SiO_2/SiCN核壳陶瓷微球的制备及表征  

Preparation and Characterization of SiO_2/SiCN Core-shell Ceramic Microspheres

作　　者：张海媛[1,2] 刘洪丽[1,2] 李婧[2] 康伟[2] ZHANG Hai-yuan LIU Hong-li LI Jing KANG Wei(Tianjin Key Laboratory of Soft Soil Characteristics and Engineering Environment, Tianjin 300384, China School of Materials Science and Engineering, Tianjin Chengjian University, Tianjin 300384, China)

机构地区：[1]天津市软土特性与工程环境重点实验室,天津300384 [2]天津城建大学材料科学与工程学院,天津300384

出　　处：《材料工程》2017年第5期7-12,共6页Journal of Materials Engineering

基　　金：国家自然科学基金资助项目(51472175);天津应用基础与前沿技术研究计划资助项目(15JZDC37200)

摘　　要：采用乳液技术和先驱体转化法相结合,利用改性后SiO_2颗粒表面的双键引发聚硅氮烷(PSN)原位聚合,得到SiO_2/PSN核壳结构微球,经高温裂解过程成功制备SiO_2/SiCN核壳陶瓷微球。研究SiO_2与PSN原料的质量比、固化时间和热解温度对核壳微球形成过程和形貌的影响,并采用SEM,EDS,TEM,FT-IR,XRD对微球的微观形貌、化学成分及物相进行表征。结果表明:SiO_2与PSN质量比为1∶4时,200℃固化4h得到表面颗粒分布均一、包覆完全的SiO_2/PSN核壳微球;经800~1200℃热处理后,得到能保持原来形貌的非晶态SiO_2/SiCN核壳陶瓷微球;1400℃热解产物发生结晶,生成了SiO_2,SiC和Si_3N_4晶相。The SiO2/PSN core-shell microspheres were prepared via an emulsion reaction combined with the polymer-derived ceramics （PDCs） method using polysilazane （PSN） in situ polymerization on the surface of SiO2 modified by silane coupling agents MPS, followed by pyrolysis process to obtain SiO2/SiCN core-shell ceramic microspheres. The effects of raw mass ratio, curing time and pyrolysis temperature on the formation and the morphology of core-shell microspheres were studied. The morphology, chemical composition and phase transformation were characterized by SEM, EDS, TEM, FT-IR and XRD. The results show that after reaction for 4h at 200℃, SiO2 completely coated PSN forms a core-shell microsphere with rough surface when the mass ratio of SiO2 and PSN is 1：4; when pyrolysis temperature is at 800-1200℃, amorphous SiO2/SiCN core-shell ceramic microspheres are prepared; at 1400℃, the amorphous phase partially crystallizes to produce SiO2, SiC and Si3N4 phase.

关 键 词：聚硅氮烷  乳液法  先驱体转化法  核壳陶瓷微球 

分 类 号：TQ174[化学工程—陶瓷工业]