镁锂合金微弧氧化膜抗腐蚀及摩擦磨损性能研究
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摘要
超轻金属材料镁锂合金具有低密度、高比强度、良好的机械性能、电磁屏蔽效果和可循环利用的特点，在汽车、宇航、电子通讯领域有广泛的应用前景，但较弱的抗腐蚀性能、摩擦磨损性能限制其进一步的发展和工业应用。本文通过微弧氧化膜的制备与浸渍后处理大大改善了镁锂合金的抗腐蚀性能和摩擦磨损性能。利用SEM、XRD、TF-XRD、EDS、XPS技术对微弧氧化膜结构、物相组成、化学组成及其形成机制进行了表征，利用动电位极化曲线、电化学阻抗谱、浸泡实验研究了覆膜合金的抗腐蚀性能，利用球-盘摩擦磨损机、磨痕轮廓仪、纳米压痕仪、SEM和OM等对覆膜镁锂合金的摩擦学行为及磨损机制进行了测试和研究。
通过碱性硅酸盐电解液添加钨酸盐或钼酸盐，用先恒流后恒压电控方式在不同镁锂合金上制备了抗腐蚀性能较好的微弧氧化膜，发现了阳极氧化阶段速度和终电压对微弧氧化膜孔径的影响。镁锂合金基体中锂含量的降低以及电解液钨酸盐或钼酸盐的添加都加快了微弧氧化膜钝化的速度，抑制了合金基体的溶解。
采用碱性高锰酸盐、钼酸盐对微弧氧化膜浸渍处理时，由于H_2O、OH–等渗透到微弧氧化膜微孔，膜层更加致密，阻抗增大。表面生成Mn_2O_3、MnO_2、MgO·MoO_2、MoO_3、MgF_2和NaF等微/纳米粒子状化合物。氯化钠中性盐短暂浸渍后含钨膜表面水化、软化、疏松。
微弧氧化膜对Si_3N_4球作干滑动摩擦实验时发现，上述微/纳米粒子或软化物质作为微弧氧化膜表面固体润滑剂，缓解了膜层表面的应力分布，避免了陶瓷质地氧化膜的脆性断裂。同时，Si_3N_4球自身硬度高，不易被磨损，对微弧氧化膜剪切作用小，大大降低了微弧氧化膜的摩擦和磨损。动电位极化实验后产生的少量腐蚀产物有益于摩擦学行为的改善，局部腐蚀微裂纹不影响摩擦磨损性能。高粗糙度、低厚度、表面无润滑粒子或大量硬脆陶瓷粒子增大了摩擦和磨损。微弧氧化膜的磨损形貌显示，Si_3N_4球对不同陶瓷氧化膜产生刮擦、微抛光、抛光、断裂和剥离磨损。微弧氧化膜对硬度低于Si_3N_4的CCr15钢球作干滑动摩擦实验时发现，钢球在摩擦过程中自身被磨损，磨屑粘着在氧化膜上，钢球粗糙度逐渐增大，不断剪切微弧氧化膜，产生大量硬磨屑，虽然微弧氧化膜上面的润滑层及粘着的铁润滑层保持对磨面稳定摩擦和磨损，但随着接触面和粗糙度继续增大或者摩擦应力超过断裂应力，膜层断裂，微弧氧化膜/钢球系统由低而稳定的摩擦转向高摩擦。CCr15球对不同微弧氧化膜除产生抛光、切削、断裂磨损外还产生粘着和氧化磨损。质量磨损率和磨痕形貌显示，高硬度微弧氧化膜造成对磨试料高磨损率。
磷酸盐、含氟锆酸钾硅酸盐电解液以及添加钛溶胶后微弧氧化膜摩擦磨损实验研究发现，微弧氧化膜含磷非晶化合物有利于减摩，钛溶胶的添加增大了微弧氧化膜的硬度和弹性模量，表面更加平滑，抗摩擦磨损性能增强。高硬度含锆硅酸盐膜有利于磨损率降低，钛溶胶的添加降低了表面粗糙度，增大了弹性模量，低转速下发生低摩擦熔融磨损。
浸渍微弧氧化膜的长期腐蚀行为研究结果表明，中性盐长时间浸泡，浸渍含钨膜表面生成更多的腐蚀产物，封闭了表面微孔，外层阻抗增大，内层阻抗减小。非含钨浸渍微弧氧化膜由于微孔较大，容易渗透腐蚀液，内层有大量腐蚀产物堆积。
Mg-Li alloys as the lightest structural materials have wide application prospect in thefields of aerospace, electronic communication and automobile due to their inherent superiorproperties such as low density, high strength to weight ratio, good machining property,electromagnetic shielding and recyclability. However, the main factors hindering furtherdevelopment and industrial application of Mg-Li alloys are very poor corrosion and wearresistance. Micro-arc oxidation (MAO) coatings have been successfully fabricated on thesurface of Mg-Li alloys, followed by post-treatment of solution immersion, and theremarkable improvement in corrosion and wear resistance were obtained in the present paper.The surface morphology, microstructure, phase composition, chemical composition andformation mechanism of the coatings were characterized by means of SEM, XRD, TF-XRD,EDS and XPS techniques. The corrosion resistance was investigated by potentiodynamicpolarization curves, EIS and immersion test. The tribological properties and wear mechanismof the coatings were measured and analyzed using ball-on-disc configuration sliding frictiontest, talysurf, nanoindentation, SEM and OM.
