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熔盐电化学法制备Fe-6.5wt%Si合金的研究

Research on Fe-6.5wt%Si Alloy Made by Electrolyte in Molten Salt

【作者】 王福佳

【导师】 杨海丽;

【作者基本信息】 河北理工大学 , 材料加工工程, 2009, 硕士

【摘要】 利用正交法研究了不同熔盐的摩尔配比、电流密度、电流的占空比和脉冲周期对硅沉积层的厚度与质量的影响规律,得到了最佳的电沉积工艺参数:熔盐的摩尔比1:1:3:0.3,电流密度60mA/cm2,占空比20%,脉冲周期1000μs。SEM表明:电流密度、电流占空比和脉冲周期对镀层质量具有重要影响。此外,施加反向电流对镀层质量也有一定的影响。对沉积层的硅含量分布曲线研究表明:沉积过程中,硅的扩散符合恒定源扩散规律;对沉积后试样的扩散退火研究发现:沉积50min的试样均匀化扩散退火需60min,退火后的硅含量为3.3%。采用GDA750型辉光放电光谱仪测量硅含量沿镀层厚度方向的分布曲线,然后利用ORIGIN软件求其积分的方法,来计算沉积层中总的含硅量。此方法计算出的试样退火后的理论硅含量与实验得到硅含量误差在10%内。对基体电沉积80min,在1200℃和94.4%Ar+5.6%H2的还原气氛下扩散退火110 min,成功制备出了硅含量为6.5%的铁硅合金。在FClNaK-SiO2体系中熔盐电沉积硅,采用脉冲电流比普通直流电源具有更好的镀层质量。FClNaK-SiO2体系中,采用电沉积法制备Fe-6.5wt%Si合金是切实可行的,且有更低的制作成本。该方法有工艺简单、操作方便和有利于环保的优点,将具有较好的应用前景。

【Abstract】 The molar ratio of molten salt, the current density, current duty ratio and the influence of the pulse interval on the thickness and the quality of the silicon deposition layer have been studied by orthogonal method, electro-deposition process parameter was obtained: the molar ratio of molten salt is 1:1:3:0.3, current density is 60 mA/cm2, duty ratio is 20%, the pulse interval is 1000μs. The SEM of deposit indicated that: the coating quality is obvious influenced by current density, duty ratio and the pulse interval, the deposit quality is also influenced by back current.The result of the distribution curve of silicon content in the silicon deposition indicates that the diffusion of silicon in deposition matches constant current diffusion rule in the process of deposition. The research of diffusion annealing on post-depositional specimen shows that: 60 minutes are needed to homogenization diffusion anneal for depositing the 50min test specimen homogenization diffusion annealing, and the silicon content approximately is about 3.3% after annealing.Survey the silicon content distribution curve by glow discharge spectrometer in this article and associate with integral method to calculate the content of silicon in deposition, the error is in 10%.After 80 minutes electro-deposition on the base, and diffusion annealing 110 minutes under 94.4%Ar+5.6%H2 reducing atmosphere at 1200℃,the ferro-silicium which the silicon content is 6.5% was made out.In the FClNaK-SiO2 system, the coating is influenced by the impulse current which is better than the ordinary direct constant source electric current treatment. In the FClNaK-SiO2 system, it is a feasible method to make Fe-6.5wt%Si alloy by electro-deposition process, and the cost of electro-deposition silicon in molten salt is low. This method will have good prospect because of simple, handing convenience and environmental protection.

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