SINTESIS LITHIUM TITANAT DENGAN METODE HIDROTERMAL DAN EFEK SUHU SINTERING PADA KARAKTERISTIK NANOSTRUKTURNYA
DOI:
https://doi.org/10.17146/jsmi.2015.17.1.4195Keywords:
Hidrotermal, Lithium titanat, Sintering, Sol-gel, Xerogel TiO2Abstract
SINTESIS LITHIUM TITANAT DENGAN METODE HIDROTERMAL DAN EFEK SUHU SINTERING PADA KARAKTERISTIK NANOSTRUKTURNYA. Lithium titanat merupakan salah satu senyawa yang digunakan sebagai material anoda pada baterai lithium ion. Senyawa ini disintesis dengan mencampurkan TiO2 anatase dan lithium karbonat (Li2CO3) dan diproses menggunakan metode hidrotermal pada suhu 120℃ selama 15 jam, selanjutnya disinter pada tiga variasi suhu sintering yaitu 550℃, 650℃ dan 750℃ untuk menghasilkan LTO fasa spinel kristalin. TiO2 anatase yang dipakai dibuat dengan metode sol-gel dengan suhu kalsinasi 300℃ selama 2 jam. Senyawa yang dihasilkan diamati dengan menggunakan X-Ray Diffraction (XRD), Brunauer Emmet Teller (BET), Spektroskopi Infra Merah (FT-IR) dan Field Emission Scanning Electron Microscope (FE-SEM). Hasil foto mikrograf FE-SEM memperlihatkan padatan senyawa lithium titanat (Li4Ti5O12), Li2TiO3, dan sisa TiO2 rutile dengan struktur morfologi tidak beraturan sebagai aglomerat. Hasil XRD dan BET menunjukkan bahwa pada suhu sintering 550℃ dihasilkan ukuran kristalit ratarata 23,45 nm, luas permukaan 6,65 m2/g, dan didominasi oleh TiO2 rutile, sementara suhu sintering 650℃ dihasilkan ukuran kristalit rata-rata 27,70 nm, luas permukaan 1,91 m2/g, dan masih didominasi oleh TiO2 rutile dan pada suhu 750℃ dihasilkan ukuran kristalit rata-rata 52,06 nm, luas permukaan sangat kecil, dan didominasi oleh litihum titanat (Li4Ti5O12). Hasil FT-IR mengkonfirmasikan keberadaan LTO spinel pada padatan hasil sintering. Ukuran kristalit yang diperoleh dalam kisaran di bawah 100 nm, sesuai dengan tujuan penelitian ini.
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References
. R. Wen. “Nanostructured Li4Ti5O12 as Anode Material for Lithium Ion Batteries.” M.Sc Thesis, Faculty of Science, The University of New South Wales, 2012.
. B. Li, F. Ning, Y. He, H. Du, Q. Yang, F. Kang, and C. Hsu. “Synthesis and Characterization of Long Life Li4Ti5O12/C Composite Using Amorphous TiO2 Nanoparticles.” International Journal of Electrochemical Science, vol. 6, pp. 3210-3223, Aug. 2011.
. C. Zhang, Y. Zhang, J. Wang, D. Wang, D. He, and Y. Xia. “Li4Ti5O12 prepared by a modified citric acid sol-gel method for lithium-ion battery.” Journal of Power Sources, vol. 236, pp. 118-125, Jan. 2013.
. T. Yuan, R. Cai, R. Ran, Y. Zhou, Z. Shao, P. Gu, and Z. Shao. “A mechanism study of synthesis of Li4Ti5O12 from TiO2 anatase.” Journal of Alloys and Compounds, vol. 505, no. 1, pp. 367-373, Aug. 2010.
. J.-W. Shin, C.-H. Hong, and D.-H. Yoon. “Effects of TiO2 Starting Materials on the Solid-State Formation of Li4Ti5O12.” Journal of the American Ceramic Society, vol. 95, no. 6, pp. 1894-1900, Jun. 2012.
. S. Han, J. H. Ryu, J. Jeong, and D. Yoon. “Solid-state synthesis of Li4Ti5O12 for high power lithium ion battery applications.” Journal of Alloys and Compounds, vol. 570, pp. 144-149, Mar. 2013.
. Y. J. Gu, Z. Guo, and H. Q. Liu. “Structure and electrochemical properties of Li4Ti5O12 with Li excess as an anode electrode material for Li-ion batteries.” Electrochimica Acta, vol. 123, pp. 576-581, Jan. 2014.
. W. Liu, D. Shao, G. Luo, Q. Gao, G. Yan, J. He, D. Chen, X. Yu, and Y. Fang. “Mesoporous Spinel Li4Ti5O12 Nanoparticles for High Rate Lithium-ion Battery Anodes.” Electrochimica Acta, vol. 133, pp. 578-582, Jul. 2014.
. H. Yan, Z. Zhu, D. Zhang, and W. Li. “A new hydrothermal synthesis of spherical Li4Ti5O12 anode material for lithium-ion secondary batteries.” Journal of Power Sources, vol. 219, pp. 45-51, Jul. 2012.
. X. Guo, C. Wang, and M. Chen. “A novel non-organic hydrothermal/hydrolysis method for preparation of well-dispersed Li4Ti5O12.” Materials Letters, vol. 83, pp. 39-41, Jun. 2012.
. Z. Zhang, L. Cao, J. Huang, D. Wang, J. Wu, and Y. Cai. “Hydrothermal synthesis of Li4Ti5O12 microsphere with high capacity as anode material for lithium ion batteries.” Ceramics International, vol. 39, no. 3, pp. 2695-2698, Sep. 2013.
