阴离子表面活性剂辅助模板途径合成介孔结构氧化锆纳米晶

Anionic Surfactant-assisted Synthesis of Mesoporous Zirconia Nanocrystallite

利用阴离子表面活性剂十二烷基磺酸钠(SDS)为辅助模板剂,成功地合成了高稳定性的介孔氧化锆纳米晶,采用DSC-FG,FT-IR,XRD,TEM,UV-Vis以及N2吸附-脱附等方法对样品进行了表征.研究表明,以阴离子型十二烷基磺酸钠合成的氧化锆经600℃煅烧后仍为纯四方相,氧化锆晶粒平均尺寸约为6.5 nm.阴离子型表面活性剂与有机锆源形成自组装协同作用,合成的氧化锆具有蠕虫状介孔结构,经过500℃煅烧后介孔结构仍然保持,且由于表面活性剂的去除,比表面积显著提高,显示了良好的热稳定性.本实验制备的氧化锆纳米晶较一般方法制备的市售纳米氧化锆有明显紫外吸收边蓝移现象.

A steady mesoporous zirconia nanocrystallite has been successfully synthesized by the anionic surfactant-assisted route. The DSC-TG, FT-IR, XRD, TEM, UV-Vis and N2 adsorption-desorption analyses have been used for the structural characterizations. The DSC-TG showed that the anionic surfactant had a significant co-operative effect on the synthesis of zirconia nanocrystallite. The XRD patterns indicate that the as-prepared zirconia took a pure tetragonal phase even calcinated at 600 ℃. The TEM analysis displays that the zirconia exhibits worm-like mesoporous structure, which can be well maintained after calcination.The pore size is about 1.8 nm, observable from the TEM images. Compared to that of the commercial sample, a significant blue shift of the UV-Vis spectra of the zirconia nanocrystallite after calcination at 500 ℃ has been demonstrated. The N2 adsorption analysis illustrates that the zirconia has an improved BET surface area after calcination, indicative of good thermal stability.