LY12铝合金表面微弧氧化膜层制备及热阻隔应用研究
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摘要
随着航天、航空工业中各种飞行器飞行速度不断提高,服役环境越来越恶劣,飞行器表面气动加热和热冲击问题十分突出。飞行器用材料要求具有足够高的强度和刚度,通常作为结构材料的铝合金难以承受如此高的热载荷,而限制了铝合金的广泛应用。因此必须对其表面进行热防护处理。微弧氧化技术在金属表面原位生长陶瓷膜,可以制备高结合强度、优良热稳定性和耐热冲击性能的膜层。本文针对微弧氧化膜层的上述特点,制备优良热阻隔性能的膜层。
本文首先选定了硅酸钠体系做为制备热阻隔膜层的电解液体系。研究了不同反正向电流比j-/j+对微弧氧化电特性、生长速率及能耗的影响。结果显示:反向电流对放电过程产生调制作用,柔化了放电过程,提高了膜层的生长速率,降低了膜层的单位能耗。通过向电解液中添加氟锆酸钾的方式,大大提高了膜层生长速率,较Na_2SiO_3-KOH体系单位能耗大大降低,随着K2ZrF6浓度的提高,膜层生长速率提高,单位能耗降低。
通过SEM及附带的能普和XRD测试分析了膜层的形貌、成分和结构。在Na_2SiO_3-KOH体系中,反向电流对微弧放电产生了柔化作用,对膜层的形貌、结构、成分产生了影响,使膜层的致密度提高。当j-/j+=0.5时,膜层中大缺陷消失,孔洞尺寸小,分布均匀,膜层质量最好,并使得膜层的晶体峰明显减少,非晶相增多。Na_2SiO_3-K_2ZrF_6-KOH体系中,反向电流的引入,改善了j-/j+=0时放电通道残留的孔洞尺寸,表面形成的“圆饼”尺寸小。截面形貌显示,与Na_2SiO_3-KOH体系中制备的膜层相比,膜层质量较好,且反向电流引入之后,膜层中的晶体相含量提高。各浓度下膜层的形貌和结构相差不大,膜层由内向外,Si和Zr元素含量逐渐升高。
经微弧氧化处理之后,铝合金的拉伸性能基本上没有受到影响;耐磨性能提高,有效地保护了铝合金基体。热冲击测试显示,膜层与基体结合良好。对比分析可知,反向电流的引入提高了膜层与基体的结合力。LY12铝合金经微弧氧化处理之后,抗高温氧化性能提高。火焰烧蚀测试结果显示,微弧氧化膜层提高了LY12铝合金基体的抗火焰烧蚀能力。Na_2SiO_3-KOH体系中不同j-/j+对膜层隔热性能的研究表明,j-/j~+=0.5时膜层的隔热性能最好,15 min之后温度为180℃,比基体15 min之后的212℃低32℃。电解液中K_2ZrF_6的引入提高膜层的隔热性能。当K_2ZrF_6浓度为7 g/L厚度为90μm的膜层隔热性能最好,15 min后比基体温度低45. 5℃。
With the increasing need of high flight speed in space industry and aircraft industry, the components frenquently work in the harsh environment and temperature-rise and thermal shock on aerocrafts surface are quite severe, thus enough strength and rigidity of the utilized materials are necessary. Aluminum alloys, frequently as structural material of aerocrafts, can not bear such high heat effects and widely limited in the high-speed applications. Consquently thermal protection process is required. The micro-arc oxidation (MAO) technique, by which a compound ceramic coating grows in situ on Al, Ti, Mg and many other valve-metals directly, has been developed rapidly in recent years. The MAO coatings exhibit excellent combination of extremely high adhesion, thermal stability and thermal shock. In view of the features above, Coatings with excellent thermal resistance performance are expected to fabricate using MAO technics.
Silicate system is chosen to prepare heat resistance coatings. The influence of different current ratio j-/j~+ (j- reprents the reverse current desity and j~+ reprents the positive current desity) on electric characteristics, growth rate and power consumption has been studied. The results show that the reverse current results in a“softer”effect on micro-discharges. The growth rate has been improved and the power consumption is reduced. By introducing K_2ZrF_6 to the solution, the growth rate is promoted greatly with lower power consumption.
Micro-structure, element distribution and phase composition has been analyzed using SEM, EDS and XRD respectively. In Na_2SiO_3-KOH solution, the reverse current, which affects micro-structure and phase composition by changing discharge characteristics, improves the density of MAO coatings with fewer large-scale defects. Micro-discharges may be interrupted suddenly when the reverse current is applied, so melt materials cool very rapidly without crystallizing. This may reduce the number of crystal peaks. In Na_2SiO_3- K_2ZrF_6-KOH solution, the discharge channel and pancake become small. The MAO coatings are of good quality prepared in Na_2SiO_3- K_2ZrF_6-KOH solution compared with that produced in Na_2SiO_3-KOH solution. The reverse current also improves the quality of MAO coatings and increases the concentration of crystal phase. The content of Si and Zr gradually increase towards the external surface of MAO coatings.
