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FeAl/Al2O3阻氚层的制备新方法与性能
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国家磁约束聚变项目(2010GB112000)


A New Preparing Method and Performances of FeAl/Al2O3 Tritium Permeation Barrier
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    摘要:

    采用室温熔盐电镀-热处理-氧化复合新技术在HR-2不锈钢上制备FeAl/Al2O3涂层,研究热处理温度与时间的影响,并表征涂层的形貌和性能。结果表明:25 ℃下,采用AlCl3-MEIC(氯化1-甲基3-乙基咪唑)室温熔盐在HR-2钢表面获得结合良好的纯铝镀层,电沉积速率为15 μm/h。650~750 ℃热处理1~30 h, 在HR-2钢表面制得成分渐变、冶金结合、无缝隙与裂纹的3~27 μm铝化物涂层,涂层截面为3层或2层结构;涂层生长速率与热处理温度的关系符合Arrhenius公式,活化能为116.9 kJ/mol;涂层的形成过程受原子扩散过程控制,其厚度随热处理时间变化呈抛物线关系。700 ℃,4 h热处理涂层在10-2 Pa O2中继续氧化80 h后,最终涂层由约30 μm厚的FeAl扩散层及约110 nm的γ-A12O3膜组成,600 ℃下该涂层使HR-2不锈钢的氘渗透率降低3个数量级;涂层可抗750 ℃~室温冷热循环20次以上。该方法有望成为ITER中氚包容容器表面阻氚层的候选制备新方法。

    Abstract:

    A new three-step method for preparing aluminum rich coating on HR-2 stainless steel was proposed, i.e. ambient temperature chloroaluminate melts electroplating followed by heat treating and artificial oxidation. In the electroplating process, aluminum deposition from AlCl3/MEIC to the surface of HR-2 steel was performed with a deposition rate of 15 μm/h. Within the aluminizing temperature range from 650 to 750 oC, aluminizing time from 1 to 30 h, the aluminized coating with thickness of 3-27 μm can be prepared, which is homogeneous and free of porosity or crack, and have good metallographic adherence to the substrate; the coating cross section exhibits a three-layer or two-layer structure. A simple Arrhenius relationship can be used to describe the effect of temperature on the coating growth rate, which gives activation energy of 116.9 kJ/mol. The relationship between the coating thickness against time1/2 is approximately linear, which is a typical feature of the diffusion controlled coating growth mechanism. To form Al2O3 film on surface, the aluminized coating treated for 4 h was oxidized in 10-2 Pa O2 for 80 h and observed by X-ray photoelectron spectroscopy (XPS) and Reflection spectrum. The finally fabricated coating shows a double-layer structure consisting of an outer γ-A12O3 layer with thickness of 110 nm and inner (Fe,Cr,Mn and Ni)Al/(Fe,Cr,Mn and Ni)3Al layer of 30 μm thickness, and is homogeneous without any defects. The deuterium permeation rate through the coated HR-2 steel is reduced by 3 orders of magnitude at 600 oC. The coating remains a perfect surface for 20 thermal cycles between 750 oC and room temperature. The method is a potential candidate for preparation of TPB on the tritium container surface in ITER.

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张桂凯,李 炬,陈长安,黄志勇,凌国平. FeAl/Al2O3阻氚层的制备新方法与性能[J].稀有金属材料与工程,2011,40(6):1120~1124.[Zhang Guikai, Li Ju, Chen Chang’an, Huang Zhiyong, Ling Guoping. A New Preparing Method and Performances of FeAl/Al2O3 Tritium Permeation Barrier[J]. Rare Metal Materials and Engineering,2011,40(6):1120~1124.]
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  • 收稿日期:2010-08-28
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