CN114196938A - 一种双层非晶碳膜及其制备方法 - Google Patents
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Abstract
本发明提供一种双层非晶碳膜及其制备方法,涉及金属涂层材料制备技术。所述所述双层非晶碳膜包括第一层非晶碳膜和第二层非晶碳膜,且所述第一层非晶碳膜为采用类石墨结构为主的GLC非晶碳膜层,所述第二层非晶碳膜为采用类金刚石为主的DLC膜层。本发明克服了现有技术的不足,通过不同结构的非晶碳的组合,避免了单一结构非晶碳膜硬度高、内应力大、摩擦系数高或者硬度低、内应力小、摩擦系数小的极端问题,有效满足精密器件的保护与装配配合度性能要求。
Description
技术领域
本发明涉及金属涂层材料制备技术,具体涉及一种双层非晶碳膜及其制备方法。
背景技术
非晶碳膜具有化学性质稳定、硬度高、耐磨性能好等特点,其可分为以SP2结构为主的类石墨非晶碳结构(GLC)和以SP3结构为主的类金刚石结构(DLC)。
类石墨结构GLC具有较好的导电性能和附着力,但硬度较低;而类金刚石结构DLC则硬度高、疏水性能好、导电性能差,二者在性能上有较大差异。
在精密器件加工领域,需要密合的精密器件部件对表面加工精度要求很高,在承受高应力的条件下,如果发生形变将严重影响器件的密合程度,因而对其表面的耐磨性能要求很高。
人们一般通过阳极氧化和电镀工艺来提高表面的磨损性能,但这些工艺对环境污染严重,另一方面,这两种工艺处理过的器件表面的精度也将下降,器件部件之间发生摩擦也会对阳极氧化层或电镀层产生破坏。此外,对于生物医学金属材料在用于夹具、螺钉和螺纹等机械接口时,往往具有较差的摩擦学性能,从而导致有限的重新定位、不均匀的扭矩参数,甚至机械接头被卡住或剥离等现象。
发明内容
针对现有技术不足,本发明提供一种双层非晶碳膜及其制备方法,通过不同结构的非晶碳的组合,避免了单一结构非晶碳膜硬度高、内应力大、摩擦系数高或者硬度低、内应力小、摩擦系数小的极端问题,有效满足精密器件的保护与装配配合度性能要求。
为实现以上目的,本发明的技术方案通过以下技术方案予以实现:
一种双层非晶碳膜,所述双层非晶碳膜包括第一层非晶碳膜和第二层非晶碳膜,所述第一层非晶碳膜和第二层非晶碳膜具有不同比率的SP2结构类石墨非晶碳和SP3结构类金刚石非晶碳,且所述第一层非晶碳膜为采用类石墨结构为主的GLC非晶碳膜层,所述第二层非晶碳膜为采用类金刚石为主的DLC膜层。
优选的,所述双层非晶碳膜是等离子体增强化学气相沉积膜。
优选的,所述第一层非晶碳膜中类石墨非晶碳与类金刚石非晶碳的组分比例为4∶1-3∶1;所述第二层非晶碳膜中类石墨非晶碳与类金刚石非晶碳的组分比例为1∶5-1∶8。
优选的,所述第一层非晶碳膜厚度为200nm-5um;所述第二层非晶碳膜厚度为500nm-1um。
所述双层非晶碳膜的制备方法包括以下步骤:
(1)第一层非晶碳膜制备:将基材于中空腔室中抽真空后,通过离子源向中空腔室内通入乙炔气体,再以石墨为溅射靶材,向溅射靶内通入氩气,同时基材施加脉冲偏压在基材表面沉积非晶碳膜层,得到第一层非晶碳膜;
(2)第二层非晶碳膜制备:将上述放置基材的中空腔室抽真空,通过离子源向中空腔室内通入乙炔气体,同时对基材施加脉冲偏压在基材上沉积第二层非晶碳膜,得到双层非晶碳膜。
优选的,所述步骤(1)中通入乙炔气体的通入流量为30-40sccm,离子源电流为0.10-0.15A。
优选的,所述步骤(1)中氩气流量为40-60sccm,氩气溅射电流为1A。
优选的,所述步骤(1)中对基材施加脉冲偏压为-150V,步骤(2)中对基材施加脉冲偏压为-200V。
优选的,所述步骤(1)中沉积时间为40min,步骤(2)中沉积时间为20min。
优选的,所述步骤(2)中乙炔气体的通入流量为30-40sccm,离子源电流为0.20-0.25A。
本发明提供一种双层非晶碳膜及其制备方法,与现有技术相比优点在于:
(1)本发明制备的双层非晶碳膜可以通过不同结构的非晶碳的组合,避免了单一结构非晶碳膜硬度高、内应力大、摩擦系数高或者硬度低、内应力小、摩擦系数小的极端问题,在第一层采用类石墨结构为主的GLC非晶碳涂层提高与基材的结合力、降低内应力,在第二层则通过类金刚石为主的DLC结构提高涂层体系的硬度、降低摩擦系数,使得本发明所制备的非晶碳膜在稳态、未润滑和环境大气条件下的摩擦系数值小于0.06;
