原子转移自由基聚合法改性纳米氮化硅粉体的制备工艺及性能

doi:10.16085/j.issn.1000-6613.2017-1411

化工进展 ›› 2018, Vol. 37 ›› Issue (05): 1881-1887.DOI: 10.16085/j.issn.1000-6613.2017-1411

原子转移自由基聚合法改性纳米氮化硅粉体的制备工艺及性能

黄李晓研, 魏铭, 王钦利, 刘晓芳

武汉理工大学化学化工与生命科学学院, 湖北武汉 430070

收稿日期:2017-07-10 修回日期:2017-11-21 出版日期:2018-05-05 发布日期:2018-05-05
通讯作者: 魏铭,副教授,研究方向为涂料与涂装技术。
作者简介:黄李晓研(1992-),男,硕士研究生。
基金资助:
国家自然科学基金项目（51272191）。

Preparation and properties of nano-Si₃N₄ powder modified by ATRP

HUANG Lixiaoyan, WEI Ming, WANG Qinli, LIU Xiaofang

School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, Hubei, China

Received:2017-07-10 Revised:2017-11-21 Online:2018-05-05 Published:2018-05-05

摘要/Abstract

摘要： 采用γ氨丙基三乙氧基硅烷（KH-550）、氯乙酰氯在氮化硅（Si₃N₄）表面引入引发基团，通过原子转移自由基聚合（ATRP）方法，以甲基丙烯酸甲酯（MMA）、甲基丙烯酸缩水甘油酯（GMA）为单体，制得表面引发的丙烯酸聚合物改性的氮化硅粉体。使用傅里叶红外光谱（FTIR）、核磁共振氢谱（¹H NMR）、凝胶渗透色谱（GPC）对ATRP法改性的氮化硅粉体进行表征，确定了改性氮化硅粉体的最佳工艺条件；使用马尔文激光粒度仪、扫描电子显微镜（SEM）、接触角测定仪对改性前后氮化硅进行性能测定。结果表明：通过此方法制备出的改性氮化硅粉体具有良好的分散性，粒径较小、团聚减少，表面接枝聚合物相对分子质量分布窄、可控。

关键词: 原子转移自由基聚合, 氮化硅, 纳米粒子, 团聚, 粒度分布

Abstract: 3-Triethoxysilylpropylamine (KH-550)and chloracetyl chloride were utilized to introduce the initiator on the surface of nano-Si₃N₄. The surface-initiated acrylic polymer modified nano-Si₃N₄ powder was prepared by atom transfer radical polymerization (ATRP)method by using methyl methacrylate (MMA)and glycidyl methacrylate (GMA)as monomer. ATRP modified nano-Si₃N₄ powders were characterized by Fourier infrared spectroscopy (FTIR),nuclear magnetic resonance spectroscopy (¹H NMR)and gel permeation chromatography (GPC),and the optimum process conditions for preparing modified Si₃N₄ were determined. Malvern laser particle size analyzer, scanning electron microscope (SEM) and contact angle tester were used to characterize the properties of the nano-Si₃N₄ powders before and after modification. The results indicate that the modified nano-Si₃N₄ powders prepared by this method have good dispersibility, while the particle size and the agglomeration of the nano-Si₃N₄ powders decreased in ethanol solution, and the molecular weight distribution of the surface graft copolymer was narrow and controllable.

Key words: atom transfer radical polymerization, silicon nitride, nanoparticles, agglomeration, particle size distribution

中图分类号:

O613.72

黄李晓研, 魏铭, 王钦利, 刘晓芳. 原子转移自由基聚合法改性纳米氮化硅粉体的制备工艺及性能[J]. 化工进展, 2018, 37(05): 1881-1887.

HUANG Lixiaoyan, WEI Ming, WANG Qinli, LIU Xiaofang. Preparation and properties of nano-Si₃N₄ powder modified by ATRP[J]. Chemical Industry and Engineering Progress, 2018, 37(05): 1881-1887.

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原子转移自由基聚合法改性纳米氮化硅粉体的制备工艺及性能

Preparation and properties of nano-Si₃N₄ powder modified by ATRP

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Preparation and properties of nano-Si₃N₄ powder modified by ATRP