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结合碘化法与电子束熔炼法制备了纯度≥4N5的高纯Ti。碘化法是利用粗Ti在卤化区(温度为800~900K)的产物TiI4与粗Ti反应生成TiI2,同时在1 200~1 400K温度下使TiI2发生裂解反应。通过SEM、EDS、GDMS方法对制得的样品进行表面形貌、微区化学成分和杂质元素含量的分析。经过实验及热力学分析,确定了卤化区与裂解区的温度及杂质Cr、Ni存在的原因,为今后控制金属杂质含量,优化实验条件提供了理论依据。
High purity Ti with purity ≥4N5 was prepared by iodination and electron beam melting. Iodination is the use of crude Ti in the halogenation zone (temperature of 800 ~ 900K) product TiI4 and crude Ti reaction TiI2, while TiI2 at 1,200 ~ 1,400 K temperature cracking reaction occurred. The prepared samples were analyzed by SEM, EDS and GDMS methods to analyze the surface morphology, the chemical composition of micro-domains and the content of impurity elements. Through experimental and thermodynamic analysis, the causes of the existence of halide and impurity regions of Cr and Ni in the halogenated zone and the pyrolysis zone were determined, which provided a theoretical basis for controlling the content of metallic impurities and optimizing the experimental conditions in the future.