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FeAl/Al2O3阻氚層的制備新方法與性能
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國家磁約束聚變項目(2010GB112000)


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

    采用室溫熔鹽電鍍-熱處理-氧化復(fù)合新技術(shù)在HR-2不銹鋼上制備FeAl/Al2O3涂層,研究熱處理溫度與時間的影響,并表征涂層的形貌和性能。結(jié)果表明:25 ℃下,采用AlCl3-MEIC(氯化1-甲基3-乙基咪唑)室溫熔鹽在HR-2鋼表面獲得結(jié)合良好的純鋁鍍層,電沉積速率為15 μm/h。650~750 ℃熱處理1~30 h, 在HR-2鋼表面制得成分漸變、冶金結(jié)合、無縫隙與裂紋的3~27 μm鋁化物涂層,涂層截面為3層或2層結(jié)構(gòu);涂層生長速率與熱處理溫度的關(guān)系符合Arrhenius公式,活化能為116.9 kJ/mol;涂層的形成過程受原子擴散過程控制,其厚度隨熱處理時間變化呈拋物線關(guān)系。700 ℃,4 h熱處理涂層在10-2 Pa O2中繼續(xù)氧化80 h后,最終涂層由約30 μm厚的FeAl擴散層及約110 nm的γ-A12O3膜組成,600 ℃下該涂層使HR-2不銹鋼的氘滲透率降低3個數(shù)量級;涂層可抗750 ℃~室溫冷熱循環(huán)20次以上。該方法有望成為ITER中氚包容容器表面阻氚層的候選制備新方法。

    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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張桂凱,李 炬,陳長安,黃志勇,凌國平. FeAl/Al2O3阻氚層的制備新方法與性能[J].稀有金屬材料與工程,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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