宽温域固体润滑材料及涂层的高温摩擦学特性研究
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摘要
室温到高温具有良好摩擦学性能的润滑材料是尖端工业领域迫切需要解决的难题。固体润滑剂与传统液体润滑剂相比在高温摩擦领域具有优势,但常用的固体润滑剂石墨、MoS2和低熔点金属在高温易氧化而失去润滑性能；一些稀土化合物和氧化物高温润滑性能好,但室温易导致磨粒磨损。合理运用多种润滑剂的协同润滑效应是实现室温到高温宽温度范围润滑的有效方法之一。以往研究通常是在金属基体中添加固体润滑剂制备复合材料或在金属基体表面沉积润滑涂层,复合材料中润滑剂添加量少对润滑性能改善效果不明显,而润滑剂添加量过多则会导致力学性能的显著下降；而润滑涂层寿命有限,一旦失效将造成灾难性后果。
本论文从润滑剂组元、表面形貌及润滑渗层等方面设计宽温度范围自润滑材料,用粉末冶金法制备含石墨、Ag、MoS2及Ce02的镍基自润滑复合材料,利用石墨或金属银在低温段润滑,利用硫化物或氧化物在高温段润滑；采用脉冲激光在镍基材料表面刻蚀微孔来存储润滑氧化物；采用双层辉光等离子渗金属技术对微孔化表面渗Mo或Mo／N复合渗处理以改善表面耐磨性能。研究多种润滑剂的协同润滑作用以及表面形貌与润滑渗层的复合运用。固体润滑复合材料表面制备润滑渗层,改善复合材料的表面力学性能和摩擦学性能,该研究对于解决极端工况下工作的转动密封、高温轴承的摩擦润滑问题具有重要的指导意义。
研究了镍基自润滑复合材料、渗Mo层以及Mo／N复合渗层的力学性能、抗氧化性能以及室温～600℃的摩擦学性能,并探讨了润滑剂添加量、温度、载荷、配副材料及微孔化、渗Mo处理对摩擦学行为的影响。采用光学显微镜、扫描电镜及X射线衍射仪观察分析镍基复合材料及渗层的微观组织形貌,采用白光干涉三维表面轮廓仪观察微孔形貌,利用扫描电子显微镜(SEM)、电子能谱(EDS)、X射线光电子能谱(XPS)分析高温磨损表面形貌及其成分。
镍基自润滑复合材料中,石墨与钨热压反应生成碳化钨,MoS2与铬反应生成CrxSx+1共晶化合物。添加一定量的MoS2,由于Mo的固溶强化,提高了复合材料的硬度和抗弯强度。添加石墨和MoS2分别有利于降低镍基合金室温段和高温段的摩擦系数,同时添加石墨和MoS2的镍基材料含有硬质相(Mo2C、WC)及润滑相(CrxSx+1、石墨)其室温到700℃的摩擦系数(0.14-0.27)低于添加单一润滑剂的复合材料,且磨损率比添加单一润滑剂的材料低一个数量级。添加MoS2的镍基复合材料,由于低熔点硫化物的摩擦熔融,获得了较低的摩擦系数。润滑剂的添加,降低了材料的抗氧化性能。随润滑剂添加量的增加,复合材料的氧化激活能线性变化。
添加金属银有利于改善镍基材料中低温段的摩擦学性能,银添加量为10%时,Ni-Ag合金室温摩擦系数降低为0.2。添加Ce02有利于高温摩擦表面致密氧化膜的形成,降低了Ni-Ag合金的高温摩擦系数和磨损率。同时添加Ag、MoS2和Ce02的镍基复合材料含有Ag、CrxSx+1、CeS等润滑相,室温～700℃的摩擦系数降低到0.16-0.26,磨损率下降了一个数量级。
双层辉光等离子渗金属技术在镍基合金表面获得了厚度为20-30μm的渗Mo层,其表面Mo浓度为34wt%,渗Mo处理提高了镍基合金表面的硬度和弹性模量,降低了合金高温段的摩擦系数和磨损率。渗Mo基础上渗氮处理,在Ni-Ag合金表面形成的MoN化合物层,提高了表面力学性能,但连续的化合物层阻碍了内部润滑剂银的释放,对摩擦学性能产生不利影响。
激光微孔化处理在镍基合金表面形成直径为150μm,深度为40～50μm,规则排列的微孔。微孔化表面渗Mo处理,Mo的高温润滑性氧化物降低了高温摩擦系数,微孔存储润滑性氧化物,并且存积硬质磨粒,降低了高温磨损率。激光微孔化表面进行Mo／N复合渗处理,Ni-Ag合金中内含的银可以通过微孔向外释放,并且硬质渗层提高了软质润滑膜的承载能力,降低了银的摩擦损耗,提高了高温摩擦学性能。
镍基复合材料和渗层的动态氧化增重抛物线常数比静态氧化增重高2个数量级。在传统的氧化磨损模型及熔融磨损模型的基础上,建立了更接近于实验值的镍基复合材料及渗层的高温氧化物熔融磨损模型,计算了复合材料的静态和动态氧化激活能,阐述了高温摩擦表面氧化物的生成、剥落／部分熔融以及致密承载层的形成等演化过程。
Solid lubrication over a wide range of temperature is a challenge for decades and has yet to overcome. Most common lubricant performs only within a narrow temperature range, such as graphite, molybdenum disulfide are effective below 400℃in air, above which they will oxidize or decompose and lose their lubricious nature. Some oxides lubricate well above 600-800℃, but are abrasive at lower temperature. The combination of two or more than two lubricants is one of the good methods to realize lubrication over a wide temperature.
In provious study, the self lubricating composite was usually prepared by adding solid lubricant in the metal matrix and lubricating coating was prepared by deposition technology. The frictional property was less affected if the adding amount of lubricant was too low. However, if the adding amount of lubricant was too high, the mechanical properties would decrease significantly. The wear life of lubricating coating was limited and its failure leaded to catastrophic incident.
