铝合金表面原位生长陶瓷膜及摩擦磨损与耐蚀研究
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摘要
针对铝合金耐磨、耐蚀性差等问题,利用双相脉冲微弧氧化电源在铝合金表面原位生长陶瓷膜,研究了不同铝合金基体氧化铝陶瓷膜组成、结构及性能;系统研究了LY12铝合金微弧氧化黑色氧化铝和氧化锆复合陶瓷膜的组成,结构及性能,探讨了合金成分对微弧氧化陶瓷膜结构、性能和颜色的影响及不同电解液体系下的氧化锆陶瓷膜的成膜机制;建立陶瓷膜抗热弹性形变应力模型,分析热冲击循环过程热应力的变化;运用加速电化学腐蚀的方法评价了三种电解液体系陶瓷膜的耐腐蚀性;研究了三种电解液体系陶瓷膜的摩擦行为。
利用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、电子探针(EPMA)、能谱(EDS)和X射线光电子能谱仪(XPS)研究膜层的相组成、形貌、元素分布和元素价态变化;利用加速的电化学方法评价膜层的耐腐蚀性;利用显微硬度仪研究膜层硬度的变化特点;利用球盘式滑动干摩擦仪(Si3N4球为摩擦副),研究铝合金和陶瓷膜的磨损率和摩擦系数。
纯Al和LC9微弧氧化膜分别由α-Al_2O_3和γ-Al_2O_3组成,LY12膜层由大量γ-Al_2O_3和少量α-Al_2O_3组成。膜层抗热震性按LC9、LY12、Al依次增强;耐腐蚀性能和与基体结合强度按Al、LC9、LY12依次增强;纯Al、LY12和LC9膜层的硬度最大值分别为33.4GPpa、22.15GPa和16.8GPa。在Na5P3O10-CrO3溶液中,LY12铝合金微弧氧化可制得黑色陶瓷膜层,膜层的Cr氧化数为0、+3价、+6,并且以非晶态存在,CrO3能促进γ-Al_2O_3向α-Al_2O_3转化、提高成膜速率、硬度、致密性及耐蚀性。
在K_2ZrF_6-NaH_2PO_2溶液中,LY12铝合金微弧氧化陶瓷膜主要由m-ZrO2、t-ZrO2和γ-Al_2O_3组成。负相电流密度增加导致电解液体系状态发生改变,使得膜层增厚及消除KZr_2(PO_4)_3相;膜层的最大努普硬度可达16.75GPa,与基体结合强度大于17.5MPa;增加NaH_2PO_2浓度均可提高膜层的耐点腐蚀性能。在NaAlO2-K_2ZrF_6电解液中,陶瓷膜主要由γ-Al_2O_3、α-Al_2O_3和少量的c-ZrO2;少量的K_2ZrF_6能加速膜层生长、致密性提高、促进γ-Al_2O_3向α-Al_2O_3转化及硬度的增大,改善了膜层的耐腐蚀性能;膜层的最大努普硬度达23.41GPa。
微弧氧化陶瓷膜一个热冲击循环经历升温、保温和降温3个阶段。K_2ZrF_6-NaH_2PO_2电解液体系陶瓷膜加热过程应力由0迅速达到575Mpa,然后缓慢变为780MPa,冲击循环38次以上出现起皮脱落;NaAlO2-K_2ZrF_6电解液体系陶瓷膜加热过程应力由0迅速达到558Mpa,然后缓慢变为994 MPa ,降温过程为升温过程的逆过程热,热冲击循环次数29次以上出现起皮剥落。
微弧氧化陶瓷膜的耐磨性同LY12铝合金相比较显著提高。K_2ZrF_6-NaH_2PO_2体系制备的膜层(载荷150g)最小磨损率为1.61×10-6g/min、摩擦系数在0.35-0.367之间变化,磨损过程由开始阶段的粘着磨损逐步过渡至脆性断裂。NaAlO2-K_2ZrF_6体系制备的膜层(载荷300g )磨损率为4.33×10-6g/min、摩擦系数最小为0.214;磨损过程由磨料磨损逐步过渡至磨料磨损和裂疲劳磨损,该体系陶瓷膜耐磨减磨效果最好。Na5P3O10-CrO3体系制备的膜层(载荷100g)磨损率为2.1×10-5g/min、摩擦系数0.306;摩擦过程表现为一定程度的塑性变形导致的光滑磨损和脆性断裂。
In order to solve the poor wear and corrosion properties, the oxide ceramic coatings were formed in-situ on aluminium alloys using the bi-pulsed micro-arc oxidation (MAO) power. The composition, structure and performance of the oxide coatings formed on different aluminium alloys were studied. The study was also conducted on the composition, structure and mechanical performance of black ceramic coating consisting of alumina and zirconia, respectively. The effect of alloy components on the structure, color and properties was discussed. The in-situ growth mechanism of oxide ceramic coatings was discussed in different electrolytes. The model of ceramic coatings’resistance to heat shock was established and used to analyze the variation of heat stress during the cycles of heat shock. The corrosion resistance, the friction behavior and wear mechanism of three kinds of coatings were estimated and discussed.
