Inorganic Chemicals Industry >
Study on preparation of battery grade ferric phosphate by co-precipitation of ferric nitrate and phosphoric acid
Received date: 2022-09-11
Online published: 2023-07-13
By using ferric nitrate and phosphoric acid as raw materials,the co-precipitation method was used to prepare the battery grade ferric phosphate.The effects of reaction temperature,reactant concentration,feeding proportion and reaction time on the yield and particle size of ferric phosphate were studied,and the optimal process conditions were obtained through orthogonal optimization:the solution concentration of Fe(NO3)3 was 1.1 mol/L,the feed ratio of phosphoric acid to ferric nitrate was 1.1,the reaction temperature was 90 ℃,and the reaction time was 8 h.The prepared iron phosphate was characterized by scanning electron microscopy(SEM),laser particle size analyzer,X-ray diffractometer(XRD) and TG-DTA.The analysis results showed that the obtained ferrophosphate dihydrate was monoclinic crystal with high purity and secondary particle size D50 of 2.41 μm,which met the requirements of battery grade ferrophosphate.The performance of LiFePO4/C prepared by the precursor system of iron phosphate was good.The initial discharge specific capacity of the battery composed of iron phosphate as cathode materials were 143.9,136.8 and 131.4 mA·h/g at 0.05C,0.1C and 1C,respectively.
WANG Zihan , LI Jun , CHEN Ming , ZHOU Qingyu . Study on preparation of battery grade ferric phosphate by co-precipitation of ferric nitrate and phosphoric acid[J]. Inorganic Chemicals Industry, 2023 , 55(7) : 51 -57 . DOI: 10.19964/j.issn.1006-4990.2022-0548
| 1 | 张克杰,陈鹏,谢旺旺,等.磷酸铁锂优缺点及改性研究进展[J].无机盐工业,2018,50(6):13-17. |
| ZHANG Kejie, CHEN Peng, XIE Wangwang,et al.Progress in modification of lithium iron phosphate and its advantages and disadvantages[J].Inorganic Chemicals Industry,2018,50(6):13-17. | |
| 2 | 梁广川.锂离子电池用磷酸铁锂正极材料[M].北京:科学出版社,2013:288-292. |
| 3 | 张婷,林森,于建国.磷酸铁锂正极材料的制备及性能强化研究进展[J].无机盐工业,2021,53(6):31-40. |
| ZHANG Ting, LIN Sen, YU Jianguo.Research progress in synthesis and performance enhancement of LiFePO4 cathode materials[J].Inorganic Chemicals Industry,2021,53(6):31-40. | |
| 4 | 刘贡钢,叶红齐,刘辉,等.前驱体磷酸铁的制备及其对磷酸 |
| 铁锂电化学性能的影响[J].应用化工,2013,42(2):225- 228. | |
| LIU Gonggang, YE Hongqi, LIU Hui,et al.Preparation of precursor FePO4 and its effects on electrochemical properties of LiFePO4 [J].Applied Chemical Industry,2013,42(2):225-228. | |
| 5 | 袁静楠.不同晶型磷酸铁的制备及与磷酸亚铁锂间的相互转换关系[D].郑州:郑州大学,2012. |
| YUAN Jingnan.Preparation of different crystal forms of iron phosphate and their conversion relationship with lithium ferrous phosphate[D].Zhengzhou:Zhengzhou University,2012. | |
| 6 | 姚停,徐婷,宋磊,等.磷酸铁形貌对磷酸铁锂倍率性能的影响[J].电池,2020,50(1):54-57. |
| YAO Ting, XU Ting, SONG Lei,et al.Effects of morphology of ferric phosphate on rate capability of lithium iron phosphate[J].Battery Bimonthly,2020,50(1):54-57. | |
| 7 | 吴康,李军,陈明.乙醇-水体系3D纳/微米球形磷酸铁的制备与表征[J].无机盐工业,2020,52(6):41-45. |
| WU Kang, LI Jun, CHEN Ming.Synthesis and characterization of 3D nano/micro spherical iron phosphate in ethanol-water system[J].Inorganic Chemicals Industry,2020,52(6):41-45. | |
| 8 | 马志鸣,肖仁贵,廖霞,等.片层纳米结构磷酸铁制备及对磷酸铁锂电性能的影响[J].材料导报,2018,32(19):3325-3331. |
| MA Zhiming, XIAO Rengui, LIAO Xia,et al.Preparation of the lameller nanostructure iron phosphate and its effect on the electrochemical performance of lithium iron phosphate[J].Materials Review,2018,32(19):3325-3331. | |
| 9 | 赵曼.水热法以磷铁制备电池级磷酸铁及改性研究[D].贵阳:贵州大学,2017. |
| ZHAO Man.Preparation of battery-grade iron phosphate from ferrophosphorus by hydrothermal method and its modification[D].Guiyang:Guizhou University,2017. | |
| 10 | 严鹏,谢刚,张春明,等.非晶态磷酸铁的沉淀反应机理及性能[J].电池,2015,45(5):241-243. |
| YAN Peng, XIE Gang, ZHANG Chunming,et al.Precipitation reaction mechanism and performance of amorphous ferric phosphate[J].Battery Bimonthly,2015,45(5):241-243. | |
| 11 | 张震,蒲薇华,任建国,等.控制结晶法制备球形磷酸铁的团聚尺寸模型[J].化学工程,2011,39(8):20-24. |
| ZHANG Zhen, PU Weihua, REN Jianguo,et al.Agglomeration-size model of ferric phosphate spherical particle prepared by controlled crystallization[J].Chemical Engineering(China),2011,39(8):20-24. | |
| 12 | 李永佳,魏润宏,鲁劲华,等.电池级磷酸铁的制备及性能[J].化工进展,2021,40(4):2227-2233. |
| LI Yongjia, WEI Runhong, LU Jinhua,et al.Preparation and performance of FePO4 precursor for LiFePO4 [J].Chemical Industry and Engineering Progress,2021,40(4):2227-2233. | |
| 13 | 郑典模,潘鹤政,伍丽萍,等.超细磷酸铁的制备及其电化学性能研究[J].电源技术,2015,39(1):58-61. |
| ZHENG Dianmo, PAN Hezheng, WU Liping,et al.Study on preparation and electrochemical of ultrafine FePO4 [J].Chinese Journal of Power Sources,2015,39(1):58-61. | |
| 14 | 李文升,樊勇利,童书辉,等.高振密球形FePO4·xH2O的合成研究[J].电源技术,2013,37(6):950-952. |
| LI Wensheng, FAN Yongli, TONG Shuhui,et al.Synthesis research on iron phosphate with spherical structure and high tap density[J].Chinese Journal of Power Sources,2013,37(6):950-952. | |
| 15 | ZHANG Tongbao, XIN Dawei, LU Yangcheng,et al.Direct precipitation for a continuous synthesis of nanoiron phosphate with high purity[J].Industrial & Engineering Chemistry Research,2014,53(16):6723-6729. |
/
| 〈 |
|
〉 |