摘要
以工业纯ZrOCl28H2O,分析纯AlCl3·6H2O,分析纯Y2O3等为原料,将AlCl36H2O 和ZrOCl2·8H2O分别配制成0.5 mol·L^-1和1 mol·L^-1的水溶液,按ZrO2和Al2O3的质量比为4456配成混合溶液;将混合溶液与用盐酸溶解稳定剂Y2O3后配制成一定浓度的YCl3溶液混合并搅拌均匀,再向均匀溶液中加入2%PEG分散剂制成母液;然后向母液中滴加过量的0.5 mol·L^-1的草酸溶液形成络合母液,滴加氨水调节其pH值.研究了pH值在4～10之间,直接沉淀法和络合沉淀法对Al2O3-ZrO2复合粉前驱体溶胶团聚及粉体粒度分布的影响.利用透射电镜（TEM）和激光粒度分析仪对溶胶和复合粉粒度组成进行了分析.结果表明：采用草酸为络合剂,氨水为沉淀剂的络合沉淀法可以明显的改善Al2O3-ZrO2复合粉前驱体溶胶的团聚,干燥后得到的复合粉体没有明显的硬团聚;反应溶液的pH值为9时效果最佳;络合沉淀法制备的Al2O3-ZrO2复合粉的平均粒径为3.704 μm,直接法制得的粉体的平均粒径为7.052 μm.
Industrial pure ZrOCl2 · 8H2O, analyzing pure AlCl3 · 6H2O and analyzing pure Y2O3 were used as starting material. AlCl3 · 6H2O and ZrOCl2· 8H2O were made into solution of 0.5 mol · L^-1 and 1 mol · L^-1 respectively,then they were mixed according to mass ratio of ZrO2 and Al2O3 44 ： 56. The mixed solution was mixed with YCl3 solution,which was obtained by dissolving Y2O3 with HCI, and then adding 2% PEG dispersant to form mother liquor. Excessive oxalic acid of 0.5 mol · L^-1 was titrated into the mother liquor and complex mother liquor was formed. Ammonia water was then added to adjust the pH value, The effects of compleximetry-precipitation method and direct-precipitation method on the agglomeration of the precursor sol and grain size distribution were studied with pH value 4 - 10. The sol and composite powder were analyzed by transmission electron microscopy（TEM） and laser grain size analyzer. The result indicates that： the compleximetry-precipitation method by using oxalic acid as complexing agent and ammonia water as precipitant can remarkably reduce the agglomeration of composite powder precursors. After drying, the composite powder appeared trivial hard agglomeration. The optimum pH value is 9 ;The average size of the composite powder is 3. 704 μm by compleximetry-precipitation method and 7. 052 μm by direct-precipitation method.
出处
《耐火材料》
CAS
北大核心
2006年第5期362-365,共4页
Refractories
基金
陕西省科技攻关项目(2003K07-G9)
西安市科技局攻关项目(DG200347)
