制备条件对镥铝石榴石纳米粉体合成的影响

Effect of preparation conditions on synthesis of Lu_3Al_5O_(12) nanopowders

采用溶剂热法研究起始材料硝酸镥(Lu(NO_3)_3·6H_2O)和硝酸铝(Al(NO_3)_3·9H_2O)中结晶水去除前后对镥铝石榴石(LuAG)纳米粉体合成的影响;比较高温热处理对LuAG纳米粉体合成的影响;利用X射线衍射仪、红外光谱仪、透射电子显微镜分析所得粉体的物相组成、微观形貌和分散情况。结果表明,对于含结晶水的起始材料采用溶剂热法能够合成纯相的LuAG纳米粉体,颗粒尺寸为100 nm左右且具有较好的分散性;高温热处理后,纳米粉体结构趋于完整,但纳米颗粒有团聚现象。认为原材料中结晶水的去除不利于溶剂热法合成LuAG纳米粉体,而高温热处理所得的LuAG纳米粉体均已结晶。

The effect of before and after removal of crystal water in starting material Lu（NO3）3·6 H2 O and Al（NO3）3·9 H2 O on synthesis of Lu3 Al5 O（12）（LuAG） nanopowders by solvothermal method was investigated. As a comparison, the obtained powders were subsequently heated at 1 000 ℃ for 2 h. The phase composition, morphology and dispersion of the powders were analyzed by X-ray diffraction（XRD）, fourier transform infrared spectroscopy（FTIR） and transmission electron microscopy（TEM）. The results show that pure phase LuAG nanopowders can be synthesized by solvothermal method using the starting materials with crystal water. The particle size is about 100 nm and has good dispersion. After heat treatment at high temperature, the structure of nanopowders tends to be complete, but has the slight agglomeration. Therefore, the removal of crystalline water in the raw materials is not conducive to the synthesis of LuAG nanopowders by solvothermal method, and the LuAG nanopowders obtained by heat treatment are well crystallized.