正向电压对氢化锆微弧氧化阻氢膜层性能的影响
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摘要
在偏铝酸钠-氢氧化钠-EDTA混合溶液中,采用恒压模式对氢化锆表面进行微弧氧化处理。借助场发射扫描电镜(FE-SEM)、X射线衍射仪(XRD)及真空脱氢实验,研究了不同正向电压(350~425 V)对微弧氧化膜层表面、截面、相结构及阻氢渗透性能的影响。分析结果表明:微弧氧化过程大致由阳极氧化、火花放电、微弧氧化和熄弧四个阶段组成。制备的膜层分为致密层和疏松层,致密层所占比例约为80%。随着正向电压的增大,晶粒尺寸增大,晶面间距减小,氢化锆表面微弧氧化膜层厚度由122μm增加至150μm,膜层的增长速度也随正向电压的增大而加快。但正向电压的改变对膜层的相结构并无显著影响,膜层由单斜相氧化锆和四方相氧化锆组成,当正向氧化电压为400 V时,氧化膜的PRF值达到最大值20。
Technology of micro-arc oxidation was applied on ZrH_(1.8) in the electrolyte composed of Na AlO_2+NaOH+ Na2 EDTA in constant voltage mode. The film was characterized by field emission scanning electron microscope(FE-SEM), X-ray diffraction(XRD), and vacuum dehydrogenation experiment, respectively. The influences of anode voltage(350 to 425 V) on surface and cross-sectional morphology, structure, and hydrogen resistance properties of the hydrogen resistance film on the surface of ZrH_(1.8) were investigated. The micro-arc oxidation process can be divided into four stages: anodic oxidation, spark discharge, micro-arc oxidation and flameout. The results reveal that film obtained in the electrolyte is composed of inner dense layer and outer loose layer, and proportion of the dense layer is about 80%. Grain sizes and growth rate of the film increase while the d-spacing decreases with the increase of the anode voltage, and the thickness of the film is increased from 122 to 150 μm. However, anode voltage has no obvious influence on the structure of the film. The prepared film is composed of M-ZrO_2 and T-ZrO_2. When the anode voltage is 400 V, the permeation reduction factor value reaches the maximum of 20.
Technology of micro-arc oxidation was applied on ZrH_(1.8) in the electrolyte composed of Na AlO_2+NaOH+ Na2 EDTA in constant voltage mode. The film was characterized by field emission scanning electron microscope(FE-SEM), X-ray diffraction(XRD), and vacuum dehydrogenation experiment, respectively. The influences of anode voltage(350 to 425 V) on surface and cross-sectional morphology, structure, and hydrogen resistance properties of the hydrogen resistance film on the surface of ZrH_(1.8) were investigated. The micro-arc oxidation process can be divided into four stages: anodic oxidation, spark discharge, micro-arc oxidation and flameout. The results reveal that film obtained in the electrolyte is composed of inner dense layer and outer loose layer, and proportion of the dense layer is about 80%. Grain sizes and growth rate of the film increase while the d-spacing decreases with the increase of the anode voltage, and the thickness of the film is increased from 122 to 150 μm. However, anode voltage has no obvious influence on the structure of the film. The prepared film is composed of M-ZrO_2 and T-ZrO_2. When the anode voltage is 400 V, the permeation reduction factor value reaches the maximum of 20.
引文
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[3]ALLEN G B,KERR M,DAYMOND M R.Measurement and modeling of strain fields in zirconium hydrides precipitated at a stress concentration.Journal of Nuclear Materials,2012,430(1/2/3):27–36.
[4]HAYASHI T,TOBITA K,NAKAMORI Y,et al.Advanced neutron shielding material using zirconium borohydride and zirconium hydride.Journal of Nuclear Materials,2009,386(2):386–388.
[5]OLANDER D,GREENSPAN E,GARKISCH H D,et al.Uranium–zirconium hydride fuel properties.Nuclear Engineering and Design,2009,239(8):1406–1424.
[6]KUMAR NAPK,SZPUNAR J A,HE Z.Preferential precipitation of hydrides in textured zircaloy-4 sheets.Journal of Nuclear Materials,2010,403(1/2/3):101–107.
