CN1584353A - 滑动件及其生产方法 - Google Patents
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Abstract
按照本发明的一种实施方式,提供一种滑动件,其包括基体和形成于所述基体上以限定在润滑作用下与相对构件滑动接触的滑动表面的硬碳涂层。所述硬碳涂层具有氢含量低于其剩余部分的最外层表面部分、或氢含量低于至少一层其它涂层的最外层涂层。
Description
技术领域
本发明涉及一种滑动件,特别涉及具有硬碳如类金刚石碳的薄涂层的滑动件,其在特定润滑剂存在下表现出优良的低摩擦特性和耐久性。本发明还涉及生产所述滑动件的方法。
背景技术
全球环境问题例如全球变暖和臭氧层破坏已近在眼前。全球变暖主要受CO2排放影响,设定CO2排放标准以降低CO2排放,已经成为每个国家关切的大事。为了降低CO2排放,改善车辆的燃料效率是非常重要的。因此,希望降低车辆发动机中的摩擦,以获得燃料效率方面的直接改善。
存在有多种可能的方法来降低发动机的摩擦。一种降低发动机摩擦的方法是提供在极端摩擦/磨损条件下具有较低摩擦系数和较高耐磨性的发动机滑动件。例如设想将硬碳涂层材料涂覆到发动机滑动件的凸轮随动件上(如起阀器和起阀器垫片)并使用一种配带有滚柱滚针轴承的所谓滚柱摇臂。已经证实类金刚石碳(DLC)涂层在空气中较氮化钛(TiN)膜和氮化铬(CrN)膜具有更低的摩擦系数,所以所述DLC涂层预期可用于发动机滑动件。另一降低发动机摩擦的方法是改善用于滑动件的润滑油的性质。设想降低润滑油的粘度,以便降低在水力润滑区中的粘性阻力和在机械滑动部分中的搅动阻力。另外还设想提供混有合适的摩擦改进剂及其它添加剂的润滑油,以便降低在混合润滑条件和边界润滑条件下发动机的摩擦损失。对于各种不同摩擦改进剂,已经进行了许多的研究,这些改进剂包括有机钼化合物,例如二硫代氨基甲酸钼(MoDTC)和二硫代磷酸钼(MoDTP),而且已经证实含有这类有机钼摩擦改进剂的润滑油在使用的早期阶段对于降低钢制滑动件间的摩擦是有效的。
所述DLC涂层的低摩擦特性和所述有机钼化合物的摩擦调节性能,已报导在KANO等人的Japan Tribology Congress 1999.5,Tokyo,Proceeding Page 11-12和KANO等人的Worid Tribology Congress2001.9,Vienna,Proceeding Page 342之中。
发明内容
但这种DLC涂层在润滑油存在下不能总是表现出低摩擦系数。即使在含有有机钼摩擦改进剂的润滑油存在下,所述DLC涂层也不能适当地表现出其低摩擦系数。
而且当所述DLC涂层具有低的氢含量时,所述DLC涂层对基底材料的粘着性易于得到改善。当所述DLC涂层不含氢时,则难以提高涂层厚度。这样,所述DLC涂层的耐久性就易于得到改善。
因此,本发明的一个目的是提供一种具有硬碳薄涂层的滑动件,其在润滑剂存在下表现出优良的低摩擦特性和耐久性,从而当用于车辆发动机时能够获得燃料效率的进一步改善。本发明的另一个目的是提供一种生产所述滑动件的方法。
作为广泛研究的结果,本申请人已经发现,具有一定结构的硬碳薄涂层与特定润滑剂组合时能够表现出优良的低摩擦特性和耐久性。本发明就是基于上述发现完成的。
根据本发明的第一方面,提供一种滑动件,其包括:基体;和形成于所述基体上用来限定在润滑作用下与相对构件进行滑动接触的滑动表面的硬碳涂层,所述硬碳涂层具有氢含量低于其剩余部分的最外层表面部分。
根据本发明的第二方面,提供一种滑动件,其包括:基体;和形成于所述基体上用来限定在润滑作用下与相对构件进行滑动接触的滑动表面的硬碳涂层,所述硬碳涂层具有沿其厚度方向层压在一起的两层或多层涂层,所述层压涂层包括氢含量低于至少一个其它涂层的最外层涂层。
根据本发明的第三方面,提供一种生产滑动件的方法,其包括:提供所述滑动件的基体;和在所述基体上形成硬碳涂层,其形成方式应使硬碳涂层具有氢含量低于其剩余部分的最外层表面部分。
根据本发明的第四方面,提供一种生产滑动件的方法,其包括:提供所述滑动件的基体;和在所述基体上形成硬碳涂层,其形成方式应使硬碳涂层具有氢含量低于至少一个其它涂层的最外层涂层。
由下述内容可进一步理解本发明的其它目的和特征。
附图说明
图1A所示为本发明一种示例性实施方式的活塞环的平面图。
图1B为图1A所示活塞环的局部截面图。
图1C为图1B所示划圈部分的放大视图。
图2为往复式摩擦/磨损测试装置的示意图。
具体实施方式
下面将对本发明作详细说明。在下述说明中,除非另有规定,所有百分比(%)都以质量表示。
本发明一种示例性实施方式的滑动件(在下文中称为“滑动件”),包括基体、形成于所述基体上用来限定与相对构件进行滑动接触的滑动表面的硬碳涂层和施用到所述滑动表面上的润滑剂薄膜,从而所述滑动件在所述相对构件上通过设置在所述滑动件和所述相对构件之间的润滑剂薄膜滑动。
