超高速液相色谱用纳米ZrO_2晶体颗粒的制备及机理

Preparation and mechanism of nano ZrO_2 crystal particles for ultra high-speed liquid chromatography

以正丁醇/水二元油包水体系形成的微乳液滴为反应器,采用正丙醇锆为锆源反应物、水为沉淀剂和硬脂酸(表面活性剂)发生反应,制备了纳米ZrO_2颗粒。采用扫描电子显微镜、Malvern粒度分布仪、X射线衍射仪、热重-差热分析仪和N2吸附-脱附仪对所得到的ZrO_2颗粒表征。结果表明,经过500和700℃焙烧,ZrO_2颗粒分别由无定型向亚稳定四方形、亚稳定四方形向单斜型转变,且制备的纳米ZrO_2颗粒为表面光滑、无孔、均一、单分散的球体,可用于超高速液相色谱材料。

Nano-ZrO_2 particles were prepared using microemulsion droplet formed with oil-water system of n-butanol/water as the reactors,zirconium n-propoxide as material,water as precipitating agent and stearic acid as surfactants.The ZrO_2 particles were characterized by SEM,Malvern particle size analyzer,XRD,TG-DTA,and N2 adsorption-desorption.The results showed that the nano-ZrO_2 particles were uniform spheres with smooth surface and non-porous structures.The phase of the ZrO_2 particles transformed from amorphous to metastable tetragonal calcined at 500 ℃ in air and from tetragonal to monoclinic zirconia calcined at 700 ℃.The nanoparticles has potential application in ultra high-speed liquid chromatography.