CN109627816B - 低摩擦碳基固体润滑涂层及其制备方法和应用 - Google Patents
低摩擦碳基固体润滑涂层及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种低摩擦碳基固体润滑涂层,该涂层包括碳薄膜,所述碳薄膜具有规则分布的裂纹,并被所述的裂纹分割成网格状;在所述的裂纹中填充有固体润滑剂。可通过包括如下步骤制得:(1)将丝网置于基体表面上;(2)在基体表面上沉积碳薄膜;(3)去除丝网,在碳薄膜上得到与丝网相对应的裂纹;(4)向裂纹中注入固体润滑剂。本发明的涂层具有低摩擦系数,在橡胶表面具有良好的灵活度和优异的结合力,可用于制备动密封件。
Description
技术领域
本发明属于密封材料领域,具体涉及用于橡胶表面的低摩擦碳基固体润滑涂层。
背景技术
现代工业设备中存在大量的密封装置,用以防止工作介质泄漏及外界灰尘和异物侵入。而密封介质一旦泄漏,会直接危及人身安全,带来巨大经济损失。目前,大多密封泄漏事故均与密封件的磨损失效有关。例如日本炼油行业发生的燃烧爆炸事故正是由于橡胶密封圈磨损失效造成的。因此,密封件磨损失效是机械设备密封系统关键共性技术问题之一。
橡胶由于其弹性模量小、伸长率高、耐密封介质腐蚀性能强,因此作为重要的动密封部件广泛应用于航空航天、汽车、化工机械等技术领域。然而,当橡胶与金属配副时会产生严重的粘着磨损,从而极大地减短橡胶密封件的实际服役寿命,同时影响系统安全性和精确性。因此,减小橡胶密封件与装配件之间的摩擦力具有重要的意义。传统降低橡胶密封件磨损的主要方法是在橡胶体与金属配副之间使用油脂润滑以降低摩擦力。但由于摩擦热效应会导致油液粘度、结构等造成致命损坏,从而导致其润滑失效。因此,探寻有效的改善橡胶密封件耐磨性的方法迫在眉睫。
由于材料摩擦磨损总是发生在材料的表面或亚表面,因此表面固体润滑薄膜改性技术无疑是最理想的方法。前期人们尝试采用金属薄膜,但金属薄膜仍会与密封件对偶发生严重粘着磨损。而碳薄膜与橡胶具有良好的化学相容性,且不会改变橡胶基底的自身属性(如柔韧性,抗拉强度等),因而是橡胶表面耐磨改性的理想材料。改性后橡胶与金属配副之间的接触转变为碳薄膜与金属配副之间的摩擦,避免了橡胶基体与摩擦副直接接触,从而有效降低了薄膜的粘着磨损。然而,橡胶是软基底而碳薄膜是硬质涂层,如何确保硬质薄膜在软基底发生形变时不至于发生脱落,且能保持橡胶基底的柔韧性(即碳薄膜灵活性)是重中之重。此外,降低涂层摩擦系数可有效延长薄膜的耐磨损寿命,提高密封设备安全性和可靠性。
发明内容
针对现有橡胶表面碳薄膜的缺陷,本发明的目的在于提供一种在能够橡胶表面实现灵活度高且摩擦系数低的固体润滑涂层。
为实现上述目的,本发明采用如下技术方案:
低摩擦碳基固体润滑涂层,包括碳薄膜,其特点在于:所述碳薄膜具有规则分布的裂纹,并被所述的裂纹分割成网格状;在所述的裂纹中填充有固体润滑剂。
优选地,所述网格为方形网格、菱形网格或圆形网格。
优选地,所述固体润滑剂为石墨、二硫化钼和聚四氟乙烯颗粒中的一种或几种,更优选地,所述颗粒的尺寸在5µm以下。
优选地,在所述的裂纹中填充有粘结剂。
优选地,所述粘结剂为聚酰亚胺粘结剂、酚醛树脂粘结剂和环氧树脂粘结剂中的一种或几种。
上述低摩擦碳基固体润滑涂层的制备方法,包括如下步骤:
(1)将丝网置于基体表面上;
(2)在基体表面上沉积碳薄膜;
(3)去除丝网,在碳薄膜上得到与丝网相对应的裂纹;
(4)向裂纹中注入固体润滑剂。
优选地,所述碳薄膜是通过等离子体增强化学气相沉积法沉积得到,沉积条件为:Ar、H2、CH4的流量分别为15sccm、10sccm、5sccm,脉冲偏压为-700V,占空比为40~50%,频率为40~50KHz,沉积气压为20Pa,沉积温度为 80℃。
基体为橡胶基体时,在沉积碳薄膜前,依次用氩等离子体和氢等离子体对橡胶基体进行轰击处理,可实现橡胶表面微纳级清洗及表面活化,其中,氩等离子体轰击的条件为:氩气流量300sccm,腔内气压为4~6Pa,脉冲偏压为-900V,占空比为50~60%,频率为60~70KHz,氢等离子体轰击的条件为:氢气流量200sccm,腔内气压为4~6Pa,脉冲偏压为-900V,占空比为50~60%,频率为60~70KHz。
