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Preparation of Spherical FePO4 by Chemical Co-precipitation Combined with Spray-Drying

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Abstract

Well-shaped spherical agglomerates of FePO4 particles were prepared by a novel method: chemical co-precipitation combined with spray-drying. Tap density analysis, Brunauer–Emmett–Teller analysis, characterizations of X-ray diffraction, scanning electron microscopy, and transmission electron microscopy confirmed that the micron-sized spherical agglomerates with high specific surface area and high tap density were composed of the uniform nano-sized particles. The effects of pH and reaction time on the morphology of the FePO4 particles were investigated by experimental and theoretical analyses. The analyses revealed that amorphous FePO4 was responsible for forming a well-shaped spherical agglomerate, and the ideal spherical particles were obtained at pH 3. The reaction time also played a significant role in controlling the size and surface morphology of the FePO4 particles, and smooth spherical FePO4 particles were obtained at a reaction time of 6 h. By this novel method, poly-porous spherical iron phosphate particles were prepared, which can be used with high efficiency in some special fields, especially as a precursor for synthesizing LiFePO4 and catalysts.

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References

  1. Mesko MG, Day DE, Bunker BC (2000) Immobilization of CsCl and SrF2 in iron phosphate glasses. Waste Manag 20(4):271–278

    Article  Google Scholar 

  2. Balmér P, Frederiksen OF (1975) A pilot-plant scale evaluation of potential precipitants in the secondary precipitation process. Water Res 9(8):721–727

    Article  Google Scholar 

  3. Lazzarin P, Bellemo S (1989) Fatigue strength of AISI304 and FePO4 steels in the presence of circular notches. Lamiera 26(10):116–123

    Google Scholar 

  4. De Latour C (1973) Magnetic separation in water pollution control. IEEE Trans Magn 9(3):314–316

    Article  Google Scholar 

  5. Lai YM, Liang XF, Yang SY et al (2011) Raman and FTIR spectra of iron phosphate glasses containing cerium. J Mol Struct 992(1–3):84–88

    Article  Google Scholar 

  6. Ye W, Otsuka K (1997) Partial oxidation of ethane by reductively activated oxygen over iron phosphate catalyst. J Catal 171(1):106–114

    Article  Google Scholar 

  7. Son D, Kim E, Kim TG et al (2004) Nanoparticle iron–phosphate anode material for Li-ion battery. Appl Phys Lett 85(24):5875–5877

    Article  Google Scholar 

  8. Croce F, D’Epifanio A, Reale P et al (2003) Ruthenium oxide-added quartz iron phosphate as a new intercalation electrode in rechargeable lithium cells. J Electrochem Soc 150(5):A576–A581

    Article  Google Scholar 

  9. Xie HM, Wang RS, Ying JR et al (2006) Optimized LiFePO4–polyacene cathode material for lithium-ion batteries. Adv Mater 18(19):2609–2613

    Article  Google Scholar 

  10. Oh SW, Myung ST, Oh SM et al (2010) Polyvinylpyrrolidone-assisted synthesis of microscale C–LiFePO4 with high tap density as positive electrode materials for lithium batteries. Electrochim Acta 55(3):1193–1199

    Article  Google Scholar 

  11. Liu QB, Liao SJ, Song HY et al (2012) LiFePO4/C microspheres with nano-micro structure, prepared by spray drying method assisted with PVA as template. Curr Nanosci 8(2):208–214

    Article  Google Scholar 

  12. Yuan LX, Wang ZH, Zhang WX et al (2011) Goodenough development and challenges of LiFePO4 cathode material for lithium-ion batteries. Energy Environ Sci 4(2):269–284

    Article  Google Scholar 

  13. Tang XC, Li LX, Lai QL et al (2009) Investigation on diffusion behavior of Li+ in LiFePO4 by capacity intermittent titration technique (CITT). Electrochim Acta 54(8):2329–2334

    Article  Google Scholar 

  14. Gao F, Tang ZY, Xue JJ (2007) Preparation and characterization of nano-particle LiFePO4 and LiFePO4/C by spray-drying and post-annealing method. Electrochim Acta 53(4):1939–1944

    Article  Google Scholar 

  15. Yu DH, Qian JS, Xue NH et al (2007) Mesoporous nanotubes of iron phosphate: synthesis, characterization, and catalytic property. Langmuir 23(2):382–386

