CN1788071A - 固体润滑剂和滑动部件 - Google Patents
固体润滑剂和滑动部件 Download PDFInfo
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Abstract
本发明提供一种在高负载条件下能够发挥与含铅固体润滑剂同等或同等以上滑动特性的无铅固体润滑剂。该润滑剂是埋入在滑动部件基体的滑动面上形成的孔或沟中的固体润滑剂,含有20~40重量%的选自烃类蜡、高级脂肪酸、高级脂肪酸酯和高级脂肪酸酰胺的1种或2种以上的蜡类、和20~40重量%的三聚氰胺氰尿酸酯、以及20~50重量%的四氟乙烯树脂。
Description
技术领域
本发明涉及固体润滑剂和滑动部件,更详细地涉及埋入在滑动部件基体的滑动面上形成的孔或沟中的固体润滑剂和滑动部件。
背景技术
在轴承等的滑动面上埋入而使用的固体润滑剂,在滑动面上形成为薄膜,发挥滑动作用。因此,该覆盖膜形成的好坏对摩擦系数和覆盖膜寿命有较大的影响。作为该种固体润滑剂,可以列举具有层状结构的、特别是以石墨为主要成分的润滑剂。石墨由于其层状结构,对负载方向显示大的阻力,但对滑动方向的阻力小。而且,是软质,在从常温至高温的范围内具有可以保持润滑性能的特性。
但是,以石墨为主要成分的固体润滑剂,覆盖膜形成性能稍有不足,并对反复摩擦的其覆盖膜寿命方面也不充分。因此,不适合低速度·高负载的用途。
另一方面,作为在高负载用途中被使用的固体润滑剂,可以列举在四氟乙烯树脂中配合铟、铅、锡等的软金属、蜡的固体润滑剂。特别是在四氟乙烯树脂中配合铅和蜡的固体润滑剂被广泛使用着。该固体润滑剂,高负载条件下的摩擦系数极低,另外,覆盖膜形成性能优异,该覆盖膜的寿命也长,更有覆盖膜的自我修复性也优异。
近年来,材料开发的动向,从对环境问题的考虑出发,向无铅方向发展。该开发动向在上述固体润滑剂上也不例外。但是,在固体润滑剂中,在满足滑动特性上,铅是重要的结构成分。特别是埋入在轴承等的滑动面上形成的孔或沟中,在高负载条件下使用时,从覆盖膜形成性能的观点出发,铅也是重要的。
作为无铅的滑动部件,使含有三聚氰胺和三聚异氰酸的附加物的树脂成形,而制成的滑动部件被揭示(参照专利文献1)。但是,以由含有三聚氰胺和三聚异氰酸的附加物的树脂制成的滑动部件组合物作为固体润滑剂使用时,在高负载条件下的摩擦系数不能说充分。因此,希望提供不含铅,在高负载条件下发挥充分的滑动特性的固体润滑剂。
专利文献1:特开昭55-108427号公报
发明内容
本发明鉴于上述情况,其目的在于提供高负载条件下,能够发挥与含铅的固体润滑剂同等或同等以上的滑动特性的、无铅的固体润滑剂。
本发明的第一方面认为是埋入在滑动部件基体的滑动面上形成的孔或沟中的固体润滑剂,其含有20~40重量%的选自烃类蜡、高级脂肪酸、高级脂肪酸酯和高级脂肪酸酰胺的1种或2种以上的蜡类、和20~40重量%的三聚氰胺氰尿酸酯、以及20~50重量%的四氟乙烯树脂。
本发明的第二方面认为在滑动部件基体的滑动面上形成的孔或沟中,埋入上述固体润滑剂制成滑动部件。
根据发明提供,埋入在滑动部件基体的滑动面上形成的孔或沟中而使用的适合的固体润滑剂,在高负载条件下,能够发挥与含铅的固体润滑剂同等或同等以上的滑动特性的、无铅的固体润滑剂。
具体实施方式
说明本发明的实施方式。首先叙述固体润滑剂。蜡类主要具有降低摩擦系数的作用。作为被使用的蜡类选自烃类蜡、高级脂肪酸、高级脂肪酸酯和高级脂肪酸酰胺的1种或2种以上。
作为烃类蜡,可以列举碳原子数24以上的链烷烃类蜡、碳原子数26以上的链烯烃类蜡、碳原子数28以上的烷基苯、结晶质的微晶蜡。这些烃类蜡可以单独或作为2种以上的混合物使用。
作为高级脂肪酸,可以列举碳原子数12以上的饱和或不饱和脂肪酸。具体的可以列举十二烷酸、十四烷酸、十六烷酸、硬脂酸、二十烷酸、二十二烷酸、二十六烷酸、二十八烷酸、三十烷酸、十二烯酸、十四烯酸、油酸、反油酸、亚油酸、亚麻酸、花生油烯酸、二十碳-9-烯酸、芥酸等。
高级脂肪酸酯是上述高级脂肪酸与一元醇或多元醇的酯。作为一元醇,可以列举辛醇、月桂醇、肉豆蔻醇、棕榈醇、硬脂醇、山萮醇等,作为多元醇,可以列举乙二醇、丙二醇、丁二醇、丙三醇、季戊四醇、山梨糖醇酐等。作为高级脂肪酸酯的具体例子,可以列举硬脂酸硬脂酯、季戊四醇四硬脂酸酯、硬脂酸单甘油酯、二十二烷酸单甘油酯等。