Nickel-based composites containing graphite, sliver, MoS2 and CeO2 were prepared by powder metallurgy (P/M) method. Ni-20Cr powders mixed with tungsten, aluminum, titanium, and different contents of graphite, molybdenum disulfides or silver were hot-pressed in a vuccum furnace. Laser surface texturing (LST) was performed on the Ni-base composite in order to modify its contact state and surface molybdenizing was carried out on the textured composite in order to improve its wear resistance. The molybdenizing and nitriding duplex-treatment was also performed on the textured nickel-base composite. The molybdenizd layer prepared on the solid lubricating composite can relize self lubrication over a wide temperature range and improve its surface mechanical properties. It is meaningful to solve the friction and lubricating problems of transport part and seal in the turbine engine and heavy vehicle, which work under an extreme environment.
The mechanical properties and anti-oxidization properties of nickel-base composite, molybdenzing and duplex-treated layer were measured. Their tribological properties from room temperature to 700℃were tested on a pin-on-disk trimometer with Al2O3 as counterfaces. The effects of lubricant addition amount, temperature, load, sliding velocity and counter face materials, texturing and molybdenizing on the tribological properties were investigated. The microstructure and morphology were analyzed by X-Ray diffraction (XRD) and scanning electrical microscope (SEM) attached with EDS. The element distributions, micro-hardness of molybdenized layer were investigated. The worn surfaces were observed by optical microscope, SEM, EDS and X-ray photoelectron spectroscopy (XPS).
Chromium sulfide and tungsten carbide were formed in the composite by adding molybdenum disulfide and graphite in the nickel-base alloy. The nickel-base composite with graphit and MoS2 consisted of hard phases (Mo2C, WC) and lubricant phases (CrxSx+1, graphite). The hardness and anti-bending strength of composites increase after adding MoS2. The high temperature oxidization resistance decreases with the increase of solid lubricant. The activity energy of oxidization increases with the increase of MoS2 adding amount.The addition of MoS2 is favored to the reduction of friction coefficient of composite at high temperature. The lowest friction coefficients (0.14～0.27) and wear rates (1.0～3.5×10-6mm3/(Nm)) from room temperature to 700℃are obtained due to synergetic lubricating action of graphite and molybdenum disulfide. The graphite plays the main role of lubrication at room temperature, while sulfides are responsible for low friction at high temperature.