    Article  Google Scholar 

  16. Wang Y, Wang XX, Su Z et al (2004) SBA-15-supported iron phosphate catalyst for partial oxidation of methane to formaldehyde. Catal Today 93–95:155–161

    Article  Google Scholar 

  17. Yu F, Zhang JJ, Yang YF et al (2010) Porous micro-spherical aggregates of LiFePO4/C nanocomposites: a novel and simple template-free concept and synthesis via sol–gel-spray drying method. J Power Sources 195(19):6873–6878

    Article  Google Scholar 

  18. Yu F, Zhang JJ, Yang YF et al (2009) Preparation and characterization of mesoporous LiFePO4/C microsphere by spray-drying assisted template method. J Power Sources 189(1):794–797

    Article  Google Scholar 

  19. Nie YH, Carey JR, Chen JS (2009) Physical and electrochemical properties of LiFePO4/C composite cathode prepared from various polymer-containing precursors. J Power Sources 193(2):822–827

    Article  Google Scholar 

  20. Mal NK, Bhaumik A, Matsukata M et al (2006) Syntheses of mesoporous hybridironoxophenyl phosphate, iron oxophosphate, and sulfonated oxophenyly phosphate. Ind Eng Chem Res 45(23):7748–7751

    Article  Google Scholar 

  21. Kandori K, Kuwae T, Ishikawa T (2006) Control on size and adsorptive properties of spherical ferric phosphate particles. J Colloid Interface Sci 300(1):225–231

    Article  Google Scholar 

  22. Wang M, Xue YH, Zhang KL et al (2011) Synthesis of FePO4·2H2O nanoplates and their usage for fabricating superior high-rate performance LiFePO4. Electrochim Acta 56(11):4294–4298

    Article  Google Scholar 

  23. Ying JR, Lei M, Jiang CY et al (2006) Preparation and characterization of high-density spherical Li0.97Cr0.01FePO4/C cathode material for lithium ion batteries. J Power Sources 158(1):543–549

    Article  Google Scholar 

  24. Zhu YM, Tang SZ, Shi HH et al (2014) Synthesis of FePO4·xH2O for fabricating submicrometer structured LiFePO4/C by a co-precipitation method. Ceram Int 40(2):2685–2690

    Article  Google Scholar 

  25. Chen ZY, Zhu HL, Zhu W et al (2010) Electrochemical performance of carbon nanotube-modified LiFePO4 cathodes for Li-ion batteries. Trans Nonferr Met Soc China 20(4):614–618

    Article  Google Scholar 

  26. Zhao B, Jiang Y, Zhang HJ et al (2009) Morphology and electrical properties of carbon coated LiFePO4 cathode materials. J Power Sources 189(1):462–466

    Article  Google Scholar 

  27. Scaccia S, Carewska M, Prosini PP (2004) Thermoanalytical study of iron(III) phosphate obtained by homogeneous precipitation from different media. Thermochim Acta 413(1–2):81–86

    Article  Google Scholar 

  28. Wilhelmy RB, Matijević E (1987) Preparation and growth kinetics of monodispersed ferric phosphate hydrosols. Colloids Surf 22(2):97–110

    Article  Google Scholar 

  29. Stanislav K, Ladislav S (1985) Handbook of chemical equilibria in analytical chemistry. Ellis Horwood Limited, Chichester

    Google Scholar 

  30. Gu YJ, Liu P, Chen YB et al (2013) Influence of pH on electrochemical performances of iron phosphate (FePO4·xH2O) particles and LiFePO4/C composites. Adv Mater Res 643:100–103

    Article  Google Scholar 

  31. Delacourt C, Wurm C, Reale P et al (2004) Low temperature preparation of optimized phosphates for Li-battery applications. Solid State Ion 173(1–4):113–118

    Article  Google Scholar 

  32. Nielsen A (1964) Kinetics of precipitation. Pergamon Press, New York

    Google Scholar 

Download references

Acknowledgements

The authors would like to thank all members of TPXIIST Lab for their support and guidance on the characterization of powders.

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Correspondence to Leping Dang.

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Dang, L., Zhang, H., Xu, X. et al. Preparation of Spherical FePO4 by Chemical Co-precipitation Combined with Spray-Drying. Trans. Tianjin Univ. 26, 57–66 (2020). https://doi.org/10.1007/s12209-019-00196-w

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  • DOI: https://doi.org/10.1007/s12209-019-00196-w

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