配位-氧化聚合-水热法制备聚苯胺/CoFe2O4纳米复合物及其微波吸收性能

doi:10.7503/cjcu20130804

高等学校化学学报 ›› 2014, Vol. 35 ›› Issue (2): 402.doi: 10.7503/cjcu20130804

配位-氧化聚合-水热法制备聚苯胺/CoFe₂O₄纳米复合物及其微波吸收性能

蒋军军, 杨春明(), 王洪波, 刘小华, 李龙浩

湖南师范大学化学化工学院, 长沙 410081

收稿日期:2013-08-15 出版日期:2014-02-10 发布日期:2013-12-26
作者简介:联系人简介: 杨春明, 男, 博士, 教授, 主要从事导电聚合物及其复合物的研究与应用. E-mail:chunmingyang@126.com
基金资助:
湖南省科技计划重点项目(批准号: 2011GK2014)和湖南省自然科学基金(批准号: 06JJ4007)资助

Preparation and Microwave Absorption Performance of Polyaniline/CoFe₂O₄ Nano-composite by Coordination-oxidative Polymerization-hydrothermal Method^†

JIANG Junjun, YANG Chunming^*(), WANG Hongbo, LIU Xiaohua, LI Longhao

College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081, China

Received:2013-08-15 Online:2014-02-10 Published:2013-12-26
Contact: YANG Chunming E-mail:chunmingyang@126.com
Supported by:
† Supported by the Key Scientific Research Fund of Hunan Provincial Science and Technology Department, China(No.2011GK2014) and the Natural Science Foundation of Hunan Provincie, China(No.06JJ4007)

摘要/Abstract

摘要：

采用“配位-氧化聚合-水热法”制备了本征态聚苯胺/CoFe₂O₄二元纳米复合物, 再以磺基水杨酸掺杂获得聚苯胺/CoFe₂O₄电磁复合物. 考察了反应物配比及掺杂酸浓度对产物电磁性能的影响. 通过透射电子显微镜(TEM)、 X射线衍射(XRD)、红外光谱(FTIR)及电磁测量等手段对聚苯胺/CoFe₂O₄的形貌、结构及性能进行了表征. 结果表明, 复合物呈现多级结构, 其中CoFe₂O₄为立方体状, 平均粒径小于20 nm. 当CoFe₂O₄的质量分数为8.86%时, 复合物的电导率约为0.43 S/cm; 当聚苯胺/CoFe₂O₄复合物厚度为2 mm时, 在16.01 GHz处最大反射损耗为-16.71 dB, 小于-10 dB的带宽达4.68 GHz; 而当聚苯胺/CoFe₂O₄复合物厚度为3.2 mm时, 在9.23 GHz处最大反射损耗达-51.81 dB, 小于-10 dB的带宽为3.69 GHz, 表明具有良好的吸波性能.

关键词: 配位-氧化聚合-水热法, 聚苯胺/CoFe2O4纳米复合物, 微波吸收, 反射损耗

Abstract:

Polyaniline/CoFe₂O₄ binary nano-composites were prepared by coordination-oxidative polymerization-hydrothermal method, and doped by sulfosalicylic acid. The influence of reactants ratio and concentration of doping acid on electromagnetic properties of resulting composites was investigated. The micrographs, structure and electromagnetic properties of polyaniline/CoFe₂O₄ composites were characterized by TEM, XRD, FTIR and electromagnetic measurements. The results indicate that the prepared composite show a multi-level structure in which CoFe₂O₄ is cube-shaped with an average particle size less than 20 nm. The optimal experimental results were as follows: the conductivity of the composite is about 0.43 S/cm when the content of CoFe₂O₄ in composite is 8.86%(mass fraction). When the thickness of PAn/CoFe₂O₄ composite is at 2 mm, a maximum reflection loss of -16.71 dB at 16.01 GHz is observed with a bandwidth of 4.68 GHz above -10 dB loss; and when the thickness of PAn/CoFe₂O₄ composite is at 3.2 mm, a maximum reflection loss of -51.81 dB at 9.23 GHz is observed with a bandwidth of 3.69 GHz above -10 dB loss. The nanocomposite exhibits excellent microwave absorbing capacity.

Key words: Coordination-oxidative polymerization-hydrothermal method, Polyaniline/CoFe2O4 nanocompo-site, Microwave absorption, Reflection loss

中图分类号:

TrendMD:

蒋军军, 杨春明, 王洪波, 刘小华, 李龙浩. 配位-氧化聚合-水热法制备聚苯胺/CoFe₂O₄纳米复合物及其微波吸收性能. 高等学校化学学报, 2014, 35(2): 402.

JIANG Junjun, YANG Chunming, WANG Hongbo, LIU Xiaohua, LI Longhao. Preparation and Microwave Absorption Performance of Polyaniline/CoFe₂O₄ Nano-composite by Coordination-oxidative Polymerization-hydrothermal Method^†. Chem. J. Chinese Universities, 2014, 35(2): 402.

图/表 10

Scheme 1 Preparation of PAn/CoFe2O4 nano-composite by coordination-oxidative polymerization-hydrothermal method

Table 1 Electrical conductivity of PAn/CoFe2O4 prepared under different amounts of aniline

Amount of aniline/mL	m(CoFe₂O₄)(%)	10² σ/(S·cm^-1)	Amount of aniline/mL	m(CoFe₂O₄)(%)	10² σ/(S·cm^-1)
0.5	20.92	2.07	2.0	8.86	6.21
1.0	14.00	8.20	2.5	8.28	2.93
1.5	12.34	1.32

Fig.1 Electrical conductivity(σ) of PAn/CoFe2O4 doped by different concentrations of SSA

Fig.2 SEM images of samples before(A) and after(B) hydrothermal reaction and TEM image of sample after removal of PAn(C)

Fig.3 XRD patterns of PAn(a) and PAn/CoFe2O4(b)

Fig.4 FTIR spectra of CoFe2O4(a), PAn/CoFe2O4(b) and doped PAn/CoFe2O4(c)

Fig.5 Dielectric loss tangent(tanδE)(A) and magnetic loss tangent(tanδM)(B) for PAn/CoFe2O4 vs. frequencyσ/(S·cm-1): a. 10-4; b. 10-3; c. 10-2; d. 10-1.

Table 2 Reflection loss values of PAn/CoFe2O4 prepared under different amount of aniline

Amount of aniline/mL	10² σ/(S·cm^-1)	R_min/dB	Amount of aniline/mL	10² σ/(S·cm^-1)	R_min/dB
0.5	2.07	-5.43	2.0	6.21	-11.15
1.0	8.20	-6.56	2.5	2.93	-8.91
1.5	1.32	-6.96

Fig.6 Frequency dependence of the reflection loss of PAn/CoFe2O4 with layers of different sample thickness

Fig.7 Reflection loss curves of PAn/CoFe2O4 prepared under different conductivity magnitudeσ/(S·cm-1): a. 10-4; b. 10-3; c. 10-2; d. 10-1.

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配位-氧化聚合-水热法制备聚苯胺/CoFe₂O₄纳米复合物及其微波吸收性能

Preparation and Microwave Absorption Performance of Polyaniline/CoFe₂O₄ Nano-composite by Coordination-oxidative Polymerization-hydrothermal Method^†

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