微波法制备LaF_3超细粉

Preparation of superfine powder of LaF_3 by microwave method

以La2O3、HCl为原料制备了LaCl3,并直接用双柱法,以LaCl3溶液同NH4HCO3溶液作用合成了粒度较小的La2(CO3)3粉体;以粉体La2(CO3)3为镧源与NH4F混合,在微波作用下经过固相化学反应,合成了LaF3超细粉;研究了不同分散剂等反应条件对合成LaF3超细粉的粒度和纯度的影响;通过X射线衍射(XRD)检测了不同途径合成的LaF3超细粉体的纯度,通过扫描电镜(SEM)、透射电镜(TEM)测试了不同途径合成的LaF3超细粉体颗粒的粒度和形貌。结果表明:用乙醇作为分散剂经微波加热固相合成得到了纯度较高,平均粒度约为50nm的LaF3超细粉。

The LaF_3 superfine powder was synthesized. Superfine powder of La_2(CO_3)_3 was first synthesized by means of double pillar method in the reaction that LaCl_3 solution(got from La_2O_3, HCl as raw material ) reacted with NH_4HCO_3 solution.Then LaF_3 superfine powder was got by means of mixing solid La_2(CO_3)_3 and NH_4F under the microwave condition when the diluent of H_2O and C_2H_5OH were used.The influence of diluent (H_2O, C_2H_5OH) on grain degree or pure degree was discussed. The crystal purity of LaF_3 superfine powder was tested by XRD.The granularity and shape of LaF_3 superfine powder was tested by SEM and TEM. The results show that the purity of LaF_3 superfine powder is very well when used C_2H_5OH by means of microwave heat, and LaF_3 superfine powder is 50 nm in size in the direct solid synthesis.