摘要本文采用硬模板法合成了二氧化锆中空介孔微球。作为模板的二氧化硅微球通过Stöber法制备得到,然后以正丁醇锆、正硅酸乙酯、浓氨水、无水乙醇为原料,合成中空介孔二氧化锆微球。用傅里叶变换红外光谱仪、扫描电镜、透射电镜、X射线衍射仪、N2吸附-脱附仪对中空二氧化锆微球的形成过程进行表征。表征数据显示,产物呈中空球形,分散性良好,粒径分布均一。原先采用的合成方法制备的二氧化锆中空介孔微球由于煅烧温度高等原因导致球体破碎较多,为解决此问题,本文在制备方法上采用煅烧前加硅保护层法解决了此问题。59858
毕业论文关键词 二氧化锆 Stöber法 中空介孔微球
毕业设计说明书(论文)外文摘要
Title The Synthesis of Hollow Mesoporous Zirconia Nanospheres
Abstract
In this thesis , hollow zirconia microspheres with a mesoporous shell were synthesized via the hard-template method with zirconium butoxide, tetraethyl orthosilicate (TEOS), aqueous ammonia and anhydrous ethanol as raw material. Silica spheres,as templates,were prepared by the Stöber method. The factors influencing the formation,structures and properties of hollow microspheres were studies in detail by Fourier Transform Infrared Spectroscopy (FTIR), scanning electron microscope (SEM), Transmission Electron Microscope (TEM), X-Ray Diffraction (XRD) and N2 adsorption-desorption. The result shows that the hollow mesoporous shells is thick and smooth, with good dispersion and even particles distribution. However, many hollow zirconia microspheres prepared by conventional techniques were broken because of high-temperature calcination. In this paper, we have solved the above issue by the “silica-protected calcination” process.
Keywords zirconia Stöber process hollow mesoporous microspheres
目 次
1 绪论 1
1.1 中空介孔材料 1
1.2 二氧化锆的制备 3
1.2.1 气相法 3
1.2.2 固相法 3
1.2.3 液相法 3
1.3 二氧化锆中空介孔微球的制备 5
1.3.1 二氧化锆中空微球的制备 5
1.3.2 介孔二氧化锆材料的制备 7
2 中空介孔二氧化锆微球的制备 8
2.1 实验药品与仪器 8
2.1.1 实验原料 8
2.1.2 主要实验仪器 8
2.2 实验原理 9
2.2.1 不同粒径二氧化硅微球的制备 9
2.2.1 不同粒径二氧化锆包覆微球的制备 9
2.2.3 二氧化硅保护最外层包覆层的制备 9
2.2.1 二氧化锆空心微球的制备 9
2.3 不同粒径二氧化锆微球的制备 10
2.4 本章小结 11
3.1 主要表征仪器 12
3.2 结果与讨论 12
3.2.1 红外光谱