The friction coefficient at room temperature decreases after adding silver in the composite. Meanwhile, the wear rates at high temperature are reduced by adding cerium oxide. The wear rates are reduced by more than one order of magnitude after adding silver and CeO2. The SEM analysis of worn surface at high temperature shows that the rare earth compound is helpful for the formation of compact oxide film, which improves the wear resistance at high temperature. The nickel-base silver-containing composite consisted of lubricant phase such as sliver, Cr3S4, and CeS. The friction coefficients of silver and CeO2 containing Ni-base composite from room temperature to 700℃are in the range of 0.16～0.26.
The molybdenized layer on nickel-base alloy is approximately 20-30μm in thickness. The content of molybdenum on the surface of molybdenized layer reaches 34% and the hardness and elastic modulus is improved by molybdenizing. The friction coefficient and wear rate of alloy decrease after molybdenizing. The diffusion of sliver and the forming of trioxide of molybdenum affected by temperature are responsible for the friction reduction at elevated temperatures. The molybdenizing and nitriding duplex-treated layer shows the similar tribological character with that of molybdenized layer. The compound MoN layer hinders the diffusion of silver.
The laser surface textured dimples on nickel-base alloy are 150μm in diameter and 45-50 u m in depth and the distances between dimples are 500μm. The friction coefficient of alloys decreases by texturing and molybdnizing duplex-treatment. The wear rate of duplex-treated alloy is one order of magnitude lower than that of pristine alloy at elevated temperature due to the lubrication of trioxides of molybdenum. Furthermore, the micro-dimples can relieve abrasive wear by storing hard wear particles, which is also responsible for the reduction of wear rates. After texturing, the dimples on the MoN layer act as diffusion channels. The MoN layer on textured surface is hard enough to carry the load and protects the silver film.
The parabolic parameter of dynamic oxidization is two orders of magnitude higher than that of static oxidization. the calculated wear rate of composite based on oxidizing wear model is lower than the experiment value while the calculated wear rate based on melt wear model is two orders of magnitude higher than experiment value. A high temperature melting wear model of oxide is developed for nickel-base composite and molybdenized layer. The oxide on high temperature frictional surface experienced formation, break or partly melt and compaction of compact layer.
本论文从润滑剂组元、表面形貌及润滑渗层等方面设计宽温度范围自润滑材料,用粉末冶金法制备含石墨、Ag、MoS2及Ce02的镍基自润滑复合材料,利用石墨或金属银在低温段润滑,利用硫化物或氧化物在高温段润滑；采用脉冲激光在镍基材料表面刻蚀微孔来存储润滑氧化物；采用双层辉光等离子渗金属技术对微孔化表面渗Mo或Mo／N复合渗处理以改善表面耐磨性能。研究多种润滑剂的协同润滑作用以及表面形貌与润滑渗层的复合运用。固体润滑复合材料表面制备润滑渗层,改善复合材料的表面力学性能和摩擦学性能,该研究对于解决极端工况下工作的转动密封、高温轴承的摩擦润滑问题具有重要的指导意义。
研究了镍基自润滑复合材料、渗Mo层以及Mo／N复合渗层的力学性能、抗氧化性能以及室温～600℃的摩擦学性能,并探讨了润滑剂添加量、温度、载荷、配副材料及微孔化、渗Mo处理对摩擦学行为的影响。采用光学显微镜、扫描电镜及X射线衍射仪观察分析镍基复合材料及渗层的微观组织形貌,采用白光干涉三维表面轮廓仪观察微孔形貌,利用扫描电子显微镜(SEM)、电子能谱(EDS)、X射线光电子能谱(XPS)分析高温磨损表面形貌及其成分。