优选地,步骤(4)的具体过程包括:将固体润滑剂、胶粘剂、固化剂和有机溶剂混合后,注入裂纹中,干燥,优选地,固体润滑剂、固化剂与胶粘剂的质量比为20~30:16~20:40。所述有机溶剂可选用丁酮、二甲苯等。
优选地,所述基体的表面光洁度Ra<200nm。
优选地,所述丝网的网孔为方形、菱形或圆形。
上述低摩擦碳基固体润滑涂层在制备动密封件中的应用。
一种动密封件,包括橡胶基体,所述橡胶基体的表面具有如上所述的低摩擦碳基固体润滑涂层。
所述橡胶基体选自氟橡胶、丁腈橡胶、硅橡胶中的任意一种。橡胶基体的表面光洁度Ra<200nm,厚度为0.5~5mm。
优选地,所述的碳薄膜中,裂纹面积占总表面积的2~20%,更优选地为2~10%。
本发明与现有技术相比具有以下优点:
1、本发明碳基固体润滑涂层的裂纹为人造的规则分布的裂纹,裂纹的大小、排列方式、间距等均可人为调节控制,从而保证了硬质碳薄膜高灵活度,避免了因橡胶形变而造成的薄膜碎裂脱落,确保了橡胶基底的柔韧性;
2、本发明设计的人造裂纹能够有效的释放薄膜中的残余应力,确保了薄膜与橡胶基底高的结合力;
3、本发明设计的碳基固体润滑涂层具有很好的灵活性和塑性,可随橡胶基体形变而发生形变。将固体润滑剂填充在碳薄膜裂纹中,避免了摩擦对偶与裂纹边缘和顶端的尖锐碰撞,从而有效的降低了薄膜摩擦系数。同时,该碳基固体润滑涂层具有优异的亲油性,油液可在其表面形成均匀成膜;
4、采用反复弯曲法对本发明的碳基固体润滑涂层进行灵活性评价。结果显示:样品在经过20~30次反复弯曲后,橡胶表面的碳基固体润滑涂层未发生脱落现象,表明本发明的涂层具有良好的灵活度和优异的结合力。
5、采用摩擦磨损试验机对本发明的碳基固体润滑涂层进行摩擦学性能评价。摩擦条件为:球-盘旋转模式,法向载荷5N,摩擦对偶为φ6mm GCr15钢球,测试环境为大气。结果显示:常规的纯碳薄膜摩擦系数较高(~0.27),而本发明碳基固体润滑涂层的摩擦系数显著降低(~0.20)。
6、本发明碳基固体润滑涂层的制备工艺简单,可操作性强,沉积温度低、易于实现大面积工业化应用。
附图说明
图1 为碳薄膜裂纹的形成示意图。
图2 为碳基固体润滑涂层结构示意图。
图3 为碳基固体润滑涂层摩擦系数曲线。
具体实施方式
实施例1橡胶表面碳基固体润滑涂层的制备方法,采用高真空多功能磁控溅射离子镀膜设备,包括以下步骤:
(1)将300×300×2mm黑色丁腈橡胶板(表面光洁度Ra<200nm,厚度为2mm)切割成30×30mm2的橡胶片,浸泡在60℃肥皂水溶液中超声清洗30min,以除去橡胶表面的油脂和污垢;然后取出并浸泡在90-95℃蒸馏水超声清洗30min,以除去可能残留的肥皂水溶液;最后用干燥氮气吹干后放置于干燥箱中120℃下再干燥20min,以蒸发掉橡胶表面残留水分。上述过程反复进行5次。
(2)待橡胶冷却至室温后,将橡胶放置于样品盘上,然后将铁丝网(方形网孔0.5×0.5mm,丝线直径0.01mm)以任意角度放置于橡胶表面,关闭真空腔门,将真空腔真空抽至≤1.0×10–3Pa。
(3)向真空腔中通入流量300sccm氩气,腔内气压为4~6Pa,打开高功率脉冲叠加直流偏压电源,利用氩等离子体对橡胶进行轰击处理,其中偏压为-900V,占空比为55%,频率为60KHz,处理时间为35min。然后抽干净氩气,再通入200sccm氢气,利用上述同样条件轰击清洗25min。
(4)处理结束后待橡胶温度降至室温,然后向真空腔中通入15sccm Ar2、10sccmH2、5sccm CH4气体,开启高功率脉冲偏压电源沉积碳薄膜,偏压为-700V,占空比为45%,频率为45KHz,沉积气压保持在20Pa,沉积时间为120min,沉积温度恒定在80℃。沉积结束后待真空腔内温度冷却至室温后取出样品,并小心剥离金属铁丝网,得到被规则排列的裂纹分割成网格状的碳薄膜;采用相同条件制备无裂纹的纯碳薄膜作为对比样品。
(5)将25wt%石墨颗粒、15wt%丁酮、40wt%双酚A型环氧树脂粘结剂和20wt%固化剂(β-羟乙基乙二胺)充分混合后,在光学显微镜下利用微纳注射器将其缓慢注入碳薄膜的裂纹中,然后充分干燥固化(即固体润滑干膜),从而在橡胶表面上得到碳基固体润滑涂层。