(2)本发明提供的双层非晶碳膜具有高附着力、低应力、低摩擦系数和高硬度,与器件结合力高、可完全满足精密器件的保护与装配配合度性能要求。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面结合本发明实施例对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:
双层非晶碳膜的制备:
(1)第一层非晶碳膜制备(类石墨非晶碳膜GLC为主):将基材不锈钢锭(直径15mm,高度7mm)放置在PECVD的中空腔室,抽真空,通过离子源向放置基材的中空腔室内通入流量为30sccm的乙炔气体,离子源电流为0.15A,然后以石墨为溅射靶材,向溅射靶内通入氩气,氩气流量为40sccm,氩气溅射电流为1A,向基材施加脉冲偏压-150V,沉积时间为40min,得到薄膜厚度为200nm~5um的非晶碳膜;
(2)第二层非晶碳膜制备(类金刚石非晶碳膜DLC为主):在上述步骤(1)结束后,将放置基材的中空腔室抽真空,然后通过离子源向中空腔室内通入流量为30sccm的乙炔气体,离子源电流为0.25A,同时施加-200V的脉冲偏压,沉积时间为20min,得到薄膜厚度为500nm~1um的非晶碳膜。
实施例2:
双层非晶碳膜的制备:
(1)第一层非晶碳膜制备(类石墨非晶碳膜GLC为主):将基材不锈钢锭(直径15mm,高度7mm)放置在PECVD的中空腔室,抽真空,通过离子源向放置基材的中空腔室内通入流量为40sccm的乙炔气体,离子源电流为0.10A,然后以石墨为溅射靶材,向溅射靶内通入氩气,氩气流量为60sccm,氩气溅射电流为1A,向基材施加脉冲偏压-150V,沉积时间为40min,得到薄膜厚度为200nm~5um的非晶碳膜;
(2)第二层非晶碳膜制备(类金刚石非晶碳膜DLC为主):在上述步骤(1)结束后,将放置基材的中空腔室抽真空,然后通过离子源向中空腔室内通入流量为40sccm的乙炔气体,离子源电流为0.20A,同时施加-200V的脉冲偏压,沉积时间为20min,得到薄膜厚度为500nm~1um的非晶碳膜。
实施例3:
双层非晶碳膜的制备:
(1)第一层非晶碳膜制备(类石墨非晶碳膜GLC为主):将基材不锈钢锭(直径15mm,高度7mm)放置在PECVD的中空腔室,抽真空,通过离子源向放置基材的中空腔室内通入流量为35sccm的乙炔气体,离子源电流为0.13A,然后以石墨为溅射靶材,向溅射靶内通入氩气,氩气流量为50sccm,氩气溅射电流为1A,向基材施加脉冲偏压-150V,沉积时间为40min,得到薄膜厚度为200nm~5um的非晶碳膜;
(2)第二层非晶碳膜制备(类金刚石非晶碳膜DLC为主):在上述步骤(1)结束后,将放置基材的中空腔室抽真空,然后通过离子源向中空腔室内通入流量为35sccm的乙炔气体,离子源电流为0.22A,同时施加-200V的脉冲偏压,沉积时间为20min,得到薄膜厚度为500nm~1um的非晶碳膜。
对比例1:
双层非晶碳膜的制备:
(1)第一层非晶碳膜制备(类石墨非晶碳膜GLC为主):将基材不锈钢锭(直径15mm,高度7mm)放置在PECVD的中空腔室,抽真空,通过离子源向放置基材的中空腔室内通入流量为35sccm的乙炔气体,离子源电流为0.13A,然后以石墨为溅射靶材,向溅射靶内通入氩气,氩气流量为20sccm,氩气溅射电流为1A,向基材施加脉冲偏压-100V,沉积时间为40min,得到薄膜厚度为200nm~5um的非晶碳膜;
(2)第二层非晶碳膜制备(类金刚石非晶碳膜DLC为主):在上述步骤(1)结束后,将放置基材的中空腔室抽真空,然后通过离子源向中空腔室内通入流量为35sccm的乙炔气体,离子源电流为0.22A,同时施加-200V的脉冲偏压,沉积时间为20min,得到薄膜厚度为500nm~1um的非晶碳膜。
对比例2:
双层非晶碳膜的制备:
