Al-Sn轴承合金的双相双尺度结构与摩擦学性能
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摘要
随着滑动轴承向着高承载能力、耐磨减摩和环保（无铅）的方向发展，开发兼具优异力学和摩擦学性能的新型Al-Sn基轴承合金成为研究热点。纳米相复合Al-Sn轴承合金因其细化的组织和较高的硬度，通常表现出较好的摩擦学性能。但是，纳米晶合金强度与塑性的倒置关系制约了其在高摩擦学性能轴承材料领域的发展和工程应用。研究发现，双相双尺结构合金可同时获得高强度和良好塑性。本文利用双相双尺度结构强韧化Al-Sn合金，为发展具有优异摩擦学性能的新一代轴承合金提供了一条全新的思路。
首先，本文将机械合金化与粉末烧结相结合制备出具有纳米晶/超细晶与微米粗晶的混合组织的双相双尺度结构Al-12wt%Sn合金，并研究了其双尺度晶粒分布的微观结构和力学性能的关系。将高能球磨制备的纳米晶Al-12wt%Sn合金粉末与未经球磨的粗晶Al-12wt%Sn粉末按照一定比例均匀混合，压制和烧结可获得双相双尺度结构Al-Sn合金，它由超细晶区域（硬）、粗晶区域（软）及其这两区域各自结构中所包含的Al相（硬）、Sn相（软），组成了两对交互耦合的“硬-软”相，是轴瓦材料理想的微观组织。针对双相双尺度合金的非均质特性，同时采用了纳米压痕、显微硬度和压缩强度对其力学性能进行表征。结果表明，双相双尺度结构Al-12wt%Sn合金的硬度和压缩强度，随着粗晶含量的增加而逐步降低，但是，其塑性却随超细晶含量的增加而逐步降低。双相双尺度结构实现了Al-Sn合金在硬度、强度和塑性等方面的可调控，并在粗晶含量为Xwt%CG（20≤X≤60）的合金能兼具优良强度和塑性的力学性能。在此基础上，本文进一步发展并研究了双相双尺度结构Al-Sn、Al-Sn-Mg和Al-Sn-Si合金的摩擦学性能。
其次，我们首次对双相双尺度结构Al-12wt%Sn合金的滑动磨损性能和磨损机理进行研究，并将其与纯超细晶结构、粗晶结构Al-12wt%Sn合金的摩擦行为进行对比。研究表明，双相双尺度Al-Sn合金在其硬度值约为HV56时具有最优摩擦学性能，其耐磨性比纯超细晶结构提高了约1.5倍，比纯粗晶结构提高约2倍，而摩擦系数也比纯粗晶结构降低13%。在研究其磨损机理时发现，一层主要由纳米晶结构氧化物组成的动态稳定的氧化摩擦层是提高纯超细晶结构和双相双尺度结构Al-Sn合金磨损性能的关键因素。而纯粗晶结构Al-Sn合金，由于其基体强度较低而难以支撑持续稳定的摩擦层的形成，导致摩擦层容易剥落，从而使合金表现出高的磨损量。但是，影响动态稳定摩擦层的磨损破坏的根本原因是合金基体的“强度-塑性”的同时配合。对于纯超细晶Al-Sn合金而言，其基体表现出的较低塑性使其磨损面难以承受应变累积，摩擦层容易出现裂纹失效，进一步阻碍了其耐磨性能的提高；对于双相双尺度Al-Sn合金而言，适当的“超细晶+粗晶”比例使其基体具有最佳的“强度-塑性”配合，有利于在磨损表面形成持续稳定的氧化摩擦层，从而获得最优的耐磨性能。这种独特的双相双尺度结构也使得Al-Sn合金的摩擦学性能可调控。
再次，为了克服烧结后强度不高和粗晶引入对超细晶Al-Sn合金减摩性能造成的降低。我们通过添加Mg和Sn-Si包覆结构组元来进一步改善双相双尺度Al-12wt%Sn合金的组织结构、力学和摩擦学性能。利用Mg与和Al颗粒表面氧化膜反应形成MgAl2O4等相，改善润湿性，有效抑制了Sn相的离异共晶和Al晶粒的长大，同时提高了烧结致密度和强度。在添加Mg的滑动磨损和纳米划痕表面观察到大量Sn纳米相的传输和生长，包括纳米颗粒和纳米线，由于其较低的剪切强度，有效降低了合金的摩擦系数；同时，较高的强度和Mg元素受摩擦热的反应，对摩擦层的形成和特性均有明显改善，从而进一步提高合金的耐磨性能。此外，利用球磨细化Sn-12wt%Si组元替代双相双尺度Al-Sn合金中的粗晶Sn相，明显改善了Al-Sn合金的组织和硬度。特别是，由于球磨导致细小的硬质Si颗粒具有较高的残余应力，在磨损过程中，这些应力作用到Si颗粒表面的Sn相上，导致磨损面也出现了大量的Sn纳米相，对合金的摩擦学性能有了显著改善。为此，文中对比研究了添加Mg和Sn-Si包覆结构组元对Al-Sn合金中形成Sn纳米线的作用机制。
最后，为了实现双相双尺度Al-Sn合金在滑动轴承上的工程应用，我们还研究了双相双尺度结构Al-12wt%-(Mg)粉末与喷涂有纯Al层的钢背的复合轧制。通过研究轧制变形量、退火和烧结工艺对轧制组织及性能的影响，得出较优的复合轧制工艺。最终获得了均匀分布的双相双尺度结构的Al-Sn-Mg合金层，并在合金层-纯Al过渡层-钢背各层之间达到了紧密的界面结合，成功将该轧制复合带材弯制成轴瓦。为双相双尺度结构Al-Sn合金的应用奠定了基础。
Along with the development of plain bearing to higher load-carrying capacity, bettertribological properties and environmentally friendly (Pb-free), there are continuousdemands for developing new Al-Sn based bearing alloys combining with excellentmechanical and wear performances. Refining microstructure and high strength of nanophasecomposite Al-Sn bearing alloys are beneficial for their tribological properties. However, astrength-ductility trade-off presenting in nanocrystallined alloy restricts its good wearperformance and engineering applicationin Al-Sn bearing alloy. It was demonstrated thatdual-phase and dual-scale structured alloys obtain a simultaneously enhanced strength andductility. In this dissertation, toughened high-strength nanostructured Al-Sn by creatingdual-scale structure provides a bran-new idea for developing new bearing alloys withexcellent wear performance.