虽然所述滑动件具有许多用途,但理想地是在极端摩擦/磨损条件下使用所述滑动件,以充分利用所述滑动件的优良低摩擦特性和耐久性。例如所述滑动件可成型为用于汽车发动机的活塞环如顶环和甩油环,如图1A、1B和1C所示。所述硬碳涂层优选形成在所述活塞环基体的相对环面1上,该面与活塞的活塞环槽(作为相对构件,图中未画出)进行接触,这样不仅可以有效降低所述活塞与所述活塞环间的摩擦,而且还可改善所述活塞的抗卡死性。而且所述硬碳涂层优选形成在所述活塞环基体部分的外围面2上,该面与发动机本体的汽缸内径(作为相对构件,图中未画出)进行滑动接触,以便有效降低所述活塞与所述汽缸壁间的摩擦。可替换地,也可以采用所述硬碳涂层涂覆整个活塞环,也可以在所述汽缸壁上形成一层硬碳涂层。
滑动件
所述基体是由任意已知基底材料形成的,如铁基(钢)材料或铝基(铝合金)材料,在用所述硬碳涂层涂覆之前,可对其进行表面处理。
一般地,所述硬碳涂层是由无定形碳制成的,其中的碳元素存在于两种sp2和sp3杂化中以形成石墨和金刚石的复合结构。所述无定形碳的具体实例包括:不含氢的无定形碳(a-C)、含氢的无定形碳(a-C:H)和/或含有金属元素钛(Ti)或钼(Mo)作为一部分的金属碳化物或金属碳(MeC)。不含氢的无定形碳和氢含量低的无定形碳也称作“类金刚石碳(DLC)”。
按照本发明的第一种实施方式,所述硬碳涂层的最外层表面部分的氢含量低于其剩余部分。利用这样的氢含量分布有可能改善所述硬碳涂层对所述基体的粘着性,并有可能提高所述硬碳涂层的厚度到足够的程度,从而保证或改善所述滑动件的低摩擦特性、耐磨性和耐久性。此处,所述硬碳涂层的“最外层表面部分”定义为在所述滑动表面以下的部分,例如在涂层厚度5%范围内延伸的部分或者在厚度为1.0μm范围内延伸的部分。
为了获得更大的降低摩擦效果,希望使第一实施方式中所述硬碳涂层的最外层表面部分中的氢含量最小。所述硬碳涂层的最外层表面部分的平均氢含量优选控制为20原子%或更低,更优选为10原子%或更低,更进一步优选为5原子%或更低,进而更优选为0.5原子%或更低,最优选基本为零。
在第一实施方式中,所述硬碳涂层的氢含量分布不受特别限制,只要所述硬碳涂层的最外层表面部分的氢含量低于剩余部分即可。考虑到涂覆方法的步骤和条件和制备成本,所述硬碳涂层的氢含量分布可以适当地根据所述硬碳涂层需要的低摩擦特性、耐磨性和耐久性而变化。虽然如此,还是希望所述硬碳涂层的氢含量沿涂层厚度方向从基体侧到滑动表面侧(即最外层涂层表面侧)是逐渐降低的。当所述硬碳涂层是由这类具有连续氢含量梯度的功能化梯度材料制成时,所述硬碳涂层的内应力得到释放。这就可能防止所述硬碳涂层中发生破裂,从而进一步改善所述硬碳涂层的耐久性。一种替代方案是,所述硬碳涂层的氢含量可按阶梯方式降低。
按照本发明的第二实施方式,所述硬碳涂层具有沿涂层厚度方向层压在一起的两层或多层,并包括氢含量低于至少一个其它层的最外层。优选地,所述硬碳涂层最外层的氢含量低于所有其它层。通过这样的层结构,可以改善所述硬碳涂层对所述基体的粘着性,并可能提高所述硬碳涂层的厚度到足够的程度,从而保证或改善所述滑动件的低摩擦特性、耐磨性和耐久性。此处,所述硬碳涂层的“层”定义为在其整个厚度内具有基本均匀的氢含量的部分。
在第二实施方式中,所述硬碳涂层的层结构不受特别限制,只要所述最外层涂层的氢含量低于任何其它涂层即可。考虑到涂覆方法的步骤和条件和制备成本,所述硬碳涂层的层结构可适当地根据所述硬碳涂层需要的低摩擦特性、耐磨性和耐久性来确定。虽然如此,还是希望所述硬碳涂层的氢含量从基体侧到滑动表面侧是逐层逐渐降低的。一种替代方案是,所述硬碳涂层的氢含量可按阶梯方式降低。
为了获得更大的降低摩擦效果,还希望使第二实施方式中所述硬碳涂层的最外层的氢含量最小。所述硬碳涂层的最外层的氢含量优选控制为20原子%或更低,更优选为10原子%或更低,更进一步优选为5原子%或更低,进而更优选为0.5原子%或更低,最优选基本为零。
在第一实施方式和第二实施方式的每一种中,所述硬碳涂层均可通过物理气相沉积(PVD)方法、化学气相沉积(CVD)方法或其组合形成。为了降低所述硬碳涂层最外层表面部分或最外层中的氢含量,在采用例如通过PVD电弧离子电镀法形成所述硬碳涂层时,降低涂覆气氛中氢的含量是有效的。
而且在用所述硬碳涂层涂覆之前,所述基体优选可通过镀铬法、氮化铬法、氮化法或其组合被赋予底涂层,以便提高所述硬碳涂层对所述基体的粘着性,改善其耐久性。
润滑剂
下述润滑油和润滑剂中的每一种都可用作润滑剂。
所述润滑油主要由基础油组成,优选含有无灰脂肪酸酯摩擦改进剂、无灰脂族胺摩擦改进剂、聚丁烯基琥珀酰亚胺、聚丁烯基琥珀酰亚胺的衍生物和二硫代磷酸锌中的至少一种物质。具体地,所述含无灰脂肪酸酯摩擦改进剂和无灰脂族胺摩擦改进剂中一种或两种的润滑油,可对于在本发明所述涂覆有硬碳薄膜的滑动件与由铁基或铝基材料制成的相对构件之间的滑动摩擦产生较大的摩擦降低效果。
