Physical and electrochemical properties of LiFePO4 nanoparticles synthesized by a combination of spray pyrolysis with wet ball-milling

Physical and electrochemical properties of LiFePO4 nanoparticles synthesized by a combination of spray pyrolysis with wet ball-milling
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DOI:
10.1016/j.jpowsour.2009.06.046
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发表时间:
2009-12
影响因子:
9.2
通讯作者:
Muxina Konarova;I. Taniguchi
Muxina Konarova;I. Taniguchi
中科院分区:
工程技术2区
文献类型:
--
作者:
Muxina Konarova;I. Taniguchi

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采用喷雾热解法(SP)和湿法球磨(WBM)相结合的方法制备了LiFePO 4纳米粒子。利用该技术,研究了球磨时间、烧结温度等工艺参数对LiFePO 4纳米颗粒的制备影响。通过X射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)、透射电子显微镜(TEM)、BET法、拉曼光谱和电化学测试等手段,研究了工艺参数对LiFePO 4物理性能和电化学性能的影响|1 M LiClO 4溶于EC:DEC=1:1|磷酸铁锂在Ar气氛中,转速为800 rpm,球磨时间为12 h,然后在N2+ 3%H2气氛中,于500°C热处理4 h,制备出几何平均粒径为58 nm的LiFePO 4纳米颗粒。在0.1和10 C的充放电速率下,样品的首次放电容量分别为164和100 mAhg − 1。在较高的充放电倍率下,Fe 2 P、Fe 3 P和α-Fe 2 O3的生成对LiFePO 4纳米粒子的电化学性能有很大影响。
A novel preparation technique was developed to synthesize LiFePO4nanoparticles through a combination of spray pyrolysis (SP) with wet ball-milling (WBM). Using this technique, the preparation of LiFePO4nanoparticles was investigated for a wide range of process parameters such as ball-milling time and sintering temperature. The effect of process parameters on the physical and electrochemical properties of LiFePO4was then discussed through analysis using by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), the Brunauer–Emmet–Teller (BET) method, Raman spectroscopy and using an electrochemical cell of Li|1M LiClO4in EC:DEC=1:1|LiFePO4. LiFePO4nanoparticles with a geometric mean diameter of 58nm were prepared at a rotating speed of 800rpm and a ball-milling time of 12h in an Ar atmosphere followed by heat treatment at 500°C for 4h in a N2+3% H2atmosphere. The sample delivered first discharge capacities of 164 and 100mAhg−1at charge–discharge rates of 0.1 and 10C in the test cells, respectively. The electrochemical properties of LiFePO4nanoparticles were strongly affected by the formation of Fe2P, Fe3P and α-Fe2O3at higher charge–discharge rates.