Firstly, a dual-phase and dual-scale Al-12wt%Sn alloy consisting of mixtures ofnanocrystalline/ultra-fine grain (NC/UFG) and coarse grain (CG) was produced by acombination of mechanical alloying and conventional powder sintering, and the correlationbetween dual-scale microstructure and mechanical properties was studied. The results showthat the milled NC Al-12wt%Snpowders were mixed with ummilled CG Al-12wt%Snpowders at a certain ratio, and then the powder mixtures were consolidated and sintered. Thefinal bulk alloys comprise of UFG (hard) and discrete CG (soft) regions, and simultaneouslyinclude Al (hard) and Sn (soft) phases in the two above regions, which forme two pairs ofcross-coupling“hard-soft” phases and develop an ideal microstructure of new bearingmaterials. Nano-indentation, micro-hardness and compressive strength are used tocharacterize mechanical properties in accordance to the heterogeneous feature of dual-scalealloys. It was found that the hardness and compressive strength of Al-12wt%Sn decreasegradually with the increasing CG content, but the ductility in opposite. The hardness, strengthand ductility of the dual-scale structured Al-Sn alloys can be adjusted by controlling theUFG/CG ratios. A simultaneously enhanced strength and ductility is achieved at a ratio of Xwt%CG（20≤X≤60）.On this basis, we further to study wear properties of dual-phase anddual-scale structured Al-Sn, Al-Sn-Mg and Al-Sn-Si alloys.
Secondly, for the first time, sliding wear properties and wear mechanism of dual-phaseand dual-scale Al-12wt%Sn alloy have been explored, and monolithic UFG and CGAl-12wt%Sn alloys were also investigated for comparison. The results show that the bestwear performance is achieved at a value of HV56hardness for the dual-phase and dual-scaleAl–Sn alloy, which has a wear resistance about1.5times greater than that of the monolithicUFG alloy, about twice that of the monolithic CG alloy. The friction coefficient decreases bynearly13%of the monolithic CG alloy. It also has been found that a dynamic steadytribolayer consisting of fine crystalline oxides plays a dominant role in improving the wearproperties of both the UFG and dual-scale alloys. For the CG alloys, poor wear properties,caused by delamination wear ofthe tribolayer, could not be maintained on the worn surface.However, the damage of the dynamic steady tribolayer is governed by the matching betweenductilityand strength of the matrix.The low ductility of the UFG alloy substrate causes thetribolayer to suffer crack damage rather easily, which limits any further improvement of itswear resistance. In contrast, the dual-scale structured alloy has excellent ductility-strengthmatching in accordance to UFG/CG ratios, and therefore a dynamic stable tribolayer caneasily be maintained on the worn surface, leading to excellent wear performance.Thediscrepant structure of dual-phase and dual-scale also provides a novel approach to controlthe wear properties of Al-Sn alloys.
