CN1332232A - 水系润滑剂及金属材料的表面处理方法 - Google Patents

水系润滑剂及金属材料的表面处理方法 Download PDF

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CN1332232A
CN1332232A CN01118416A CN01118416A CN1332232A CN 1332232 A CN1332232 A CN 1332232A CN 01118416 A CN01118416 A CN 01118416A CN 01118416 A CN01118416 A CN 01118416A CN 1332232 A CN1332232 A CN 1332232A
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resin
lubricant
molybdenumdisulphide
millimicron
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川越亮助
藤井政明
吉田昌之
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NIPPON BACALAIJINGU CO Ltd
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Abstract

本发明公开了一种在金属材料表面上形成滑动润滑性优良薄膜用的水系润滑剂及其表面的处理方法,该水系润滑剂特征在于其中含有平均粒径0.5～10毫微米的二硫化钼,以及断裂强度为300千克/平方厘米以上、断裂延伸率在10%以下、平均分子量在5000～50000的水系树脂,所述的水系树脂是聚酯树脂或水性聚氨酯树脂。

Description

水系润滑剂及金属材料的表面处理方法
本发明涉及在金属材料表面上形成一种滑动润滑性优良薄膜用的水系润滑剂及其表面的处理方法。更具体讲，本发明涉及由二硫化钼和具有特定性质的树脂组成的水系润滑剂，以及使用这种润滑剂的金属材料表面的处理方法。
二硫化钼自古以来就作为固体润滑剂使用，即使现在也还在以各种汽车部件为首的各种用途中使用。过去一般采用的方法是，将二硫化钼润滑剂和聚酰胺酰亚胺粘合剂溶解在有机溶剂中，将其喷涂后进行烧结。然而，近年来从保护地球环境观点来看，人们强烈地希望开发不用有机溶剂的水系润滑剂。
另一方面，在二十世纪四十年代，磷酸锰处理作为钢铁用防锈处理就已实用化，其后逐渐将磷酸锰薄膜作为滑动薄膜使用。因为与其它化成膜相比，坚硬、耐磨损性优良、初期磨合性好而且是多孔物质，能够使材料表面保持润滑油，具有润滑油保持特性。因为未实施表面处理的滑动部分会有金属间接触，局部产生高温和高压。在这种状态下滑动时局部将出现显著磨损，使构件劣化。因此，防止金属间直接接触是十分重要的，而表面上形成磷酸锰薄膜对于防止这种金属间的直接接触是有效的，实际上已经用于许多滑动部件上。但是，近年来人们对滑动部件的使用条件(荷载)提出了许多更严格要求，而且希望部件的使用寿命长。因此许多场合下，传统的磷酸锰薄膜已不能单独获得所需的充分性能。
为了改善薄膜的摩擦学特性，有人提出在磷酸锰上形成二硫化钼罩面涂层的方法。例如，特公平7-113401号公报(真空环境用齿轮传动机构)中公开了一种真空环境用齿轮传动机构，其特征在于它是至少在齿轮的啮合部分由合金工具钢制成，在此啮合部分依次形成磷酸锰底层和固定润滑膜固体的润滑齿轮，而固体润滑膜优选由二硫化钼形成。但是，关于形成固体润滑膜的润滑剂用粘合剂却没有任何记载。而特开平9-184079号公报(耐磨损构件)公开了一种耐磨损构件，其中至少在压力环的上下表面上设有磷酸锰层，以及在其晶粒间隙间分散有平均粒径1～2毫微米的二硫化钼的润滑剂层。在公开的此方法中，作为优选的粘合剂举出了聚酰胺酰亚胺、环氧树脂、聚酰亚胺和聚四氟乙烯，但是却未触及该树脂的机械性质。其实施例中使用聚酰胺酰亚胺作粘合剂，采用的是有机溶剂系的涂装方法。
本发明是为解决现有技术中存在的这些问题而提出的，具体而言本发明目的在于提供一种以低成本和在环境污染小的条件下形成新颖的水系润滑剂及其表面的处理方法。
本发明人就上述现有技术存在问题的解决手段进行深入研究，结果发现由特定粒径的二硫化钼和具有特定机械特性的树脂组成的水系润滑剂以及使用这种润滑剂的表面处理方法，此外还发现使之形成特定磷酸锰薄膜层和润滑剂层组成的复合膜的方法。