(1)第一层非晶碳膜制备(类石墨非晶碳膜GLC为主):将基材不锈钢锭(直径15mm,高度7mm)放置在PECVD的中空腔室,抽真空,通过离子源向放置基材的中空腔室内通入流量为35sccm的乙炔气体,离子源电流为0.13A,然后以石墨为溅射靶材,向溅射靶内通入氩气,氩气流量为50sccm,氩气溅射电流为1A,向基材施加脉冲偏压-150V,沉积时间为40min,得到薄膜厚度为200nm~5um的非晶碳膜;
(2)第二层非晶碳膜制备(类金刚石非晶碳膜DLC为主):在上述步骤(1)结束后,将放置基材的中空腔室抽真空,然后通过离子源向中空腔室内通入流量为20sccm的乙炔气体,离子源电流为0.22A,同时施加-200V的脉冲偏压,沉积时间为20min,得到薄膜厚度为500nm~1um的非晶碳膜。
检测:
通过球盘式摩擦磨损试验机(JLTB-02,J&L Tech.,Korean)测试上述实施例1-3和对比例1-2中所制得的样品涂层的摩擦系数;通过残余应力仪过残余应力仪(StressTester,J<ech.,Korean)测试各组样品涂层的内应力;通过维氏硬度计测试各组样品涂层的硬度;通过WS-2005型划痕仪测试样品涂层的结合力;通过拉曼光谱测试涂层中不同结构的比例,结果如下表1所示。
表1:不同实施例样品涂层性能比较
从上表1中可以看出,实施例样品摩擦系数均较低,实施例的样品硬度均较大(大于17GPa),对比例则较小,同时,实施例的结合力也较大(大于35N),而对比例1则较小,可见,通过涂层的结构设计,实施例实现了涂层高硬度和高结合力的结合。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下,由语句“包括一个……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。
以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种双层非晶碳膜,其特征在于:所述双层非晶碳膜包括第一层非晶碳膜和第二层非晶碳膜,所述第一层非晶碳膜和第二层非晶碳膜具有不同比率的SP2结构类石墨非晶碳和SP3结构类金刚石非晶碳,且所述第一层非晶碳膜为采用类石墨结构为主的GLC非晶碳膜层,所述第二层非晶碳膜为采用类金刚石为主的DLC膜层。
2.一种双层非晶碳膜,其特征在于:所述双层非晶碳膜是等离子体增强化学气相沉积膜。
3.一种双层非晶碳膜,其特征在于:所述第一层非晶碳膜中类石墨非晶碳与类金刚石非晶碳的组分比例为4∶1-3∶1;所述第二层非晶碳膜中类石墨非晶碳与类金刚石非晶碳的组分比例为1∶5-1∶8。
4.一种双层非晶碳膜,其特征在于:所述第一层非晶碳膜厚度为200nm-5um;所述第二层非晶碳膜厚度为500nm-1um。
5.一种双层非晶碳膜的制备方法,其特征在于,所述双层非晶碳膜的制备方法包括以下步骤:
(1)第一层非晶碳膜制备:将基材于中空腔室中抽真空后,通过离子源向中空腔室内通入乙炔气体,再以石墨为溅射靶材,向溅射靶内通入氩气,同时基材施加脉冲偏压在基材表面沉积非晶碳膜层,得到第一层非晶碳膜;
(2)第二层非晶碳膜制备:将上述放置基材的中空腔室抽真空,通过离子源向中空腔室内通入乙炔气体,同时对基材施加脉冲偏压在基材上沉积第二层非晶碳膜,得到双层非晶碳膜。
6.根据权利要求5所述的一种双层非晶碳膜的制备方法,其特征在于:所述步骤(1)中通入乙炔气体的通入流量为30-40sccm,离子源电流为0.10-0.15A。
7.根据权利要求5所述的一种双层非晶碳膜的制备方法,其特征在于:所述步骤(1)中氩气流量为40-60sccm,氩气溅射电流为1A。
8.根据权利要求5所述的一种双层非晶碳膜的制备方法,其特征在于:所述步骤(1)中对基材施加脉冲偏压为-150V,步骤(2)中对基材施加脉冲偏压为-200V。
9.根据权利要求5所述的一种双层非晶碳膜的制备方法,其特征在于:所述步骤(1)中沉积时间为40min,步骤(2)中沉积时间为20min。
10.根据权利要求5所述的一种双层非晶碳膜的制备方法,其特征在于:所述步骤(2)中乙炔气体的通入流量为30-40sccm,离子源电流为0.20-0.25A。
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