高级脂肪酸酰胺是上述高级脂肪酸与一元或多元胺的酰胺。作为一元或多元胺,可以列举辛胺、月桂基胺、肉豆蔻胺、棕榈胺、硬脂胺、亚甲基二胺、亚乙基二胺、六甲基二胺等。作为高级脂肪酸酰胺的具体例子,可以列举棕榈酸酰胺、硬脂酸酰胺、油酸酰胺、芥酸酰胺等。
蜡类的配合比例,通常是20~40重量%,优选是20~30重量%。配合比例小于20重量%时,得不到所希望的低摩擦特性,另外,大于40重量%时,成形性变差,并成形体的强度下降。
三聚氰胺氰尿酸酯是三聚氰胺和三聚氰酸或三聚异氰酸的附加化合物,六元环结构的三聚氰胺分子与三聚氰酸(三聚异氰酸)分子,由氢键配列为平面状,该平面以弱的粘合力重叠为层状,可以认为具有二硫化钼和石墨那样的解理性。该三聚氰胺氰尿酸酯,具有使耐磨损性、耐负载性提高的作用,其配合比例通常是20~40重量%,优选是30~40重量%。配合比例小于20重量%时,得不到所希望的耐磨损性、耐负载性提高的效果,大于40重量%时,使耐磨损性下降。
四氟乙烯树脂(PTFE)主要具有赋予低摩擦性的作用。本发明中使用的四氟乙烯树脂,大致区别为:在以制模粉末或细粉末为主成形用中被使用的四氟乙烯树脂(以下简称为“高分子量PTFE”);和由放射线照射等分解高分子量PTFE或四氟乙烯树脂聚合时调节分子量,比高分子量PTFE分子量小的容易粉碎或分散性好的、主要作为添加材料使用的四氟乙烯树脂(以下简称为“低分子量PTFE”)。四氟乙烯树脂可以单独使用高分子量PTFE或作为高分子量PTFE与低分子量PTFE的混合物使用。作为混合物的高分子量PTFE与低分子量PTFE的混合比例(重量),通常为1∶1~3∶1。
作为制模粉末用高分子量PTFE,可以列举三井杜邦氟化学公司生产的“テフロン(注册商标)7-J”、“テフロン(注册商标)7A-J”、“テフロン(注册商标)70-J”等、大金工业公司生产的“ポリフロンM-12(商品名)”等、旭硝子公司生产的“フルオンG163(商品名)”、“フルオンG190(商品名)”等。作为细粉末用高分子量PTFE,可以列举三井杜邦氟化学公司生产的“テフロン(注册商标)6CJ”等、大金工业公司生产的“ポリフロンF201(商品名)”等、旭硝子公司生产的“フルオンCD076(商品名)”、“フルオンCD090(商品名)”等。
另外,作为高分子量PTFE,除上述高分子量PTFE以外,可以使用以苯乙烯类、丙烯酸酯类、甲基丙烯酸酯类、丙烯腈类聚合物等改性了高分子量PTFE的物质,具体的、可以列举三菱丽阳公司生产的“メタブレンA-3000”等。作为低分子量PTFE,可以列举三井杜邦氟化学公司生产的“TLP-10F(商品名)”等、大金工业公司生产的“ルブロンL-5(商品名)”等、旭硝子公司生产的“フルオンL169J(商品名)”等、喜多村公司生产的“KTL-8N(商品名)”等。
PTFE的配合比例,通常是20~50重量%,优选是20~40重量%。配合比例小于20重量%时,得不到所希望的低摩擦特性,大于50重量%时,耐磨损性变差,并保形性变差,成形体的强度下降。
本发明的固体润滑剂中,作为补加成分,也可以加入金属皂和/或聚乙烯树脂和/或磷酸盐。
金属皂是上述高级脂肪酸与碱金属或碱土类金属的盐。具体的可以列举硬脂酸锂、硬脂酸钙等。该金属皂具有使耐磨损性提高,使摩擦系数下降,并使热稳定性提高的作用。其配合比例,通常是5~20重量%,优选是10~15重量%。配合比例小于5重量%时,得不到所希望的摩擦系数下降和耐磨损性与热稳定性提高的效果,配合比例大于20重量%时,成形性变差。
聚乙烯树脂具有使耐磨损性提高,并提高形成固体润滑剂的各成分组成粘合力的作用。作为被使用的聚乙烯树脂,可以列举高压法低密度聚乙烯(HPLD)、直链状低密度聚乙烯(LLDPE)、超低密度聚乙烯(VLDPE)、高密度聚乙烯(HDPE)、超高分子量聚乙烯(UHMWPE)、由超高分子量聚乙烯与低分子量乃至高分子量聚乙烯组成的高分子量聚乙烯(HMWPE)等。
