具有大尺度无缺陷垂直孔道的介孔二氧化硅薄膜在生物材料、电化学和光学传感器中具有重要应用价值。本文采用电化学辅助自组装(EASA)工艺制备大面积(5×5 cm2)孔道垂直定向的介孔二氧化硅薄膜,利用循环伏安曲线(CV),扫描电子显微镜(SEM)、原子力显微镜(AFM)、高分辨透射电子显微镜(HRTEM)、二维掠入射小角X射线散射(2D-GISAXS)等手段对薄膜渗透性、表面宏观形貌,及介孔孔道的结构等进行了表征,并通过同步辐射反射率计测试了该薄膜在极紫外波段的光学性能。结果表明,采用EASA法在大面积基底上成功制备出了具有垂直取向孔道且渗透性良好的介孔二氧化硅薄膜,其孔径和晶胞参数大小分别为2.83 nm和4.1 nm,且其在极紫外波段(5~11 nm)的反射率最高可达75%。

Mesoporous silica films with defect-free vertical channels on large length scales have great significance in biomaterials, electrochemical and optical sensors. Herein, mesoporous silica films with vertical orientation on large area (5×5 cm2) substrates were successfully prepared by electrochemical assisted self-assembly (EASA) process. The film permeability, surface macroscopic morphology and mesoporous pore structure were characterized by cyclic voltammetry (CV), scanning electron microscope (SEM), atomic force microscope (AFM), high resolution transmission electron microscope(HRTEM), and 2D grazing incidence small-angle X-ray scattering (2D-GISAXS), respectively. In addition, the optical properties of the films in the extreme ultraviolet region were tested by albedometer. The results show that the obtained film on a large area substrate exhibites good permeability,which suggests that the mesochannels in silica films are vertically oriented, and the mesopore diameter and cell parameters are 2.83 nm and 4.1 nm, respectively. Moreover, the reflectivity reaches up to 75% in the extreme ultraviolet wavelengths (5-11 nm).