.1016/S0927-796X(01)00030-4 [3] Leonidov, I.A., Leonidova, O.N., Perelyaeva, L.A., Samigullina, R.F., Kovyazina, S.A. and Patrakeev, M.V. (2003) Structure, Ionic Conduction, and Phase Transformations in Lithium Titanate Li4Ti5O12. Physics of the Solid State, 45, 2183-2188.
http://dx.doi.org/10.1134/1.1626760 [4] Belharouak, I., Sun, Y.-K., Lu, W. and Amine, K. (2007) On the Safety of the Li4Ti5O12∕LiMn2O4 Lithium-Ion Battery System. Journal of the Electrochemical Society, 154, A1083-A1087.
http://dx.doi.org/10.1149/1.2783770 [5] Roth, E.P. and Doughty, D.H. (2004) Thermal Abuse Performance of High-Power 18650 Li-Ion Cells. Journal of Power Sources, 128, 308-318.
http://dx.doi.org/10.1016/j.jpowsour.2003.09.068 [6] Abraham, D.P., Roth, E.P., Kostecki, R., McCarthy, K., MacLaren, S. and Doughty, D.H. (2006) Diagnostic Examination of Thermally Abused High-Power Lithium-Ion Cells. Journal of Power Sources, 161, 648-657.
http://dx.doi.org/10.1016/j.jpowsour.2006.04.088 [7] Gao, J., Ying, J., Jiang, C. and Wan, C. (2007) High-Density Spherical Li4Ti5O12/C Anode Material with Good Rate Capability for Lithium Ion Batteries. Journal of Power Sources, 166, 255-259.
http://dx.doi.org/10.1016/j.jpowsour.2007.01.014 [8] Huang, J. and Jiang, Z. (2008) The Preparation and Characterization of Li4Ti5O12/Carbon Nano-Tubes for Lithium Ion Battery. Electrochimica Acta, 53, 7756-7759.
http://dx.doi.org/10.1016/j.electacta.2008.05.031 [9] Hao, Y.-J., Lai, Q.-Y., Lu, J.-Z., Liu, D.-Q. and Ji, X.-Y. (2007) Influence of Various Complex Agents on Electrochemical Property of Li4Ti5O12 Anode Material. Journal of Alloys and Compounds, 439, 330-336.
http://dx.doi.org/10.1016/j.jallcom.2006.08.082 [10] Pierre, K., Aurélie, G., Manfred, W., Laurent, A., Josette, O.-F., Pierre-Emmanuel, L. and Jean-Claude, J. (2003) Phase Transition in the Spinel Li4Ti5O12 Induced by Lithium Insertion: Influence of the Substitutions Ti/V, Ti/Mn, Ti/F. Journal of Power Sources, 119, 626-630. [11] Chen, C.H., Vaughey, J.T., Jansen, A.N., Dees, D.W., Kahaian, A.J., Goacher, T. and Thackeray, M.M. (2001) Studies of Mg-Substituted Li4xMgxTi5O12 Spinel Electrodes (0≤x≤1) for Lithium Batteries. Journal of The Electrochemical Society, 148, A102-A104.
http://dx.doi.org/10.1149/1.1344523 [12] Robertson, A.D., Trevino, L., Tukamoto, H. and Irvine, J.T.S. (1999) New Inorganic Spinel Oxides for Use as Negative Electrode Materials in Future Lithium-Ion Batteries. Journal of Power Sources, 81, 352-357.
http://dx.doi.org/10.1016/S0378-7753(98)00217-1 [13] Mukai, K., Ariyoshi, K. and Ohzuku, T. (2005) Comparative Study of Li[CrTi]O4, Li[Li1/3Ti5/3]O4 and Li1/2Fe1/2 [Li1/2Fe1/2Ti]O4 in Non-Aqueous Lithium Cells. Journal of Power Sources, 146, 213-216.
http://dx.doi.org/10.1016/j.jpowsour.2005.03.019 [14] Huang, S.H., Wen, Z.Y., Zhang, J.C., Gu, Z.H. and Xu, X.H. (2006) Li4Ti5O12/Ag Composite as Electrode Materials for Lithium-Ion Battery. Solid State Ionics, 177, 851-855.
http://dx.doi.org/10.1016/j.ssi.2006.01.050 [15] Gao, J., Jiang, C.Y., Ying, J.R. and Wan, C.R. (2006) Preparation and Characterization of High-Density Spherical Li4Ti5O12 Anode Material for Lithium Secondary Batteries. Journal of Power Sources, 155, 364-367.
http://dx.doi.org/10.1016/j.jpowsour.2005.04.008 [16] Hao, Y.J., Lai, Q.Y., Lu, J.Z., Wang, H.L., Chen, Y.D. and Ji, X.Y. (2006) Synthesis and Characterization of Spinel Li4Ti5O12 Anode Material by Oxalic Acid-Assisted Sol-Gel Method. Journal of Power Sources, 158, 1358-1364.