Furthermore, in order to overcome the low strength of sintering and the reducinganti-friction by introducing of CG part, we attempted to further promote microstructure,mechanical and wear properties of the dual-phase and dual-scale structured Al–12wt%Snalloys by Mg and Sn-Si composite structure addition. Mg addition can disrupt the oxide filmof Al through the formation of MgAl2O4, which increases of wet-ability and reduces divorcedeutectics between Al and Sn, and simultaneously improves sintering density and strength. Mgaddition also enhances the transportation and growth of Sn nanophases, includingnaoparticles and nanowires, towards sliding worn and nanoscratch surfaces, which effectivelyreduces the friction coefficient due to their lower shear strength. Simultaneously, both theenhanced strength and heating reaction of Mg addition have an obvious improvement in theformation and features of tribolayer, and cause further promotion of wear resistance. Inaddition, employing milled Sn-12wt%Si to replace CG Sn in dual-phase and dual-scale Al-Sn alloy achieves a simultaneously enhanced microstructure and hardness. In particular, A largeresidual stresses in hard Si particles induced by ball milling act as the drive forces, which areimposed on the Sn phase. It leads to large amounts of Sn nanophases in the worn surface andobtains a significant improvement of wear properties. Therefore, the theories of the presenceof Sn nanowires or whiskers in the worn surface for both Mg and Sn-Si composite structurecontaining alloys were also investigated for comparison.
Finally, in order to achieve the engineering application of dual-phase and dual-scaleAl-Sn alloy in sliding bearing. The rolling bonding between the dual-phase and dual-scalestructured Al-12wt%Sn-(Mg) powders and steel with spraying Al coating also has beeninvestigated. After researching the effect of rolling deformation, annealing and sinteringtechnology on microstructure and properties, we obtain an optimum rolling technology.Finally, a homogeneous dual-phase and dual-scale structure in Al-Sn-Mg alloy layer wasprepared. The interfaces of Al-Sn-Mg layer/spraying Al layer/steel can achieve a closebonding. And the rolling strip was also successfully bended to be bearing. It establishes afoundation for the application of dual-phase and dual-scale Al-Sn alloy.
