十六烷基膦酸表面修饰纳米镍粉及其复合材料的制备和性能

doi:10.7503/cjcu20130631

摘要/Abstract

摘要：

以十六烷基膦酸作为修饰剂, 对纳米镍粉进行表面改性处理, 通过溶液共混的方法制备改性镍粉与聚丙烯的聚合物基复合材料. 利用X射线光电子能谱(XPS)、 X射线衍射(XRD)及透射电子显微镜(TEM)等测试手段研究改性镍粉的表面形态; 利用扫描电子显微镜(SEM)研究复合材料断面形貌; 利用介电频谱分析系统对复合材料的介电常数和介电损耗等进行了测试. 结果表明, 纳米镍粉表面形成厚度为2~4 nm的十六烷基膦酸包覆层, 使纳米镍粉由亲水性变为亲油性; 聚丙烯基复合材料中, 改性镍粉均匀分散; 复合材料的介电常数在镍填充量为40%时, 可以达到纯聚丙烯的近10倍.

关键词: 纳米镍, 十六烷基膦酸, 表面修饰, 聚合物基复合材料

Abstract:

Through the modification of nano-Ni particles with n-hexadecylphosphonic acid(HDPA) as surface modifier, Ni/HDPA hybrid particles were prepared. Composite of polypropylene(PP) and Ni/HDPA was prepared by solution blending. The dispersion of Ni in PP, the compatibility and stability of Ni and PP, the dielectric performance of composite were discussed. The X-ray photoelectron spectroscopy(XPS), X-ray diffraction(XRD) and transmission electron microscope(TEM) results showed the surface morphology of Ni/HDPA, while the fracture surface morphology and the dielectric properties of composite were demonstrated by scanning electron microscope(SEM) and the dielectric spectrum analysis system. It is found that a coverage layer, which is 2—4 nm thick, of n-hexadecylphosphonic can be formed on the surface of nano-Ni. In the presence of the coverage layer, nano-Ni was changed from hydrophilicity into lipophilicity, in results of which the Ni/HDPA disperses well in the PP matrix. At the Ni/HDPA volume fraction of 40%, permittivity of composite can be as high as 10 times of pure PP.

Key words: Nano-Ni, n-Hexadecylphosphonic acid, Surface modification, Polymer matrix composite

中图分类号:

TrendMD:

尚光远, 李明. 十六烷基膦酸表面修饰纳米镍粉及其复合材料的制备和性能. 高等学校化学学报, 2014, 35(2): 427.

SHANG Guangyuan, LI Ming. Preparation and Properties of Surface Modified Nano-Ni Particles with n-Hexadecylphosphonic and Its Composites. Chem. J. Chinese Universities, 2014, 35(2): 427.

图/表 12

Fig.1 XPS spectra of Ni(a) and Ni/HDPA(b—d) m(Ni)∶m(HDPA): b. 1∶0.024; c. 1∶0.072; d. 1∶0.24.

Fig.2 Ni2p XPS spectra of Ni(a) and Ni/HDPA(b—d)m(Ni)∶m(HDPA): b. 1∶0.024; c. 1∶0.072;d. 1∶0.24.

Fig.3 Ni2p XPS spectra of Ni/HDPA [m(Ni)∶m(HDPA)=1∶0.24](a) and nickel hexadecylphosphates(b)

Fig.4 XRD patterns of Ni(a) and Ni/HDPA[m(Ni)∶m(HDPA)=1∶0.24](b)

Fig.5 XRD patterns of nickel hexadecylphosphates(a) and Ni/HDPA [m(Ni)∶m(HDPA)=1∶0.24](b)

Fig.6 TEM of Ni(A) and Ni/HDPA(B, C)m(Ni)∶m(HDPA): (B) 1∶0.024; (C) 1∶0.24.

Fig.7 Dispersion of Ni/HDPA(A) and Ni(B) in water and cyclohexane

Fig.8 SEM images of Ni/HDPA/PP and Ni/PP(A) 5%Ni/HDPA; (B) 10%Ni/HDPA; (C) 15%Ni/HDPA; (D) 5%Ni; (E) 10%Ni; (F) 15%Ni.

Fig.9 Relationship between permittivity(ε) of Ni/HDPA/PP composites and frequency(f)Volume fraction of Ni(%): a. 5; b. 10; c. 15; d. 20; e. 25; f. 30; g. 35; h. 40; i. 50.

Fig.10 Relationship between dielectric loss(tanδ) of Ni/HDPA/PP composites and frequency(f)Volume fraction of Ni(%): a. 5; b. 10; c. 15; d. 20; e. 25; f. 30; g. 35; h. 40; i. 50.

Fig.11 Relationship between dielectric properties(ε and tanδ) of Ni/HDPA/PP composites and Ni volume fraction

Fig.12 Relationship between DC conductivity of Ni/HDPA/PP composites and Ni volume fraction

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