也就是说，本发明涉及一种水系润滑剂，其特征在于其中含有平均粒径0.5～10毫微米的二硫化钼，以及断裂强度为300千克/平方厘米以上、断裂延伸率在10％以下、平均分子量在5000～50000的水系树脂。其中所说的水系树脂优选聚酯树脂或水性聚氨酯树脂。此外，本发明还提供了一种金属材料的表面处理方法，其特征在于使用所述的水系润滑剂与清洁的金属材料表面接触，形成含有以钼计0.1～5.0克/平方米二硫化钼，以碳计0.1～5.0克/平方米树脂的水系润滑剂薄膜层，然后在100～250℃下进行烧结。本发明也提供了一种金属材料的表面处理方法，其特征在于使用所述的润滑剂与薄膜厚度为1～15毫微米、结晶粒径为0.5～30毫微米、表面粗糙度(Rz)为0.5～20毫微米的被晶状磷酸锰薄膜覆盖的金属表面接触，使之形成含有以钼计0.1～5.0克/平方米二硫化钼，以碳计0.1～5.0克/平方米树脂的水系润滑剂薄膜层后，在100～250℃下进行烧结，使之形成由磷酸锰薄膜层和润滑薄膜层组成的复合膜。
以下详细说明本发明。
对用作本发明处理对象的材料并无特别限制，主要适用于钢铁材料，例如炭素钢、铬合金钢、铬钼合金钢、高碳铬合金钢、铝、铝合金等。
本发明的水系润滑剂可以采用使二硫化钼和水系树脂分散在水中的方法制造。本发明的水系润滑剂中使用二硫化钼的平均粒径必须处于0.5～10毫微米范围内。用平均粒径处于此范围内的二硫化钼可以获得优良滑动特性。低于0.5毫微米时在性能上虽无问题，但是成本增高，不好。另一方面若超过10毫微米，在润滑剂中的分散就会恶化，也不好。本发明水系润滑剂中用的水系树脂，是能在水中溶解或分散使用的一些树脂，例如聚酯树脂、聚氨酯树脂、多酚树脂等。特别优选聚酯树脂或水性聚氨酯树脂(分散液)。聚酯系树脂可以举出用对苯二甲酸或间苯二甲酸的砜化物作为共聚成份的聚酯树脂；而聚氨酯系树脂可以举出以聚醚多元醇、聚酯多元醇等多元醇，以及联甲苯胺二异氰酸酯、苄撑二异氰酸酯等聚异氰酸酯为基料的水性聚氨酯树脂。这些树脂必须使用断裂强度为300千克/平方厘米以上、断裂延伸率在10％以下、平均分子量5000～50000的，因为断裂强度高而延伸率低的树脂有优良的耐磨损性。其中平均分子量对处理剂的分散性有影响，所以必须处于此范围内。
以下说明用上述水系润滑剂处理金属材料表面的方法。这种金属材料的表面处理方法是：首先使所说的水系润滑剂与清洁的金属材料表面接触，形成含有以钼计0.1～5.0克/平方米的二硫化钼，以碳计0.1～5.0克/平方米树脂的水系润滑剂薄膜层，然后在100～250℃下进行烧结。通过这种烧结，使金属材料表面形成含有以钼计0.1～5.0克/平方米钼和以碳计0.1～5.0克/平方米碳的润滑剂薄膜。经过这种烧结干燥后，钼和碳的各自附着量低于0.1克/平方米时得不到足够的滑动性，而钼和碳的各自附着超过5.0克/平方米虽然没有特别问题，但经济性却变差。
对水系润滑剂与金属材料的接触方法没有特别限制，可以采用浸渍法和喷涂法等。其中包括使水系润滑剂以原液形式或者以稀释处理液形式接触。而且也可以并用表面活性剂，以便使二硫化钼均一涂布。对这种处理液中二硫化钼和树脂的浓度没有特别限制，其各自浓度通常0.1～1％左右较优。浓度低于0.1％时，涂布次数少时不能获得预定涂布量，因此使工序延长在经济上不合算。反之一旦超过1％，就会使处理液的稳定性劣化也不好。
然后在100～250℃温度下进行烧结和干燥，使之形成润滑薄膜层。这种烧结干燥的目的在于挥发水份，使所用的树脂流动，即树脂将软化平滑，具有更高的附着性，所以烧结干燥温度必须处于上述范围，更处于150～200℃范围较优。
对钢铁材料实施上述金属材料表面处理方法时，从滑动润滑性、附着性和耐腐蚀性角度看，应当首先在表面上形成磷酸锰薄膜，形成的磷酸锰薄膜控制在1～15毫微米薄膜厚度内，晶粒直径为0.5～30毫微米，表面粗糙度(Rz)为0.5～20毫微米范围内较优。薄膜厚度低于1毫微米时，耐烧伤程度降低，不好。薄膜厚度超过15毫微米时，性能上虽然没有差别但是经济性却变差。晶粒直径低于0.5毫微米时耐荷载不充分，而超过30毫微米时摩擦系数增高，也不好。表面粗糙度(Rz)低于0.5毫微米时附着性降低，而超过20毫微米时表面粗糙度增大，润滑薄膜的覆盖性差，所以都不好。
以下就本发明特定的上述薄膜厚度、晶粒直径、表面粗糙度、钼附着量和碳附着量的测定方法进行说明。也就是说，磷酸锰薄膜的薄膜厚度，是将化成处理后的构件剖开后，用金属显微镜观察断面的方法测定的。而晶粒直径是用市售的扫描电子显微镜(SEM)表面观察的方法测定的。表面粗糙度是用市售的表面粗糙度计测定的。