所述基础油不作特别的限制,它可选自任意常用的基础油化合物,如矿物油、合成油和脂肪。
所述矿物油的具体实例包括正链烷烃油和链烷烃基油或环烷烃基油,它们是通过常压蒸馏或减压蒸馏从石油中提取润滑油馏分、然后采用任意的下述处理方法对所得到的润滑油馏分进行纯化而制得的:溶剂脱沥青、溶剂提取、加氢裂化、溶剂脱蜡、加氢精制、蜡异构化、硫酸处理和白土精制。虽然所述润滑油馏分一般通过加氢精制或溶剂精制进行纯化,但优选使用通过深度加氢裂化或GTL(气体到液体)蜡异构化方法降低所述油中芳烃含量来纯化所述润滑油馏分而制得的矿物油。
所述合成油的具体实例包括;聚α-烯烃(PAO),如1-辛烯低聚物、1-癸烯低聚物和乙烯-丙烯低聚物及其加氢产物;异丁烯低聚物及其加氢产物;异链烷烃;烷基苯;烷基萘;二酯,如戊二酸二(十三烷基)酯、己二酸二辛基酯、己二酸二异癸基酯、己二酸二(十三烷基)酯和癸二酸二辛基酯;多元醇酯,如三羟甲基丙烷酯(例如三羟甲基丙烷辛酸酯、三羟甲基丙烷壬酸酯和三羟甲基丙烷异硬脂酸酯)和季戊四醇酯(例如己酸季戊四醇-2-乙基酯和壬酸季戊四醇酯);聚氧亚烷基乙二醇;二烷基二苯基醚;和聚苯基醚。在这些合成油化合物中,优选的为聚α-烯烃,如1-辛烯低聚物和1-癸烯低聚物及其加氢产物。
上述基础油化合物可以单独使用,也可组合使用。在使用由两种或更多种基础油化合物的混合物作为基础油时,对于基础油化合物的混合比不作特别限定。
所述基础油的硫含量不受特别限制,基于所述基础油的总质量,优选为0.2%或更低,更优选为0.1%或更低,更进一步优选为0.05%或更低。希望使用加氢精制矿物油或合成油,这是因为加氢精制矿物油和合成油每种都具有不多于0.005%的硫含量,或基本不含硫(不多于5ppm)。
所述基础油的芳烃含量不受特别限制。此处,所述芳烃含量定义为按照ASTM D2549测得的芳烃馏分的含量。为了在延长的时间期限内使所述润滑油保持适合用于内燃机的低摩擦特性,基础油的芳烃含量基于基础油的总质量优选为15%或更低,更优选为10%或更低,更进一步优选为5%或更低。当基础油的芳烃含量超过15%时,润滑油的氧化稳定性将不利地发生劣化。
所述基础油的运动粘度不受特别限制。为了在内燃机中使用所述润滑油,所述基础油的运动粘度优选为2mm2/s或更高,更优选为3mm2/s或更高,并且同时优选为20mm2/s或更低,更优选为10mm2/s或更低,更进一步优选为8mm2/s或更低,它们都是在100℃时测得的。当所述基础油的运动粘度在100C低于2mm2/s时,所述润滑油就有可能不能提供充足的耐磨性,并引起相当大的蒸发损失。当所述基础油的运动粘度在100℃超过20mm2/s时,所述润滑油就有可能不能提供低摩擦特性,并使低温性能发生劣化。在组合使用两种或多种基础油化合物时,不需要限定每种基础油化合物的运动粘度均在这一特定范围内,只要所述基础油化合物的混合物在100℃时的运动粘度处于上述规定范围内即可。
所述基础油的粘度指数不受特别限制,为了在内燃机中使用所述润滑油,所述粘度指数优选为80或更高,更优选为100或更高,最优选为120或更高。当所述基础油具有较高粘度指数时,所述润滑油可以改善油耗性能和低温粘度性能。
至于脂肪酸酯摩擦改进剂和脂族胺摩擦改进剂,可以使用每个都具有C6-C30直链或支链烃链的脂肪酸酯和脂族胺,优选具有C8-C24直链或支链烃链,更优选具有C10-C20直链或支链烃链。当所述摩擦改进剂烃链的碳数不在6-30范围内时,可能不能产生想要的摩擦降低效果。所述脂肪酸酯和脂族胺摩擦改进剂的C6-C30直链或支链烃链的具体实例包括:烷基如己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基、十九烷基、二十烷基、二十一烷基、二十二烷基、二十三烷基、二十四烷基、二十五烷基、二十六烷基、二十七烷基、二十八烷基、二十九烷基和三十烷基;链烯基如己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一碳烯基、十二碳烯基、十三碳烯基、十四碳烯基、十五碳烯基、十六碳烯基、十七碳烯基、十八碳烯基、十九碳烯基、二十碳烯基、二十一碳烯基、二十二碳烯基、二十三碳烯基、二十四碳烯基、二十五碳烯基、二十六碳烯基、二十七碳烯基、二十八碳烯基、二十九碳烯基和三十碳烯基。上述烷基和链烯基均包括所有可能的异构体。
所述脂肪酸酯优选的例子有具有上述C6-C30烃基的脂肪酸和单羟基或多羟基脂族醇的酯。这类脂肪酸酯的具体实例包括甘油单油酸酯、甘油二油酸酯、山梨聚糖单油酸酯和山梨聚糖二油酸酯。