HPLD是由高压法制造的乙烯均聚物,除乙基等的短链分支还含有长链分支,其密度通常是0.910~0.940g/cm3。LLDPE是由中·低压法制造的乙烯与其以外的α-链烯烃(丙烯、丁烯-1、4-甲基戊烯-1、辛烯-1等)的共聚物,其密度通常是0.900~0.940g/cm3。其中,密度为0.925~0.940g/cm3的共聚物被称为中密度聚乙烯(MDPE)。VLDPE是将LLDPE再低密度化的物质,其密度是0.880~0.910g/cm3。HDPE是由中·低压法制造的乙烯的均聚物,其密度通常是0.940~0.970g/cm3。UHMWPE是由低压法制造的分子量为100万以上的物质,其密度通常是0.940g/cm3。
聚乙烯树脂的配合比例,通常为5~20重量%,优选为10~15重量%。配合比例小于5重量%时,作为粘合材料的作用不能被充分发挥,另外,配合比例大于20重量%时,形成固体润滑剂的各成分的配合比例变少,得到良好润滑性能变得困难。
作为磷酸盐,可以列举碱金属或碱土类金属的磷酸三盐、磷酸氢盐、焦磷酸盐、亚磷酸盐、偏磷酸盐等。具体的,可以列举磷酸三锂、磷酸氢二锂、焦磷酸锂、磷酸三钙、磷酸一氢钙、焦磷酸钙、偏磷酸锂、偏磷酸镁、偏磷酸钙等。磷酸盐其本身不显示润滑性,在与对象材料的滑动中,发挥有助于向对象材料表面形成润滑覆盖膜的效果。由此,在对象材料表面经常保持形成良好的润滑覆盖膜,维持良好的滑动特性。
磷酸盐的配合比例,通常是5~15重量%,优选是10~15重量%。配合比例小于5重量%时,不能发挥有助于向对象材料表面形成润滑覆盖膜的效果,大于20重量%时,向对象材料表面形成润滑覆盖膜的移动量变得过多,耐磨损性下降。
本发明的固体润滑剂,可以由亨舍尔混合机、超级混合机、球摩机、转鼓等的混合机混合上述各成分的规定量,成形得到的混合物而得到。成形方法没有特别限定,优选采用将上述混合物供给挤出机,以蜡类熔融的温度熔融混炼,制作小球,将该小球供给射出成形机而成形的方法。
本发明的滑动部件在由金属材料或合成树脂等构成的滑动部件基体的滑动面上形成的孔或沟中,埋入由上述制造方法得到的固体润滑剂而制成。作为在基材上形成的孔或沟中埋入固体润滑剂的方法,可以列举压入固定的方法、在固体润滑剂上涂布粘合剂、将其在孔或沟中固定的方法等。
实施例
以下由实施例更详细地说明本发明,但本发明在不超出其要点的范围内,不被以下的实施例所限定。
实施例1:
在亨舍尔混合机中投入50重量%的作为四氟乙烯树脂的高分子量PTFE(旭硝子公司生产的“フルオンG163(商品名)”)、10重量%的作为蜡类的烃类蜡的聚乙烯蜡(Clariant Japan公司生产的“リコヮツクスPE520(商品名)”、和10重量%的石蜡(日本精蜡公司生产的“150(商品名)”)、以及30重量%的三聚氰胺氰尿酸酯(三菱化学公司生产的“MCA(商品名)”),制作混合物。将得到的混合物导入挤出成形机,制作带状成形物后,较细地切断该成形物,制作由该混合物构成的小球。然后,将该小球供给射出成形机,制作直径6mm、长5mm的圆柱状固体润滑剂。
实施例2~23及对照例1与3:
实施例1中,如表2~表8所示那样地变更组成以外,由与实施例1同样的方法,制作直径6mm、长5mm的圆柱状固体润滑剂。表2~表8表示成分组成。
对照例2:
混合搅拌50体积%的PTFE粉末(三井杜邦氟化学公司生产的“テフロン(注册商标)7A-J”和40体积%的雾化铅粉末,得到混合物。由压力成形机将该混合物加压成形,制作直径6mm、长5mm的圆柱状固体润滑剂。然后,将该圆柱状固体润滑剂浸渍在加入了润滑油(美孚公司生产的“DTEエキストラヘビ一オィル(商品名)”)的油槽,含浸10体积%的润滑油(以重量换算PTFE为18.8重量%、铅79.6重量%、润滑油1.6重量%)。
在由铜合金制成的平板状基体的滑动面上形成的孔中埋入上述实施例和对照例中得到的固体润滑剂,作为滑动部件试验片,由推力试验试验该滑动部件试验片的滑动性能。表1表示试验条件。表2~表8表示滑动特性。
表1
试验片材质 | 高力黄铜铸件4种 |
对象材料材质 | 不锈钢(SUS403) |
在滑动部件试验片的滑动面上所占的固体润滑剂的面积比例 | 30% |
滑动速度 | 0.5m/min |
负载 | 300kgf/cm2 |
润滑 | 无润滑 |
试验时间 | 10小时 |
表2
实施例1 | 实施例2 | 实施例3 | 实施例4 | ||