实施例2硅橡胶表面碳基固体润滑涂层的制备方法,包括以下步骤:
(1)硅橡胶预清洗步骤同实施例1。其中:硅橡胶表面光洁度Ra<200 nm,厚度为3mm。
(2)~(3)同实施例1。丝网采用镍丝网(菱形网孔,开孔率94%)。
(4)处理结束后硅橡胶温度降至室温,然后向真空腔中通入15sccm Ar2、10sccmH2、5sccm CH4气体,开启高功率脉冲偏压电源沉积碳薄膜,偏压为-700V,占空比为50%,频率为50KHz,沉积气压保持在20Pa,沉积时间为120min,沉积温度恒定在80℃。沉积结束后待真空腔内温度冷却至室温后取出样品,并小心剥离镍丝网,得到被规则排列的裂纹分割成网格状的碳薄膜。
(5)将20wt%石墨颗粒、20wt%二甲苯、40wt%酚醛树脂粘结剂和20wt%固化剂(β-羟乙基乙二胺)充分混合后,在光学显微镜下利用微纳注射器将其缓慢注入碳薄膜的裂纹中,然后充分干燥固化,从而在硅橡胶表面上得到碳基固体润滑涂层。
实施例3硅橡胶表面碳基固体润滑涂层的制备方法,包括以下步骤:
(1)硅橡胶预清洗步骤同实施例1。其中:硅橡胶表面光洁度Ra<200 nm,厚度为3mm。
(2)~(3)同实施例1。丝网采用尼龙丝网(圆形网孔,开孔率85%)。
(4)处理结束后待基底温度降至室温,然后向真空腔中通入15sccm Ar2、10sccmH2、5sccm CH4气体,开启高功率脉冲偏压电源沉积碳薄膜,偏压为-700V,占空比为40%,频率为40KHz,沉积气压保持在20Pa,沉积时间为120min,沉积温度恒定在80℃。沉积结束后待真空腔内温度冷却至室温后取出样品,并小心剥离尼龙丝网,得到被规则排列的裂纹分割成网格状的碳薄膜。
(5)将30wt%二硫化钼颗粒、14wt%二甲苯和40wt%聚酰亚胺粘结剂和16wt%固化剂(β-羟乙基乙二胺)充分混合后,在光学显微镜下利用微纳注射器将其缓慢注入碳薄膜的裂纹中,然后充分干燥固化,从而在硅橡胶表面上得到碳基固体润滑涂层。
Claims (11)
1.低摩擦碳基固体润滑涂层,包括碳薄膜,其特征在于:所述碳薄膜具有规则分布的裂纹,并被所述的裂纹分割成网格状;在所述的裂纹中填充有固体润滑剂和粘结剂,其中,固体润滑剂与粘结剂的质量比为20~30:40。
2.如权利要求1所述的低摩擦碳基固体润滑涂层,其特征在于:所述网格为方形网格、菱形网格或圆形网格。
3.如权利要求1所述的低摩擦碳基固体润滑涂层,其特征在于:所述固体润滑剂为石墨颗粒、二硫化钼颗粒和聚四氟乙烯颗粒中的一种或几种。
4.如权利要求3所述的低摩擦碳基固体润滑涂层,其特征在于:所述颗粒的尺寸在5µm以下。
5.如权利要求1所述的低摩擦碳基固体润滑涂层,其特征在于:所述粘结剂为聚酰亚胺粘结剂、酚醛树脂粘结剂和环氧树脂粘结剂中的一种或几种。
6.权利要求1~5任一所述的低摩擦碳基固体润滑涂层的制备方法,包括如下步骤:
(1)将丝网置于基体表面上;
(2)在基体表面上沉积碳薄膜;
(3)去除丝网,在碳薄膜上得到与丝网相对应的裂纹;
(4)向裂纹中注入固体润滑剂。
7.如权利要求6所述的制备方法,其特征在于:所述碳薄膜是通过等离子体增强化学气相沉积法沉积得到,沉积条件为:Ar、H2、CH4的流量分别为15sccm、10sccm、5sccm,脉冲偏压为-700V,占空比为40~50%,频率为40~50KHz,沉积气压为20Pa,沉积温度为 80℃。
8.如权利要求6所述的制备方法,其特征在于:步骤(4)的具体过程包括:将固体润滑剂、粘结剂、固化剂和有机溶剂混合后,注入裂纹中。
9.如权利要求8所述的制备方法,其特征在于:固体润滑剂、固化剂与粘结剂的质量比为20~30:16~20:40。
10.权利要求1~5任一所述的低摩擦碳基固体润滑涂层的应用,所述的低摩擦碳基固体润滑涂层在制备动密封件中的应用。
11.一种动密封件,包括橡胶基体,其特征在于:所述橡胶基体的表面具有如权利要求1~5任一所述的低摩擦碳基固体润滑涂层。
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