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<p>Lithium iron phosphate (LiFePO<sub>4</sub>, LFP) is well-established and one of the commercially dominant cathode materials for Li-ion batteries due to its safety, stability, and low cost, but its low electronic and ionic conductivity limits performance. Reducing particle size represents an effective strategy to address this drawback and thereby improve charge-transfer kinetics and lithium-ion diffusion. Spray drying offers a scalable route to produce such fine, homogeneous particles, making it a suitable technique for LFP synthesis. In this paper, we examined the influence of two iron precursors—ferric citrate and ferric acetylacetonate. Our results indicate that ferric citrate was unsuitable for this method, likely due to phase separation that occurred during the drying process, which led to phosphorus deficiency and the formation of iron oxide/spinel impurities. In contrast, ferric acetylacetonate enabled the synthesis of phase-pure olivine LiFePO<sub>4</sub>. A&#xa0;comparative analysis with a commercial single-crystal-like reference revealed that the spray-dried material formed polycrystalline secondary agglomerates composed of sintered nanocrystallites (~ 42&#xa0;nm) with significant lattice strain. Although this nanostructure facilitated lithium diffusion, electrochemical impedance spectroscopy (EIS) confirmed that the high grain boundary density led to particle isolation and increased inter-particle resistance upon cycling. These findings demonstrate the impact of precursor chemistry and highlight the necessity of optimizing polycrystalline morphology resulting from spray drying synthesis to address the kinetic limitations associated with grain boundaries. Identification of these kinetic limitations provides the necessary groundwork for future optimization strategies aimed at achieving performance in spray-dried LFP that meets commercial standards.</p> Graphical Abstract <p></p>

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Effect of iron precursor selection on spray drying synthesis of LiFePO4 cathodes

  • 期刊论文

  • 发表日期：

    2026年6月3日

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  • Hana Hálová,
  • Lukáš Preisler,
  • Marek Kunz,
  • David Trochta,
  • Pavel Čudek,
  • Ladislav Chladil

摘要

Lithium iron phosphate (LiFePO4, LFP) is well-established and one of the commercially dominant cathode materials for Li-ion batteries due to its safety, stability, and low cost, but its low electronic and ionic conductivity limits performance. Reducing particle size represents an effective strategy to address this drawback and thereby improve charge-transfer kinetics and lithium-ion diffusion. Spray drying offers a scalable route to produce such fine, homogeneous particles, making it a suitable technique for LFP synthesis. In this paper, we examined the influence of two iron precursors—ferric citrate and ferric acetylacetonate. Our results indicate that ferric citrate was unsuitable for this method, likely due to phase separation that occurred during the drying process, which led to phosphorus deficiency and the formation of iron oxide/spinel impurities. In contrast, ferric acetylacetonate enabled the synthesis of phase-pure olivine LiFePO4. A comparative analysis with a commercial single-crystal-like reference revealed that the spray-dried material formed polycrystalline secondary agglomerates composed of sintered nanocrystallites (~ 42 nm) with significant lattice strain. Although this nanostructure facilitated lithium diffusion, electrochemical impedance spectroscopy (EIS) confirmed that the high grain boundary density led to particle isolation and increased inter-particle resistance upon cycling. These findings demonstrate the impact of precursor chemistry and highlight the necessity of optimizing polycrystalline morphology resulting from spray drying synthesis to address the kinetic limitations associated with grain boundaries. Identification of these kinetic limitations provides the necessary groundwork for future optimization strategies aimed at achieving performance in spray-dried LFP that meets commercial standards.

Graphical Abstract