具有介孔孔壁的三维有序大孔氧化铝的制备与表征

Synthesis and characterization of three-dimensional ordered macroporous Al_2O_3 materials with mesoporous wall

以260 nm的聚苯乙烯胶体微球组装的胶体晶体作为模板,采用硝酸铝为原料制备了γ晶相的三维有序大孔(3DOM)Al2O3。首先将Al(NO3)3.9H2O溶解在体积分数70%的甲醇溶液中并填充到胶体晶体模板中,然后取出模板室温干燥,再用质量分数10%的稀氨水浸泡并干燥,最后经550℃焙烧3 h得到3DOMAl2O3。所得材料具有三维有序的大孔孔道,大孔之间由小窗口连通,构成内部交联的大孔网络。3DOMAl2O3孔壁由10 nm左右的Al2O3纳米粒子组成,形成丰富的介孔孔隙,并使材料构成大孔/介孔多级孔道体系,材料的BET比表面积达到315 m2/g。

Three-dimensional ordered macroporous Al2O3 materials （3DOM Al2O3 ） with mesoporous wall are successfully synthesized using Al（ NO3 ）3·9H2O as precursor and 260 nm polystyrene colloid crystal as template. Al（NO3）3·9H2O dissolved in 70% methanol solution, is filled in the voids of colloid crystal template. The impregnated template is dried at room temperature for 30 minutes. Then, the composites are infiltrated with 10% of ammonium hydroxide solution. At last, the template is removed through calcinations at 550℃ for 3 hours. The resulted materials have three-dimensional ordered macroporous structure. At the same time, the macropores keep interconnected through small windows. The walls of 3DOM Al2O3 are made up of nano-particles of about 10 nm diameter, which results into rich mesoporous and high surface area of 315 m2/g. The XRD spectrum of 3DOM Al2O3 shows the sample consisting of polycrystal γ-Al2O3.