成分组成 | PTFE·高分子量PTFE·低分子量PTFE | 50- | 40- | 30- | 50- |
蜡类(烃类蜡)·聚乙烯蜡·石蜡·微晶蜡(高级脂肪酸)·硬脂酸 | 1010-- | 1010-- | 1515-- | --20- | |
三聚氰胺氰尿酸酯 | 30 | 40 | 40 | 30 | |
金属皂·硬脂酸锂·硬脂酸锌·硬脂酸钙 | --- | --- | --- | --- | |
聚乙烯树脂·HDPE·LDPE·HMWPE | --- | --- | --- | --- | |
磷酸盐·焦磷酸钙·磷酸三钙 | -- | -- | -- | -- | |
各项特性 | 摩擦系数 | 0.072~0.085 | 0.086~0.093 | 0.088~0.096 | 0.078~0.088 |
磨损量(μm) | 4 | 4 | 4 | 4 |
表3
实施例5 | 实施例6 | 实施例7 | 实施例8 | ||
成分组成 | PTFE·高分子量PTFE·低分子量PTFE | 2525 | 2020 | 1515 | 2525 |
蜡类(烃类蜡)·聚乙烯蜡·石蜡·微晶蜡(高级脂肪酸)·硬脂酸 | 1010-- | 1010-- | 1515-- | --20- | |
三聚氰胺氰尿酸酯 | 30 | 40 | 40 | 30 | |
金属皂·硬脂酸锂·硬脂酸锌·硬脂酸钙 | --- | --- | --- | --- | |
聚乙烯树脂·HDPE·LDPE·HMWPE | --- | --- | --- | --- | |
磷酸盐·焦磷酸钙·磷酸三钙 | -- | -- | -- | -- | |
各项特性 | 摩擦系数 | 0.086~0.094 | 0.092~0.100 | 0.093~0.110 | 0.090~0.098 |
磨损量(μm) | 4 | 4 | 4 | 4 |
表4
实施例9 | 实施例10 | 实施例11 | ||
成分组成 | PTFE·高分子量PTFE·低分子量PTFE | 20- | 30- | 40- |
蜡类(烃类蜡)·聚乙烯蜡·石蜡·微晶蜡(高级脂肪酸)·硬脂酸 | 1515-10 | 1010-10 | 1010-10 | |
三聚氰胺氰尿酸酯 | 40 | 40 | 30 | |
金属皂·硬脂酸锂·硬脂酸锌·硬脂酸钙 | --- | --- | --- | |
聚乙烯树脂·HDPE·LDPE·HMWPE | --- | --- | --- | |
磷酸盐·焦磷酸钙·磷酸三钙 | -- | -- | -- | |
各项特性 | 摩擦系数 | 0.073~0.085 | 0.088~0.097 | 0.073~0.085 |
磨损量(μm) | 0.5 | 1 | 3 |
表5
实施例12 | 实施例13 | 实施例14 | 实施例15 | ||
成分组成 | PTFE·高分子量PTFE·低分子量PTFE | 20- | 20- | 20- | 20- |
蜡类(烃类蜡)·聚乙烯蜡·石蜡·微晶蜡(高级脂肪酸)·硬脂酸 | 30--- | 1515-- | -30-- | --30- | |
三聚氰胺氰尿酸酯 | 40 | 40 | 40 | 40 | |
金属皂·硬脂酸锂·硬脂酸锌·硬脂酸钙 | 10-- | -10- | --10 | --10 | |
聚乙烯树脂·HDPE·LDPE·HMWPE | --- | --- | --- | --- | |
磷酸盐·焦磷酸钙·磷酸三钙 | -- | -- | -- | -- | |
各项特性 | 摩擦系数 | 0.094~0.096 | 0.088~0.095 | 0.080~0.085 | 0.083~0.087 |
磨损量(μm) | 2 | 2 | 1 | 1 |
表6
实施例16 | 实施例17 | 实施例18 | 实施例19 | ||
成分组成 | PTFE·高分子量PTFE·低分子量PTFE | 20- | 20- | 20- | 20- |
蜡类(烃类蜡)·聚乙烯蜡·石蜡·微晶蜡(高级脂肪酸)·硬脂酸 | 1010-10 | 1515-10 | -20-10 | --2010 | |