所述脂族胺优选的例子有每个均具有上述C6-C30烃基的脂族单胺及其环氧烷加合物、脂族多胺、咪唑啉及其衍生物。这类脂族胺的具体实例包括:脂族胺化合物如月桂基胺、月桂基二乙胺、月桂基二乙醇胺、十二烷基二丙醇胺、棕榈胺、硬脂胺、硬脂基四亚乙基五胺、油基胺、油基亚丙基二胺、油基二乙醇胺和N-羟乙基油基咪唑啉(N-hydroxyethyloleylimidazolyne);上述脂族胺化合物的环氧烷加合物,如N,N-二聚氧化烯-N-烷基或链烯基(C6-C28)胺和酸改性的化合物(通过使上述脂族胺化合物与C2-C30一元羧酸如脂肪酸或C2-C30多元羧酸(如草酸、苯二酸、偏苯三酸和1,2,4,5-苯四酸)反应以中和或酰胺化全部或部分的剩余氨基和/或亚氨基而制得)。其中N,N-二聚氧亚乙基-N-油基胺是优选使用的。
所述脂肪酸酯摩擦改进剂和/或脂族胺摩擦改进剂在润滑油中的含量不受特别限制,基于所述润滑油总质量,优选为0.05-3.0%,更优选为0.1-2.0%,最优选为0.5-1.4%。当润滑油中脂肪酸酯摩擦改进剂和/或脂族胺摩擦改进剂的含量低于0.05%时,就有可能不能获得足够的摩擦降低效果。当润滑油中脂肪酸酯摩擦改进剂和/或脂族胺摩擦改进剂的含量超过3.0%时,所述基础油中摩擦改进剂的溶解度就有可能变得很低,以致使所述润滑贮存稳定性劣化,引起沉淀。
至于聚丁烯基琥珀酰亚胺,可以使用由下述通式(1)和(2)表示的化合物:
在通式(1)和(2)中,PIB表示衍生自数均分子量为900-3500聚丁烯的聚丁烯基团,优选分子量为1000-2000,它可通过在氟化硼催化剂或氯化铝催化剂存在下聚合高纯异丁烯或1-丁烯和异丁烯的混合物而制得。当所述聚丁烯的数均分子量低于900时,就有可能不能提供充分的清洁作用。当所述聚丁烯的数均分子量超过3500时,所述聚丁烯基琥珀酰亚胺的低温流动性倾向于劣化。在用于制备聚丁烯基琥珀酰亚胺之前,聚丁烯可通过采用任意合适的处理方法(如吸附方法或洗涤方法)除去源自聚丁烯制备催化剂的痕量氟和氯残余物而对其进行纯化,由此来控制聚丁烯中氟和氯残余物的含量为50ppm或更低,希望为10ppm或更低,更希望为1ppm或更低。
而且考虑到清洁效果,在通式(1)和(2)中,n表示1-5的整数,优选为2-4的整数。
所述聚丁烯基琥珀酰亚胺的制备方法不受特别限制。例如所述聚丁烯基琥珀酰亚胺可通过下述方法制得:使聚丁烯的氯化物或聚丁烯(氟和氯残余物已经从中充分除去)与马来酸酐在100-200℃反应形成聚丁烯基琥珀酸酯,然后使所述聚丁烯基琥珀酸酯与多胺(如二亚乙基三胺、三亚乙基四胺、四亚乙基五胺或五亚乙基六胺)进行反应。
至于聚丁烯基琥珀酰亚胺衍生物,它们可使用硼或酸改性的化合物,可通过使通式(1)或(2)所述聚丁烯基琥珀酰亚胺与硼化合物或含氧有机化合物进行反应以中和或酰胺化全部或部分的剩余氨基和/或酰亚胺而制得。其中含硼聚丁烯基琥珀酰亚胺,尤其是含硼二(聚丁烯基)琥珀酰亚胺,是优选使用的。在含硼聚丁烯基琥珀酰亚胺化合物中氮与硼的含量之比(B/N)以质量计通常为0.1-3,优选为0.2-1.
用于制备聚丁烯基琥珀酰亚胺衍生物的硼化合物可以为硼酸、硼酸盐或硼酸酯。所述硼酸的具体实例包括原硼酸、偏硼酸和四硼酸。所述硼酸盐的具体实例包括:铵盐如硼酸铵,例如偏硼酸铵、四硼酸铵、五硼酸铵和八硼酸铵。所述硼酸酯的具体实例包括:硼酸和烷基醇(优选为C1-C6烷基醇)的酯,如硼酸单甲基酯、硼酸二甲基酯、硼酸三甲基酯、硼酸单乙基酯、硼酸二乙基酯、硼酸三乙基酯、硼酸单丙基酯、硼酸二丙基酯、硼酸三丙基酯、硼酸单丁基酯、硼酸二丁基酯和硼酸三丁基酯。
用于制备聚丁烯基琥珀酰亚胺衍生物的含氧有机化合物可以为任意C1-C30一元羧酸,如甲酸、乙酸、乙二醇酸、丙酸、乳酸、丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、十一烷酸、月桂酸、十三烷酸、肉豆蔻酸、十五烷酸、棕榈酸、十七烷酸、硬脂酸、油酸、十九烷酸、二十烷酸;C2-C30多元羧酸,如草酸、苯二甲酸、偏苯三酸和1,2,4,5-苯四酸,其酸酐和酯;C2-C6环氧烷;和羟基(多)氧亚烷基碳酸酯。
所述聚丁烯基琥珀酰亚胺和/或聚丁烯基琥珀酰亚胺衍生物存在于所述润滑油中的含量不受特别限制,基于所述润滑油总质量,优选为0.1-15%,更优选为1.0-12%。当所述润滑油中聚丁烯基琥珀酰亚胺和/或聚丁烯基琥珀酰亚胺衍生物的含量低于0.1%时,就有可能不能获得充分的清洁效果。当所述润滑油中聚丁烯基琥珀酰亚胺和/或聚丁烯基琥珀酰亚胺衍生物的含量超过15%时,所述润滑油的反乳化能力可能劣化。另外,在所述润滑油中添加如此大量的所述聚丁烯基琥珀酰亚胺和/或聚丁烯基琥珀酰亚胺衍生物,也是不经济的。
对于所述二硫代磷酸锌,它可以采用由下述通式(3)表示的化合物:
