CN111270516A - 一种抗高能辐照自润滑织物衬垫及制备方法、自润滑织物复合材料 - Google Patents
一种抗高能辐照自润滑织物衬垫及制备方法、自润滑织物复合材料 Download PDFInfo
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Abstract
本发明提供了一种抗高能辐照自润滑织物衬垫及制备方法、自润滑织物复合材料,涉及功能材料技术领域。本发明以g‑C3N4和多层石墨烯为复合固体润滑剂,实现自润滑织物衬垫对低摩擦、耐磨损的需求。同时,g‑C3N4和多层石墨烯独特的六元环结构,赋予了自润滑织物衬垫一定的耐辐照性能,从而延长了其使用寿命。此外,利用二氧化铈中的铈元素化学价态的灵活转化,有效提高了基体树脂(酚醛树脂)的耐辐照性能。另外,该自润滑织物衬垫的制备方法简单,环保无污染。此外,由抗高能辐照自润滑织物衬垫形成的自润滑织物复合材料具有优异的抗高能辐照能力和摩擦学性能。
Description
技术领域
本发明涉及功能材料技术领域,尤其涉及一种抗高能辐照自润滑织物衬垫及制备方法、自润滑织物复合材料。
背景技术
自润滑织物衬垫以聚合物自身的润滑特性、相对较轻的重量和容易加工等优点,被广泛应用于自润滑关节轴承的设计与制备。而在医学、航空航天、核工业以及武器系统等领域中,自润滑材料会不可避免的暴露在高能射线的辐照下(如电子束辐照、X射线辐照和γ射线辐照等),其中具备极强穿透能力的γ射线辐照对材料的损伤更是致命的。长期处于γ射线辐照中的聚合物材料,其分子链吸收电离能后会产生自由基,进一步引发交联、接枝和断链等反应,特别是在较高辐照剂量以及有氧环境下,聚合物材料会发生严重氧化降解,致使其性能大幅下降、使用寿命缩短且可靠性降低,最终导致材料的功能失效,造成安全隐患。
查阅相关资料,多数专利报道自润滑织物衬垫材料常选用酚醛树脂作为基体,主要源于酚醛具有抗张、抗冲击、耐湿热老化等优异性能,同时也考虑到成本以及成型工艺的需求。然而,关于以酚醛树脂为基体的自润滑织物衬垫材料在高能射线的辐照下的应用至今尚未报道。归结其原因,一方面考虑到酚醛树脂自身较弱的耐辐照性能;另一方面,未曾发现合适的固体润滑剂。
发明内容
有鉴于此,本发明的目的在于提供一种抗高能辐照自润滑织物衬垫及制备方法、自润滑织物复合材料,本发明提供的抗高能辐照自润滑织物具有优异的抗高能辐照能力和摩擦学性能。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种抗高能辐照自润滑织物衬垫,包括预处理混纺纤维布和负载在所述预处理混纺纤维布上的复合固体润滑剂、二氧化铈和酚醛树脂,所述复合固体润滑剂为石墨相氮化碳和多层石墨烯。
优选地,所述复合固体润滑剂、二氧化铈和酚醛树脂的质量之和为预处理混纺纤维布质量的30~65%。
优选地,所述复合固体润滑剂的质量为酚醛树脂质量的15~52%。
优选地,所述复合固体润滑剂中石墨相氮化碳和多层石墨烯的质量比为1:1~7:1。
优选地,所述石墨相氮化碳的粒径为10~100nm。
优选地,所述多层石墨烯的层数为10~30层。
优选地,所述二氧化铈的质量为酚醛树脂质量的1.5~8%。
优选地,所述二氧化铈的粒径为20~50nm。
本发明还提供了上述技术方案所述的抗高能辐照自润滑织物衬垫的制备方法,包括以下步骤:
