无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2012, Vol. 44 ›› Issue (9): 59-.

• 论文 • 上一篇    

超临界水快速连续制备纳米磷酸铁锂正极材料

宋续明,毛志强,赵亚平   

  1. 上海交通大学化学化工学院,上海 200240
  • 发布日期:2012-09-11

Continuous and rapid synthesis of LiFePO4 nanoparticles in supercritical water

 SONG  Xu-Ming, MAO  Zhi-Qiang, ZHAO  Ya-Ping   

  1. School of Chemistry and Chemical Engineering,Shanghai Jiao Tong University,Shanghai 200240,China
  • Published:2012-09-11

摘要: 建立了超临界水快速连续合成磷酸铁锂纳米颗粒的工艺。研究了反应物浓度、反应温度和反应压力等因素对磷酸铁锂颗粒的大小、结晶度和形貌的影响并解释了相关机理,采用扫描电镜(SEM)、动态光散射(DLS)粒度分析和X射线衍射(XRD)等手段表征了目标产物的颗粒大小、形貌和结晶度。结果表明,在所研究的过程参数范围内,均获得了纳米尺度的磷酸铁锂。在超临界范围内,提高反应温度会使颗粒尺寸变大,但粒度分布更加均匀;预热温度对磷酸铁锂的结晶度有明显的影响,升高预热温度有利于提高磷酸铁锂纳米颗粒的结晶度;较高的反应压力、较低的反应物浓度有利于得到更小的纳米颗粒。在反应温度为380 ℃、预热温度为405 ℃、反应压力为27 MPa、二价铁离子浓度为0.015 mol/L条件下,获得了平均粒度为105 nm的高结晶度、橄榄石状的球形磷酸铁锂颗粒。

关键词: 连续合成, 磷酸铁锂, 纳米颗粒, 超临界水

Abstract: A rapid and continuous method for synthesis of LiFePO4 nanoparticles in supercritical water was established.The effects of reactant concentration,temperature,and pressure etc. on size,crystallinity degree,and morphology of LiFePO4 particles were investigated and possible reasons for this behavior were also given.The crystallinity degree,size,and morphology of objective product were characterized by SEM,DLS,and XRD.Results showed,nano-sized LiFePO4 were obtained in all the researched parameter ranges.In the supercritical range,with the reaction temperature increased,the particle size became bigger,but distribution more uniform;the pre-heating temperature had a significant impact on crystallinity degree and higher pre-heating temperatures were found to be in favor of improving the crystallinity degree of LiFePO4 nanoparticles; higher pressure and lower reactant concentration could get smaller nanoparticles;and olivine-like spherical LiFePO4 nanoparticles with average size of 105 nm and high crystallinity degree were obtained under the conditions of reaction temperature of 380 ℃,pre-heating temperature of 405 ℃,reaction pressure of 27 MPa,and Fe2+ concentration of 0.015 mol/L.

Key words: continuous synthesis, LiFePO4, nanoparticle, supercritical water

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