离子交换法制备Ag/Ag1.69Sb2.27O6.25光催化纳米粉末的表征与光催化性能

Characterization and photocatalytic properties of Ag/Ag1.69Sb2.27O6.25 photocatalytic nano-powder synthesized by ion exchange method

以K2H2Sb2O74·H2O和AgNO3为原料,采用离子交换法合成Ag/Ag1.69Sb2.27O6.25光催化纳米粉体材料,利用X射线衍射仪、扫描电镜、透射电镜、X射线光电子能谱、紫外漫反射及紫外可见-分光光度计等,分析和测试不同煅烧温度下所得纳米粉体的物相、形貌、结构以及光学性能,并通过对盐酸四环素(TC-HCl)的可见光下光降解实验测定材料的光催化性能。结果表明:Ag/Ag1.69Sb2.27O6.25颗粒直径约为100~150nm,颗粒表面附着有尺寸为10nm的球状单质纳米Ag颗粒。随煅烧温度升高,Ag/Ag1.69Sb2.27O6.25纳米颗粒表面的凹陷变小,逐渐转变为完整球状,粉末颜色从灰色转变为黄色。煅烧温度为250℃的Ag/Ag1.69Sb2.27O6.25纳米材料(Ag/ASO-250)的光催化活性最高,为900℃煅烧材料的催化活性的7倍。光催化降解反应进行到90min时,AgSbO3-ssr,N-TiO2,和Ag/ASO-250催化降解TC-HCl的降解率分别为65%,77%和90%,这表明与固相烧结的AgSbO3和N-TiO2相比,Ag/ASO-250具有更强的光催化活性。

Ag/Ag1.69Sb2.27O6.25 photocatalytic nano-powders were synthesized by ion exchange method using K2H2Sb2O7 4H2O and AgNO3 as raw materials. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, ultraviolet diffuse reflectance and ultraviolet-visible-spectrophotometer were used to analyze and test the phase, morphology, structure and optical properties of the nano-powders obtained at different calcination temperatures. The photocatalytic properties of the nano-powders were measured by photodegradation experiments of tetracycline hydrochloride (TC-HCl) under visible light. The results show that the diameter of Ag/Ag1.69Sb2.27O6.25 particles is about 100 150 nm, and the surface of Ag1.69Sb2.27O6.25 is coated with spherical Ag particles with a size of 10 nm. With the increase of calcination temperature, the depression of Ag/ Ag1.69Sb2.27O6.25 nanoparticles becomes smaller, and the powder color changes from gray to yellow. The photocatalytic activity of Ag/ Ag1.69Sb2.27O6.25 nano-materials prepared at 250 ℃ is the highest, which is 7 times higher than that of the materials (Ag/ASO-250) prepared at 900 ℃. Moreover, the percentage of TC-HCl degradation by AgSbO3-ssr, N-TiO2 and Ag/ASO-250 is 65%, 77%, and 90% respectively when the photocatalytic degradation reaction lasts 90 minutes. This indicates that Ag/ASO-250 has strong photocatalytic activity compared with AgSbO3-ssr and N-TiO2.