将所述复合固体润滑剂、二氧化铈、酚醛树脂胶粘剂和稀释剂混合分散,得到自润滑浸渍液;
将所述自润滑浸渍液涂敷于预处理混纺纤维布,干燥,得到所述抗高能辐照自润滑织物衬垫。
本发明还提供了一种自润滑织物复合材料,所述自润滑织物复合材料由层叠设置的抗高能辐照自润滑织物衬垫、酚醛树脂和金属基材经固化成型得到;
所述抗高能辐照自润滑织物衬垫为上述技术方案所述的抗高能辐照自润滑织物衬垫或上述技术方案所述的制备方法制得的抗高能辐照自润滑织物衬垫。
本发明提供了一种抗高能辐照自润滑织物衬垫,包括预处理混纺纤维布和负载在所述预处理混纺纤维布上的复合固体润滑剂、二氧化铈和酚醛树脂,所述复合固体润滑剂为石墨相氮化碳和多层石墨烯。本发明以石墨相氮化碳(g-C3N4)以及多层石墨烯为复合固体润滑剂,实现自润滑织物衬垫对低摩擦、耐磨损的需求。同时,g-C3N4和多层石墨烯独特的六元环结构,赋予了自润滑织物衬垫一定的耐辐照性能,从而延长了其使用寿命。除此之外,利用二氧化铈中的铈元素化学价态的灵活转化,有效提高了基体树脂(酚醛树脂)的耐辐照性能。实施例的数据表明:经过高能辐照后的自润滑织物复合材料的摩擦系数均有所下降,而且随着辐照剂量的增大,摩擦系数有所升高,证明设计的自润滑织物复合材料在辐照条件下仍然具有润滑性能。
本发明还提供了上述技术方案所述的抗高能辐照自润滑织物衬垫的制备方法,包括以下步骤:将所述复合固体润滑剂、二氧化铈、酚醛树脂胶粘剂和稀释剂混合分散,得到自润滑浸渍液;将所述自润滑浸渍液涂敷于预处理混纺纤维布,干燥,得到所述抗高能辐照自润滑织物衬垫。本发明的预处理混纺纤维布具有较高的纳米粒子负载量;另外采用浸渍法将自润滑浸渍涂敷于预处理混纺纤维布上,保证了自润滑浸渍液对预处理混纺纤维布的浸渍量,保证了最终抗高能辐照自润滑织物衬垫的性能。同时,制备方法简单、环保无污染。
本发明还提供了一种自润滑织物复合材料,所述自润滑织物复合材料由层叠设置的抗高能辐照自润滑织物衬垫、酚醛树脂和金属基材经固化成型得到。本发明将抗高能辐射自润滑织物衬垫黏贴到金属基材上,形成了自润滑织物复合材料,使其具有优异的摩擦性能和抗高强辐照能力。
附图说明
图1为实施例5所得自润滑织物复合材料的摩擦效果图;其中(a)为实施例5所得自润滑织物复合材料未经辐照的摩擦效果图,(b)为实施例5所得自润滑织物复合材料经1000Gy剂量辐照后的摩擦效果图,(c)为实施例5所得自润滑织物复合材料经2200Gy剂量辐照后的摩擦效果图。
具体实施方式
本发明提供了一种抗高能辐照的自润滑织物衬垫,包括预处理混纺纤维布和负载在所述预处理混纺纤维布上的复合固体润滑剂、二氧化铈和酚醛树脂,所述复合固体润滑剂为石墨相氮化碳和多层石墨烯。
在本发明中,所述复合固体润滑剂、二氧化铈和酚醛树脂的质量之和优选为预处理混纺纤维布质量的30~65%,进一步优选为40~60%,更优选为45~50%。本发明将复合固体润滑剂、二氧化铈和酚醛树脂的质量之和控制为预处理混纺纤维布质量的30~65%,提高了接枝混纺纤维布的承载能力,同时改善了自润滑织物衬垫的摩擦磨损,保证了其与金属基体很好的粘结力。
在本发明中,所述复合固体润滑剂的质量优选为酚醛树脂质量的15~52%,进一步优选为25~40%;所述复合固体润滑剂中石墨相氮化碳(g-C3N4)和多层石墨烯的质量比优选为1:1~7:1,进一步优选为3:1~5:1。