在通式(3)中,R4、R5、R6和R7中每个均表示C1-C24烃基。所述C1-C24烃基优选为C1-C24直链或支链烷基、C3-C24直链或支链链烯基、C5-C13环烷基或直链或支链烷基环烷基、C6-C18芳基或直链或支链烷基芳基或C7-C19芳基烷基。上述烷基或链烯基可为伯、仲或叔基。R4、R5、R6和R7的具体实例包括:烷基如甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基、十九烷基、二十烷基、二十一烷基、二十二烷基、二十三烷基和二十四烷基;链烯基如丙烯基、异丙烯基、丁烯基、丁二烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一碳烯基、十二碳烯基、十三碳烯基、十四碳烯基、十五碳烯基、十六碳烯基、十七碳烯基、十八碳烯基(油基)、十九碳烯基、二十碳烯基、二十一碳烯基、二十二碳烯基、二十三碳烯基和二十四碳烯基;环烷基如环戊基、环己基和环庚基;烷基环烷基如甲基环戊基、二甲基环戊基、乙基环戊基、丙基环戊基、乙基甲基环戊基、三甲基环戊基、二乙基环戊基、乙基二甲基环戊基、丙基甲基环戊基、丙基乙基环戊基、二丙基环戊基、丙基乙基甲基环戊基、甲基环己基、二甲基环己基、乙基环己基、丙基环己基、乙基甲基环己基、三甲基环己基、二乙基环己基、乙基二甲基环己基、丙基甲基环己基、丙基乙基环己基、二丙基环己基、丙基乙基甲基环己基、甲基环庚基、二甲基环庚基、乙基环庚基、丙基环庚基、乙基甲基环庚基、三甲基环庚基、二乙基环庚基、乙基二甲基环庚基、丙基甲基环庚基、丙基乙基环庚基、二丙基环庚基和丙基乙基甲基环庚基;芳基如苯基和萘基;烷基芳基如甲苯基、二甲苯基、乙基苯基、丙基苯基、乙基甲基苯基、三甲基苯基、丁基苯基、丙基甲基苯基、二乙基苯基、乙基二甲基苯基、四甲基苯基、戊基苯基、己基苯基、庚基苯基、辛基苯基、壬基苯基、癸基苯基、十一烷基苯基和十二烷基苯基;和芳基烷基,如苄基、甲基苄基、二甲基苄基、苯乙基、甲基苯乙基和二甲基苯乙基。上述烃基包括所有可能的异构体。尤其优选的是C1-C18直链或支链烷基和C6-C18芳基或直链或支链烷基芳基。
所述二硫代磷酸锌化合物优选的例子有:二异丙基二硫代磷酸锌、二异丁基二硫代磷酸锌、二仲丁基二硫代磷酸锌、二仲戊基二硫代磷酸锌、二正己基二硫代磷酸锌、二仲己基二硫代磷酸锌、二辛基二硫代磷酸锌、二-2-乙基己基二硫代磷酸锌、二正癸基二硫代磷酸锌、二正十二烷基二硫代磷酸锌和二异十三烷基二硫代磷酸锌。
所述润滑油中所述二硫代磷酸锌的含量不受特别限制。为了获得更大的摩擦降低效果,所述二硫代磷酸锌的含量基于所述润滑油总质量以所述磷元素计优选为0.1%或更低,更优选为0.06%或更低,最优选为最小有效量。当所述润滑油中二硫代磷酸锌含量超过0.1%时,就有可能抑制无灰脂肪酸酯摩擦改进剂和/或无灰脂族胺摩擦改进剂的摩擦降低效果,特别是对于所述DLC涂覆的滑动件与所述铁基相对构件之间的滑动摩擦。
所述二硫代磷酸锌的制备方法不受特别限制,所述二硫代磷酸锌可通过任意已知方法制得。例如所述二硫代磷酸锌可通过使具有上述R4、R5、R6和R7烃基的醇或酚与五硫化磷(P2O5)反应形成二硫代磷酸,然后用氧化锌中和二硫代磷酸而制得。要指出的是,二硫代磷酸锌的分子结构会随着用作制备所述二硫代磷酸锌的原料的醇或酚而不同。
上述二硫代磷酸锌化合物可以单独使用,也可以使用两种或多种化合物的混合物。在组合使用两种或多种二硫代磷酸锌化合物时,对于所述二硫代磷酸锌化合物的混合比不作特别限定。
为了改善用于内燃机的润滑油的性能,所述润滑油还可含有其它添加剂,如金属清洁剂、抗氧化剂、粘度指数改进剂、不同于上述提及的脂肪酸酯摩擦改进剂和脂族胺摩擦改进剂的摩擦改进剂、不同于上述提及的聚丁烯基琥珀酰亚胺和聚丁烯基琥珀酰亚胺衍生物的无灰分散剂、耐磨剂或极压剂、防锈剂、非离子型表面活性剂、破乳剂、金属钝化剂和/或消泡剂。
所述金属清洁剂可选自任意的常用于发动机润滑剂的金属清洁剂化合物。所述金属清洁剂的具体实例包括诸如钠(Na)和钾(K)之类碱金属或诸如钙(Ca)和镁(Mg)之类碱土金属的磺酸盐、酚盐和水杨酸盐;及其两种或多种的混合物。其中钠和钙的磺酸盐、钠和钙的酚盐和钠和钙的水杨酸盐是适合使用的。所述金属清洁剂的总碱值和含量可根据润滑油所需要的性能进行选择。所述金属清洁剂的总碱值通常为0-500mgKOH/g,优选为150-400mgKOH/g,它是按照ISO 3771利用高氯酸测得的。所述金属清洁剂的含量通常为所述润滑油总质量的0.1-10%。
所述抗氧化剂可选自任意的常用于发动机润滑油的抗氧化剂化合物。所述抗氧化剂的具体实例包括:酚类抗氧化剂,如4,4’-亚甲基二(2,6-二-叔丁基苯酚)和十八烷基-3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯;氨基抗氧化剂,如苯基-α-萘胺、烷基苯基-α-萘胺和烷基二苯基胺;及其两种或多种的混合物。所述抗氧化剂的含量通常为所述润滑油总质量的0.01-5%。