The X-ray diffraction (XRD), scanning electron microscope (SEM), electrode probe microscope analysis (EPMA), energy dispersive spectroscopy (EDS) and X-ray photoelectron spectroscope (XPS) were used to study the composition, morphology, the element distribution and variation of element valence. The corrosion resistance was studied by electrochemical methods. The coating hardness was measured by micro-hardness instrument. The wear lost and friction coefficient of aluminium alloys and ceramic coatings were studied by a ball-on-disk tester under the dry sliding conditions.
It was shown that the MAO coating formed on pure aluminium and LC9 consisted ofα-Al_2O_3 andγ-Al_2O_3, respectively. The coating formed on LY12 was composed of large numbers ofγ-Al_2O_3 and littleα-Al_2O_3. The heat shock resistance was increased by the followed orders: LC9﹤LY12﹤Al, and the corrosion resistance was increased by the subsequence of Al, LC9 and LY12. Coatings’maximal hardness of Al, LY12 and LC9 were 33.4 MPa, 22.15 MPa and 16.8 MPa, respectively. The black Al_2O_3 ceramic coating was prepared on LY12 aluminium alloys in solution of Na5P3O10-CrO3. The chromium was not crystal and had the valence of 0, +3, +6. CrO3 benefited to the transformation ofγ-Al_2O_3 toα-Al_2O_3 and increased the growth, hardness, thickness and corrosion resistance, and improved the compactness.
The coating consisting of m-ZrO2、t-ZrO2、γ-Al_2O_3 was prepared on LY12 in K_2ZrF_6-NaH_2PO_2. The proper increase of negative current density was in favor of the thickness increase of the coating and eliminated KZr2(PO3)3. The maximum of Knoop hardness could reach 16.75Gpa. The adherent strength of coating to substrate was beyond 17.5Mpa. Increasing the concentration of NaH_2PO_2 could improve the dot-corrosion resistance of the coating. The coating was mainly composed ofγ-Al_2O_3、α-Al_2O_3 and a little c-ZrO2. A small quantity of K_2ZrF_6 accelerated the coating growth and increased the compactness, promoted the transformation fromγ-Al_2O_3 toα-Al_2O_3 and consequently improved the corrosion resistance. The maximum Knoop hardness could reach 23.41Gpa.
The heat shock cycle experiment includes three stages: heat uprising, heat preservation and heat decreasing. During the heat shock process, the stress prepared in K_2ZrF_6-NaH_2PO_2 was increased quickly to 575Mpa, and then up to 780 MPa slowly, and there was no strip peered off after 38 cycles of heat shock. The heat stress of coating prepared in NaAlO2-K_2ZrF_6 was quickly increased to 558Mpa, and then up to 994 MPa slowly, and there was no strip peered off after 29 cycles of heat shock. The heat shock resistance of coating prepared in K_2ZrF_6-NaH_2PO_2 was better.
The LY12 aluminium alloys had the most rate of wear and tear and grinding abrasion occurred against Si3N4 ball on ball-on-disk tester with the rate of 1000 r/min under dry friction conditions. However, the wear resistance of the ceramic coatings was enhanced remarkably. The ceramic coating prepared in the solution of K_2ZrF_6-NaH_2PO_2 had the friction coefficient between 0.35 and 1.367 and minimum wear rate was 1.61×10-6g/min under a 150g load. The wear mechanism gradually converted from abrasion wear and adhesive abrasion to fatigue wear. The ceramic coating prepared in the NaAlO2-K_2ZrF_6 solution had the minimum friction coefficient of 0.214 and wear rate of 4.33×10-6g/min under a 300g load. The wear mechanism changed from abrasion wear to fatigue wear and abrasion wear. The high-wear-resistance friction pairs Si3N4 were badly worn, and Si from friction pairs was found in the wear scar on the ceramic coating. The ceramic coating prepared in the solution of Na5P3O10-CrO3had the friction coefficient of 0.306 and wear rate of 2.1×10-5g/min under a 100g load. Plastic deformation occurred to some extent, which induced smooth abrasion and brittle rupture of the coating.