. Z. Zhang, L. Cao, J. Huang, D. Wang, Y. Meng, and Y. Cai. “Temperature effect on spinel Li4Ti5O12 as anode materials for lithium ion batteries.” Electrochimica Acta, vol. 88, pp. 443-446, Jan. 2013.
. S. Kim, S. Fang, Z. Zhang, J. Chen, L. Yang, J. E. Penner-Hahn, and A. Deb. “The electrochemical and local structural analysis of the mesoporous Li4Ti5O12 anode.” Journal of Power Sources, vol. 268, pp. 294-300, Dec. 2014.
. R. P. Maloney, H. J. Kim, and J. S. Sakamoto. “Lithium Titanate Aerogel for Advanced Lithium-Ion Batteries.” Applied Material & Interfaces, vol. 4, pp. 2318-2321, Apr. 2012.
. I. Bilecka and M. Niederberger. “New developments in the nonaqueous and/or non-hydrolytic sol-gel synthesis of inorganic nanoparticles.” Electrochimica Acta, vol. 55, no. 26, pp. 7717-7725, Nov. 2010.
. B. Priyono, A. H. Yuwono, B. Munir, A. Rahman, A. Maulana, and H. Abimanyu. “Synthesis of Highly-Ordered TiO2 through CO2 Supercritical Extraction for Dye-Sensitized Solar Cell Application.” Advanced Materials Research, vol. 789, pp. 28-32, Sep. 2013.
. D.-S. Seo, J.-K. Lee, and H. Kim. “Preparation of nanotube-shaped TiO2 powder.” Journal of Crystal Growth, vol. 229, no. 1-4, pp. 428-432, Jul. 2001.
. E. Morgado, M. A. S. de Abreu, O. R. C. Pravia, B. A. Marinkovic, P. M. Jardim, F. C. Rizzo, and A. S. Araújo. “A study on the structure and thermal stability of titanate nanotubes as a function of sodium content.” Solid State Sciences, vol. 8, no. 8, pp. 888-900, Aug. 2006.
. G. H. Du, Q. Chen, R. C. Che, Z. Y. Yuan, and L. M. Peng. “Preparation and structure analysis of titanium oxide nanotubes.” Applied Physics Letters, vol. 79, no. 22, pp. 3702-3704, Sep. 2001.
. K. Byrappa and M. Yoshimura. Handbook of Hydrothermal Technology, A Technology for Crystal Growth and Materials Processing. 2001.
. J. Ortiz-Landeros, C. Gómez-Yáñez, R. López-Juárez, I. Dávalos-Velasco, and H. Pfeiffer. “Synthesis of advanced ceramics by hydrothermal crystallization and modified related methods.” Journal of Advanced Ceramics, vol. 1, no. 3, pp. 204-220, Aug. 2012.
. A. H. Sun, P. J. Guo, Z. X. Li, Y. Li, and P. Cui. “Low temperature synthesis of anatase and rutile titania nanopowders by hydrolysis of TiCl4 using ammonia gas.” Journal of Alloys and Compounds, vol. 481, pp. 605-609, Mar. 2009.
. Y. Hu, H. L. Tsai, and C. L. Huang. “Effect of brookite phase on the anatase-rutile transition in titania nanoparticles.” Journal of the European Ceramic Society, vol. 23, no. 5, pp. 691-696, Jun. 2003.
. D. C. L. Vasconcelos, V. C. Costa, E. H. M. Nunes, A. C. S. Sabioni, M. Gasparon, and W. L. Vasconcelos. “Infrared Spectroscopy of Titania Sol-Gel Coatings on 316L Stainless Steel.” Materials Sciences and Applications, vol. 02, no. 10, pp. 1375-1382, Mar. 2011.
. A. Verma, S. B. Samanta, A. K. Bakhshi, and S. A. Agnihotry. “Effect of stabilizer on structural, optical and electrochemical properties of sol-gel derived spin coated TiO2 films.” Solar Energy Materials and Solar Cells, vol. 88, no. 1, pp. 47-64, Jan. 2005.
. H. Yan, Z. Zhu, D. Zhang, W. Li, and Qilu. “A new hydrothermal synthesis of spherical Li4Ti5O12 anode material for lithium-ion secondary batteries.” Journal of Power Sources, vol. 219, pp. 45-51, Jul. 2012.
. J. W. W. Shin, C. H. H. Hong, and D. H. H. Yoon. “Effects of TiO2 Starting Materials on the Solid-State Formation of Li4Ti5O12.” Journal of the American Ceramic Society, vol. 95, no. 6, pp. 1894-1900, Jun. 2012.
. S. W. Han, J. W
. Shin, and D. H. Yoon. “Synthesis of pure nano-sized Li4Ti5O12 powder via solid-state reaction using very fine grinding media.” Ceramics International, vol. 38, no. 8, pp. 6963-6968, May. 2012.
. C. H. Hong, A. Noviyanto, J. H. Ryu, J. Kim, and D. H. Yoon. “Effects of the starting materials and mechanochemical activation on the properties of solid-state reacted Li4Ti5O12 for lithium ion batteries.” Ceramics International, vol. 38, no. 1, pp. 301-310, Jan. 2012.
. S. Speakman. “Estimating Crystallite Size Using XRD.” MIT Center for Materials Science and Engineering, 2015. [Online]. Available: http://prism.mit.edu/xray/. [Accessed: 19-May-2015].
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