在本发明中,所述石墨相氮化碳的粒径优选为10~100nm;本发明对所述石墨相氮化碳的来源不做具体限定,采用本领域技术人员熟知的市售产品即可。在本发明中,所述多层石墨烯的层数优选为10~30层,进一步优选为20层。本发明对所述多层石墨烯的来源不做具体限定,采用本领域技术人员熟知的市售产品即可。
在本发明中,所述复合固体润滑剂优选由包括以下步骤的方法制得:
将石墨相氮化碳和多层石墨烯球磨混合后,洗涤、干燥,得到所述复合固体润滑剂。
在本发明中,所述球磨混合的时间优选为8~72h,进一步优选为12~24h。在本发明中,所述洗涤用试剂优选为无水乙醇,所述洗涤的次数优选为1~3次。
在本发明中,所述干燥的温度优选为80~100℃,时间优选为2~10h。
在本发明中,所述二氧化铈的质量优选为酚醛树脂质量的1.5~8%,进一步优选为4~6%;所述二氧化铈的粒径优选为20~50nm。
在本发明中,所述预处理混纺纤维布优选由包括以下步骤的方法制得:
将3,4-二羟苯乙胺、三(羟基甲基)氨基甲烷和水混合,得到混合液;将混纺纤维布浸渍于所述混合液中进行预处理,干燥,得到所述预处理混纺纤维布。
在本发明中,所述混纺纤维布优选为聚四氟乙烯纤维和聚间苯二甲酰间苯二胺纤维按按重量比1:1混纺而成的布,所述混纺纤维布的厚度为0.1~0.4mm。
在本发明中,所述3,4-二羟苯乙胺和三(羟基甲基)氨基甲烷的质量比优选为4:3;所述3,4-二羟苯乙胺和三(羟基甲基)氨基甲烷的质量之和与水的质量比优选为1:10。
在本发明中,所述预处理的温度优选为室温,即既不需要额外加热也不需要冷却;所述预处理的时间优选为60min。在本发明中,所述干燥的温度优选为100℃,时间优选为24h;所述干燥优选在鼓风烘箱中进行。
本发明对所述混纺纤维布做预处理,能够在混纺纤维布引入一些活性基团比如羟基,能够提高混纺纤维布的负载量及负载活性。
本发明提供抗高能辐照自润滑织物衬垫中以g-C3N4以及多层石墨烯为复合固体润滑剂,实现自润滑织物衬垫对低摩擦、耐磨损的需求。同时,g-C3N4和多层石墨烯独特的六元环结构,赋予了自润滑织物衬垫一定的耐辐照性能,从而延长了其使用寿命。除此之外,利用二氧化铈(CeO2)中的Ce元素化学价态的灵活转化,有效提高了基体树脂(酚醛树脂)的耐辐照性能。
本发明还提供了上述技术方案所述的抗高能辐照自润滑织物衬垫的制备方法,包括以下步骤:
将所述复合固体润滑剂、二氧化铈、酚醛树脂胶粘剂和稀释剂混合分散,得到自润滑浸渍液;
将所述自润滑浸渍液涂敷于预处理混纺纤维布,干燥,得到所述抗高能辐照自润滑织物衬垫。
本发明将所述复合固体润滑剂、二氧化铈、酚醛树脂胶粘剂和稀释剂混合分散,得到自润滑浸渍液。
在本发明中,所述复合固体润滑剂的获得方式与上述技术方案一致,在此不再赘述。
在本发明中,所述酚醛树脂胶粘剂优选为酚醛-丁腈胶粘剂、酚醛-缩醛胶粘剂或酚醛-改性环氧胶粘剂,即所述酚醛树脂胶粘剂由酚醛树脂和溶剂构成,其中酚醛树脂胶粘剂中的溶剂当自润滑浸渍液涂敷到预处理混纺纤维布上后,在后续的干燥过程中会挥发,只有其中的酚醛树脂会留在预处理混纺纤维布上。在本发明中,所述酚醛树脂胶粘剂的固含量优选为≥75%,进一步优选为75%;所述酚醛树脂胶粘剂的固含量为酚醛树脂占酚醛树脂胶粘剂总质量的比例。
在本发明中,所述稀释剂优选为乙醇、丙酮、乙酸乙酯或四氢呋喃。在本发明中,所述稀释剂在自润滑浸渍液涂敷到预处理混纺纤维布上后,在后续的干燥过程中会挥发,所以在最终的抗高辐照自润滑织物衬垫上是不存在稀释剂的。
