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Synthesis of LiFePO4 powder by the organic–inorganic steric entrapment method

Published online by Cambridge University Press:  27 July 2015

Daniel Ribero Open the ORCID record for Daniel Ribero [Opens in a new window]  and
Waltraud M. Kriven
Daniel Ribero
Affiliation:
Department of Materials Science and Engineering, University of Illinois at Urbana-Champaign, Illinois 61801, USA
Waltraud M. Kriven*
Affiliation:
Department of Materials Science and Engineering, University of Illinois at Urbana-Champaign, Illinois 61801, USA
*
a)Address all correspondence to this author. e-mail: kriven@illinois.edu
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Abstract

A nanoscale and pure, olivine-structured LiFePO4 was synthesized at ∼300 °C using an organic–inorganic steric entrapment method. Normally, when calcined and crystallized in air, this method leads to the synthesis of compounds where the cations are in their highest oxidation state. However, in this study, we found a way to produce compounds having lower oxidation states (e.g., compounds containing Fe2+), which may have wider applications in the synthesis of other compounds with complex chemistry that have variable oxidation states and, therefore, potential applications in electronic ceramics. The resulting LiFePO4 or (Li2O·2FeO·P2O5) was characterized by thermogravimetric analysis/differential thermal analysis, x-ray diffractometry, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma emission spectroscopy, specific surface area by Brunauer–Emmett–Teller nitrogen absorption, and particle size analysis.

Keywords

powder processingnanostructureoxidescombustion synthesisparticulates
Type
Articles
Information
Journal of Materials Research , Volume 30 , Issue 14 , 28 July 2015 , pp. 2133 - 2143
Copyright
Copyright © Materials Research Society 2015 

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References

REFERENCES

Nazri, G. and Pistoia, G.: Lithium Batteries: Science and Technology (Kluwer Academic Publishers, Boston, 2004); pp. 708.Google Scholar
Meligrana, G., Gerbaldi, C., Tuel, A., Bodoardo, S., and Penazzi, N.: Hydrothermal synthesis of high surface LiFePO4 powders as cathode for Li-ion cells. J. Power Sources 160(1), 516–522 (2006).Google Scholar
Chen, J., Vacchio, M., Wang, S., Chernova, N., and Zavalij, P.: The hydrothermal synthesis and characterization of olivines and related compounds for electrochemical applications. Solid State Ionics 178(31–32), 1676–1693 (2008).CrossRefGoogle Scholar
Lin, Y., Pan, H., Gao, M., and Liu, Y.: Effects of reductive conditions on the microstructure and electrochemical properties of sol-gel derived LiFePO4/C. J. Electrochem. Soc. 154(12), A1124–A1128 (2007).CrossRefGoogle Scholar
Hu, S., Zhang, T., Cao, H., Zhang, H., and Li, Z.: Glycine-assisted sol–gel synthesis of LiFePO4/C cathode materials for lithium-ion batteries. Funct. Mater. Lett. 3(3), 217–221 (2010).Google Scholar
Jugović, D., Mitrić, M., Kuzmanović, M., Cvjetićanin, N., Škapin, S., Cekić, B., Ivanovski, V., and Uskoković, D.: Preparation of LiFePO4/C composites by co-precipitation in molten stearic acid. J. Power Sources 196(10), 4613–4618 (2011).CrossRefGoogle Scholar
Liu, A., Hu, Z., Wen, Z., Lei, L., and An, J.: LiFePO4/C with high capacity synthesized by carbothermal reduction method. Ionics 16(4), 311–316 (2010).Google Scholar
Gomez, L.S., de Meatza, I., Martin, M.I., Bengoechea, M., and Cantero, I.: Morphological, structural and electrochemical properties of lithium iron phosphates synthesized by spray pyrolysis. Electrochim. Acta 55(8), 2805–2809 (2010).Google Scholar
Zhang, Y. and Urquidi-Macdonald, M.: Hydrophobic ionic liquids based on the 1-butyl-3-methylimidazolium cation for lithium/seawater batteries. J. Power Sources 144(1), 191–196 (2005).CrossRefGoogle Scholar
Lu, Z., Chen, H., Robert, R., and Deng, J.: Citric acid and ammonium mediated morphological transformations of olivine LiFePO4 particles. Chem. Mater. 23(11), 2848–2859 (2011).CrossRefGoogle Scholar
Arnold, G., Garche, J., Hemmer, R., Ströbele, S., Vogler, C., and Wohlfahrt-Mehrens, M.: Fine-particle lithium iron phosphate LiFePO4 synthesized by a new low-cost aqueous precipitation technique. J. Power Sources 119–121, 247–251 (2003).Google Scholar
Wang, Q., Zhang, W., Yang, Z., Weng, S., and Jin, Z.: Solvothermal synthesis of hierarchical LiFePO4 microflowers as cathode materials for lithium ion batteries. J. Power Sources 196(23), 10176–10182 (2011).CrossRefGoogle Scholar
Tarascon, J.M., Recham, N., Armand, M., Chotard, J., Barpanda, P., and Walker, W.: Hunting for better Li-based electrode materials via low temperature inorganic synthesis. Chem. Mater. 22(3), 724–739 (2010).Google Scholar
Liu, W., Farrington, G.C., Chaput, F., and Dunn, B.: Synthesis and electrochemical studies of spinel phase LiMn2O4 cathode materials prepared by the Pechini process. J. Electrochem. Soc. 143(3), 879–884 (1996).Google Scholar
Recham, N., Chotard, J., Jumas, J., Laffont, L., Armand, M., and Tarascon, J.M.: Ionothermal synthesis of Li-based fluorophosphates electrodes. Chem. Mater. 22(3), 1142–1148 (2010).Google Scholar
Gülgün, M.A., Nguyen, M.H., and Kriven, W.M.: Polymerized organic-inorganic synthesis of mixed oxides. J. Am. Ceram. Soc. 82(3), 556–560 (1999).Google Scholar
Jung, C., Lee, S., Kriven, W., Park, J., and Ryu, W.: A polymer solution technique for the synthesis of nano-sized Li2TiO3 ceramic breeder powders. J. Nucl. Mater. 373, 194–198 (2008).Google Scholar
Lee, S. and Kriven, W.M.: Preparation of ceramic powders by a solution-polymerization route employing PVA solution. Ceram. Eng. Sci. Proc. 19(4), 469–476 (1998).Google Scholar
Rosczyk, B.R., Kriven, W.M., and Mason, T.O.: Solid oxide fuel cell materials synthesized by an organic steric entrapment method. Ceram. Eng. Sci. Proc. 24(3), 287–292 (2003).Google Scholar
Gülgün, M.A., Kriven, W.M., and Nguyen, M.H.: Processes for Preparing Mixed-Oxide Powders. U.S. Patent No. 6,482,387, November 19, 2002.Google Scholar
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