MAO coatings with high corrosion resistance were prepared on the different Mg-Lialloys by the addition of tungstate or molybdate into the alkaline silicate, using a modeinvolving an initially constant current mode, followed by a constant voltage mode. The size ofmicropores on MAO coatings was mostly found to be influenced by the speed of anodizedphase and final voltage. With the decrease in Li content of Mg-Li alloy substrate and theaddition of tungstate or molybdate into the alkaline silicate the fast speed of passivationoccurs and the dissolution of Li the is suppressed.
It was demonstrated that MAO coatings have more compact microstructural features andthe impedance increases due to the penetration of H_2O and OH–into the pores and holes onMAO coatings after the immersion into alkaline permanganate or molybdate.Micro/nanoparticles containing Mn_2O_3, MnO_2(or MgO·MoO_2, MoO_3), MgF_2and NaFcompounds are generated on the surface of the coatings. The outer layer appears to behydrated, intenerated and loosened after the immersion of the immersed coatingsW-containing into neutral NaCl for short time.
By the dry sliding friction test of MAO coatings against the countermaterial Si_3N_4it wasfound that above described micro/nanoparticles or intenerated substance, which is chieflyresponsible for moderating the stress distribution and avoiding the brittle fracture of ceramiccoatings are regarded as solid lubricant. At the same time, Si_3N_4ball is insusceptible to beabraded due to its high hardness and the shear effect on MAO coating is small, which leads toreduce the friction and wear. After potentiodynamic polarization test a small amount ofcorrosion products generated on the surface of MAO coatings is favourable for improving thetribological behavior, which is independent of the partial corrosion microcracks formed in thepolarization test. The high roughness, low thickness, the surface without lubricative layer andhard ceramic particle may bring about more serious friction and wear of the coatings. Thewear morphologies of MAO coatings suggest that Si_3N_4ball results in micro-polishing,polishing, fracturation and detaching wear of the coating. By the dry sliding friction test ofMAO coatings against the countermaterial CCr15ball with lower hardness as compared withSi_3N_4ball it was found that CCr15ball is abraded and debris is transferred into the coating.With the increase of the roughness of CCr15ball, the MAO coatings are continuously shearedand a large amount of debris is generated. Although micro/nanoparticles and Fe-containingtransferred layer as solid lubricant may keep stable friction and wear, MAO coating isfractured and MAO coating/CCr15ball friction system is transferred from low friction to highfriction when the contact area and the surface roughness get higher or the friction stressexceeds the fracture stress. CCr15ball results in the adhesion wear and oxidation wear,besides the polishing, the flaking and fracturation wear of MAO coating. The wear rate andwear morphologies show that the high hardness of MAO coating results in high wear of thecountermaterials.
We examined the friction and wear properties of MAO coatings before and after theaddition of titania-sol into the alkaline phosphate or silicate containing K2ZrF6electrolyte. Itwas found that the amorphous P-containing compound imparts the beneficial effect on thereducing friction of MAO coating, and the addition of titania-sol into alkaline phosphateincreases the hardness and elastic modulus of MAO coating and gets surface flat and smooth,leading to enhancing the antifriction and wear resistance. The high hardness of MAO coatingcontaining ZrO2and Mg2SiO4is beneficial for reducing wear. The addition of titania-sol intoalkaline silicate electrolyte reduces roughness and increases elastic modulus of MAO coating, it was demonstrated that the melted wear reducing friction and wear occurs at low rotatespeed.
