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A novel synthesis of LiFePO4/C from Fe2O3 without extra carbon or carbon-containing reductant

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Abstract

A novel synthesis of LiFePO4/C from Fe2O3 with no extra carbon or carbon-containing reductant was introduced: Fe2O3 (+NH4H2PO4)→Fe2P2O7(+Li2CO3+glucose)→LiFePO4/C. X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) were utilized to characterize relevant products obtained in the synthetic procedure. The reaction of Fe2P2O7 and Li2CO3 was investigated by thermo-gravimetric and differential thermal analysis (TGA-DTA). Fe2O3 is completely reduced to Fe2P2O7 by NH4H2PO4 at 700 °C and Fe2P2O7 fully reacts with Li2CO3 to form LiFePO4 in the temperature range of 663.4–890 °C. The primary particles of LiFePO4/C samples prepared at 670, 700 and 750 °C respectively exhibit uniform morphology and narrow size distribution, 0.5–3 μm for those obtained at 670 and 700 °C and 0.5–5 μm for those obtained at 750 °C. LiFePO4/C (carbon content of 5.49%, mass fraction) made at 670 °C shows an appreciable average capacity of 153.2 mA·h/g at 0.1C in the first 50 cycles.

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References

  1. HU Guo-rong, XIAO Zheng-wei, PENG Zhong-dong, DU Ke, DENG Xin-rong. Preparation of LiFePO4 for lithium ion battery using Fe2P2O7 as precursor [J]. Journal of Central South University of Technology, 2008, 15(4): 531–534.

    Article  Google Scholar 

  2. KIM J, KIM H, PARK I, PARK Y U, YOO J K, PARK K Y, LEE S, KANG K. LiFePO4 with an alluaudite crystal structure for lithium ion batteries [J]. Energy & Environmental Science, 2013, 6(3): 830–834.

    Article  Google Scholar 

  3. SHIN J H, HENDERSON W A, SCACCIC S, PROSINI P P, PASSERINI S. Solid-state Li/LiFePO4 polymer electrolyte batteries incorporating an ionic liquid cycled at 40 °C [J]. Journal of Power Sources, 2006, 156(2): 560–566.

    Article  Google Scholar 

  4. XIAO Zheng-wei, HU Guo-rong, DU Ke, PENG Zhong-dong, DENG Xin-rong. High density LiFePO4/C composite cathode material for lithium ion batteries [J]. The Chinese Journal of Nonferrous Metals, 2007, 17(12): 2040–2045. (in Chinese)

    Google Scholar 

  5. CHEN Quan-qi, LI Xiao-shuan, WANG Jian-ming. Electrochemical performance of LiFePO4/(C+Fe2P) composite cathode material synthesized by sol-gel method [J]. Journal of Central South University of Technology, 2011, 18(4): 978–984.

    Article  Google Scholar 

  6. DELACOURT C, WURM C, LAFFONT L, LERICHE J B, MASQUELIER C. Electrochemical and electrical properties of Nb-and/or C-containing LiFePO4 composite [J]. Solid State Ionics, 2006, 177(3/4): 333–341.

    Article  Google Scholar 

  7. ZHONG M, ZHOU Z. Preparation of high tap-density LiFePO4/C composite cathode materials by carbothermal reduction method using two kinds of Fe3+ precursors [J]. Materials Chemistry and Physics, 2010, 119(3): 428–431.

    Article  Google Scholar 

  8. ZHANG J, XIE J, WU C, CAO G, ZHAO X. In-situ one-pot preparation of LiFePO4/carbon-nanofibers composites and their electrochemical performance [J]. Journal of Materials Science and Technology, 2011, 27(11): 1001–1005.

    Article  Google Scholar 

  9. HUANG Y, REN H, PENG Z, ZHOU Y. Synthesis of LiFePO4/carbon composite from nano-FePO4 by a novel stearic acid assisted rheological phase method [J]. Electrochimica Acta, 2009, 55(1): 311–315.

    Article  Google Scholar 

  10. GAO J, LI J, HE X, JIANG C, WAN C. Synthesis and electrochemical characteristics of LiFePO4/C cathode materials from different precursors [J]. International Journal of Electrochemical Science, 2011, 6: 2818–2825.

    Google Scholar 

  11. YUAN S, DAI K. A novel method with low-cost Fe2O3 to synthesize small size LiFePO4 by carbothermal reduction method [J]. Russian Journal of Electrochemistry, 2011, 47(9): 1144–1147.

    Google Scholar 

  12. TOPRAKCI O, JI L, LIN Z, TOPRAKCI H, ZHANG X. Fabrication and electrochemical characteristics of electrospun LiFePO4/carbon composite fibers for lithium-ion batteries [J]. Journal of Power Sources, 2011, 196(18): 7692–7699.

