氯铪酸钾的制备及表征  

Preparation and Characterization of Hexachlorohafnate of Potassium

作　　者：柳旭[1] 王鑫[1] 彭家庆[1] 王力军[1] 陈松[1] 吴延科[1] 陈洋[1] 

机构地区：[1]北京有色金属研究总院,北京100088

出　　处：《稀有金属材料与工程》2014年第2期450-454,共5页Rare Metal Materials and Engineering

基　　金：国家科技支撑计划项目(2012BAB10B00);北京有色金属研究总院青年基金(53141)

摘　　要：以氯化钾和四氯化铪为原料,通过气-固反应直接制备出了氯铪酸钾。首先考察了氯化钾与四氯化铪混合同一坩埚内加热及分别放入不同的坩埚加热两种加料方式对产物的影响,结果表明采取后一种加料方式反应较充分;之后分析原料配比、反应温度及时间对产物的影响,并对得到的产物进行XRD、EDS及SEM分析。XRD结果表明,产物为氯铪酸钾,由EDS分析可知,产物中钾原子与铪原子的摩尔比为2.11(nK:nHf=2.11),与纯氯铪酸钾中钾与铪的摩尔比2:1接近,说明产物中大部分为氯铪酸钾。制备氯铪酸钾较理想的反应条件为:采用分开放料的加料方式,氯化钾与四氯化铪的质量比为1:2,反应温度为450℃,反应时间为3 h。Hexachlorohafnate of potassium has been prepared using potassium chloride and hafnium chloride as raw materials by gas-solid reaction. The influence of two mixing methods, namely putting the mixed raw materials in a crucible and putting the raw materials in different crucibles, was analyzed first. It has been found that more sufficient reaction was got by the latter method. Then the effects of materials ratio, reaction temperature and reaction time were investigated; moreover the product was examined by X-ray diffraction, SEM and EDS methods. The result of XRD reveals that the product is mainly hexachlorohafnate of potassium. The result of EDS analysis further shows that most of the product are hexachlorohafnate of potassium because the atom ratio of potassium to hafnium equals to 2.11（nK：nHf=2.11）, which is very close to the theoretical ratio in pure hexachlorohafnate of potassium. The optimal conditions of preparing hexachlorohafnate of potassium are as follows： adopting of the latter method, e.g. raw materials in different crucibles, KC1/HfCl4 mass ratio with 1：2, reaction temperature with 450 ℃ and reaction time with 3 h

关 键 词：氯铪酸钾 制备 表征 

分 类 号：TQ131.13[化学工程—无机化工] TF044[冶金工程—冶金物理化学]