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研究了化学共沉淀法合成Nd:Sc2O3纳米粉的工艺。以Sc2O3为基质材料,掺杂0.5%(原子分数)的Nd3+,添加适量聚乙二醇(PEG)和(NH4)2SO4作为分散剂,以氨水(NH3.H2O)和碳酸氢铵(NH4HCO3)混合溶液作复合沉淀剂,采用化学共沉淀法获得了碱式稀土碳酸盐前躯体,在1100℃下煅烧该前躯体4 h,制备出性能良好的Nd:Sc2O3纳米粉。采用热重-差热分析仪(TG/DSC)、红外光谱分析仪(IR)、X射线衍射仪(XRD)、透射电子显微镜(TEM)等测试手段对Nd:Sc2O3前躯体和煅烧后的粉体进行表征。实验结果表明:在室温下,用氨水和碳酸氢铵混合溶液作为复合沉淀剂合成出的前躯体为碱式稀土碳酸盐。通过XRD和EDS能谱分析,Nd3+完全固溶于Sc2O3的立方晶格中,这将有利于制备激光透明陶瓷。在1100℃的温度下煅烧此前躯体得到的Nd:Sc2O3纳米粉具有颗粒粒度小(约50 nm)、分散性好、团聚程度轻、结晶良好的性能。因此,采用此工艺合成的粉体将有可能制备出的Nd:Sc2O3透明陶瓷。
The technology of synthesizing Nd: Sc2O3 nanopowders by chemical coprecipitation was studied. Doped with 0.5% (atomic fraction) Nd3 + and polyethylene glycol (PEG) and (NH4) 2SO4 as dispersants and mixed with ammonia water (NH3.H2O) and ammonium bicarbonate (NH4HCO3) Solution as a composite precipitant, a basic rare earth carbonate precursor was obtained by chemical coprecipitation, and the precursor was calcined at 1100 ° C for 4 h to prepare a good performance Nd: Sc2O3 nanopowder. The mechanical properties of Nd: Sc2O3 precursors and calcined powders were investigated by means of TG / DSC, IR, XRD and TEM. Body to characterize. The experimental results show that the precursors synthesized with ammonia and ammonium bicarbonate as the composite precipitant are basic rare earth carbonates at room temperature. By XRD and EDS EDS analysis, Nd3 + is completely dissolved in the cubic lattice of Sc2O3, which will be helpful for the preparation of laser transparent ceramics. The Nd: Sc2O3 nanopowder obtained by calcining the precursor at a temperature of 1100 ℃ has the characteristics of small particle size (about 50 nm), good dispersibility, light agglomeration degree and good crystallization. Therefore, the powder synthesized by this process will be possible to prepare Nd: Sc2O3 transparent ceramic.