对于所述粘度指数改进剂,可以使用的有:非分散型聚甲基丙烯酸酯粘度指数改进剂,如一种或多种甲基丙烯酸的共聚物及其加氢产物;分散型聚甲基丙烯酸酯粘度指数改进剂,如还含有氮化合物的甲基丙烯酸酯的共聚物;及其它粘度指数剂,如乙烯和α-烯(例如丙烯、1-丁烯和1-戊烯)的共聚物及其加氢产物、聚异丁烯及其加氢产物、苯乙烯-二烯加氢共聚物、苯乙烯-马来酸酐共聚物和聚烷基苯乙烯。考虑到剪切稳定性,需要对所述粘度指数改进剂的分子量进行选择。例如所述粘度指数改进剂的数均分子量,对于所述分散型或非分散型聚甲基丙烯酸酯来说,希望在5000-1000000范围内,更希望为100000-800000;对于所述聚异丁烯或其加氢产物来说,该分子量在800-5000范围内;对于所述乙烯/α-烯烃共聚物或其加氢产物来说,该分子量在800-300000范围内,更优选为10000-200000。上述粘度指数改进化合物可以单独使用,也可以以其两种或多种的混合物形式使用。所述粘度指数改进剂的含量优选为所述润滑油总质量的0.1-40.0%。
所述不同于上述提及的脂肪酸酯摩擦改进剂和脂族胺摩擦改进剂的摩擦改进剂,可以列举的有:无灰摩擦改进剂,如硼酸酯、更高级的醇和脂族醚,和金属摩擦改进剂,如二硫代磷酸钼、二硫代氨基甲酸钼和二硫化钼。
所述不同于上述提及聚丁烯基琥珀酰亚胺和聚丁烯基琥珀酰亚胺衍生物的无灰分散剂,可为任意一种具有数均分子量为900-3500的聚丁烯基的聚丁烯基苄胺和聚丁烯基胺、具有数均分子量低于900的聚丁烯基的聚丁烯基琥珀酰亚胺及其衍生物。
对于所述耐磨剂或极压剂,可以使用:二硫化物、硫化脂肪、烯烃硫化物、具有1-3个C2-C20烃基的磷酸酯、硫代磷酸酯、亚磷酸酯、硫代亚磷酸酯和这些酯的胺盐。
对于所述防锈剂,可以使用:烷基苯磺酸酯、二壬基萘磺酸酯、烯基琥珀酸的酯和多元醇的酯。
对于所述非离子型表面活性剂和破乳剂,可以使用:非离子型聚亚烷基二醇表面活性剂,如聚氧亚乙基烷基醚、聚氧亚乙基烷基苯基醚和聚氧亚乙基烷基萘基醚。
所述金属钝化剂可以列举的有:咪唑啉、嘧啶衍生物、噻唑和苯并三唑。
所述消泡剂可以列举的有:硅酮、氟代硅酮和氟代烷基醚。
所述不同于脂肪酸酯和脂族胺摩擦改进剂的摩擦改进剂、所述不同于聚丁烯基琥珀酰亚胺和聚丁烯基琥珀酰亚胺衍生物的无灰分散剂、所述耐磨剂或极压剂、所述防锈剂和所述破乳剂中,每种物质的含量通常均为所述润滑油总质量的0.01-5%,所述金属钝化剂的含量通常为所述润滑油总质量的0.005-1%,所述消泡剂的含量通常为所述润滑油总质量的0.0005-1%。
所述润滑剂主要由具有羟基的化合物组成,它能够对本实施方式所述涂覆有硬碳涂层的滑动件与由铁基或铝基材料制成的相对构件之间的滑动摩擦产生较大的摩擦降低效果。所述含羟基化合物的具体实例包括醇。在各种醇中,甘油或乙二醇优选用作所述润滑剂。
参考下述实施例,对本发明进行更详细的说明。但需要指出的是,下述实施例仅是例证性的,而不是对本发明的限制。
[准备测试样品]
实施例1
首先从S45C钢材(按照JIS G4051)上切割下基本为半圆柱状的钢件(作为基体),其尺寸为8×12×40mm。采用CVD法,在所述切割件的半圆柱状面上形成一层氢含量为20原子%和厚度为10μm的DLC涂层(作为内涂层)。然后采用PVD电弧离子电镀法,形成另一层氢含量为5原子%和厚度为0.5μm的DLC涂层(作为外涂层),从而得到测试样品。然后,采用不含添加剂的聚α-烯烃油作为润滑油,对所述测试样品进行下述的摩擦/磨损测试。
实施例2
首先从S45C钢材(按照JIS G4051)上切割下基本为半圆柱状的钢件(作为基体),其尺寸为8×12×40mm。采用CVD法,在所述切割件的半圆柱状面上形成一层氢含量为20原子%和厚度为10μm的DLC涂层(作为内涂层)。然后采用PVD电弧离子电镀法,形成另一层氢含量为0.5原子%和厚度为0.5μm的DLC涂层(作为外涂层),从而得到测试样品。然后,采用不含添加剂的聚α-烯烃油作为润滑油,对所述测试样品进行摩擦/磨损测试。
实施例3
首先从S45C钢材(按照JIS G4051)上切割下基本为半圆柱状的钢件(作为基体),其尺寸为8×12×40mm。采用CVD法,在所述切割件的半圆柱状面上形成一层氢含量为20原子%和厚度为10μm的DLC涂层(作为内涂层)。然后采用PVD电弧离子电镀法,形成另一层氢含量为0.5原子%和厚度为0.5μm的DLC涂层(作为外涂层),从而得到测试样品。然后,采用混有1质量%甘油单油酸酯(作为无灰脂肪酸酯摩擦改进剂)的聚α-烯烃油作为润滑油,对所述测试样品进行摩擦/磨损测试。
实施例4
首先从S45C钢材(按照JIS G4051)上切割下基本为半圆柱状的钢件(作为基体),其尺寸为8×12×40mm。采用CVD法,在所述切割件的半圆柱状面上形成一层氢含量为20原子%和厚度为10μm的DLC涂层(作为内涂层)。然后采用PVD电弧离子电镀法,形成另一层氢含量为0.5原子%和厚度为0.5μm的DLC涂层(作为外涂层),从而得到测试样品。然后,采用甘油作为润滑剂,对所述测试样品进行摩擦/磨损测试。
对比例1
从S45C钢材(按照JIS G4051)上切割下基本为半圆柱状的钢件(作为基体),其尺寸为8×12×40mm。在所述切割件的半圆柱状面上形成一层厚度为50μm的镀铬涂层,从而得到测试样品。然后,采用不含添加剂的聚α-烯烃油作为润滑油,对所述测试样品进行摩擦/磨损测试。