http://dx.doi.org/10.1016/j.jpowsour.2005.09.063 [17] Hao, Y.J., Lai, Q.Y., Xu, Z.H., Liu, X.Q. and Ji, X.Y. (2005) Synthesis by TEA Sol-Gel Method and Electrochemical Properties of Li4Ti5O12 Anode Material for Lithium-Ion Battery. Solid State Ionics, 176, 1201-1206.
http://dx.doi.org/10.1016/j.ssi.2005.02.010 [18] Kosovaa, N.V., Anufrienkob, V.F., Larinab, T.V., Rougierc, A., Aymardc, L. and Tarasconc, J.M. (2002) Disordering and Electronic State of Cobalt Ions in Mechanochemically Synthesized LiCoO2. Journal of Solid State Chemistry, 165, 56-64.
http://dx.doi.org/10.1006/jssc.2002.9493 [19] Balaz, P. (2004) Mechanochemistry of Sulphides. Journal of Materials Science, 39, 5097-5102.
http://dx.doi.org/10.1023/B:JMSC.0000039190.72325.cf [20] Georgina, I. and Anthony, R.W. (1980) Phase Equilibria in the System Li2O-TiO2. Materials Research Bulletin, 15, 1655-1660.
http://dx.doi.org/10.1016/0025-5408(80)90248-2 [21] Leonidov, I.A., Leonidova, O.N., Perelyaeva, L.A., Samigullina, R.F., Kovyazina, S.A. and Patrakeev M.V. (2003) Structure, Ionic Conduction, and Phase Transformations in Lithium Titanate Li4Ti5O12. Physics of the Solid State, 45, 2183-2188.
http://dx.doi.org/10.1134/1.1626760 [22] Lee, S.S., Byun, K.T., Park, J.P., Kim, S.K., Kwak, H.Y. and Shim, I.W. (2007) Preparation of Li4Ti5O12 Nanoparticles by a Simple Sonochemical Mehod. Dalton Transactions, 37, 4182-4184.
http://dx.doi.org/10.1039/b707164g [23] Kim, J. and Cho, J. (2007) Spinel Li4Ti5O12 Nanowires for High-Rate Li-Ion Intercalation Electrode. Electrochemical and Solid-State Letters, 10, A81-A84.
http://dx.doi.org/10.1149/1.2431242
[1] Tsutomu, O., Atsushi, U. and Norihiro, Y. (2005) Zero-Strain Insertion Material Insertion Material of Li[Lil/3Ti5/3]O4 for Rechargeable Lithium Cells. Journal of the Electrochemical Society, 142, 1431-1435. [2] Masataka, W. (2001) Recent Developments in Lithium Ion Batteries. Materials Science and Engineering: R: Reports, 33, 109-134.
http://dx.doi.org/10.1016/S0927-796X(01)00030-4 [3] Leonidov, I.A., Leonidova, O.N., Perelyaeva, L.A., Samigullina, R.F., Kovyazina, S.A. and Patrakeev, M.V. (2003) Structure, Ionic Conduction, and Phase Transformations in Lithium Titanate Li4Ti5O12. Physics of the Solid State, 45, 2183-2188.
http://dx.doi.org/10.1134/1.1626760 [4] Belharouak, I., Sun, Y.-K., Lu, W. and Amine, K. (2007) On the Safety of the Li4Ti5O12∕LiMn2O4 Lithium-Ion Battery System. Journal of the Electrochemical Society, 154, A1083-A1087.
http://dx.doi.org/10.1149/1.2783770 [5] Roth, E.P. and Doughty, D.H. (2004) Thermal Abuse Performance of High-Power 18650 Li-Ion Cells. Journal of Power Sources, 128, 308-318.
http://dx.doi.org/10.1016/j.jpowsour.2003.09.068 [6] Abraham, D.P., Roth, E.P., Kostecki, R., McCarthy, K., MacLaren, S. and Doughty, D.H. (2006) Diagnostic Examination of Thermally Abused High-Power Lithium-Ion Cells. Journal of Power Sources, 161, 648-657.
http://dx.doi.org/10.1016/j.jpowsour.2006.04.088 [7] Gao, J., Ying, J., Jiang, C. and Wan, C. (2007) High-Density Spherical Li4Ti5O12/C Anode Material with Good Rate Capability for Lithium Ion Batteries. Journal of Power Sources, 166, 255-259.
http://dx.doi.org/10.1016/j.jpowsour.2007.01.014 [8] Huang, J. and Jiang, Z. (2008) The Preparation and Characterization of Li4Ti5O12/Carbon Nano-Tubes for Lithium Ion Battery. Electrochimica Acta, 53, 7756-7759.
http://dx.doi.org/10.1016/j.electacta.2008.05.031 [9] Hao, Y.-J., Lai, Q.-Y., Lu, J.-Z., Liu, D.-Q. and Ji, X.-Y. (2007) Influence of Various Complex Agents on Electrochemical Property of Li4Ti5O12 Anode Material. Journal of Alloys and Compounds, 439, 330-336.