Tensile strength of aluminum substrates rarely changes and anti-wear performance has been enhanced after MAO process. This may protect LY12 aluminium alloy from severe wear.
The thermal shock experiment shows high adhesion between substrate and coatings. Coatings prepared in Na_2SiO_3-K_2ZrF_6-KOH solution have higher adhesion, due to the effect of the reverse current. In the high temperature oxidation experiment the weight of the control samples increases quickly at the beginning and then slowly with increasing oxidation time. In contrast, the weight of the samples with MAO coatings decreases and then keeps unchangeable. Flame ablation experiment shows the MAO coatings may effectively protect substrates from flame ablation, j-/j~+ of 0.5 leads to the best heat insulation performance of coatings fabricated in Na_2SiO_3-KOH solution. By introducing K_2ZrF_6 to the solution, the heat insulation performance is improved. The 90μm coatings produced with the K_2ZrF_6 concentration of 7 g/L has the best heat insulation properties, i.e. the temperature on the surface is lower 45.5℃than that of untreated samples after 15 min exposure to 500℃.
本文首先选定了硅酸钠体系做为制备热阻隔膜层的电解液体系。研究了不同反正向电流比j-/j+对微弧氧化电特性、生长速率及能耗的影响。结果显示:反向电流对放电过程产生调制作用,柔化了放电过程,提高了膜层的生长速率,降低了膜层的单位能耗。通过向电解液中添加氟锆酸钾的方式,大大提高了膜层生长速率,较Na_2SiO_3-KOH体系单位能耗大大降低,随着K2ZrF6浓度的提高,膜层生长速率提高,单位能耗降低。
通过SEM及附带的能普和XRD测试分析了膜层的形貌、成分和结构。在Na_2SiO_3-KOH体系中,反向电流对微弧放电产生了柔化作用,对膜层的形貌、结构、成分产生了影响,使膜层的致密度提高。当j-/j+=0.5时,膜层中大缺陷消失,孔洞尺寸小,分布均匀,膜层质量最好,并使得膜层的晶体峰明显减少,非晶相增多。Na_2SiO_3-K_2ZrF_6-KOH体系中,反向电流的引入,改善了j-/j+=0时放电通道残留的孔洞尺寸,表面形成的“圆饼”尺寸小。截面形貌显示,与Na_2SiO_3-KOH体系中制备的膜层相比,膜层质量较好,且反向电流引入之后,膜层中的晶体相含量提高。各浓度下膜层的形貌和结构相差不大,膜层由内向外,Si和Zr元素含量逐渐升高。
经微弧氧化处理之后,铝合金的拉伸性能基本上没有受到影响;耐磨性能提高,有效地保护了铝合金基体。热冲击测试显示,膜层与基体结合良好。对比分析可知,反向电流的引入提高了膜层与基体的结合力。LY12铝合金经微弧氧化处理之后,抗高温氧化性能提高。火焰烧蚀测试结果显示,微弧氧化膜层提高了LY12铝合金基体的抗火焰烧蚀能力。Na_2SiO_3-KOH体系中不同j-/j+对膜层隔热性能的研究表明,j-/j~+=0.5时膜层的隔热性能最好,15 min之后温度为180℃,比基体15 min之后的212℃低32℃。电解液中K_2ZrF_6的引入提高膜层的隔热性能。当K_2ZrF_6浓度为7 g/L厚度为90μm的膜层隔热性能最好,15 min后比基体温度低45. 5℃。
With the increasing need of high flight speed in space industry and aircraft industry, the components frenquently work in the harsh environment and temperature-rise and thermal shock on aerocrafts surface are quite severe, thus enough strength and rigidity of the utilized materials are necessary. Aluminum alloys, frequently as structural material of aerocrafts, can not bear such high heat effects and widely limited in the high-speed applications. Consquently thermal protection process is required. The micro-arc oxidation (MAO) technique, by which a compound ceramic coating grows in situ on Al, Ti, Mg and many other valve-metals directly, has been developed rapidly in recent years. The MAO coatings exhibit excellent combination of extremely high adhesion, thermal stability and thermal shock. In view of the features above, Coatings with excellent thermal resistance performance are expected to fabricate using MAO technics.
Silicate system is chosen to prepare heat resistance coatings. The influence of different current ratio j-/j~+ (j- reprents the reverse current desity and j~+ reprents the positive current desity) on electric characteristics, growth rate and power consumption has been studied. The results show that the reverse current results in a“softer”effect on micro-discharges. The growth rate has been improved and the power consumption is reduced. By introducing K_2ZrF_6 to the solution, the growth rate is promoted greatly with lower power consumption.
