CN109182997B - 一种掺Si的类金刚石涂层的制备方法 - Google Patents
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Abstract
本发明公开了一种掺Si的DLC涂层的制备方法，将预处理后的工件放入镀膜设备真空室中的转架杆上，该转架杆随转架台转动，采用安置在炉体内壁上的溅射靶作为掺Si的物质源，用脉冲电源的功率控制Si的溅射率，高纯Ar和高纯CH4通过离子源进入真空室；然后进行沉积Si底层、SiC过渡层和掺Si的DLC涂层，所得到的掺Si的DLC涂层比传统掺金属的DLC涂层的硬度高、结合力强、耐磨及减摩性能好，可满足于严酷工作条件的零部件表面耐磨减摩涂层的性能设计要求。
Description
技术领域
本发明属于涂层制备技术领域，具体涉及一种掺Si的类金刚石涂层的制备方法。
背景技术
类金刚石涂层(Diamond-like Carbon，简称DLC)是碳基涂层的典型代表，其高硬度、低摩擦系数和良好的化学稳定性引起人们的广泛关注。DLC涂层是金刚石结构(sp3键)和石墨结构(sp2键)混合的非晶态亚稳物质，其中，碳原子主要以sp3和sp2杂化键结合，通过调控化学键组成比例，可优化涂层的耐磨和减摩性能，从而有望在航空、汽车、电子等行业的关键零部件、切削刀具及成型模具表面改性领域获得广泛应用。
DLC涂层具有极低的摩擦系数(≤0.2)，保证了它具有优异的减摩性能以及自润滑性能。然而，要使DLC涂层在保持优异减摩性能的同时，也能兼具良好的耐磨性能，仍面临巨大的技术挑战，主要困难在于DLC涂层自身内应力大、韧性差、硬度低，在使用过程中会发生磨损，开裂，甚至涂层剥落等。为此，研究人员开发的各种掺金属的DLC涂层，通过金属打底层和过渡层设计，以及金属颗粒强化等，不同程度解决了涂层内应力大、结合力弱和硬度相对偏低等技术难题，DLC涂层耐磨损性能得到一定改善，并已开始在工业实际中应用。
申请人在长期的研究过程中，曾发明了各种掺金属的DLC涂层的设计方案及制备技术，例如：掺Cr的DLC涂层(中国专利号：ZL201210421250.3)，掺Ti的DLC涂层(中国专利号：ZL201210423173.5),以及掺W的DLC涂层(中国专利号：ZL201310344882.9)等，已在高速缝纫机针杆、滑块，制冷压缩机曲轴及铝合金切削刀具上取得成功应用。但这些含氢的掺金属的DLC涂层的硬度基本在HV3000以下，当应用于更加严酷的耐磨减摩零件时，摩檫学性能仍显不足，这主要是硬度相对较低造成的。
申请人也曾发明了纳米复合TiAlSiN超硬涂层技术实现方案及制备工艺(中国专利号：ZL201210139265.0)，该涂层硬度达到HV4000及以上，其技术实现方案就是在真空气相沉积TiAlN硬质涂层中加入非金属Si，在沉积过程中形成了纳米颗粒的Si3N4物质相，通过纳米颗粒弥散强化将TiAlN涂层硬度从HV3000，提高到TiAlSiN涂层的HV4000以上，与国内外研究者大多采用掺金属的传统技术方案不同。
发明内容
本发明的目的在于，提供一种掺Si的类金刚石涂层的制备方法，所得到的掺Si的DLC涂层比传统掺金属的DLC涂层的硬度高、结合力强、耐磨及减摩性能好，可满足于严酷工作条件的零部件表面耐磨减摩涂层的性能设计要求。
为了实现上述任务，本发明采取如下的技术解决方案：
一种掺Si的DLC涂层的制备方法，其特征在于，按下列步骤进行：
1)将预处理后的工件放入镀膜设备真空室中的转架杆上，该转架杆随转架台转动，以保证镀膜过程的均匀性；
2)使用安置在炉体内壁上的溅射靶作为掺Si的物质源，用脉冲电源的功率控制Si的溅射率，高纯Ar和高纯CH4通过离子源进入真空室；
3)涂层制备工艺参数：
A.工件等离子清洗：
Ar气体流量30sccm，真空度1.0×10-1Pa，离子源功率1.5kW，工件负偏压600V，用Ar离子轰击工件表面，时间60min；
B.沉积Si底层：
Ar流量50sccm，真空度1.5×10-1Pa，离子源功率0.5kW，工件负偏压60V，开启溅射靶，溅射靶功率1.2kW，沉积时间10min；
C.沉积SiC过渡层：
将CH4通过离子源通入真空室，CH4流量30sccm，Ar流量60sccm，真空度2.0×10- 1Pa，离子源功率1.0kW，工件负偏压60V，溅射靶功率2.0kW，沉积时间20min；
