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以八水氧氯化锆(ZrOCl2·8H2O)为原料,以氨水(NH3·H2O)、氢氧化钠(NaOH)溶液为沉淀剂,采用溶胶-凝胶法制备纳米级氧化锆粉体,对前驱体加入不同的稳定剂,通过吸滤、干燥、煅烧等工艺,得到以四方氧化锆晶相为主、不同粒度组成、不同四方相含量的样品.利用激光纳米粒度分析仪、X-射线衍射(XRD)等分析手段分别对粉体的粒径、物相组成进行表征,分别采用晶面公式、谢乐公式对四方相含量、晶粒尺寸进行计算.分析了室温下加入不同稳定剂制备的氧化锆纳米粉体中四方相含量和颗粒粒径之间的关系.结果表明:氧化钇稳定的氧化锆纳米粉粒度更细、粒度分布更均匀.经400~1000 ℃×2 h煅烧后,通过氧化锆纳米粉晶粒尺寸累积分布与四方相含量的关系可以得出以氧化镁、氧化钙、氧化钇为稳定剂制备的氧化锆纳米粉相变临界粒径分别为24~28 nm、26~33.6 nm、18~22.6 nm.

Nano-sized zirconia powders were prepared by sol-gel method using ZrOCl2·8H2O as the starting material, NH3·H2O and NaOH solution as precipitants.Different stabilizers were added into the precursor.Tetragonal zirconia samples with different particle sizes and tetragonal phase content were obtained after filtration, drying and calcination.The particle size and phase composition of the powders were characterized by a laser nano particle analyzer and XRD respectively.The content of tetragonal phase and grain size were calculated using Scherer formula and crystal face formula.The relationship between tetragonal phase content and particle size of zirconia powders added into different stabilizers at room temperature was analyzed.The results indicate that Nano-zirconia powder stabilized with Y2O3 is finer in particle size and more uniformity in particle size distribution.After calcine at 400-1000 ℃ for 2 h, the critical particle sizes of phase transition of nano-zirconia powder stabilize with MgO, CaO, Y2O3 are respectively 24-28 nm, 26-33.6 nm, 18-22.6 nm , based on the relationship between tetragonal phase content and cumulative distribution of particle size in nano-sized zirconia powders.