Micro-structure, element distribution and phase composition has been analyzed using SEM, EDS and XRD respectively. In Na_2SiO_3-KOH solution, the reverse current, which affects micro-structure and phase composition by changing discharge characteristics, improves the density of MAO coatings with fewer large-scale defects. Micro-discharges may be interrupted suddenly when the reverse current is applied, so melt materials cool very rapidly without crystallizing. This may reduce the number of crystal peaks. In Na_2SiO_3- K_2ZrF_6-KOH solution, the discharge channel and pancake become small. The MAO coatings are of good quality prepared in Na_2SiO_3- K_2ZrF_6-KOH solution compared with that produced in Na_2SiO_3-KOH solution. The reverse current also improves the quality of MAO coatings and increases the concentration of crystal phase. The content of Si and Zr gradually increase towards the external surface of MAO coatings.
Tensile strength of aluminum substrates rarely changes and anti-wear performance has been enhanced after MAO process. This may protect LY12 aluminium alloy from severe wear.
The thermal shock experiment shows high adhesion between substrate and coatings. Coatings prepared in Na_2SiO_3-K_2ZrF_6-KOH solution have higher adhesion, due to the effect of the reverse current. In the high temperature oxidation experiment the weight of the control samples increases quickly at the beginning and then slowly with increasing oxidation time. In contrast, the weight of the samples with MAO coatings decreases and then keeps unchangeable. Flame ablation experiment shows the MAO coatings may effectively protect substrates from flame ablation, j-/j~+ of 0.5 leads to the best heat insulation performance of coatings fabricated in Na_2SiO_3-KOH solution. By introducing K_2ZrF_6 to the solution, the heat insulation performance is improved. The 90μm coatings produced with the K_2ZrF_6 concentration of 7 g/L has the best heat insulation properties, i.e. the temperature on the surface is lower 45.5℃than that of untreated samples after 15 min exposure to 500℃.
引文
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67 R. Arrabal, E. Matykina, T. Hashimoto, et al. Characterization of AC PEO coatings on magnesium alloys, Surface and Coatings Technology. 2009, 203(16): 2207~2220
68 Magurova. Yu V, Timoshenko.A V Zashch. Met. 1995 (31):414 (in Russian) (for English translation see Prot. Met. ISSN 0033~1732)
69 A L Yerokhin, L O Snizhko, N L Gurevina et al. Discharge characterization in plasma electrolytic oxidation of aluminium. Journal of Physics D: Applied. Physics. 2003, 36: 2110~2120
70 L.Dujardin, A.Viola, J.Beauvir. Tailored aluminium oxide layers by bipolar current adjustment in the Plasma Electrolytic Oxidation (PEO) process. Surface and Coating Technology. 2007, 201:8677~8682
71 Xuetong Sun, Zhaohua Jiang, Zhongping Yao et al. The effects of anodic and cathodic processes on the characteristics of ceramic coatings formed on titanium alloy through the MAO coating technology. Applied Surface Science. 2005, 252: 441~447
72 Shigang Xin, Lixin Song, Ronggen Zhao et al. Influence of cathodic current on composition, structure and properties of Al2O3 coatings on aluminum alloy prepared by micro-arc oxidation process. Thin Solid Films. 2006, 515:326 ~332
73骆海贺. AZ91D镁合金微弧氧化ZrO2-Y2O3复合陶瓷膜层的制备表征及性能研.华中科技大学博士论文. 2009:23
74张欣盟,陈东方,巩春志,等. K2ZrF6添加对LY12铝合金微弧氧化膜层结构调制及隔热性能影响,无机材料学报, 1000-324X(2010)01-0000-06
75 Zhong ping Yao, Zhao hua Jiang, Xue tong Sun, et al. Influences of current density on structure and corrosion resistance of ceramic coating sonTi-6Al-
4V alloy by micro-plasma oxidation, Thin Solid Films. 2004, 468:120~125
76陈宏,郝建民.负脉冲对铝合金微弧氧化膜耐蚀性影响的研究,材料保护. 2007, 40(9):17~19
77 S. Moon, Y. Jeong. Generation mechanism of microdischarges during plasma electrolytic oxidation of Al in aqueous solutions. Corrosion Science. 2009, (51): 1506~1512
78 Wenbin Xue, Zhiwei Deng, Ruyi Chen et al. Growth regularity of ceramic coatings formed by microarcoxidation on Al-Cu-Mg alloy. Thin Solid Films. 2000, 372:114~117
79 XiShu Wang, XiQiao Feng, XingWu Guo. Failure behavior of anodized coating-magnesium alloy substrate structures. Key Engineering Materials Vols. 2004, 261-263:363~368
80 K. Wu, Y.Q. Wang, M.Y. Zheng. Effects of microarc oxidation surface treatment on the mechanical properties of Mg alloy and Mg matrix composites. Materials Science and Engineering A. 2007, 447: 227~232
81 P.A. Dearnley, J. Gummersbach, H. Weiss, et al. The sliding wear resistance and frictional characteristics of surface modified aluminium alloys under extreme pressure. Wear, 1999, (225–229): 127~134
82 Yongjun Xu, Zhongping Yao, Fangzhou Jia et al. Preparation of PEO ceramic coating on Ti alloy and its high temperature oxidation resistance. Current Applied Physics, 2010, 10:698~702