Hydrothermal Method for Synthesizing and Characterizing LiMn2O4 as a Cathode Material for Rechargeable (Li-ion) Battery Applications
DOI:
https://doi.org/10.24237/ASJ.03.02.862DKeywords:
hydrothermal method, CV, Warburg Impedance, the Coulombic efficiency.Abstract
This research involved the production of the spinel compound LiMn2O4 as the cathode active substance for Li-ion cells using the hydrothermal method. The field-emission scanning electron microscope (FESEM) was employed for an evaluative analysis of the external surface morphology of the synthesized material. The crystal structure of the spinel material was confirmed using X-ray diffractometry (XRD). The XRD graph exhibited no signs of impurity peaks, confirming a singular crystal structure phase. As per the Scherrer equation, the crystal size was estimated at 12.65 nm. The energy-dispersive X-ray spectroscopy (EDX) spectra for the equipped sample showed the existence of manganese and oxygen, and the concentrations were very close to the elemental composition used. Electrochemical attributes were investigated through galvanostatic charge–discharge (GCD) cycling and cyclic voltammetry (CV) in a specific voltage range. The LiMn2O4sample displayed a charge capacity of 111.6 mAhg-1 and a discharge capacity of 109.9 mAhg-1. The Coulombic efficiency exhibited by this electrode was 98.4%. After 100 cycles, the capacity retention was as high as 57.1%. The electrochemical impedance spectroscopy (EIS) measurements of the LiMn2O4 electrode, including the electrolyte bulk resistance (Rs), charge transfer resistance (Rct), and Warburg Impedance (Wo), were 8.1 ohms, 127.5 ohms, and 0.86 ohms, respectively.
References
Kang, K., Meng, Y. S., Breger, J., Grey, C. P., Ceder, G., Electrodes with high power and high capacity for rechargeable lithium batteries, Science, 311(5763), 977-980, (2006)
Tarascon, J. M., Armand, M., Issues and challenges facing rechargeable lithium batteries, nature, 414(6861), 359-367, (2001)
Yunjian, L., Xinhai, L., Huajun, G., Zhixing, W., Qiyang, H., Wenjie, P., Yong, Y., Electrochemical performance and capacity fading reason of LiMn2O4/graphite batteries stored at room temperature, Journal of Power Sources, 189(1), 721-725, (2009)
Xu, B., Qian, D., Wang, Z., Meng, Y. S., Recent progress in cathode materials research for advanced lithium ion batteries, Materials Science and Engineering: R: Reports, 73(5-6), 51-65, (2012)
Goodenough, J. B., Park, K. S., The Li-ion rechargeable battery: a perspective, Journal of the American Chemical Society, 135(4), 1167-1176, (2013)
Wan, C., Wu, M., Wu, D., Synthesis of spherical LiMn2O4 cathode material by dynamic sintering of spray-dried precursors, Powder technology, 199(2), 154-158, (2010)
Taniguchi, I., Fukuda, N., Konarova, M., Synthesis of spherical LiMn2O4 microparticles by a combination of spray pyrolysis and drying method:, Powder Technology, 181(3), 228-236, (2008)
H.W. Chan, J.G. Duh, S.R. Sheen, LiMn2O4 cathode doped with excess lithium and synthesized by co-precipitation for Li-ion batteries, Journal of Power Sources, 115, 110-118, (2003)
Xia, Y., Sakai, T., Fujieda, T., Yang, X. Q., Sun, X., Ma, Z. F., ... Yoshio, M., Correlating Capacity Fading and Structural Changes in Li1+yMn2−yO4−δ Spinel Cathode Materials: A Systematic Study on the Effects of Li/Mn Ratio and Oxygen Deficiency, Journal of The Electrochemical Society, 148(7), A723, (2001)
Shim, J., Kostecki, R., Richardson, T., Song, X., Striebel, K. A., Electrochemical analysis for cycle performance and capacity fading of a lithium-ion battery cycled at elevated temperature, Journal of power sources, 112(1), 222-230, (2002)
Kim, D. K., Muralidharan, P., Lee, H. W., Ruffo, R., Yang, Y., Chan, C. K., ... Cui, Y., Spinel LiMn2O4 nanorods as lithium ion battery cathodes, Nano letters, 8(11), 3948-3952, (2008)
Li, N., Patrissi, C. J., Che, G., Martin, C. R., Rate capabilities of nanostructured LiMn2O4 electrodes in aqueous electrolyte, Journal of the electrochemical Society, 147(6), 2044, (2000)
Curtis, C. J., Wang, J., Schulz, D. L., Preparation and Characterization of LiMn2O4 Spinel Nanoparticles as Cathode Materials in Secondary Li Batteries, Journal of the Electrochemical Society, 151(4), A590., (2004)