    Article  Google Scholar 

  13. BARKER J, SAIDI M Y, SWOYET J L. Lithium ion (II) phospho-olivines prepared by a novel carbothermal reduction method [J]. Electrochemical and Solid-State Letters, 2003, 6(3): A53–A55.

    Article  Google Scholar 

  14. REN Q, YANG Y. Effects of Co2+ doping on the crystal structure and electrochemical performance of LiFePO4 [J]. Chinese Journal of Structural Chemistry, 2011, 30(10): 1477–1482.

    MathSciNet  Google Scholar 

  15. ZHANG L, LIANG C, PENG G, HUANG Y, WANG L, QIE L, CROFT M C, IGNATOV A, GOODENOUGH J B. Insight into Fe incorporation in Li3V2(PO4)3/C cathode material [J]. Journal of Electrochemical Society, 2012, 159(10): A1573–A1576.

    Article  Google Scholar 

  16. BARAN E J, BOTTO I L, NORD A G. The vibrational spectrum and the conformation of the P2O7 4-anion in Fe2P2O7 [J]. Journal of Molecular Structure, 1986, 143: 151–154.

    Article  Google Scholar 

  17. RAVET N, GAUTHIER M, ZAGHIB K, GOODENOUGH J B, MAUGER A, GENDRON F, JULIEN C M. Mechanism of the Fe3+ reduction at low temperature for LiFePO4 synthesis from a polymeric additive [J]. Chemistry of Materials, 2007, 19(10): 2595–2602.

    Article  Google Scholar 

  18. BURBA C M, FRECH R. Raman and FTIR spectroscopic study of LixFePO4 (0≤x≤1) [J]. J Journal of Electrochemical Society, 2004, 151(7): A1032–A1038

    Article  Google Scholar 

  19. ZHI X, LIANG G, WANG L, CUI J, YANG L. Synthesis and electrochemical performance of nano-metastructured LiFePO4/C cathode material [J]. Journal of Nanoscience and Nanotechnology, 2010, 10(11): 7676–7679.

    Article  Google Scholar 

  20. YU F, ZHANG J, YANG Y, SONG G. Porous micro-spherical aggregates of LiFePO4/C nanocomposites: A novel and simple template-free concept and synthesis via sol-gel-spray drying method [J]. Journal of Power Sources, 2010, 195(19): 6873–6878.

    Article  Google Scholar 

  21. ZHANG X, HE W, YUE Y, WANG R, SHEN J, LIU S, MA J, XU F. Bio-synthesis participated mechanism of mesoporous LiFePO4/C nanocomposite microspheres for lithium ion battery [J]. Journal of Materials Chemistry, 2012, 37(22): 19948–19956.

    Article  Google Scholar 

  22. JUNG H G, JANG M W, HASSOUN J, SUN Y K, SCROSATI B. A high-rate long-life Li4Ti5O12/Li[Ni0.45Co0.1Mn1.45]O4 lithium-ion battery [J]. Nature Communications, 2011, 2(516): 1–5.

    Google Scholar 

  23. CHUNG S Y, BLOKING J T, CHIANG Y M. Electronically conductive phospho-olivines as lithium storage electrodes [J]. Nature Materials, 2002, 1(2): 123–128.

    Google Scholar 

  24. HOSONO E, WANG Y G, KIDA N, ENOMOTO M, KOJIMA N, OKUBO M, MATSUDA H, SAITO Y, KUDO T, HONMA I, ZHOU H S. Synthesis of triaxial LiFePO4 nanowire with a VGCF core column and a carbon shell through the electrospinning method [J]. Applied Materials & Interfaces, 2010, 2(1): 212–217.

    Article  Google Scholar 

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Authors and Affiliations

  1. Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming, 650093, China

    Zheng-wei Xiao  (肖政伟)

  2. School of Metallurgy and Environment, Central South University, Changsha, 410083, China

    Guo-rong Hu  (胡国荣)

Authors
  1. Zheng-wei Xiao  (肖政伟)
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  2. Guo-rong Hu  (胡国荣)
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Corresponding author

Correspondence to Zheng-wei Xiao  (肖政伟).

Additional information

Foundation item: Project(2010ZC051) supported by the Natural Science Foundation of Yunnan Province, China; Project(2009-041) supported by Analysis and Testing Foundation from Kunming University of Science and Technology, China; Project(14118245) supported by the Starting Research Fund from Kunming University of Science and Technology, China

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Xiao, Zw., Hu, Gr. A novel synthesis of LiFePO4/C from Fe2O3 without extra carbon or carbon-containing reductant. J. Cent. South Univ. 21, 2143–2149 (2014). https://doi.org/10.1007/s11771-014-2164-4

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  • DOI: https://doi.org/10.1007/s11771-014-2164-4

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