Study on the mechanism of liquid-phase regulated preparation of battery-grade iron phosphate

IF 3 4区 材料科学 Q3 CHEMISTRY, PHYSICAL Solid State Ionics Pub Date : 2024-11-23 DOI:10.1016/j.ssi.2024.116740
Haijing Cui , Changjiang Yang , Yankun Wang , Zehang Qin , Jun Chang
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Abstract

LiFePO4 batteries play a crucial role in energy storage and electric vehicles, with their precursor, FePO4, directly determining the electrochemical performance of LiFePO4. The key to preparing high-quality FePO4 is the precise regulation of crystal morphology. This study investigates the inter-ionic interaction of Fe3+ in a complex phosphate system to form monoclinic FePO4 with high crystallinity by precisely controlling process parameters such as pH and reaction temperature. The optimized process parameters are as follows: during the leaching stage, a P/Fe feeding ratio of 3:1 and a reaction temperature of 90 °C; during the oxidation stage, a 140 % excess of H2O2 and a reaction temperature of 50 °C; and during the crystallization stage, a pH of 1.5 and a reaction temperature of 90 °C, with an aging time of 1 h. The resulting FePO4 has a round cake morphology with a diameter of approximately 1.5 μm and a thickness of about 0.5 μm. The particle size distribution is narrow, with a D50 of 2.64 μm. The products exhibit consistent crystalline morphology, high crystallinity, an Fe content of 36.595 %, a P content of 20.676 %, and an Fe/P ratio of 0.981. The synthesized LiFePO4/C derived from this FePO4 shows a discharge capacity of 154 mAh/g at 0.2C. The proposed preparation mechanism has significant theoretical implications for the efficient and environmentally friendly production of FePO4 in the industry.
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电池级磷酸铁的液相调控制备机理研究
磷酸铁锂电池在储能和电动汽车中发挥着至关重要的作用,其前驱体磷酸铁直接决定了磷酸铁锂电池的电化学性能。制备高质量磷酸铁锂的关键是精确调节晶体形态。本研究通过精确控制 pH 值和反应温度等工艺参数,研究了复杂磷酸盐体系中 Fe3+ 的离子间相互作用,以形成具有高结晶度的单斜 FePO4。优化的工艺参数如下:在浸出阶段,P/Fe 进料比为 3:1,反应温度为 90 °C;在氧化阶段,过量的 H2O2 为 140 %,反应温度为 50 °C;在结晶阶段,pH 为 1.5,反应温度为 90 °C,老化时间为 1 h。粒度分布较窄,D50 为 2.64 μm。产品的结晶形态一致,结晶度高,铁含量为 36.595%,磷含量为 20.676%,铁磷比为 0.981。由这种 FePO4 合成的 LiFePO4/C 在 0.2C 下的放电容量为 154 mAh/g。所提出的制备机理对于在工业中高效、环保地生产 FePO4 具有重要的理论意义。
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来源期刊
Solid State Ionics
Solid State Ionics 物理-物理:凝聚态物理
CiteScore
6.10
自引率
3.10%
发文量
152
审稿时长
58 days
期刊介绍: This interdisciplinary journal is devoted to the physics, chemistry and materials science of diffusion, mass transport, and reactivity of solids. The major part of each issue is devoted to articles on: (i) physics and chemistry of defects in solids; (ii) reactions in and on solids, e.g. intercalation, corrosion, oxidation, sintering; (iii) ion transport measurements, mechanisms and theory; (iv) solid state electrochemistry; (v) ionically-electronically mixed conducting solids. Related technological applications are also included, provided their characteristics are interpreted in terms of the basic solid state properties. Review papers and relevant symposium proceedings are welcome.
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