在本发明中,所述复合固体润滑剂的质量优选为酚醛树脂胶粘剂中酚醛树脂质量的15~52%,进一步优选为25~40%。
在本发明中,所述二氧化铈的质量优选为酚醛树脂胶粘剂中酚醛树脂质量的1.5~8%,进一步优选为4~6%。
在本发明中,所述自润滑浸渍液的固含量优选为10~35%。在本发明中,所述自润滑浸渍液的固含量为自润滑浸渍液中复合固体润滑剂、二氧化铈和酚醛树脂胶粘剂中酚醛树脂的质量之和占自润滑浸渍液总质量的比例。
在本发明中,所述混合分散的转速优选为10000~21000r/min,进一步优选为15000~18000r/min;所述混合分散优选在高速分散乳化机中进行。
得到自润滑浸渍液后,本发明将所述自润滑浸渍液涂敷于预处理混纺纤维布,干燥,得到所述抗高能辐照自润滑织物衬垫。
在本发明中,所述预处理混纺纤维布的制备方法与上述技术方案一致,在此不再赘述。
在本发明中,所述干燥的温度优选为80~100℃,时间优选为0.5~2h;所述干燥优选在鼓风烘箱中进行。
在本发明中,所述抗高能辐照自润滑织物衬垫的重量相比所述预处理混纺纤维布的重量增加30~65%,进一步优选为40~60%,更优选为45~50%。
在本发明中,当所述抗高能辐照自润滑织物衬垫的重量相比所述预处理混纺纤维布的重量没有增加30~65%,优选重复步骤“将所述自润滑浸渍液涂敷于所述预处理混纺纤维布,干燥”,以使抗高能辐照自润滑织物衬垫达到增重要求。
本发明提供的抗高辐照自润滑织物衬垫的制备方法简单,原料来源广,且环保无污染。
本发明还提供了一种自润滑织物复合材料,所述自润滑织物复合材料由层叠设置的上述抗高能辐照自润滑织物衬垫、酚醛树脂和金属基材经固化成型得到。
本发明对所述酚醛树脂的用量不做具体限定,只要能够充分覆盖金属基材即可,具体地,一般涂敷2~3次。在本发明中,所述固化成型的压力优选为0.01~0.03MPa,进一步优选为0.02MPa,温度优选为80~200℃,进一步优选为120~180℃,更优选为150℃;时间优选为1.5~8h,进一步优选为3~5h。在本发明中,所述金属基材的材质优选为钛合金、304钢、铝以或轴承钢;所述金属基材的尺寸优选为18×18×2mm。
本发明提供的自润滑织物复合材料具有优异的抗高辐照能力和摩擦性能。
下面结合实施例对本发明提供的高能辐照自润滑织物衬垫及制备方法、自润滑织物复合材料进行详细的说明,但是不能把它们理解为对本发明保护范围的限定。
实施例1
1、8g3,4-二羟苯乙胺和6g三(羟基甲基)氨基甲烷溶于140g去离子水中,得到混合液;将混纺纤维布浸渍于混合液中进行预处理60min,取出后100℃鼓风烘箱中干燥24h,得到预处理混纺纤维布;
2、将10gg-C3N4和10g多层石墨烯球磨混合8h后,取出用乙醇洗涤2次,然后80℃条件下干燥10h,得到复合固体润滑剂;
3、将10g酚醛-丁腈胶粘剂(固含量75%)、0.11g纳米CeO2以及步骤2制备的1.875g复合固体润滑剂分散在35.5g乙酸乙酯中,在高速分散乳化机中以10000r/min的速度进行充分混合,得到自润滑浸渍液;
4、将所述自润滑浸渍液涂敷于预处理混纺纤维布上,然后移至80℃鼓风烘箱中干燥0.5h,并重复该过程至预处理混纺纤维布增重30%,得到抗高能辐照自润滑织物衬垫;
