熔盐电解制备Mg-Zr和Mg-Zn-Zr合金工艺及阴极过程研究
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摘要
锆是镁合金中的主要合金化元素之一,其在镁合金中有着强烈的品粒细化作用。传统的制备含锆镁合金的方法有对掺法和热还原法等,由于金属锆的熔点很高且在镁合金中溶解度较小,致使含锆的镁合金制备存在工艺操作比较复杂,生产成本较高等弊端。本课题以金属化合物为原料采用熔盐电解的方法在低温条件下直接制备镁锆合金和镁锌锆合金,并研究了镁锆合金和镁锌锆合金的电化学形成过程及锆离子在实验体系下的电化学还原机理。
首先,采用循环伏安法和方波伏安法等电化学方法研究了在MgCl2-KCl-K2ZrF6熔盐体系中Zr(Ⅳ)离子在钼电极上的电化学还原过程。循环伏安实验结果表明Zr(Ⅳ)离子的还原过程是通过两步电子转移反应完成的。为了进一步研究Zr(Ⅳ)离子的电子转移过程,通过方波伏安法对电子转移数的计算,证明其电化学反应历程是：Zr(Ⅳ)+ 2e→Zr(Ⅱ)；Zr(Ⅱ)+2e→Zr.在上述熔盐体系中添加Zr02的循环伏安曲线表明在熔盐电解过程中添加Zr02促进Zr(Ⅳ)离子的还原过程。
在MgCl2-KCl-KF-K2ZrF6-ZrO2熔盐体系中制备镁锆合金,通过对原料配比、电流密度和电解温度等电解工艺参数的研究,确定了采用熔盐电解法制备镁锆合金的较佳工艺条件。在较佳工艺条件下可得到锆的质量含量为0.8%的Mg-Zr合金。XRD分析结果表明合金中含有Mg相和Zr相。通过扫描电镜及EDS能谱分析可以看出锆元素在合金内部多以单质锆的形式存在,这与XRD的分析结果相一致,面扫描显示合金内部化学成分均匀。从合金的金相照片可以看出锆对镁合金的晶粒细化作用明显,品粒大小由100～2001μm细化到10～501μm。
其次,采用循环伏安法和计时电流法研究在低温熔融MgCl2-KCl熔盐体系中Mg2+、Zr(Ⅳ)和Zn2+离子在钼电极上的电化学还原过程。循环伏安法实验结果表明Mg2+、Zr(Ⅳ)和Zn2+离子在钼电极上的析出电位分别为：1.8V、1.3V和0.7V。通过计时电流法进一步证实了上述循环伏安的实验结果。
在MgCl2-KCl-KF-ZnCl2-K2ZrF6-ZrO2熔盐体系中制备镁锌锆合金,通过对电流密度和电解温度等电解工艺参数的研究,确定了熔盐电解法制备镁锌锆合金的较佳工艺条件。XRD分析结果表明合金中含有Mg相、Mg7Zn3相和Zr相。EDS分析表明Mg7Zn3合金化合物和单质锆在合金中均分布在晶界处。面扫描可以看出合金内部化学成分均匀。
Zirconium, which is one of the main alloying elements, exhibits obvious grain refining in the magnesium alloys. The traditional preparation methods mainly include metal casting and thermoreduction. Because of high melting point of zirconium metal and its low solubility in magnesium alloy, there are many disadvantages like complex technical operation and high production cost if use these two methods for preparation magnesium alloys containing zirconium. In this paper, we have studied preparation of Mg-Zr and Mg-Zn-Zr alloys in molten salt at low temperature. The formation process and electrochemical reduction mechanism have been investigated using these elements' compounds as raw materials.
Cyclic voltammetry, square wave voltammetry and other electrochemical methods have been used in the MgCl2-KCl-K2ZrF6 molten salt to investigate the reduction mechanism of Zr (Ⅳ) ion in the Mo cathode. Cyclic voltammetry results show that Zr (IV) ion reduction is two steps of electron transfer process and the addition of ZrO2 promote the reduction of Zr (Ⅳ) ions. For further study of the electron transfer process of Zr (IV) ion, quare wave voltammetry has been used to calculate the electron transfer number. The value of electron transfer number proves the reduction processes are Zr (IV)+2e= Zr (II); Zr (II)+2e= Zr.
In the MgCl2-KCl-KF-K2ZrF6-ZrO2 electrolysis system, the optimum conditions of proparation Mg-Zr alloys has been determined by investigation of the ratio of raw materials, current density and electrolysis temperature. The Mg-Zr alloy which is obtained in the optimal conditions contained 0.8% zirconium in the alloy. XRD analysis showed that these alloys contain Mg phase and Zr phase. Scanning electron microscopy and EDS spectrum analysis indicate that Zr element exist in the form of simple substance. This result is consistent with that of XRD analysis. The surface scanning show that internal chemical composition is homogeneous in the alloys. From metallographic photographs, we can see that Zr brings good grain refinement in magnesium alloys. The grain size was dwindled from 100-200μm to 10～50μm.
In another section, we have investigated electrochemical reduction process of Mg+2, Zr (IV) and Zn+2 ions in the Mo electrode by cyclic voltammetry and chronoamperometry in MgCl2-KCl melt at low temperature. The deposition potentials of Mg+2, Zr (IV) and Zn+2 ions on molybdenum electrode were detected at 1.8V,1.3V and 0.7V, respectively. Mg-Zn-Zr alloys are prepared by electrolysis in MgCl2-KCl-KF-ZnCl2-K2ZrF6-ZrO2 melt. The optimum proparation conditions have been determined by investigation of electrolytic parameters like current density and electrolysis temperature. In these alloys, Mg phase, Mg7Zn3 phase and Zr phase were observed by XRD. These phases Mg7Zn3 and Zr metal mainly exist in the grain boundaries. From surface scan we can see that the internal every chemical composition distribute homogeneity in the alloys.