Du, K., Zhang, H., Preparation and performance of spinel LiMn2O4 by a citrate route with combustion, Journal of alloys and compounds, 352(1-2), 250-254, (2003)
Nieto, S., Majumder, S. B., Katiyar, R. S., Improvement of the cycleability of nano-crystalline lithium manganate cathodes by cation co-doping, Journal of power sources, 136 (1), 88-98, (2004)
Guo, H. J., Li, X. Q., He, F. Y., Li, X. H., Wang, Z. X., Peng, W. J. , Effects of sodium substitution on properties of LiMn2O4 cathode for lithium ion batteries, Transactions of Nonferrous Metals Society of China, 20(6), 1043-1048, (2010)
Chen, Y. C., Xie, K., Pan, Y., Zheng, C. M., Wang, H. L., High power nano-LiMn2O4 cathode materials with high-rate pulse discharge capability for lithium-ion batteries, Chinese Physics B, 20(2), 028201, (2011)
Zhu, C., Nobuta, A., Saito, G., Nakatsugawa, I., Akiyama, T., Solution combustion synthesis of LiMn2O4 fine powders for lithium ion batteries, Advanced Powder Technology, 25(1), 342-347, (2014)
O. A. Hussein, Synthesis and Characterization of (Polypyrrole-Ferrites) Nanocomposites for Multi-Applications, Ph.D. Thesis, University of Diyala, Diyala, Iraq (2022)
Peng, C., Huang, J., Guo, Y., Li, Q., Bai, H., He, Y., Guo, J., Electrochemical performance of spinel LiAlxMn2−xO4 prepared rapidly by glucose-assisted solid-state combustion synthesis, Vacuum, 120, 121-126, (2015)
Mao, L., Du, S., Li, S., Ren, Z., Excellent stability of Al-doped LiMn2O4 prepared by a sol-gel method, In 2016 5th International Conference on Environment, Materials, Chemistry and Power Electronics. Atlantis Press, (2016)
Ahmad, M., Shahid, M., Alanazi, Y. M., ur Rehman, A., Asif, M., Dunnill, C. W., Lithium ferrite (Li0.5Fe2.5O4): synthesis, structural, morphological and magnetic evaluation for storage devices, journal of materials research and technology, 18, 3386-3395, (2022)
Goldstein, J. I., Newbury, D. E., Michael, J. R., Ritchie, N. W., Scott, J. H. J., Joy, D. C., Scanning electron microscopy and X-ray microanalysis, springer, (2017)
Homada, H. T., Alia, N. M., Al-Jubourib, O. A., Al-Timimia, M. H., Synthesis and characterization of LiCo1-xNixO2 nanoparticles by urea route as cathode for lithium-ion battery, Journal of Ovonic Research, 19(6), 783-791, (2023)
Elgrishi, N., Rountree, K. J., Mccarthy, B. D., Rountree, E. S., Eisenhart, T. T., Dempsey, J. L., A practical beginner’s guide to cyclic voltammetry, Journal of chemical education, 95(2), 197-206, (2018)
Abou-Rjeily, J., Bezza, I., Laziz, N. A., Autret-Lambert, C., Sougrati, M. T., Ghamouss, F., High-rate cyclability and stability of LiMn2O4 cathode materials for lithium-ion batteries from low-cost natural β−MnO2, Energy Storage Materials, 26, 423-432, (2020)
Song, H., Liu, Y., Zhang, C., Liu, C., Cao, G., Mo-doped LiV3O8 nanorod-assembled nanosheets as a high performance cathode material for lithium ion batteries, Journal of Materials Chemistry A, 3(7), 3547-3558, (2015)
Wang, J. L., Li, Z. H., Yang, J., Tang, J. J., Yu, J. J., Nie, W. B., ... Xiao, Q. Z., Effect of Al-doping on the electrochemical properties of a three-dimensionally porous lithium manganese oxide for lithium-ion batteries, Electrochimica acta, 75, 115-122, (2012)
Madhu, M., Venkateswara Rao, A., Mutyala, S., La and Ni Co-doping effect in LiMn2O4 on structural and electrochemical properties for lithium-ion batteries, Journal of Electronic Materials, 50(9), 5141-5149, (2021)
Zhang, J., Shen, J., Wei, C., Tao, H., Yue, Y., Synthesis and enhanced electrochemical performance of the honeycomb TiO2/LiMn2O4 cathode materials, Journal of Solid State Electrochemistry, 20, 2063-2069, (2016)
Lazanas, A. C., Prodromidis, M. I., Electrochemical Impedance Spectroscopy, A Tutorial. ACS Measurement Science Au, (2023)
Sharifi, H., Mosallanejad, B., Mohammadzad, M., Hosseini-Hosseinabad, S. M., Ramakrishna, S., Cycling performance of LiFePO4/graphite batteries and their degradation mechanism analysis via electrochemical and microscopic techniques, Ionics, 1-16, (2022)
Priyono, S., Hardiyani, S., Syarif, N., Subhan, A., Suhandi, A., Electrochemical performanceof LiMn2O4 with varying thickness of cathode sheet, In Journal of Physics: Conference Series (Vol. 1191, No. 1, p. 012022). IOP Publishing, (2019)
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