5、最后用酚醛树脂将所述抗高能辐照自润滑织物衬垫粘贴于钛合金基材表面,并施加0.03MPa的压力,于80℃下保温固化8h成型,得自润滑织物复合材料。
实施例2
1、按照实施例1步骤1的方法制备预处理混纺纤维布;
2、将35gg-C3N4和5g多层石墨烯球磨混合72h,取出后用乙醇洗涤2次,100℃条件下干燥2h,得到复合固体润滑剂;
3、将10g酚醛-改性环氧胶粘剂(固含量75%)、0.6g纳米CeO2以及步骤2制备3.9g的复合固体润滑剂分散在65.5g四氢呋喃中,在高速分散乳化机中以21000r/min的速度进行充分混合,得到自润滑浸渍液;
4、将所述自润滑浸渍液涂敷于预处理混纺纤维布上,然后移至100℃鼓风烘箱中干燥2h,并重复该过程至预处理混纺纤维布增重65%,得到抗高能辐照自润滑织物衬垫;
5、最后用酚醛树脂将上述烘干后的织物粘贴于304钢表面,并施加0.01MPa的压力,于200℃下保温固化2h成型,得自润滑织物复合材料。
实施例3
1、按照实施例1步骤1的方法制备预处理混纺纤维布;
2、将25gg-C3N4和5g多层石墨烯球磨混合24h后,取出用乙醇洗涤2次,在100℃条件下干燥2h,得到复合固体润滑剂;
2、将10g酚醛-改性环氧胶粘剂(固含量75%)、0.6g纳米CeO2以及步骤2制备1.875g的复合固体润滑剂分散在37.5g丙酮中,在高速分散乳化机中以15000r/min的速度进行充分混合,得到自润滑浸渍液;
4、将所述自润滑浸渍液涂敷于预处理混纺纤维布上,然后移至100℃鼓风烘箱中干燥2h,并重复该过程至预处理混纺纤维布增重50%,得到抗高能辐照自润滑织物衬垫;
5、最后用酚醛树脂将上述抗高能辐照自润滑织物衬垫粘贴于铝基材表面,并施加0.01MPa的压力,于150℃下保温固化2h成型,得自润滑织物复合材料。
实施例4
1、按照实施例1步骤1的方法制备预处理混纺纤维布;
2、将24gg-C3N4和8g多层石墨烯球磨混合12h后,取出用乙醇洗涤2次,80℃条件下干燥2h,得到复合固体润滑剂;
3、将10g酚醛-缩醛胶粘剂(固含量75%)、0.11g纳米CeO2以及步骤2制备3.9g复合固体润滑剂分散在19g乙醇中,在高速分散乳化机中以18000r/min的速度进行充分混合,得到自润滑浸渍液;
4、将上述自润滑浸渍液涂敷于预处理混纺纤维布,然后移至100℃鼓风烘箱中干燥2h,并重复该过程至预处理混纺纤维布增重65%,得到抗高能辐照自润滑织物衬垫;。
5、最后用酚醛树脂将上述抗高能辐照自润滑织物衬垫粘贴于轴承钢表面,并施加0.03MPa的压力,于180℃下保温固化2h成型,得自润滑织物复合材料。
实施例5
1、按照实施例1步骤1的方法制备预处理混纺纤维布;
2、将25gg-C3N4和5g多层石墨烯球磨混合24h后,取出用乙醇洗涤2次,在100℃条件下干燥2h,得到复合固体润滑剂;
3、将10g酚醛-改性环氧胶粘剂(固含量75%)、0.3g纳米CeO2以及步骤2制备3g复合固体润滑剂分散在41g乙酸乙酯中,在高速分散乳化机中以18000r/min的速度进行充分混合,得到自润滑浸渍液;
4、将上述自润滑浸渍液涂敷于预处理混纺纤维布,然后移至100℃鼓风烘箱中干燥2h,并重复该过程至预处理混纺纤维布增重50%,得到抗高能辐照自润滑织物衬垫;
5、最后用酚醛树脂将上述抗高能辐照自润滑织物衬垫粘贴于轴承钢表面,并施加0.01MPa的压力,于180℃下保温固化1.5h成型,得自润滑织物复合材料。