镍基自润滑复合材料中,石墨与钨热压反应生成碳化钨,MoS2与铬反应生成CrxSx+1共晶化合物。添加一定量的MoS2,由于Mo的固溶强化,提高了复合材料的硬度和抗弯强度。添加石墨和MoS2分别有利于降低镍基合金室温段和高温段的摩擦系数,同时添加石墨和MoS2的镍基材料含有硬质相(Mo2C、WC)及润滑相(CrxSx+1、石墨)其室温到700℃的摩擦系数(0.14-0.27)低于添加单一润滑剂的复合材料,且磨损率比添加单一润滑剂的材料低一个数量级。添加MoS2的镍基复合材料,由于低熔点硫化物的摩擦熔融,获得了较低的摩擦系数。润滑剂的添加,降低了材料的抗氧化性能。随润滑剂添加量的增加,复合材料的氧化激活能线性变化。
添加金属银有利于改善镍基材料中低温段的摩擦学性能,银添加量为10%时,Ni-Ag合金室温摩擦系数降低为0.2。添加Ce02有利于高温摩擦表面致密氧化膜的形成,降低了Ni-Ag合金的高温摩擦系数和磨损率。同时添加Ag、MoS2和Ce02的镍基复合材料含有Ag、CrxSx+1、CeS等润滑相,室温～700℃的摩擦系数降低到0.16-0.26,磨损率下降了一个数量级。
双层辉光等离子渗金属技术在镍基合金表面获得了厚度为20-30μm的渗Mo层,其表面Mo浓度为34wt%,渗Mo处理提高了镍基合金表面的硬度和弹性模量,降低了合金高温段的摩擦系数和磨损率。渗Mo基础上渗氮处理,在Ni-Ag合金表面形成的MoN化合物层,提高了表面力学性能,但连续的化合物层阻碍了内部润滑剂银的释放,对摩擦学性能产生不利影响。
激光微孔化处理在镍基合金表面形成直径为150μm,深度为40～50μm,规则排列的微孔。微孔化表面渗Mo处理,Mo的高温润滑性氧化物降低了高温摩擦系数,微孔存储润滑性氧化物,并且存积硬质磨粒,降低了高温磨损率。激光微孔化表面进行Mo／N复合渗处理,Ni-Ag合金中内含的银可以通过微孔向外释放,并且硬质渗层提高了软质润滑膜的承载能力,降低了银的摩擦损耗,提高了高温摩擦学性能。
镍基复合材料和渗层的动态氧化增重抛物线常数比静态氧化增重高2个数量级。在传统的氧化磨损模型及熔融磨损模型的基础上,建立了更接近于实验值的镍基复合材料及渗层的高温氧化物熔融磨损模型,计算了复合材料的静态和动态氧化激活能,阐述了高温摩擦表面氧化物的生成、剥落／部分熔融以及致密承载层的形成等演化过程。
Solid lubrication over a wide range of temperature is a challenge for decades and has yet to overcome. Most common lubricant performs only within a narrow temperature range, such as graphite, molybdenum disulfide are effective below 400℃in air, above which they will oxidize or decompose and lose their lubricious nature. Some oxides lubricate well above 600-800℃, but are abrasive at lower temperature. The combination of two or more than two lubricants is one of the good methods to realize lubrication over a wide temperature.
In provious study, the self lubricating composite was usually prepared by adding solid lubricant in the metal matrix and lubricating coating was prepared by deposition technology. The frictional property was less affected if the adding amount of lubricant was too low. However, if the adding amount of lubricant was too high, the mechanical properties would decrease significantly. The wear life of lubricating coating was limited and its failure leaded to catastrophic incident.
Nickel-based composites containing graphite, sliver, MoS2 and CeO2 were prepared by powder metallurgy (P/M) method. Ni-20Cr powders mixed with tungsten, aluminum, titanium, and different contents of graphite, molybdenum disulfides or silver were hot-pressed in a vuccum furnace. Laser surface texturing (LST) was performed on the Ni-base composite in order to modify its contact state and surface molybdenizing was carried out on the textured composite in order to improve its wear resistance. The molybdenizing and nitriding duplex-treatment was also performed on the textured nickel-base composite. The molybdenizd layer prepared on the solid lubricating composite can relize self lubrication over a wide temperature range and improve its surface mechanical properties. It is meaningful to solve the friction and lubricating problems of transport part and seal in the turbine engine and heavy vehicle, which work under an extreme environment.