对比例2
从S45C钢材(按照JIS G4051)上切割下基本为半圆柱状的钢件(作为基体),其尺寸为8×12×40mm。在所述切割件的半圆柱状面上形成一层厚度为20μm的氮化钛(TiN)涂层,从而得到测试样品。然后,采用不含添加剂的聚α-烯烃油作为润滑油,对所述测试样品进行摩擦/磨损测试。
对比例3
从S45C钢材(按照JIS G4051)上切割下基本为半圆柱状的钢件(作为基体),其尺寸为8×12×40mm。在所述切割件的半圆柱状面上形成一层厚度为20μm的氮化铬(CrN)涂层,从而得到测试样品。然后,采用不含添加剂的聚α-烯烃油作为润滑油,对所述测试样品进行摩擦/磨损测试。
对比例4
从S45C钢材(按照JIS G4051)上切割下基本为半圆柱状的钢件(作为基体),其尺寸为8×12×40mm。采用CVD法,在所述切割件的半圆柱状面上形成一层氢含量为20原子%和厚度为10μm的DLC涂层,从而得到测试样品。然后,采用混有1质量%甘油单油酸酯(作为无灰脂肪酸酯摩擦改进剂)的聚α-烯烃油作为润滑油,对所述测试样品进行摩擦/磨损测试。
[根据摩擦/磨损测试进行性能评价]
摩擦/磨损测试是在下述条件下使用一种往复式摩擦/磨损测试器进行的。在所述摩擦/磨损测试器中,各实施例1-4和对比例1-4中的测试样品(10)按图2所示进行放置,从而当所述测试样品(10)的半圆柱状部分(10a)于负荷L下在板状相对样品(11)的区域A上滑动时,其能够沿方向S和T进行往复运动。此处,所述相对样品是由FC250铸铁(按照JIS G5501)制成的。在测试中,在所述测试样品(10)与所述相对样品(11)之间的摩擦系数是在所述区域A的转向端测得的。而且所述测试样品(10)的磨损量是在测试之后测得的。测量结果如表中所示。在该表中,实施例1、2和4和对比例1-4的测试样品的磨损量是参照实施例3的测试样品的磨损量(1.0)进行表示的。
(测试条件)
测试样品(10):由S45C钢制基体及其上的涂层形成并具有8×12×40
mm尺寸的半圆柱状件
相对样品(11):由FC250铸铁制成并具有40×60×7mm尺寸的板状件
测试装置: 往复摩擦/磨损测试器
往复运动: 600循环/分钟
测试温度: 25℃
施加负载(P): 98N
测试时间: 60min
实施例1-4的滑动件比对比例1-4的滑动件具有更低的摩擦系数和更小的磨损量,而且本发明的意料不到的结果清楚地显示在该表中。其中考虑到实施例4的滑动件比实施例1-3的具有更低摩擦系数和更小磨损量的事实,认为实施例4提供了最好的结果。
如上所述,通过本发明的确定结构的硬碳涂层和特定润滑剂的组合,所述滑动件表现出优良的低摩擦特性和耐久性。因此,通过在内燃机中使用本发明的滑动件,有可能比使用较早技术的用含有机钼化合物的润滑油润滑钢制滑动件获得燃料效率的更大改善。
日本专利申请No.2003-206809(2003年8月8日申请)和申请No.2004-225411(2004年8月2日申请)的全部内容引入此处作为参考。
虽然已经参考本发明的特定实施方式对本发明进行了说明,但本发明并不局限于上述实施方式。根据上述教导,本领域技术人员将会对上述实施方式进行各种不同的改进和改变。本发明的范围由所附权利要求进行限定。
表
摩擦系数 | 磨损量 | |
实施例1 | 0.07 | 1.5 |
实施例2 | 0.06 | 1.2 |
实施例3 | 0.04 | 1.0(参比) |
实施例4 | 0.02 | 1.0 |
对比例1 | 0.18 | 5.4 |
对比例2 | 0.17 | 3.5 |
对比例3 | 0.15 | 2.0 |
对比例4 | 0.13 | 1.8 |
Claims (31)
1.一种滑动件,包括:
基体;和
硬碳涂层,其形成于所述基体上以限定在润滑作用下与相对构件滑动接触的滑动表面,所述硬碳涂层的最外层表面部分的氢含量低于其剩余部分。
2.权利要求1所述滑动件,其中所述硬碳涂层的最外层表面部分的氢含量为20原子%或更低。
3.权利要求2所述滑动件,其中所述硬碳涂层的最外层表面部分的氢含量为10原子%或更低。
4.权利要求3所述滑动件,其中所述硬碳涂层的最外层表面部分的氢含量为5原子%或更低。
5.权利要求4所述滑动件,其中所述硬碳涂层的最外层表面部分的氢含量为0.5原子%或更低。
6.权利要求1所述滑动件,其中所述硬碳涂层的氢含量沿其厚度方向从基体侧到滑动表面侧逐渐降低。
7.一种滑动件,包括:
基体;和
硬碳涂层,其形成于所述基体上以限定在润滑作用下与相对构件滑动接触的滑动表面,所述硬碳涂层具有沿其厚度方向层压在一起的两层或多层涂层,所述层压涂层包括氢含量低于至少一个其它涂层的最外层涂层。
8.权利要求7所述滑动件,其中所述最外层涂层的氢含量低于所有其它涂层。
9.权利要求7所述滑动件,其中所述最外层涂层的氢含量为20原子%或更低。
10.权利要求9所述滑动件,其中所述最外层涂层的氢含量为10原子%或更低。