辐照条件为:Co60的放射源,辐照剂量率为50Gy/h,辐照总剂量分别为1000Gy、2200Gy,环境条件为空气氛围。先将自润滑织物复合材料辐照后再进行摩擦实验表征。
摩擦方式为环-块接触方式,摩擦实验表征分析的测试条件为:8rpm/50N、266rpm/200N,测试时间为30min,对偶材料为GCr15轴承钢。
表1为实施例5所得自润滑织物复合材料的摩擦系数和经过辐照后的自润滑织物复合材料的摩擦系数结果。
表1实施例5所得自润滑织物复合材料的摩擦系数和经过辐照后的自润滑织物复合材料的摩擦系数结果
从表1可以看出:经过高能辐照后的自润滑织物复合材料的摩擦系数均有所下降,而且随着辐照剂量的增大,摩擦系数有所升高,证明设计的自润滑织物复合材料在辐照条件下仍然具有润滑性能。
图1为实施例5所得自润滑织物复合材料的摩擦效果图;其中(a)为实施例5所得自润滑织物复合材料未经辐照的摩擦效果图,(b)为实施例5所得自润滑织物复合材料经1000Gy剂量辐照后的摩擦效果图,(c)为实施例5所得自润滑织物复合材料经2200Gy剂量辐照后的摩擦效果图。从图1可以看出:经过辐照后,自润滑织物复合材料的表面没有任何的损伤,证明制备的自润滑织物复合材料具备良好的抗高能辐射性能。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种抗高能辐照自润滑织物衬垫,其特征在于,包括预处理混纺纤维布和负载在所述预处理混纺纤维布上的复合固体润滑剂、二氧化铈和酚醛树脂,所述复合固体润滑剂为石墨相氮化碳和多层石墨烯。
2.根据权利要求1所述的抗高能辐照自润滑织物衬垫,其特征在于,所述复合固体润滑剂、二氧化铈和酚醛树脂的质量之和为预处理混纺纤维布质量的30~65%。
3.根据权利要求1所述的抗高能辐照自润滑织物衬垫,其特征在于,所述复合固体润滑剂的质量为酚醛树脂质量的15~52%。
4.根据权利要求1或2或3所述的抗高能辐照自润滑织物衬垫,其特征在于,所述复合固体润滑剂中石墨相氮化碳和多层石墨烯的质量比为1:1~7:1。
5.根据权利要求1或2或3所述的抗高能辐照自润滑织物衬垫,其特征在于,所述石墨相氮化碳的粒径为10~100nm。
6.根据权利要求1或2或3所述的抗高能辐照自润滑织物衬垫,其特征在于,所述多层石墨烯的层数为10~30层。
7.根据权利要求1所述的抗高能辐照自润滑织物衬垫,其特征在于,所述二氧化铈的质量为酚醛树脂质量的1.5~8%。
8.根据权利要求1或2或7所述的抗高能辐照自润滑织物衬垫,其特征在于,所述二氧化铈的粒径为20~50nm。
9.权利要求1~8任一项所述的抗高能辐照自润滑织物衬垫的制备方法,其特征在于,包括以下步骤:
将所述复合固体润滑剂、二氧化铈、酚醛树脂胶粘剂和稀释剂混合分散,得到自润滑浸渍液;
将所述自润滑浸渍液涂敷于预处理混纺纤维布,干燥,得到所述抗高能辐照自润滑织物衬垫。
10.一种自润滑织物复合材料,其特征在于,所述自润滑织物复合材料由层叠设置的抗高能辐照自润滑织物衬垫、酚醛树脂和金属基材经固化成型得到;
所述抗高能辐照自润滑织物衬垫为权利要求1~8任一项所述的抗高能辐照自润滑织物衬垫或权利要求9所述的制备方法制得的抗高能辐照自润滑织物衬垫。
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