首先,采用循环伏安法和方波伏安法等电化学方法研究了在MgCl2-KCl-K2ZrF6熔盐体系中Zr(Ⅳ)离子在钼电极上的电化学还原过程。循环伏安实验结果表明Zr(Ⅳ)离子的还原过程是通过两步电子转移反应完成的。为了进一步研究Zr(Ⅳ)离子的电子转移过程,通过方波伏安法对电子转移数的计算,证明其电化学反应历程是：Zr(Ⅳ)+ 2e→Zr(Ⅱ)；Zr(Ⅱ)+2e→Zr.在上述熔盐体系中添加Zr02的循环伏安曲线表明在熔盐电解过程中添加Zr02促进Zr(Ⅳ)离子的还原过程。
在MgCl2-KCl-KF-K2ZrF6-ZrO2熔盐体系中制备镁锆合金,通过对原料配比、电流密度和电解温度等电解工艺参数的研究,确定了采用熔盐电解法制备镁锆合金的较佳工艺条件。在较佳工艺条件下可得到锆的质量含量为0.8%的Mg-Zr合金。XRD分析结果表明合金中含有Mg相和Zr相。通过扫描电镜及EDS能谱分析可以看出锆元素在合金内部多以单质锆的形式存在,这与XRD的分析结果相一致,面扫描显示合金内部化学成分均匀。从合金的金相照片可以看出锆对镁合金的晶粒细化作用明显,品粒大小由100～2001μm细化到10～501μm。
其次,采用循环伏安法和计时电流法研究在低温熔融MgCl2-KCl熔盐体系中Mg2+、Zr(Ⅳ)和Zn2+离子在钼电极上的电化学还原过程。循环伏安法实验结果表明Mg2+、Zr(Ⅳ)和Zn2+离子在钼电极上的析出电位分别为：1.8V、1.3V和0.7V。通过计时电流法进一步证实了上述循环伏安的实验结果。
在MgCl2-KCl-KF-ZnCl2-K2ZrF6-ZrO2熔盐体系中制备镁锌锆合金,通过对电流密度和电解温度等电解工艺参数的研究,确定了熔盐电解法制备镁锌锆合金的较佳工艺条件。XRD分析结果表明合金中含有Mg相、Mg7Zn3相和Zr相。EDS分析表明Mg7Zn3合金化合物和单质锆在合金中均分布在晶界处。面扫描可以看出合金内部化学成分均匀。
Zirconium, which is one of the main alloying elements, exhibits obvious grain refining in the magnesium alloys. The traditional preparation methods mainly include metal casting and thermoreduction. Because of high melting point of zirconium metal and its low solubility in magnesium alloy, there are many disadvantages like complex technical operation and high production cost if use these two methods for preparation magnesium alloys containing zirconium. In this paper, we have studied preparation of Mg-Zr and Mg-Zn-Zr alloys in molten salt at low temperature. The formation process and electrochemical reduction mechanism have been investigated using these elements' compounds as raw materials.
Cyclic voltammetry, square wave voltammetry and other electrochemical methods have been used in the MgCl2-KCl-K2ZrF6 molten salt to investigate the reduction mechanism of Zr (Ⅳ) ion in the Mo cathode. Cyclic voltammetry results show that Zr (IV) ion reduction is two steps of electron transfer process and the addition of ZrO2 promote the reduction of Zr (Ⅳ) ions. For further study of the electron transfer process of Zr (IV) ion, quare wave voltammetry has been used to calculate the electron transfer number. The value of electron transfer number proves the reduction processes are Zr (IV)+2e= Zr (II); Zr (II)+2e= Zr.
In the MgCl2-KCl-KF-K2ZrF6-ZrO2 electrolysis system, the optimum conditions of proparation Mg-Zr alloys has been determined by investigation of the ratio of raw materials, current density and electrolysis temperature. The Mg-Zr alloy which is obtained in the optimal conditions contained 0.8% zirconium in the alloy. XRD analysis showed that these alloys contain Mg phase and Zr phase. Scanning electron microscopy and EDS spectrum analysis indicate that Zr element exist in the form of simple substance. This result is consistent with that of XRD analysis. The surface scanning show that internal chemical composition is homogeneous in the alloys. From metallographic photographs, we can see that Zr brings good grain refinement in magnesium alloys. The grain size was dwindled from 100-200μm to 10～50μm.
In another section, we have investigated electrochemical reduction process of Mg+2, Zr (IV) and Zn+2 ions in the Mo electrode by cyclic voltammetry and chronoamperometry in MgCl2-KCl melt at low temperature. The deposition potentials of Mg+2, Zr (IV) and Zn+2 ions on molybdenum electrode were detected at 1.8V,1.3V and 0.7V, respectively. Mg-Zn-Zr alloys are prepared by electrolysis in MgCl2-KCl-KF-ZnCl2-K2ZrF6-ZrO2 melt. The optimum proparation conditions have been determined by investigation of electrolytic parameters like current density and electrolysis temperature. In these alloys, Mg phase, Mg7Zn3 phase and Zr phase were observed by XRD. These phases Mg7Zn3 and Zr metal mainly exist in the grain boundaries. From surface scan we can see that the internal every chemical composition distribute homogeneity in the alloys.
引文
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