首先，本文将机械合金化与粉末烧结相结合制备出具有纳米晶/超细晶与微米粗晶的混合组织的双相双尺度结构Al-12wt%Sn合金，并研究了其双尺度晶粒分布的微观结构和力学性能的关系。将高能球磨制备的纳米晶Al-12wt%Sn合金粉末与未经球磨的粗晶Al-12wt%Sn粉末按照一定比例均匀混合，压制和烧结可获得双相双尺度结构Al-Sn合金，它由超细晶区域（硬）、粗晶区域（软）及其这两区域各自结构中所包含的Al相（硬）、Sn相（软），组成了两对交互耦合的“硬-软”相，是轴瓦材料理想的微观组织。针对双相双尺度合金的非均质特性，同时采用了纳米压痕、显微硬度和压缩强度对其力学性能进行表征。结果表明，双相双尺度结构Al-12wt%Sn合金的硬度和压缩强度，随着粗晶含量的增加而逐步降低，但是，其塑性却随超细晶含量的增加而逐步降低。双相双尺度结构实现了Al-Sn合金在硬度、强度和塑性等方面的可调控，并在粗晶含量为Xwt%CG（20≤X≤60）的合金能兼具优良强度和塑性的力学性能。在此基础上，本文进一步发展并研究了双相双尺度结构Al-Sn、Al-Sn-Mg和Al-Sn-Si合金的摩擦学性能。
其次，我们首次对双相双尺度结构Al-12wt%Sn合金的滑动磨损性能和磨损机理进行研究，并将其与纯超细晶结构、粗晶结构Al-12wt%Sn合金的摩擦行为进行对比。研究表明，双相双尺度Al-Sn合金在其硬度值约为HV56时具有最优摩擦学性能，其耐磨性比纯超细晶结构提高了约1.5倍，比纯粗晶结构提高约2倍，而摩擦系数也比纯粗晶结构降低13%。在研究其磨损机理时发现，一层主要由纳米晶结构氧化物组成的动态稳定的氧化摩擦层是提高纯超细晶结构和双相双尺度结构Al-Sn合金磨损性能的关键因素。而纯粗晶结构Al-Sn合金，由于其基体强度较低而难以支撑持续稳定的摩擦层的形成，导致摩擦层容易剥落，从而使合金表现出高的磨损量。但是，影响动态稳定摩擦层的磨损破坏的根本原因是合金基体的“强度-塑性”的同时配合。对于纯超细晶Al-Sn合金而言，其基体表现出的较低塑性使其磨损面难以承受应变累积，摩擦层容易出现裂纹失效，进一步阻碍了其耐磨性能的提高；对于双相双尺度Al-Sn合金而言，适当的“超细晶+粗晶”比例使其基体具有最佳的“强度-塑性”配合，有利于在磨损表面形成持续稳定的氧化摩擦层，从而获得最优的耐磨性能。这种独特的双相双尺度结构也使得Al-Sn合金的摩擦学性能可调控。
再次，为了克服烧结后强度不高和粗晶引入对超细晶Al-Sn合金减摩性能造成的降低。我们通过添加Mg和Sn-Si包覆结构组元来进一步改善双相双尺度Al-12wt%Sn合金的组织结构、力学和摩擦学性能。利用Mg与和Al颗粒表面氧化膜反应形成MgAl2O4等相，改善润湿性，有效抑制了Sn相的离异共晶和Al晶粒的长大，同时提高了烧结致密度和强度。在添加Mg的滑动磨损和纳米划痕表面观察到大量Sn纳米相的传输和生长，包括纳米颗粒和纳米线，由于其较低的剪切强度，有效降低了合金的摩擦系数；同时，较高的强度和Mg元素受摩擦热的反应，对摩擦层的形成和特性均有明显改善，从而进一步提高合金的耐磨性能。此外，利用球磨细化Sn-12wt%Si组元替代双相双尺度Al-Sn合金中的粗晶Sn相，明显改善了Al-Sn合金的组织和硬度。特别是，由于球磨导致细小的硬质Si颗粒具有较高的残余应力，在磨损过程中，这些应力作用到Si颗粒表面的Sn相上，导致磨损面也出现了大量的Sn纳米相，对合金的摩擦学性能有了显著改善。为此，文中对比研究了添加Mg和Sn-Si包覆结构组元对Al-Sn合金中形成Sn纳米线的作用机制。
最后，为了实现双相双尺度Al-Sn合金在滑动轴承上的工程应用，我们还研究了双相双尺度结构Al-12wt%-(Mg)粉末与喷涂有纯Al层的钢背的复合轧制。通过研究轧制变形量、退火和烧结工艺对轧制组织及性能的影响，得出较优的复合轧制工艺。最终获得了均匀分布的双相双尺度结构的Al-Sn-Mg合金层，并在合金层-纯Al过渡层-钢背各层之间达到了紧密的界面结合，成功将该轧制复合带材弯制成轴瓦。为双相双尺度结构Al-Sn合金的应用奠定了基础。
Along with the development of plain bearing to higher load-carrying capacity, bettertribological properties and environmentally friendly (Pb-free), there are continuousdemands for developing new Al-Sn based bearing alloys combining with excellentmechanical and wear performances. Refining microstructure and high strength of nanophasecomposite Al-Sn bearing alloys are beneficial for their tribological properties. However, astrength-ductility trade-off presenting in nanocrystallined alloy restricts its good wearperformance and engineering applicationin Al-Sn bearing alloy. It was demonstrated thatdual-phase and dual-scale structured alloys obtain a simultaneously enhanced strength andductility. In this dissertation, toughened high-strength nanostructured Al-Sn by creatingdual-scale structure provides a bran-new idea for developing new bearing alloys withexcellent wear performance.