The corrosion behavior of immersed MAO coating was investigated under theimmersion into neutral NaCl for long-term, the results show that for immersed W-containingcoating more corrosive products are accumulated on the surface and micropores are sealed,hence the outer impedance rises and inner one falls. For the immersed coating without W thecorrosion solution enters inner layer due to the large pores and a large amount of corrosionproducts are accumulated in inner layer.
通过碱性硅酸盐电解液添加钨酸盐或钼酸盐，用先恒流后恒压电控方式在不同镁锂合金上制备了抗腐蚀性能较好的微弧氧化膜，发现了阳极氧化阶段速度和终电压对微弧氧化膜孔径的影响。镁锂合金基体中锂含量的降低以及电解液钨酸盐或钼酸盐的添加都加快了微弧氧化膜钝化的速度，抑制了合金基体的溶解。
采用碱性高锰酸盐、钼酸盐对微弧氧化膜浸渍处理时，由于H_2O、OH–等渗透到微弧氧化膜微孔，膜层更加致密，阻抗增大。表面生成Mn_2O_3、MnO_2、MgO·MoO_2、MoO_3、MgF_2和NaF等微/纳米粒子状化合物。氯化钠中性盐短暂浸渍后含钨膜表面水化、软化、疏松。
微弧氧化膜对Si_3N_4球作干滑动摩擦实验时发现，上述微/纳米粒子或软化物质作为微弧氧化膜表面固体润滑剂，缓解了膜层表面的应力分布，避免了陶瓷质地氧化膜的脆性断裂。同时，Si_3N_4球自身硬度高，不易被磨损，对微弧氧化膜剪切作用小，大大降低了微弧氧化膜的摩擦和磨损。动电位极化实验后产生的少量腐蚀产物有益于摩擦学行为的改善，局部腐蚀微裂纹不影响摩擦磨损性能。高粗糙度、低厚度、表面无润滑粒子或大量硬脆陶瓷粒子增大了摩擦和磨损。微弧氧化膜的磨损形貌显示，Si_3N_4球对不同陶瓷氧化膜产生刮擦、微抛光、抛光、断裂和剥离磨损。微弧氧化膜对硬度低于Si_3N_4的CCr15钢球作干滑动摩擦实验时发现，钢球在摩擦过程中自身被磨损，磨屑粘着在氧化膜上，钢球粗糙度逐渐增大，不断剪切微弧氧化膜，产生大量硬磨屑，虽然微弧氧化膜上面的润滑层及粘着的铁润滑层保持对磨面稳定摩擦和磨损，但随着接触面和粗糙度继续增大或者摩擦应力超过断裂应力，膜层断裂，微弧氧化膜/钢球系统由低而稳定的摩擦转向高摩擦。CCr15球对不同微弧氧化膜除产生抛光、切削、断裂磨损外还产生粘着和氧化磨损。质量磨损率和磨痕形貌显示，高硬度微弧氧化膜造成对磨试料高磨损率。
磷酸盐、含氟锆酸钾硅酸盐电解液以及添加钛溶胶后微弧氧化膜摩擦磨损实验研究发现，微弧氧化膜含磷非晶化合物有利于减摩，钛溶胶的添加增大了微弧氧化膜的硬度和弹性模量，表面更加平滑，抗摩擦磨损性能增强。高硬度含锆硅酸盐膜有利于磨损率降低，钛溶胶的添加降低了表面粗糙度，增大了弹性模量，低转速下发生低摩擦熔融磨损。
浸渍微弧氧化膜的长期腐蚀行为研究结果表明，中性盐长时间浸泡，浸渍含钨膜表面生成更多的腐蚀产物，封闭了表面微孔，外层阻抗增大，内层阻抗减小。非含钨浸渍微弧氧化膜由于微孔较大，容易渗透腐蚀液，内层有大量腐蚀产物堆积。
Mg-Li alloys as the lightest structural materials have wide application prospect in thefields of aerospace, electronic communication and automobile due to their inherent superiorproperties such as low density, high strength to weight ratio, good machining property,electromagnetic shielding and recyclability. However, the main factors hindering furtherdevelopment and industrial application of Mg-Li alloys are very poor corrosion and wearresistance. Micro-arc oxidation (MAO) coatings have been successfully fabricated on thesurface of Mg-Li alloys, followed by post-treatment of solution immersion, and theremarkable improvement in corrosion and wear resistance were obtained in the present paper.The surface morphology, microstructure, phase composition, chemical composition andformation mechanism of the coatings were characterized by means of SEM, XRD, TF-XRD,EDS and XPS techniques. The corrosion resistance was investigated by potentiodynamicpolarization curves, EIS and immersion test. The tribological properties and wear mechanismof the coatings were measured and analyzed using ball-on-disc configuration sliding frictiontest, talysurf, nanoindentation, SEM and OM.
