类球形低硫磷酸铁的制备技术研究
收稿日期: 2019-11-11
网络出版日期: 2020-05-21
基金资助
中低品位磷矿及其共伴生资源高效利用国家重点实验室开放基金课题(WFKF2017-02)
Study of the method for the preparation of spherical-like and low sulfur FePO4
Received date: 2019-11-11
Online published: 2020-05-21
磷酸铁(FePO4)是锂电池正极材料磷酸铁锂(LiFePO4)的核心前驱体,FePO4形貌及硫含量对合成的LiFePO4材料性能有重要影响。为得到类球形低硫FePO4产品,在传统液相沉淀法技术基础上做了改进优化,添加十六烷基三甲基溴化铵(CTAB)作为形貌助剂提高产品球形度,添加氨水作为配体形成磷酸铁铵配合物改善结晶过程,降低产品硫含量。结果表明:所制备的FePO4产品硫质量分数低,达到2.6×10 -5,形貌为均一的微米类球形颗粒,D50=11.4 μm,振实密度达到1.22 g/cm 3,有望成为制备高压实密度LiFePO4材料的核心前驱体。
郭举 , 贾双珠 . 类球形低硫磷酸铁的制备技术研究[J]. 无机盐工业, 2020 , 52(5) : 31 -34 . DOI: 10.11962/1006-4990.2019-0367
FePO4 is the core precursor of LiFePO4.The morphology and sulfur content of FePO4 products have important ef-fects on the properties of the synthesized LiFePO4 materials.To obtain spherical-like and low-sulfur FePO4 products,the tradi-tional liquid phase precipitation method was improved and optimized.Adding CTAB as a morphology additive to improve the sphericity of the products,and adding ammonia water as a ligand to form the ammonium ferric phosphate complex in order to improve the crystallization process and reduce the sulfur content of the product.The results showed that the prepared FePO4 products have low sulfur content of up to 2.6×10 -5 and were homogeneous micro-spherical-like particles with D50=11.4 μm and tap density of 1.22 g/cm 3 that are expected to be the core precursors for the preparation of high compacted deasity LiFePO4 materials.
Key words: cathode material; low sulfur; iron phosphate; LiFePO4
[1] | Xia Y, Zhang W K, Huang H , et al. Selfassembled mesoporous LiPO4 with hierarchical spindlelike architectures for highperformance lithiumion batteries[J]. Journal of Power Sources, 2011,196:5651-5658. |
[2] | Kim D Y, Ju S H, Kang Y C . Finesized LiCoO2 particles prepared by spraypyrolysis from polymeric precursor solution[J]. Materials Research Bulletin, 2007,42:362-370. |
[3] | Zhang L Q, Noguchi H, Li D C , et al. Synjournal and electrochemistry of cubic rocksalt Li-Ni-Ti-O compounds in the phase diagram of LiNO2-LiTiO2-Li[Li1/3Ti2/3]O2[J]. Journal of Power Sources, 2008,185:534-541. |
[4] | Ravet N, Chouinard Y, Magnan J F , et al. Electroaetivity of Nature and synthetic tripbyl Re[J]. Power Sources, 2001,97/98:503-507. |
[5] | 苗萌, 马冬梅, 贺狄龙 . 磷酸铁锂动力电池失效的研究进展[J]. 电源技术, 2016,40(2):458-460. |
[6] | Massarotti V, Capsoni D, Bini M . Nanosized from mechanically ac-tivated solid-state synjournal[J]. Journal of Solid State Chemistry, 2006,179(2):590-596. |
[7] | Wang Y G, Wang Y R, Hosono E J , et al. The design of a LiFePO4/carbon nanocomposite with a core-shell structure and its synjournal by an in situpolymerization restriction method[J]. Angewandte Chemie International Edition, 2008,47(39):7461-7465. |
[8] | Palomares V, Larramendi I R, Alonso J , et al. LiFePO4 thin films grown by pulsed laser deposition:Effect of the substrate on the film structure and morphology[J]. Appilied Surface Science, 2010,256(8):2563-2568. |
[9] | 应皆荣, 高剑, 姜长印 , 等. 控制结晶法制备球形锂离子电池正极材料的研究进展[J]. 无机材料学报, 2006,21(2):291-297. |
[10] | 韩翀, 沈湘黔, 周建新 . LiFePO4/Ni复合微球的制备[J]. 硅酸盐学报, 2008,36(4):559-564. |
[11] | Lou X M, Zhang Y X . Synjournal of LiFePO4/C cathode materials with bothhighrate capability and high tap density for lithiumion batteries[J]. J Mater. Chem., 2011,21:4156-4160. |
[12] | 时喜喜, 郭春雨, 易炜 , 等. 关于提高LiFePO4振实密度的研究进展[J]. 电源技术, 2010,48(3):848-851. |
[13] | 雷敏, 应皆荣, 姜长印 , 等. 高密度球形LiFePO4的合成及其性能[J]. 电源技术, 2006,30(1):11-13. |
[14] | Liang Y C, Wen K C, Mao Y W , et al. Shape and size control of LiFePO4 for high-performance lithium-ion batteries[J]. Chem.Elec-trol.Chem., 2015,2(9):1227-1237. |
[15] | Zhao J, He J, Zhou J , et al. Facile synjournal for LiFePO4 nanospheres in tridimensional porous carbon framework for lithium ion batteries[J]. The Journal of Physical Chemistry C, 2011,115(6):2888-2894. |
[16] | Omenya F, Chernova N A, Zhang R , et al. Why substitution enhances the reactivity of LiFePO4[J]. Chemistry of Materials, 2012,25(1):85-89. |
[17] | Oh S W, Myung S T, Oh S M , et al. Double carbon coating of LiFePO4 as high rate electrode for rechargeable lithium batteries[J]. Advanced Materials, 2010,22(43):4842-4845. |
[18] | Fey G T K, Chen Y G, Kao H M . Electrochemical properties of LiFePO4 prepared via ball-milling[J]. Journal of Power Sources, 2009,189(1):169-178. |
[19] | 骆艳华, 何楠, 佘世杰 , 等. 硫含量对LiFePO4电化学性能的影响[J]. 现代化工, 2015,35(7):82-85. |
[20] | 雷敏, 应皆荣, 姜长印 , 等. 高密度球形LiFePO4的合成及其性能[J]. 电源技术, 2006,30(1):11-13. |
[21] | Oh S W, Myung S T, Oh S M , et al. Polyvinylpyrrolidone assisted synjournal of microscale C-LiFePO4 with high tap density as positive electrode materials for lithium batteries[J]. Electrochim Acta, 2010,55:1193-1199. |
/
〈 |
|
〉 |