The mechanical properties and anti-oxidization properties of nickel-base composite, molybdenzing and duplex-treated layer were measured. Their tribological properties from room temperature to 700℃were tested on a pin-on-disk trimometer with Al2O3 as counterfaces. The effects of lubricant addition amount, temperature, load, sliding velocity and counter face materials, texturing and molybdenizing on the tribological properties were investigated. The microstructure and morphology were analyzed by X-Ray diffraction (XRD) and scanning electrical microscope (SEM) attached with EDS. The element distributions, micro-hardness of molybdenized layer were investigated. The worn surfaces were observed by optical microscope, SEM, EDS and X-ray photoelectron spectroscopy (XPS).
Chromium sulfide and tungsten carbide were formed in the composite by adding molybdenum disulfide and graphite in the nickel-base alloy. The nickel-base composite with graphit and MoS2 consisted of hard phases (Mo2C, WC) and lubricant phases (CrxSx+1, graphite). The hardness and anti-bending strength of composites increase after adding MoS2. The high temperature oxidization resistance decreases with the increase of solid lubricant. The activity energy of oxidization increases with the increase of MoS2 adding amount.The addition of MoS2 is favored to the reduction of friction coefficient of composite at high temperature. The lowest friction coefficients (0.14～0.27) and wear rates (1.0～3.5×10-6mm3/(Nm)) from room temperature to 700℃are obtained due to synergetic lubricating action of graphite and molybdenum disulfide. The graphite plays the main role of lubrication at room temperature, while sulfides are responsible for low friction at high temperature.
The friction coefficient at room temperature decreases after adding silver in the composite. Meanwhile, the wear rates at high temperature are reduced by adding cerium oxide. The wear rates are reduced by more than one order of magnitude after adding silver and CeO2. The SEM analysis of worn surface at high temperature shows that the rare earth compound is helpful for the formation of compact oxide film, which improves the wear resistance at high temperature. The nickel-base silver-containing composite consisted of lubricant phase such as sliver, Cr3S4, and CeS. The friction coefficients of silver and CeO2 containing Ni-base composite from room temperature to 700℃are in the range of 0.16～0.26.
The molybdenized layer on nickel-base alloy is approximately 20-30μm in thickness. The content of molybdenum on the surface of molybdenized layer reaches 34% and the hardness and elastic modulus is improved by molybdenizing. The friction coefficient and wear rate of alloy decrease after molybdenizing. The diffusion of sliver and the forming of trioxide of molybdenum affected by temperature are responsible for the friction reduction at elevated temperatures. The molybdenizing and nitriding duplex-treated layer shows the similar tribological character with that of molybdenized layer. The compound MoN layer hinders the diffusion of silver.
The laser surface textured dimples on nickel-base alloy are 150μm in diameter and 45-50 u m in depth and the distances between dimples are 500μm. The friction coefficient of alloys decreases by texturing and molybdnizing duplex-treatment. The wear rate of duplex-treated alloy is one order of magnitude lower than that of pristine alloy at elevated temperature due to the lubrication of trioxides of molybdenum. Furthermore, the micro-dimples can relieve abrasive wear by storing hard wear particles, which is also responsible for the reduction of wear rates. After texturing, the dimples on the MoN layer act as diffusion channels. The MoN layer on textured surface is hard enough to carry the load and protects the silver film.
The parabolic parameter of dynamic oxidization is two orders of magnitude higher than that of static oxidization. the calculated wear rate of composite based on oxidizing wear model is lower than the experiment value while the calculated wear rate based on melt wear model is two orders of magnitude higher than experiment value. A high temperature melting wear model of oxide is developed for nickel-base composite and molybdenized layer. The oxide on high temperature frictional surface experienced formation, break or partly melt and compaction of compact layer.
引文
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