钼附着量用市售荧光X射线分析装置(XRF)定量测定。首先测定不同钼附着量已知的数个样品，然后根据得到的强度绘制强度一附着量工作曲线。进而在同样条件下将本发明表面处理方法处理过的样品切成适当大小(φ3厘米左右)后测定。根据上述工作曲线将这些测得的强度换算成钼附着量。碳附着量的测定用市售的表面碳分析装置(TOC)进行。将本发明表面处理方法处理的样品切成适当大小(20～50厘米左右)制成样品。表面碳分析装置的工作原理是，样品升温时表面上存在的碳氧化气化，用红外吸收光谱分析法(IR)进行定量测定。测定时采用能使表面上碳氧化气化的条件，一般优选的条件是400℃下测定5分钟。
以下列举几个实施例与比较例以便说明本发明的有用性。材料：
对下述钢铁材料进行了处理。
平板：S45C，尺寸：30mm×80mm，厚度1mm
滑动润滑试验片(SRV)：SUJ2  24×8mm前处理
洗涤处理：用市售洗涤剂(注册商标Finecleaner-4360，日本PARKERIZING股份有限公司制)的2％水溶液60℃下浸渍3分钟后，自来水洗涤30秒钟。
磷酸锰处理：洗涤处理后，浸渍在市售的表面调整剂(注册商标-Prepalan 55(实施例3)或Prepalan VM(实施例4和对照例2)，均为日本PARKERIZING股份有限公司制)的3％水溶液中，接着用市售的磷酸锰化成剂(注册商标Parhos M1A，PARKERIZING股份有限公司制)的15％水溶液在95℃下作5分钟浸渍处理。其后水洗和干燥。
实施例一：
在上述洗涤处理过的钢铁材料表面上涂布下述表面处理液1后，在160℃下进行10分钟烧结。
表面处理液1；
二硫化钼：平均粒径2.0毫微米
水系树脂：聚酯系树脂
树脂断裂强度：350千克/平方厘米
树脂延伸率：2％
树脂的平均分子量：10000
处理液1是将二硫化钼粉末分散在聚酯树脂水分散液中制成的。
实施例二：
在上述洗涤处理过的钢铁材料表面上涂布下述表面处理液2后，在200(下进行10分钟烧结。
表面处理液2：
二硫化钼(平均粒径)：4.0毫微米
水系树脂：聚酯系树脂
树脂断裂强度：320千克/平方厘米
树脂延伸率：1％
树脂的平均分子量：12000
处理液2是将二硫化钼粉末分散在聚酯树脂水分散液中制成的。
实施例三：
对上述洗涤处理过的钢铁材料实施磷酸锰处理，然后在表面上涂布下述表面处理液3，最后在220℃下进行5分钟烧结。
表面处理液3：
二硫化钼(平均粒径)：20毫微米
水系树脂：水性聚氨酯树脂
树脂断裂强度：310千克/平方厘米
树脂延伸率：5％
树脂的平均分子量：8000
处理液3是二硫化钼粉末分散在聚酯树脂水性分散液中制成的。
实施例四：
将上述洗涤处理过的钢铁材料，在加热到65℃的下述表面处理液4中浸渍处理10分钟。接着水洗和干燥。然后涂布实施例三使用的表面处理液3，180℃下进行10分钟烧结。
表面处理液4：
二硫化钼(平均粒径)：15毫微米
水系树脂：水性聚氨酯树脂
树脂断裂强度：350千克/平方厘米
树脂延伸率：3％
树脂的平均分子量：15000
处理液4是二硫化钼粉末分散在聚酯树脂水性分散液中制成。比较例1：
仅进行上述洗涤处理，不实施其后的表面处理。比较例2；
仅进行上述洗涤处理及磷酸锰处理，未实施其后的表面处理。
表1所示有关实施例一～四以及对照例1和2中磷酸锰层薄膜厚度、粒径和粗糙度、表面处理后形成的润滑薄膜层中钼量和碳量、以及滑动润滑评价结果。滑动润滑试验用以下方法进行。滑动润滑试验
用市售SRV试验机进行了评价。将处理过的试验片和未处理的钢球(SUJ2，直径10毫米)组合，在100牛顿载荷、50赫兹振动频率、2毫米振幅下不涂油滑动。测定摩擦系数及摩擦系数达到0.6前所需的时间。此时间越长，润滑性越好。
表1所示的资料说明，本发明可以得到优良的润滑性。
表1
         磷酸锰薄膜层     润滑薄膜层 滑动润滑评价
   厚度(μm)    粒径(μm)   粗糙度(μm)     Mo(g/m2)     C(g/m2) SRV滑动时间(秒)
实施例一     -     -     -     1.5     1.5     200
实施例二     -     -     -     2.0     2.0     200
实施例三     3     2    1.5     3.0     3.0     300
实施例四     10     20     8     4.0     4.0     300
比较例1     0     0      0      0       5
比较例2     10     8     8      0      0      25
本发明采用特定的水系树脂制成水系润滑剂，然后用此水系润滑剂进行金属材料表面处理，这样能在低成本和环境污染小的条件下使金属材料表面形成具有极优良滑动润滑特性的薄膜，产生优良效果。