三聚氰胺氰尿酸酯 | 40 | 30 | 40 | 40 | |
金属皂·硬脂酸锂·硬脂酸锌·硬脂酸钙 | --- | --- | --- | --- | |
聚乙烯树脂·HDPE·LDPE·HMWPE | 10-- | -10- | -10- | --10 | |
磷酸盐·焦磷酸钙·磷酸三钙 | -- | -- | -- | -- | |
各项特性 | 摩擦系数 | 0.092~0.100 | 0.086~0.098 | 0.094~0.110 | 0.096~0.120 |
磨损量(μm) | 1 | 1 | 2 | 2 |
表7
实施例20 | 实施例21 | 实施例22 | 实施例23 | ||
成分组成 | PTFE·高分子量PTFE·低分子量PTFE | 20- | 20- | 20- | 20- |
蜡类(烃类蜡)·聚乙烯蜡·石蜡·微晶蜡(高级脂肪酸)·硬脂酸 | 1010-10 | 1010-10 | 20--10 | --2010 | |
三聚氰胺氰尿酸酯 | 30 | 30 | 30 | 30 | |
金属皂·硬脂酸锂·硬脂酸锌·硬脂酸钙 | --- | --- | --- | --- | |
聚乙烯树脂·HDPE·LDPE·HMWPE | 10-- | -10- | -10- | --10 | |
磷酸盐·焦磷酸钙·磷酸三钙 | 10- | 10- | -10 | 10- | |
各项特性 | 摩擦系数 | 0.076~0.080 | 0.074~0.082 | 0.084~0.098 | 0.086~0.096 |
磨损量(μm) | 4 | 3 | 3 | 4 |
表8
对照例1 | 对照例2 | 对照例3 | ||
成分组成 | PTFE·高分子量PTFE·低分子量PTFE | -10.5 | 18.8- | 50- |
蜡类·石蜡 | 2 | - | 40 | |
三聚氰胺氰尿酸酯 | ||||
金属皂·硬脂酸锂 | 1 | - | 10 | |
聚乙烯树脂·LDPE | 1.5 | - | - | |
铅 | 85 | 79.6 | - | |
润滑油 | - | 1.6 | - | |
各项特性 | 摩擦系数 | 0.099~0.110 | 0.089~0.120 | 0.100~0.145 |
磨损量(μm) | 2 | 8 | 35 |
表中,作为低分子量PTFE,使用大金工业公司的“ルブロンL-5(商品名)”,作为微晶蜡,使用日本精蜡公司生产的“Hi-Mic-1080(商品名)”,作为HDPE,使用三井化学公司生产的“ハィゼツクス(商品名)”,作为LDPE,使用住友精化公司生产的“フロ一センG701(商品名)”,作为HMWPE,使用三井化学公司生产的“リュブマ一(商品名)”。
从以上试验结果可知,在滑动面上埋入本发明的固体润滑剂从而构成的滑动部件,显示低速度·高负载条件下优异的滑动特性,显示与埋入对照例1和对照例2中显示的现有含铅固体润滑剂的滑动部件同等或同等以上的性能。其它,在滑动面埋入的不含三聚氰胺氰尿酸酯的对照例3的固体润滑剂的滑动部件,摩擦系数高,磨损量多、滑动特性差。
Claims (5)
1.一种固体润滑剂,用于埋入在滑动部件基体的滑动面上形成的孔或沟中,其特征在于:
含有20~40重量%的选自烃类蜡、高级脂肪酸、高级脂肪酸酯以及高级脂肪酸酰胺的1种或2种以上的蜡类、和20~40重量%的三聚氰胺氰尿酸酯以及20~50重量%的四氟乙烯树脂。
2.如权利要求1所述的固体润滑剂,其特征在于:
含有5~20重量%的金属皂。
3.如权利要求1或2所述的固体润滑剂,其特征在于:
含有5~20重量%的聚乙烯树脂。
4.如权利要求1~3任一项所述的固体润滑剂,其特征在于:
含有5~15重量%的磷酸盐。
5.一种在滑动部件基体的滑动面上形成的孔或沟中埋入如权利要求1~4任一项所述的固体润滑剂而构成的滑动部件。
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BR112014026612B1 (pt) | 2012-04-26 | 2021-10-26 | Minebea Mitsumi Inc | Composição de resina curável em luz ultravioleta para forro autolubrificante, membro corrediço e respectivo método de fabricação |