MAO coatings with high corrosion resistance were prepared on the different Mg-Lialloys by the addition of tungstate or molybdate into the alkaline silicate, using a modeinvolving an initially constant current mode, followed by a constant voltage mode. The size ofmicropores on MAO coatings was mostly found to be influenced by the speed of anodizedphase and final voltage. With the decrease in Li content of Mg-Li alloy substrate and theaddition of tungstate or molybdate into the alkaline silicate the fast speed of passivationoccurs and the dissolution of Li the is suppressed.
It was demonstrated that MAO coatings have more compact microstructural features andthe impedance increases due to the penetration of H_2O and OH–into the pores and holes onMAO coatings after the immersion into alkaline permanganate or molybdate.Micro/nanoparticles containing Mn_2O_3, MnO_2(or MgO·MoO_2, MoO_3), MgF_2and NaFcompounds are generated on the surface of the coatings. The outer layer appears to behydrated, intenerated and loosened after the immersion of the immersed coatingsW-containing into neutral NaCl for short time.
By the dry sliding friction test of MAO coatings against the countermaterial Si_3N_4it wasfound that above described micro/nanoparticles or intenerated substance, which is chieflyresponsible for moderating the stress distribution and avoiding the brittle fracture of ceramiccoatings are regarded as solid lubricant. At the same time, Si_3N_4ball is insusceptible to beabraded due to its high hardness and the shear effect on MAO coating is small, which leads toreduce the friction and wear. After potentiodynamic polarization test a small amount ofcorrosion products generated on the surface of MAO coatings is favourable for improving thetribological behavior, which is independent of the partial corrosion microcracks formed in thepolarization test. The high roughness, low thickness, the surface without lubricative layer andhard ceramic particle may bring about more serious friction and wear of the coatings. Thewear morphologies of MAO coatings suggest that Si_3N_4ball results in micro-polishing,polishing, fracturation and detaching wear of the coating. By the dry sliding friction test ofMAO coatings against the countermaterial CCr15ball with lower hardness as compared withSi_3N_4ball it was found that CCr15ball is abraded and debris is transferred into the coating.With the increase of the roughness of CCr15ball, the MAO coatings are continuously shearedand a large amount of debris is generated. Although micro/nanoparticles and Fe-containingtransferred layer as solid lubricant may keep stable friction and wear, MAO coating isfractured and MAO coating/CCr15ball friction system is transferred from low friction to highfriction when the contact area and the surface roughness get higher or the friction stressexceeds the fracture stress. CCr15ball results in the adhesion wear and oxidation wear,besides the polishing, the flaking and fracturation wear of MAO coating. The wear rate andwear morphologies show that the high hardness of MAO coating results in high wear of thecountermaterials.
We examined the friction and wear properties of MAO coatings before and after theaddition of titania-sol into the alkaline phosphate or silicate containing K2ZrF6electrolyte. Itwas found that the amorphous P-containing compound imparts the beneficial effect on thereducing friction of MAO coating, and the addition of titania-sol into alkaline phosphateincreases the hardness and elastic modulus of MAO coating and gets surface flat and smooth,leading to enhancing the antifriction and wear resistance. The high hardness of MAO coatingcontaining ZrO2and Mg2SiO4is beneficial for reducing wear. The addition of titania-sol intoalkaline silicate electrolyte reduces roughness and increases elastic modulus of MAO coating, it was demonstrated that the melted wear reducing friction and wear occurs at low rotatespeed.
The corrosion behavior of immersed MAO coating was investigated under theimmersion into neutral NaCl for long-term, the results show that for immersed W-containingcoating more corrosive products are accumulated on the surface and micropores are sealed,hence the outer impedance rises and inner one falls. For the immersed coating without W thecorrosion solution enters inner layer due to the large pores and a large amount of corrosionproducts are accumulated in inner layer.
引文
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