氧氯化锆直接热分解制备三维有序大孔氧化锆

Three Dimensional Ordered Macroporous ZrO_2 Prepared by Directly Calcining ZrOCl_2

以聚苯乙烯微球胶晶为模板,氧氯化锆的甲醇溶液为前驱物,通过直接热分解的方法制备了三维有序大孔氧化锆(3DOM-ZrO2);利用SEM、TEM、EDS和BET等技术对其进行了表征,并探讨了实验条件对大孔结构与形态的影响.结果表明,过低或过高的氧氯化锆浓度都不利于形成长程有序的三维大孔结构;增加填充次数只有在较高的氧氯化锆浓度下才能有效增加填充量;合适的焙烧温度在600￣700℃之间;BET分析表明3DOM-ZrO2孔壁具有非多孔结构,与TEM观察结果非常一致.

Three dimensional ordered macroporous （3DOM） zirconium dioxides with pore diameters of about 500 nm are successfully prepared via a direct calcining step, using a methanol solution of ZrOCl2·8H2O as filling precursor and polystyrene sphere （PS） colloid crystals as templates. The method of synthesis is simple, quicker than other synthesis, and based on readily available precursors. Precursor concentration and a second filling of the 3D packed polystyrene spheres are important parameters in fine tuning the mechanical properties of the walls and achieving long range ordered materials. Low calcination temperature （≤ 500℃） introduces impurities in the wall structure of zirconia and crystallite phase transformation in the crystal structure. Excess high calcination temperature （≥800℃） leads the 3D wall structure destroyed and collapse. The BET behaviour of 3DOM-ZrO2 shows that pore wall has a non-porous structure, which agrees with the TEM results.