JP5981765B2 (ja) | 2012-05-09 | 2016-08-31 | オイレス工業株式会社 | 固体潤滑剤及び固体潤滑剤を埋め込んだ摺動部材 |
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JP7028476B2 (ja) * | 2020-06-10 | 2022-03-02 | 能瀬精工株式会社 | 固形潤滑剤及び転がり軸受 |
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-
2003
- 2003-05-13 JP JP2003133923A patent/JP2004339259A/ja active Pending
-
2004
- 2004-05-07 EP EP04731713A patent/EP1637579B1/en active Active
- 2004-05-07 CA CA2525027A patent/CA2525027C/en active Active
- 2004-05-07 KR KR1020057021061A patent/KR101130026B1/ko active IP Right Grant
- 2004-05-07 US US10/556,077 patent/US20070004843A1/en not_active Abandoned
- 2004-05-07 WO PCT/JP2004/006028 patent/WO2004101718A1/ja active Application Filing
- 2004-05-07 DE DE602004032139T patent/DE602004032139D1/de active Active
- 2004-05-07 CN CNB2004800127863A patent/CN100387694C/zh active Active
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2011
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101522874B (zh) * | 2006-09-06 | 2013-06-05 | 奥依列斯工业株式会社 | 固体润滑剂和滑动部件 |
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Publication number | Publication date |
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CN100387694C (zh) | 2008-05-14 |
KR101130026B1 (ko) | 2012-03-28 |
EP1637579A1 (en) | 2006-03-22 |
EP1637579A4 (en) | 2007-10-03 |
WO2004101718A1 (ja) | 2004-11-25 |
US20070004843A1 (en) | 2007-01-04 |
DE602004032139D1 (de) | 2011-05-19 |
CA2525027C (en) | 2012-01-03 |
EP1637579B1 (en) | 2011-04-06 |
CA2525027A1 (en) | 2004-11-25 |
KR20060009301A (ko) | 2006-01-31 |
US20110190178A1 (en) | 2011-08-04 |
JP2004339259A (ja) | 2004-12-02 |
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