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-Si_3N_4 powder modified by ATRP

作　　者：黄李晓研 魏铭 王钦利 刘晓芳 HUANG Lixiaoyan;WEI Ming;WANG Qinli;LIU Xiaofang(School of Chemistry,Chemical Engineering and Life Sciences,Wuhan University of Technology,Wuhan 430070,Hubei,China)

机构地区：[1]武汉理工大学化学化工与生命科学学院,湖北武汉430070

出　　处：《化工进展》2018年第5期1881-1887,共7页Chemical Industry and Engineering Progress

基　　金：国家自然科学基金项目(51272191)

摘　　要：采用γ氨丙基三乙氧基硅烷(KH-550)、氯乙酰氯在氮化硅(Si_3N_4)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。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.

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 

分 类 号：O613.72[理学—无机化学]