[7]OLANDER D.Nuclear fuels–present and future.Journal of Nuclear Materials,2009,389(1):1–22.
[8]LIU X Z,HUANG Q R,DU J J,et al.Study on permeation of hydrogen through HR-1 austenitic stainless steel with Cr2O3 and Ti N thin film coatings.Chinese Journal of Nuclear Science and Engineering,1997,17(3):281–284.
[9]MA H R,FU X G,QIN B.Research on prevention method of hydrogen release of zirconium hydride at high temperature.Atomic Energy Science and Technology,2016,50(11):2023–2026.
[10]CHEN Y L,XUE Z G,WANG Q,et al.New findings on properties of plasma electrolytic oxidation coatings from study of an Al-Cu-Li alloy.Electrochimica Acta,2013,107(3):358–378.
[11]CHEN M A,OU Y C,YU C Y,et al.Corrosion performance of epoxy/BTESPT/MAO coating on AZ31 alloy.Surface Engineering,2016,32(1):38–46.
[12]XIONG W M,NING C Y,GU Y H,et al.Effect of positive voltage on phase structure of micro-arc oxidation films of magnesium alloy.Rare Metal Materials and Engineering,2011,40(12):2236–2240.
[13]KHANMOHAMMADI H,ALLAHKARAM S R,TOWHIDI N,et al.Preparation of PEO coating on Ti6Al4V in different electrolytes and evaluation of its properties.Surface Engineering,2016,32(6):448–456.
[14]MARTIN J,LEONE P,NOMINE A,et al.Influence of electrolyte ageing on the plasma electrolytic oxidation of aluminium.Surface and Coatings Technology,2015,269(1):36–46.
[15]CHEN M,MA Y Z,MA Y,et al.Effects of voltage increment on performances of micro-arc oxidation coatings of magnesium alloys.Rare Metal Materials and Engineering,2010,39(11):1943–1947.
[16]ABBASI S,BAYATI M R,GOLESTANI F F,et al.Micro arc oxidized HAp–Ti O2 nanostructured hybrid layers-part I:effect of voltage and growth time.Applied Surface Science,2011,257(14):5944–5949.
[17]WANG S,GUO F,LIU L,et al.Effect of process parameters on thickness and morphology of micro-arc oxidation ceramic coating of zirconium alloy.Rare Metal Materials and Engineering,2008,37(8):1466–1470.
[18]XUE W B,JIN Q,ZHU Q Z,et al.Preparation and properties of ceramic coating formed by microarc oxidation on zirconium alloy.Transactions of Materials and Heat Treatment,2010,31(2):119–122.
[19]吴汉华.铝、钛合金微弧氧化陶瓷膜的制备表征及其特性研究.长春:吉林大学博士学位论文,2004.
[20]FANG D R,WANG J H,YANG J,et al.Electrolyte optimization of microarc oxidation of magnesium alloy.Transactions of Materials and Heat Treatment,2004,25(5b):1072–1075.
[21]ZHONG X K,YAN G Q,CHEN W D,et al.Effect of Na5P3O10addition on the MAO coating on the surface of Zr H1.8.Rare Metal Materials and Engineering,2012,41(S2):541–544.
[22]HE J,YE J,LAVERNIA E J,et al.Quantitative analysis of grain size in bimodal powders by X-ray diffraction and transmission electron microscopy.Journal of Materials Science,2004,39(23):6957–6964.
[23]YANG G L,LV X Y,BAI Y Z,et al.The effects of current density on the phase composition and microstructure properties of microarc oxidation coating.Journal of Alloys and Compounds,2002,345(1/2):196–200.
[24]王俐艳.CO2反应法制备氢化锆表面氢渗透阻挡层的研究.成都:西华大学博士学位论文,2007.
[25]YAN S F,LIU X D,CHEN W D,et al.Influence of oxidation time on MAO film on the surface of Zr H1.8 in a phosphate system.Rare Metal Materials and Engineering,2014,43(7):1717–1721.