摘要
采用硬模板法与溶胶-凝胶法相结合的工艺,以自制的聚苯乙烯(PS)为模板,十六烷基三甲基溴化铵(CTAB)为阳性表面活性剂,正硅酸四乙酯(TEOS)为硅源制备SiO_(2)空心微球。重点研究升温速率及CTAB、TEOS、氨水用量等工艺参数对SiO_(2)空心微球形貌的影响规律。采用XRD、TEM、SEM、TG、FTIR对微球的物相、微观形貌及介孔结构等进行表征。结果表明:SiO_(2)空心微球粒径为2~5μm、壁厚为117 nm;SiO_(2)空心微球壁会随着升温速率的增加而出现破损现象;随CTAB用量增加,纳米球数量增加且粒径减小;随TEOS用量增加,球壁变厚直至形成纳米球;氨水小于4 mL时,二氧化硅空心微球不能成形,氨水大于4 mL时,二氧化硅空心微球表面粗糙,有实心颗粒;当升温速率为0.5℃/min、CTAB用量为0.05 g、TEOS用量为0.3 mL、氨水用量为4 mL时,且经过抽滤清洗的SiO_(2)空心微球的形貌最佳。
The hollow SiO_(2) microspheres were prepared through the hard template method and sol-gel method by using self-made polystyrene(PS)as template,cetyltrimethyl ammonium bromide(CTAB)as cationic surfactant and Tetraethyl orthosilicate(TEOS)as silica source.Effects of heating rate,content of CTAB,TEOS and ammonia on the morphology of hollow Si O;microspheres were discussed.The phase,morphology and mesoporous structure of hollow Si O;microspheres were characterized by XRD,TEM,SEM,TG and FTIR,which shows the successful preparation of hollow silica sphere.The particle sizes of hollow SiO_(2) microspheres are 2-5μm and the thickness is 117 nm.The hollow SiO_(2) microsphere wall damage with the increase of heating rate.With increasing CTAB content,the number of nanospheres increase and the particle sizes of nanospheres decrease.With increasing TEOS content,the thicknesses of spheres increase until nanospheres are formed.When ammonia is less than 4 mL,hollow SiO_(2) microsphere cannot be formed.When ammonia is greater than 4 mL,hollow SiO_(2) microsphere have rough surface with solid particles.The optimized conditions are determined as follows:the heating rate is 0.5℃/min,the amount of CTAB is 0.05 g,the amount of TEOS is 0.3 mL,the amount of ammonia is 4 mL and then hollow SiO_(2) microspheres are treated through filtering and cleaning.
作者
文素芬
邹金住
周学凡
罗行
WEN Sufen;ZOU Jinzhu;ZHOU Xuefan;LUO Hang(Research Institute of Powder Metallurgy,Central South University,Changsha 410083,China)
出处
《粉末冶金材料科学与工程》
2022年第3期336-344,共9页
Materials Science and Engineering of Powder Metallurgy
基金
国家重点研发计划资助项目(2020YFA0711700)
湖南省创新型省份建设专项资金资助项目(2020GK2062)。