利用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、电子探针(EPMA)、能谱(EDS)和X射线光电子能谱仪(XPS)研究膜层的相组成、形貌、元素分布和元素价态变化;利用加速的电化学方法评价膜层的耐腐蚀性;利用显微硬度仪研究膜层硬度的变化特点;利用球盘式滑动干摩擦仪(Si3N4球为摩擦副),研究铝合金和陶瓷膜的磨损率和摩擦系数。
纯Al和LC9微弧氧化膜分别由α-Al_2O_3和γ-Al_2O_3组成,LY12膜层由大量γ-Al_2O_3和少量α-Al_2O_3组成。膜层抗热震性按LC9、LY12、Al依次增强;耐腐蚀性能和与基体结合强度按Al、LC9、LY12依次增强;纯Al、LY12和LC9膜层的硬度最大值分别为33.4GPpa、22.15GPa和16.8GPa。在Na5P3O10-CrO3溶液中,LY12铝合金微弧氧化可制得黑色陶瓷膜层,膜层的Cr氧化数为0、+3价、+6,并且以非晶态存在,CrO3能促进γ-Al_2O_3向α-Al_2O_3转化、提高成膜速率、硬度、致密性及耐蚀性。
在K_2ZrF_6-NaH_2PO_2溶液中,LY12铝合金微弧氧化陶瓷膜主要由m-ZrO2、t-ZrO2和γ-Al_2O_3组成。负相电流密度增加导致电解液体系状态发生改变,使得膜层增厚及消除KZr_2(PO_4)_3相;膜层的最大努普硬度可达16.75GPa,与基体结合强度大于17.5MPa;增加NaH_2PO_2浓度均可提高膜层的耐点腐蚀性能。在NaAlO2-K_2ZrF_6电解液中,陶瓷膜主要由γ-Al_2O_3、α-Al_2O_3和少量的c-ZrO2;少量的K_2ZrF_6能加速膜层生长、致密性提高、促进γ-Al_2O_3向α-Al_2O_3转化及硬度的增大,改善了膜层的耐腐蚀性能;膜层的最大努普硬度达23.41GPa。
微弧氧化陶瓷膜一个热冲击循环经历升温、保温和降温3个阶段。K_2ZrF_6-NaH_2PO_2电解液体系陶瓷膜加热过程应力由0迅速达到575Mpa,然后缓慢变为780MPa,冲击循环38次以上出现起皮脱落;NaAlO2-K_2ZrF_6电解液体系陶瓷膜加热过程应力由0迅速达到558Mpa,然后缓慢变为994 MPa ,降温过程为升温过程的逆过程热,热冲击循环次数29次以上出现起皮剥落。
微弧氧化陶瓷膜的耐磨性同LY12铝合金相比较显著提高。K_2ZrF_6-NaH_2PO_2体系制备的膜层(载荷150g)最小磨损率为1.61×10-6g/min、摩擦系数在0.35-0.367之间变化,磨损过程由开始阶段的粘着磨损逐步过渡至脆性断裂。NaAlO2-K_2ZrF_6体系制备的膜层(载荷300g )磨损率为4.33×10-6g/min、摩擦系数最小为0.214;磨损过程由磨料磨损逐步过渡至磨料磨损和裂疲劳磨损,该体系陶瓷膜耐磨减磨效果最好。Na5P3O10-CrO3体系制备的膜层(载荷100g)磨损率为2.1×10-5g/min、摩擦系数0.306;摩擦过程表现为一定程度的塑性变形导致的光滑磨损和脆性断裂。
In order to solve the poor wear and corrosion properties, the oxide ceramic coatings were formed in-situ on aluminium alloys using the bi-pulsed micro-arc oxidation (MAO) power. The composition, structure and performance of the oxide coatings formed on different aluminium alloys were studied. The study was also conducted on the composition, structure and mechanical performance of black ceramic coating consisting of alumina and zirconia, respectively. The effect of alloy components on the structure, color and properties was discussed. The in-situ growth mechanism of oxide ceramic coatings was discussed in different electrolytes. The model of ceramic coatings’resistance to heat shock was established and used to analyze the variation of heat stress during the cycles of heat shock. The corrosion resistance, the friction behavior and wear mechanism of three kinds of coatings were estimated and discussed.
