合成介孔纳米晶体氧化锆的新方法

摘要

通过一种新颖的方法,即软模板-固液技术(CSSL)合成具有高比表面积的介孔纳米晶体氧化锆.首先,通过软模板法以1-十六烷基-3-甲基咪唑溴(C16mim+Br-)为结构导向剂,硫酸锆为无机前驱物合成了介观相氧化锫杂化物,然后该杂化物与固体硝酸铜无机盐研磨并进行热处理.在600℃焙烧后所得到的氧化锆材料具有蠕虫状介孔结构,且孔壁由尺寸约为2.50nm的四方相氧化锆纳米粒子组成.该材料的比表面积为240.0 m2·g-1,孔径为4.10 nm.与之对应,使用单一的软模板法在相同的温度焙烧后,所得到的氧化锆材料介孔结构坍塌,比表面积仅为9.5m2·g-1.%A novel strategy involving the combination of soft-templating and the solid-liquid method (CSSL) is presented for the synthesis of mesoporous nanocrystalline zirconia with a high specific surface area.The mesostructured zirconia hybrid is firstly synthesized by the soft-templating method using 1-hexadecyl-3-methylimidazolium bromide (C16mim+Br-)as the structure-directing agent and zirconium sulphate as an inorganic precursor.It is then ground in the presence of solid copper nitrate followed by heat-treatment in air.The resulting zirconia material，after calcination at 600℃，possesses a wormlike arrangement of mesopores surrounded by tetragonal ZrO2 nanocrystallites of ca 2.50 nm diameter.The Brunauer-Emmett-Teller(BET)surface area is 240.0 m2·g-1 and the pore size is 4.10 nm.However，no mesoporous structure exists in the obtained zirconia material that was produced using the simple soft-templating rnmethod at the same calcination temperature.The BET surface area is only 9.5 m2·g-1 for this material.