11.权利要求10所述滑动件,其中所述最外层涂层的氢含量为5原子%或更低。
12.权利要求11所述滑动件,其中所述最外层涂层的氢含量为0.5原子%或更低。
13.权利要求1或7所述滑动件,还包括施用到所述滑动表面上的润滑油,所述润滑油中含有至少一种选自无灰脂肪酸酯摩擦改进剂和无灰脂族胺摩擦改进剂的摩擦改进剂。
14.权利要求13所述滑动件,其中所述至少一种摩擦改进剂具有C6-C30烃基,其含量基于所述润滑油总质量计为0.05-3.0%。
15.权利要求13所述滑动件,其中所述润滑油含有聚丁烯基琥珀酰亚胺和/或其衍生物。
16.权利要求15所述滑动件,其中所述聚丁烯基琥珀酰亚胺和/或其衍生物的含量基于所述润滑油总质量计为0.1-15%。
17.权利要求13所述滑动件,其中所述润滑油含有二硫代磷酸锌,其含量基于所述润滑油总质量以磷的质量计为0.1%或更低。
18.权利要求1或7所述滑动件,还包括施用到所述滑动表面上的润滑剂,所述润滑剂主要由含羟基化合物组成。
19.权利要求18所述滑动件,其中所述含羟基化合物是醇。
20.权利要求19所述滑动件,其中所述醇为甘油或乙二醇。
21.权利要求1或7所述滑动件,其中在形成所述硬碳涂层之前,所述基体已经通过选自镀铬法、氮化铬法和氮化法的至少一种方法被赋予底涂层。
22.权利要求1或7所述滑动件,其中所述滑动件是发动机活塞环。
23.权利要求22所述滑动件,其中所述活塞环是顶环和甩油环中的至少一种。
24.一种生产滑动件的方法,包括:
提供所述滑动件的基体;和
在所述基体上形成硬碳涂层,其形成方式应使所述硬碳涂层的最外层表面部分的氢含量低于其剩余部分。
25.权利要求24所述方法,其中所述形成步骤包括控制最外层表面部分的氢含量为20原子%或更低。
26.权利要求24或25所述方法,还包括向所述硬碳涂层上施用润滑油,其中所述润滑油中含有至少一种选自无灰脂肪酸酯摩擦改进剂和无灰脂族胺摩擦改进剂的摩擦改进剂。
27.权利要求24或25所述方法,还包括向所述硬碳涂层上施用润滑剂,其中所述润滑剂主要由含羟基化合物组成。
28.一种生产滑动件的方法,包括:
提供所述滑动件的基体;和
在所述基体上形成硬碳涂层,其形成方式应使所述硬碳涂层的最外层涂层的氢含量低于至少一个其它涂层。
29.权利要求28所述方法,其中所述形成步骤包括控制最外层涂层的氢含量为20原子%或更低。
30.权利要求28或29所述方法,还包括向所述硬碳涂层上施用润滑油,其中所述润滑油中含有至少一种选自无灰脂肪酸酯摩擦改进剂和无灰脂族胺摩擦改进剂的摩擦改进剂。
31.权利要求28或29所述方法,还包括向所述硬碳涂层上施用润滑剂,其中所述润滑剂主要由含羟基化合物组成。
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Cited By (4)
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CN104955984B (zh) * | 2013-01-28 | 2018-06-12 | 日产自动车株式会社 | 滑动构件和其制造方法 |
CN107923533A (zh) * | 2015-08-10 | 2018-04-17 | 日本Itf株式会社 | 活塞环及其制造方法 |
CN109595453A (zh) * | 2017-10-03 | 2019-04-09 | 丰田自动车株式会社 | 滑动系统 |
CN110894605A (zh) * | 2018-12-21 | 2020-03-20 | 纳峰真空镀膜(上海)有限公司 | 耐腐蚀碳基涂层 |
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EP1505322A1 (en) | 2005-02-09 |
US20050100701A1 (en) | 2005-05-12 |
EP1505322B1 (en) | 2008-10-08 |
EP1990564B1 (en) | 2009-12-16 |
JP2005089735A (ja) | 2005-04-07 |
JP4973971B2 (ja) | 2012-07-11 |
US8575076B2 (en) | 2013-11-05 |
DE602004016923D1 (de) | 2008-11-20 |
US20090054277A1 (en) | 2009-02-26 |
CN100344890C (zh) | 2007-10-24 |
US7458585B2 (en) | 2008-12-02 |
DE602004024728D1 (de) | 2010-01-28 |
EP1990564A1 (en) | 2008-11-12 |
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