电纺FeMnO3纳米纤维毛毡的制备及电化学性能研究

doi:10.15541/jim20180409

无机材料学报 ›› 2019, Vol. 34 ›› Issue (7): 709-714.DOI: 10.15541/jim20180409

电纺FeMnO₃纳米纤维毛毡的制备及电化学性能研究

孙晓璐¹,宋肖飞¹,刘艳华¹,吴越¹,蔡以兵^1,²(),赵宏梅²

^1. 江南大学生态纺织教育部重点实验室, 无锡 214122
^2. 仪征盛大纺织新材料有限公司, 仪征 225002

收稿日期:2018-09-06 修回日期:2018-11-25 出版日期:2019-07-20 网络出版日期:2019-06-26
作者简介:孙晓璐(1995-), 女, 硕士研究生. E-mail:xiaoluS0611@163.com
基金资助:
中央高校基本科研业务费专项资金(JUSRP51621A);江苏高校"青蓝工程"优秀青年骨干教师培养对象资助项目苏教师(【2016】15号);江苏省"双创计划"科技副总项目(FZ20180843);江南大学大学生创新训练计划项目(2018224Y)

Electrospun FeMnO₃ Nanofibrous Mats: Preparation and Electrochemical Property

SUN Xiao-Lu¹,SONG Xiao-Fei¹,LIU Yan-Hua¹,WU Yue¹,CAI Yi-Bing^1,²(),ZHAO Hong-Mei²

^1. Key Laboratory of Eco-Textiles, Ministry of Education, Jiangnan University, Wuxi 214122, China
^2. Yizheng Shengda Textile Material Co., Ltd, Yizheng 225002, China

Received:2018-09-06 Revised:2018-11-25 Published:2019-07-20 Online:2019-06-26
Supported by:
Fundamental Research Funds for Central Universities(JUSRP51621A);Vice President of Science and Technology of Jiangsu Province Double Plan(【2016】15号);Jiangsu Universities "Qing Lan"Project(FZ20180843);Undergraduate Innovation and Training Program of Jiangnan University(2018224Y)

摘要/Abstract

摘要：

本研究以聚乙烯吡咯烷酮(PVP)、九水硝酸铁和四水合醋酸锰为原料, 无水乙醇和N,N-二甲基甲酰胺为溶剂, 配置了均一稳定的前驱体纺丝液, 利用静电纺丝技术制备了PVP/Mn(COOH)₂/Fe(NO₃)₃复合纳米纤维, 高温煅烧后得到了锰酸铁(FeMnO₃)纳米纤维毛毡, 用其作为锂电池负极材料。利用红外光谱(FT-IR)、X射线衍射(XRD)、扫描电镜(SEM)和BET比表面积分析仪等研究样品的表观形貌与晶型结构。结果表明: 煅烧后制得的FeMnO₃纳米纤维毛毡具有良好的形貌结构, 比表面积为9.9 m2/g, 当温度达到470 ℃后, 曲线变得平缓, 热重损失不明显。充放电、循环伏安以及循环性能测试结果表明, FeMnO₃纳米纤维毛毡具有良好的电化学性能及电稳定性, 首次充电比容量为1264 mAh/g, 在50 mA/g电流密度下经过37次循环后其比容量仍保持在533 mAh/g; 在循环50次后, 阻抗约为170 Ω, 基本保持不变。

关键词: 静电纺丝, FeMnO₃纳米纤维毛毡, 锂电池, 电化学性能

Abstract:

A uniform and stable precursor spinning solution was prepared by using polyvinylpyrrolidone (PVP), ferric nitrate nonahydrate and manganese acetate tetrahydrate as raw materials, anhydrous ethanol and N,N-dimethylformamide as solvent, followed by magnetically stirred. The PVP/Mn(COOH)₂/Fe(NO₃)₃ composite nanofibers were prepared by electrospinning technology. FeMnO₃ nanofibrous mats were obtained after high temperature calcination, which was used as anode material for lithium battery. Apparent morphology and crystal structure of the samples were investigated by FT-IR, XRD, SEM, and BET specific surface area analyzers. All results showed that the fabricated FeMnO₃ nanofibrous mats possessed good structural morphology with the specific surface area of 9.9 m ²/g. TG analysis showed that when temperature reaches 470 ℃, the TG curve becomes gentle while the mass loss is not obvious. Results form charge and discharge, cyclic voltammetry, and cycle performance tests, indicated that FeMnO₃ nanofibrous mats had good electrochemical performance and electrical stability, with a specific capacity of 533 mAh/g at 50 mA/g after 37 cycles. After 50 cycles, the impedance is approximately 170 Ω, which remains essentially unchanged.

Key words: electrospinning, FeMnO₃ nanofibrous mats, lithium battery, electrochemical performance

中图分类号:

TQ340

孙晓璐,宋肖飞,刘艳华,吴越,蔡以兵,赵宏梅. 电纺FeMnO₃纳米纤维毛毡的制备及电化学性能研究[J]. 无机材料学报, 2019, 34(7): 709-714.

SUN Xiao-Lu,SONG Xiao-Fei,LIU Yan-Hua,WU Yue,CAI Yi-Bing,ZHAO Hong-Mei. Electrospun FeMnO₃ Nanofibrous Mats: Preparation and Electrochemical Property[J]. Journal of Inorganic Materials, 2019, 34(7): 709-714.

图/表 8

图1 PVP/Mn(COOH)2/Fe(NO3)3复合纳米纤维的TG和DTG曲线

Fig. 1 TG and DTG curves of PVP/Mn(COOH)2/Fe(NO3)3 composite nanofibers

图2 样品煅烧前(a)后(b)的红外光谱图

Fig. 2 Infrared spectra of samples before and after calcination (a) PVP/Mn(COOH)2/Fe(NO3)3 composite nanofibers; (b) FeMnO3 nanofibrous mats

图3 FeMnO3纳米纤维毛毡的XRD图谱

Fig. 3 XRD pattern of FeMnO3 nanofibrous mats

图4 (a) PVP/Mn(COOH)2/Fe(NO3)3复合纳米纤维的SEM照片; 煅烧后FeMnO3纳米纤维毛毡SEM(b)和TEM(c)照片

Fig. 4 (a) SEM image of PVP/Mn(COOH)2/Fe(NO3)3 composite nanofibers, and (b) SEM and (c) TEM images of FeMnO3 nanofibrous mats after calcination

图5 FeMnO3纳米纤维毛毡的N2等温吸附-脱附曲线

Fig. 5 N2 adsorption-desorption isotherm of FeMnO3 nanofibrous mats

图6 FeMnO3纳米纤维毛毡的循环伏安曲线

Fig. 6 Cyclic voltammograms of FeMnO3 nanofibrous mats

图7 FeMnO3纳米纤维毛毡的(a)充放电曲线和(b)循环性能曲线

Fig. 7 (a) Charge-discharge and (b) cycle performance curves of FeMnO3 nanofibrous mats

图8 FeMnO3纳米纤维毛毡的交流阻抗图谱

Fig. 8 AC impedance diagram of FeMnO3 nanofibrous mats

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电纺FeMnO₃纳米纤维毛毡的制备及电化学性能研究

Electrospun FeMnO₃ Nanofibrous Mats: Preparation and Electrochemical Property

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