http://dx.doi.org/10.1016/j.jallcom.2006.08.082 [10] Pierre, K., Aurélie, G., Manfred, W., Laurent, A., Josette, O.-F., Pierre-Emmanuel, L. and Jean-Claude, J. (2003) Phase Transition in the Spinel Li4Ti5O12 Induced by Lithium Insertion: Influence of the Substitutions Ti/V, Ti/Mn, Ti/F. Journal of Power Sources, 119, 626-630. [11] Chen, C.H., Vaughey, J.T., Jansen, A.N., Dees, D.W., Kahaian, A.J., Goacher, T. and Thackeray, M.M. (2001) Studies of Mg-Substituted Li4xMgxTi5O12 Spinel Electrodes (0≤x≤1) for Lithium Batteries. Journal of The Electrochemical Society, 148, A102-A104.
http://dx.doi.org/10.1149/1.1344523 [12] Robertson, A.D., Trevino, L., Tukamoto, H. and Irvine, J.T.S. (1999) New Inorganic Spinel Oxides for Use as Negative Electrode Materials in Future Lithium-Ion Batteries. Journal of Power Sources, 81, 352-357.
http://dx.doi.org/10.1016/S0378-7753(98)00217-1 [13] Mukai, K., Ariyoshi, K. and Ohzuku, T. (2005) Comparative Study of Li[CrTi]O4, Li[Li1/3Ti5/3]O4 and Li1/2Fe1/2 [Li1/2Fe1/2Ti]O4 in Non-Aqueous Lithium Cells. Journal of Power Sources, 146, 213-216.
http://dx.doi.org/10.1016/j.jpowsour.2005.03.019 [14] Huang, S.H., Wen, Z.Y., Zhang, J.C., Gu, Z.H. and Xu, X.H. (2006) Li4Ti5O12/Ag Composite as Electrode Materials for Lithium-Ion Battery. Solid State Ionics, 177, 851-855.
http://dx.doi.org/10.1016/j.ssi.2006.01.050 [15] Gao, J., Jiang, C.Y., Ying, J.R. and Wan, C.R. (2006) Preparation and Characterization of High-Density Spherical Li4Ti5O12 Anode Material for Lithium Secondary Batteries. Journal of Power Sources, 155, 364-367.
http://dx.doi.org/10.1016/j.jpowsour.2005.04.008 [16] Hao, Y.J., Lai, Q.Y., Lu, J.Z., Wang, H.L., Chen, Y.D. and Ji, X.Y. (2006) Synthesis and Characterization of Spinel Li4Ti5O12 Anode Material by Oxalic Acid-Assisted Sol-Gel Method. Journal of Power Sources, 158, 1358-1364.
http://dx.doi.org/10.1016/j.jpowsour.2005.09.063 [17] Hao, Y.J., Lai, Q.Y., Xu, Z.H., Liu, X.Q. and Ji, X.Y. (2005) Synthesis by TEA Sol-Gel Method and Electrochemical Properties of Li4Ti5O12 Anode Material for Lithium-Ion Battery. Solid State Ionics, 176, 1201-1206.
http://dx.doi.org/10.1016/j.ssi.2005.02.010 [18] Kosovaa, N.V., Anufrienkob, V.F., Larinab, T.V., Rougierc, A., Aymardc, L. and Tarasconc, J.M. (2002) Disordering and Electronic State of Cobalt Ions in Mechanochemically Synthesized LiCoO2. Journal of Solid State Chemistry, 165, 56-64.
http://dx.doi.org/10.1006/jssc.2002.9493 [19] Balaz, P. (2004) Mechanochemistry of Sulphides. Journal of Materials Science, 39, 5097-5102.
http://dx.doi.org/10.1023/B:JMSC.0000039190.72325.cf [20] Georgina, I. and Anthony, R.W. (1980) Phase Equilibria in the System Li2O-TiO2. Materials Research Bulletin, 15, 1655-1660.
http://dx.doi.org/10.1016/0025-5408(80)90248-2 [21] Leonidov, I.A., Leonidova, O.N., Perelyaeva, L.A., Samigullina, R.F., Kovyazina, S.A. and Patrakeev M.V. (2003) Structure, Ionic Conduction, and Phase Transformations in Lithium Titanate Li4Ti5O12. Physics of the Solid State, 45, 2183-2188.
http://dx.doi.org/10.1134/1.1626760 [22] Lee, S.S., Byun, K.T., Park, J.P., Kim, S.K., Kwak, H.Y. and Shim, I.W. (2007) Preparation of Li4Ti5O12 Nanoparticles by a Simple Sonochemical Mehod. Dalton Transactions, 37, 4182-4184.
http://dx.doi.org/10.1039/b707164g [23] Kim, J. and Cho, J. (2007) Spinel Li4Ti5O12 Nanowires for High-Rate Li-Ion Intercalation Electrode. Electrochemical and Solid-State Letters, 10, A81-A84.
http://dx.doi.org/10.1149/1.2431242