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.
作者
张海媛
刘洪丽
李婧
康伟
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)
出处
《材料工程》
EI
CAS
CSCD
北大核心
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)
关键词
聚硅氮烷
乳液法
先驱体转化法
核壳陶瓷微球
polysilazane emulsion method polymer-derived ceramics method core-shell ceramic microsphere