The X-ray diffraction (XRD), scanning electron microscope (SEM), electrode probe microscope analysis (EPMA), energy dispersive spectroscopy (EDS) and X-ray photoelectron spectroscope (XPS) were used to study the composition, morphology, the element distribution and variation of element valence. The corrosion resistance was studied by electrochemical methods. The coating hardness was measured by micro-hardness instrument. The wear lost and friction coefficient of aluminium alloys and ceramic coatings were studied by a ball-on-disk tester under the dry sliding conditions.
It was shown that the MAO coating formed on pure aluminium and LC9 consisted ofα-Al_2O_3 andγ-Al_2O_3, respectively. The coating formed on LY12 was composed of large numbers ofγ-Al_2O_3 and littleα-Al_2O_3. The heat shock resistance was increased by the followed orders: LC9﹤LY12﹤Al, and the corrosion resistance was increased by the subsequence of Al, LC9 and LY12. Coatings’maximal hardness of Al, LY12 and LC9 were 33.4 MPa, 22.15 MPa and 16.8 MPa, respectively. The black Al_2O_3 ceramic coating was prepared on LY12 aluminium alloys in solution of Na5P3O10-CrO3. The chromium was not crystal and had the valence of 0, +3, +6. CrO3 benefited to the transformation ofγ-Al_2O_3 toα-Al_2O_3 and increased the growth, hardness, thickness and corrosion resistance, and improved the compactness.
The coating consisting of m-ZrO2、t-ZrO2、γ-Al_2O_3 was prepared on LY12 in K_2ZrF_6-NaH_2PO_2. The proper increase of negative current density was in favor of the thickness increase of the coating and eliminated KZr2(PO3)3. The maximum of Knoop hardness could reach 16.75Gpa. The adherent strength of coating to substrate was beyond 17.5Mpa. Increasing the concentration of NaH_2PO_2 could improve the dot-corrosion resistance of the coating. The coating was mainly composed ofγ-Al_2O_3、α-Al_2O_3 and a little c-ZrO2. A small quantity of K_2ZrF_6 accelerated the coating growth and increased the compactness, promoted the transformation fromγ-Al_2O_3 toα-Al_2O_3 and consequently improved the corrosion resistance. The maximum Knoop hardness could reach 23.41Gpa.
The heat shock cycle experiment includes three stages: heat uprising, heat preservation and heat decreasing. During the heat shock process, the stress prepared in K_2ZrF_6-NaH_2PO_2 was increased quickly to 575Mpa, and then up to 780 MPa slowly, and there was no strip peered off after 38 cycles of heat shock. The heat stress of coating prepared in NaAlO2-K_2ZrF_6 was quickly increased to 558Mpa, and then up to 994 MPa slowly, and there was no strip peered off after 29 cycles of heat shock. The heat shock resistance of coating prepared in K_2ZrF_6-NaH_2PO_2 was better.
The LY12 aluminium alloys had the most rate of wear and tear and grinding abrasion occurred against Si3N4 ball on ball-on-disk tester with the rate of 1000 r/min under dry friction conditions. However, the wear resistance of the ceramic coatings was enhanced remarkably. The ceramic coating prepared in the solution of K_2ZrF_6-NaH_2PO_2 had the friction coefficient between 0.35 and 1.367 and minimum wear rate was 1.61×10-6g/min under a 150g load. The wear mechanism gradually converted from abrasion wear and adhesive abrasion to fatigue wear. The ceramic coating prepared in the NaAlO2-K_2ZrF_6 solution had the minimum friction coefficient of 0.214 and wear rate of 4.33×10-6g/min under a 300g load. The wear mechanism changed from abrasion wear to fatigue wear and abrasion wear. The high-wear-resistance friction pairs Si3N4 were badly worn, and Si from friction pairs was found in the wear scar on the ceramic coating. The ceramic coating prepared in the solution of Na5P3O10-CrO3had the friction coefficient of 0.306 and wear rate of 2.1×10-5g/min under a 100g load. Plastic deformation occurred to some extent, which induced smooth abrasion and brittle rupture of the coating.
引文
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