Firstly, a dual-phase and dual-scale Al-12wt%Sn alloy consisting of mixtures ofnanocrystalline/ultra-fine grain (NC/UFG) and coarse grain (CG) was produced by acombination of mechanical alloying and conventional powder sintering, and the correlationbetween dual-scale microstructure and mechanical properties was studied. The results showthat the milled NC Al-12wt%Snpowders were mixed with ummilled CG Al-12wt%Snpowders at a certain ratio, and then the powder mixtures were consolidated and sintered. Thefinal bulk alloys comprise of UFG (hard) and discrete CG (soft) regions, and simultaneouslyinclude Al (hard) and Sn (soft) phases in the two above regions, which forme two pairs ofcross-coupling“hard-soft” phases and develop an ideal microstructure of new bearingmaterials. Nano-indentation, micro-hardness and compressive strength are used tocharacterize mechanical properties in accordance to the heterogeneous feature of dual-scalealloys. It was found that the hardness and compressive strength of Al-12wt%Sn decreasegradually with the increasing CG content, but the ductility in opposite. The hardness, strengthand ductility of the dual-scale structured Al-Sn alloys can be adjusted by controlling theUFG/CG ratios. A simultaneously enhanced strength and ductility is achieved at a ratio of Xwt%CG（20≤X≤60）.On this basis, we further to study wear properties of dual-phase anddual-scale structured Al-Sn, Al-Sn-Mg and Al-Sn-Si alloys.
Secondly, for the first time, sliding wear properties and wear mechanism of dual-phaseand dual-scale Al-12wt%Sn alloy have been explored, and monolithic UFG and CGAl-12wt%Sn alloys were also investigated for comparison. The results show that the bestwear performance is achieved at a value of HV56hardness for the dual-phase and dual-scaleAl–Sn alloy, which has a wear resistance about1.5times greater than that of the monolithicUFG alloy, about twice that of the monolithic CG alloy. The friction coefficient decreases bynearly13%of the monolithic CG alloy. It also has been found that a dynamic steadytribolayer consisting of fine crystalline oxides plays a dominant role in improving the wearproperties of both the UFG and dual-scale alloys. For the CG alloys, poor wear properties,caused by delamination wear ofthe tribolayer, could not be maintained on the worn surface.However, the damage of the dynamic steady tribolayer is governed by the matching betweenductilityand strength of the matrix.The low ductility of the UFG alloy substrate causes thetribolayer to suffer crack damage rather easily, which limits any further improvement of itswear resistance. In contrast, the dual-scale structured alloy has excellent ductility-strengthmatching in accordance to UFG/CG ratios, and therefore a dynamic stable tribolayer caneasily be maintained on the worn surface, leading to excellent wear performance.Thediscrepant structure of dual-phase and dual-scale also provides a novel approach to controlthe wear properties of Al-Sn alloys.
Furthermore, in order to overcome the low strength of sintering and the reducinganti-friction by introducing of CG part, we attempted to further promote microstructure,mechanical and wear properties of the dual-phase and dual-scale structured Al–12wt%Snalloys by Mg and Sn-Si composite structure addition. Mg addition can disrupt the oxide filmof Al through the formation of MgAl2O4, which increases of wet-ability and reduces divorcedeutectics between Al and Sn, and simultaneously improves sintering density and strength. Mgaddition also enhances the transportation and growth of Sn nanophases, includingnaoparticles and nanowires, towards sliding worn and nanoscratch surfaces, which effectivelyreduces the friction coefficient due to their lower shear strength. Simultaneously, both theenhanced strength and heating reaction of Mg addition have an obvious improvement in theformation and features of tribolayer, and cause further promotion of wear resistance. Inaddition, employing milled Sn-12wt%Si to replace CG Sn in dual-phase and dual-scale Al-Sn alloy achieves a simultaneously enhanced microstructure and hardness. In particular, A largeresidual stresses in hard Si particles induced by ball milling act as the drive forces, which areimposed on the Sn phase. It leads to large amounts of Sn nanophases in the worn surface andobtains a significant improvement of wear properties. Therefore, the theories of the presenceof Sn nanowires or whiskers in the worn surface for both Mg and Sn-Si composite structurecontaining alloys were also investigated for comparison.
Finally, in order to achieve the engineering application of dual-phase and dual-scaleAl-Sn alloy in sliding bearing. The rolling bonding between the dual-phase and dual-scalestructured Al-12wt%Sn-(Mg) powders and steel with spraying Al coating also has beeninvestigated. After researching the effect of rolling deformation, annealing and sinteringtechnology on microstructure and properties, we obtain an optimum rolling technology.Finally, a homogeneous dual-phase and dual-scale structure in Al-Sn-Mg alloy layer wasprepared. The interfaces of Al-Sn-Mg layer/spraying Al layer/steel can achieve a closebonding. And the rolling strip was also successfully bended to be bearing. It establishes afoundation for the application of dual-phase and dual-scale Al-Sn alloy.
引文
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