Claims (4)

1.一种水系润滑剂，其特征在于：含有平均粒径在0.5～10毫微米的二硫化钼和断裂强度在300千克/平方厘米以上、断裂延伸率在10％以下、平均分子量在5000～50000的水系树脂。
2.根据权利要求1所述的水系润滑剂，其特征在于：所述的水系树脂是聚酯树脂或水性聚氨酯树脂。
3.一种金属材料的表面处理方法，其特征在于：用如权利要求1或2所述的水系润滑剂与清洁的金属材料表面接触，形成含有以钼计0.1～5.0克/平方米的二硫化钼，以碳计0.1～5.0克/平方米树脂的水系润滑剂薄膜层后，在100～250℃温度下进行烧结。
4.一种金属材料的表面处理方法，其特征在于：用如权利要求1或2所述的水系润滑剂与薄膜厚度为1～15毫微米、结晶粒径在0.5～30毫微米、表面粗糙度(Rz)为0.5～20毫微米的被晶状磷酸锰薄膜覆盖的金属表面接触，形成含有以钼计0.1～5.0克/平方米的二硫化钼，以碳计0.1～5.0克/平方米树脂的水系润滑剂薄膜层后，在100～250℃下进行烧结，使之形成由磷酸锰薄膜层和润滑薄膜层组成的复合膜层。
CN01118416A 2000-06-28 2001-05-30 水系润滑剂及金属材料的表面处理方法 Pending CN1332232A (zh)

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CN101205499B (zh) * 2007-11-28 2010-06-09 周贤言 一种铝镁合金拉丝润滑剂
CN105315741A (zh) * 2014-08-05 2016-02-10 东莞金太阳研磨股份有限公司 一种水性环保防堵塞涂层

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JP4671609B2 (ja) * 2004-01-26 2011-04-20 日本パーカライジング株式会社 潤滑性水系ポリウレタン樹脂組成物、それを用いる亜鉛系メッキ鋼板の表面潤滑処理方法及びその表面処理鋼板
JP2008069413A (ja) * 2006-09-14 2008-03-27 Nippon Steel & Sumikin Stainless Steel Corp 潤滑鋼板
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