熔盐电解法制备铝钪锆合金.docVIP

doi: 10.3969/j.issn.2095-1744.2016.06.005 熔盐电解制备Al-Sc-Zr合金 钱 义，，， (北京科技大学 冶金与生态工程学院，北京 100083) 摘 要： 关键词：熔盐电解中图分类号：; TG164.4 文献标志码：A 文章编号：2095-1744(2016)06-0000-00 Molten Salt Electrolysis QIAN Yi, XUE Ji-lai, XIANG Xue-mei, GAO Xing-yu (School of Metallurgical and Ecological Engineering, University of Science and Technology Beijing, Beijing 100083, China) Abstract: Al-Sc-Zr alloy is prepared by molten salt electrolysis in Na3AlF6-4%MgF2-2%CaF2-Sc2O3-ZrO2 electrolyte system. The effect of oxide additive and electrolysis time on alloying element content is investigated. The effect of Sc and Zr content on the grain sizes of the alloys is studied by the optical microscope observation and Image J analysis software. The results indicate that Al-Sc-Zr alloys with Sc content of 0.186%~0.526% and Zr content of 0.116%~0.556% can be prepared by adjustment of the electrolysis condition. The grain sizes of the alloy is decreased with the increase of w(Sc)/w(Zr). The primary precipitate in the alloy is Al3(Sc, Zr) by the SEM-EDS analysis. The atomic ratio of Sc and Zr in the Al3(Sc,Zr) grains is corresponding to the content of Sc and Zr in the alloys. The effect of the precipitate with varying proportion of Sc and Zr atoms on the refinement of the microstructure is different. Key words: Al-Sc-Zr alloy; molten salt electrolysis; grain size; Al3(Sc,Zr) 钪稀土过渡族元素，最有效，添加微量能显著[4-6]，钪与其他过渡金属元素复合添加时。Al-Sc-Zr合金的主要制备Al-Sc中间合金和Al-Zr中间合金熔炼制。合金中钪锆分布均匀性较差。1实验方法 熔盐电解装置如图1所示。Φ15 mm小槽，盛放10 g铝为阴极。用Φ15 mm高纯石墨棒做阳极。将装有熔盐的坩埚置于电阻炉的恒温带之中，将热电偶、石墨阳极及阴极引线在炉盖上插好，将炉盖与炉子接触密封好。通入氩气，氩气流量为60 mL/min，完全把炉子中剩余的气体排出。温度到达960℃后，开始电解，电流密度为1 A/cm2。 电解结束后，将坩埚取出淬火，取出合金，对合金试样进行取样、磨样、抛光、浸蚀处理后拍摄金相照片，利用Image J图像分析软件分析晶粒尺寸。合金试样中的钪和锆含量由ICP-AES方法检测。 图1Fig.1 Scheme of experimental device electrolysis cell 1—不锈钢导杆；2—气体出口；3—水冷炉盖；4—热电偶；5—炉管；6—刚玉坩埚；7—石墨阳极；8—熔盐电解质；9—液态铝阴极；10—石墨坩埚；11—不锈钢导杆；12—气体入口 2试验结果与讨论 2.1ICP-AES检测结果。从表1可知，当电解质中ZrO2含量大于0.05%时，合金中的锆含量大于0.4%，这与目标合金成分相差较大。这是因为ZrO2的理论分解电压比Sc2O3的理论分解电压小，在施加电流后，ZrO2先分解成锆，随后Sc2O3分解出钪。随着