化工新型材料

化工新型材料 ›› 2022, Vol. 50 ›› Issue (9) : 174-178. DOI: 10.19817/j.cnki.issn1006-3536.2022.09.035

科学研究

纳米SiO₂微球的粒径调控及影响因素研究

作者信息 +

Study on particle size regulation and influencing factor of nano-SiO₂ microsphere

Du Heng, Li Xin, Guan Fanglan, Luan Xiaowan, Sun Ailin, Yang Tianci

Author information +

文章历史 +

Received		Published
2021-05-07		2022-09-20
Issue Date	Revised Date
2022-09-27	2021-05-07

PDF

摘要

采用改进的Stöber溶胶-凝胶法,以氨水为碱性催化剂,通过改变乙醇和水的比例,制备出粒径范围为230～430nm的均匀SiO₂微球,并探究了反应时间、正硅酸乙酯(TEOS)滴定速度对其粒径和均匀度的影响。扫描电镜(SEM)及动态光散射测试显示,改变乙醇和水的比例、反应时间及TEOS的滴定速率可以很好地调控SiO₂微球的尺寸和圆滑度。研究结果表明,随着乙醇浓度的增大,SiO₂粒径减小;随着TEOS滴定速率的减小,SiO₂粒径相对减小且更加均匀圆滑;反应时间延长,粒径逐渐变大,最后在4h后粒径逐渐趋于稳定且保持不变。同时,微球通过垂直自组装法形成的光子晶体薄膜具有明显的结构色,进一步验证了改变乙醇和水的比例能得到尺寸均一、高圆滑度的SiO₂微球。

Abstract

Improved Stöber sol-gel method was used to prepare uniform SiO₂ microspheres with particle size ranging from 230 to 430nm by changing the ratio of ethanol to water and used ammonia water as alkaline catalyst.The effects of reaction time and titration rate of ethyl orthosilicate (TEOS) on the particle size and uniformity were investigated.The results of scanning electron microscopy (SEM) and dynamic light scattering (DLS) showed that the size and roundness of SiO₂ microspheres could be well controlled by changing the ratio of ethanol to water,the reaction time and the titration rate of TEOS.The results shown that SiO₂ particle size decreased with the increase of ethanol concentration.With the decrease of TEOS titration speed,the particle size of SiO₂ decreased and the shape became more uniform.As the reaction time prolongs,the particle size gradually became larger,and finally,after 4 hours,the particle size gradually became stable and remained unchanged.At the same time,the photonic crystal film formed by the microspheres through the vertical self-assembly method had obvious structural color,which further verified that the SiO₂ microspheres with uniform size and high smoothness can be obtained by changing the ratio of ethanol and water.

关键词

二氧化硅 / 纳米微球 / Stöber法 / 光子晶体 / 结构色

Key words

silica / nanosphere / Stöber method / photonic crystal / structure color

引用本文

引用格式 ▾

纳米SiO₂微球的粒径调控及影响因素研究[J]. 化工新型材料, 2022, 50(9): 174-178 DOI:10.19817/j.cnki.issn1006-3536.2022.09.035

登录浏览全文

4963

注册一个新账户忘记密码

参考文献

原文顺序 | 出版日期 | 本文引用

[1] 姜小阳.纳米二氧化硅的制备及表面修饰[D].青岛:青岛科技大学,2012.
[2] 蔡亮珍,杨挺.纳米SiO₂在高分子领域中的应用[D].北京:中国蓝星集团蓝星化工科技总院中央实验室,2002.
[3] Unger K K,Kumar D,Grün M,et al.Synthesis of spherical porous silicas in the micron and submicron size range:challenges and opportunities for miniaturized high-resolution chromatographic and electrokinetic separations[J].Journal of Chromatography A,2000,892(1-2):47-55.
[4] Leder G,Ladwig T,Valter V,et al.New effects of fumed silica in modern coatings[J].Progress in Organic Coatings,2002,45(2-3):139-144.
[5] Acks M D,Tseng T Y.Preparation of SiO₂ glass from model powder compacts:I,formation and characterization of powders,suspensions,and green compacts[J].Journal of the American Ceramic Society,1984,67(8):526-532.
[6] Xia Y,Gates B,Yin Y,et al.Monodispersed colloidal spheres:old materials with new applications[J].Advanced Materials,2000,12(10):693-713.
[7] Lu Z,Owens H.Optimum processing parameters for coating polyester with silica nanoparticles using gravity sedimentation[J].Journal of Nanoparticle Research,2019,21(10):1-10.
[8] Gao W,Rigout M,Owens H.The structural coloration of textile materials using self-assembled silica nanoparticles[J].Journal of Nanoparticle Research,2017,19(9):1-11.
[9] 孟佳意,何萌,杨晟,等.SiO₂@DV复合光子晶体的制备及电致变色性能研究[J].北京服装学院学报(自然科学版),2017,37(4):1-6.
[10] 吴燕,孟佳意,李昕,等.聚(3,4-二溴噻吩)复合光子晶体的制备及电致变色性能[J].高分子材料科学与工程,2019,35(8):55-60.
[11] 梁飞跃,李昕,赵宁,等.SiO₂@PANI光子晶体的制备及电致变色性能研究[J].高分子学报,2014(6):860-864.
[12] 王岩岩,唐美瑶,申赫,等.基于芘功能化核壳型磁性二氧化硅纳米微球的荧光传感器及其对水溶液中汞离子的检测和去除[J].发光学报,2018,39(12):1799.
[13] Zhang A,Yuan W,Zhou N,et al.Structural color and its application prospect in dyeing and finishing industry(Ⅰ)[J].Dyeing & Finishing,2012,38(13):44-47.
[14] Liu Z,Zhang Q,Wang H Z,et al.Magnetic field induced formation of visually structural colored fiber in micro-space[J].J Colloid Interf Sci,2013,406:18-23.
[15] 谢京励,邓旭.基于裂纹生长的胶体颗粒自组装结构色纤维[J].四川轻化工大学学报(自然科学版),2020,33(3):7-12.
[16] 赵莉,杜蘅,刘虎,等.纳米SiO₂微球在PMMA凝胶聚合物电解质中的尺寸效应及其在全固态电致变色器件中的应用[J].复合材料学报,2021,38(5):1446-1454.