D.沉积掺Si的DLC涂层：
Ar流量80sccm，CH4流量60sccm，真空度5×10-1Pa，离子源功率2.0kW，工件负偏压30V，溅射靶功率0.2kW，沉积时间150min，获得掺Si的DLC涂层。
本发明的掺Si的DLC涂层的制备方法，采用了非金属Si作为底层和SiC作为过渡层的设计方案，使DLC涂层结合力显著提高。同时，在DLC涂层中还形成了2％左右体积的纳米颗粒SiC相，通过纳米颗粒SiC相的弥散强化作用，使硬度大幅增加，达到了兼具耐磨性能和减摩性能的涂层设计要求。
所获得的掺Si的DLC涂层，其微观结构组成为：Si底层/SiC过渡层/掺Si的DLC(～2％SiC)涂层。
经测试，上述制备的掺Si的DLC涂层，外观呈黑色，表面致密，手感光滑，硬度HV3500，膜基结合力80N，厚度2.5μm，当摩擦副为Al2O3时，涂层的干摩擦系数为0.1。
附图说明
图1为本发明采用的镀膜设备结构示意图。
以下结合附图和实施例对本发明作进一步的详细说明。
具体实施方式
借鉴中国专利号：ZL201210139265.0的研究成果，申请人近期在DLC涂层制备技术研究中，创造性的提出加入非金属Si，通过大量工艺优化实验，采用离子源增强磁控溅射方法，成功制备出新型高硬度、低摩擦的掺Si的DLC涂层，有望进一步应用到严酷工作条件的零部件表面耐磨减摩领域。
本实施例给出一种采用离子源增强磁控溅射掺Si的DLC涂层的制备方法。需要说明的是，本发明的方法制备的掺Si的DLC涂层，可以在任何选用的基体材料上进行，并不限于该实施例。
本实施例给出的掺Si的DLC涂层的制备方法的具体实施过程是：
(1)采用碳化钨类的硬质合金YG15制成的试块(成分(％)WC:85，Co:15，硬度HRA87)作为基体样品，首先对样品进行预处理，即将样品表面抛光后浸入丙酮中超声波清洗，酒精脱水，待用。
(2)将样品放入镀膜设备中，镀膜设备如图1所示，镀膜设备至少包括有真空室1、转台架2、偏压3、转架杆4、溅射靶5、永磁体6、离子源7、加热器8、泵组9。
将预处理后的样品置于真空室1中的转架杆4上,转架杆4随转架台2转动，以保证镀膜过程的均匀性；溅射靶5采用尺寸为435mm×95mm×10mm的一对平面Si靶，以对称的方式分别安置在炉体左右内壁上，并通过电源功率控制溅射靶5的溅射率。
(3)离子源7采用阳极层矩形气体离子源，高纯Ar和高纯CH4通过离子源7进入真空室。
(4)涂层制备工艺参数：
A.工件等离子清洗：
Ar气体流量30sccm，真空度1.0×10-1Pa，离子源功率1.5kW，工件负偏压600V，用Ar离子轰击工件表面，时间60min；
B.沉积Si底层：
Ar流量50sccm，真空度1.5×10-1Pa，离子源功率0.5kW，工件负偏压60V，开启溅射靶5，溅射靶5功率1.2kW，沉积时间10min；
C.沉积SiC过渡层：
将CH4通过离子源通入真空室，CH4流量30sccm，Ar流量60sccm，真空度2.0×10- 1Pa，离子源功率1.0kW，工件负偏压60V，溅射靶5功率2.0kW，沉积时间20min；
D.沉积掺Si的DLC涂层：
Ar流量80sccm，CH4流量60sccm，真空度5×10-1Pa，离子源功率2.0kW，工件负偏压30V，溅射靶功率0.2kW，沉积时间150min，获得掺Si的DLC涂层。
本实施例制备的掺Si的DLC涂层，外观呈黑色，表面致密，手感光滑，硬度HV3500，膜基结合力80N，厚度2.5μm，当摩擦副为Al2O3时，涂层的干摩擦系数为0.1。
相对于传统的掺金属的DLC涂层，本实施例制备的这类新型掺Si的DLC涂层，由于非金属Si的独特作用，进一步提高了涂层硬度、降低了涂层摩擦系数，解决了兼具优异的减摩性能和良好的耐磨损性能的设计要求，是严酷工作条件零部件表面耐磨减摩的理想涂层。
Claims (2)
1.一种掺Si的DLC涂层的制备方法，其特征在于，该制备方法采用离子源增强磁控溅射方法，按下列步骤进行：
1)将预处理后的工件放入镀膜设备真空室中的转架杆上，该转架杆随转架台转动，以保证镀膜过程的均匀性；
2)安置在炉体内壁上的溅射靶作为掺Si的物质源，用脉冲电源的功率控制Si的溅射率，高纯Ar和高纯CH4通过离子源进入真空室；
3)涂层制备工艺参数：
A.工件等离子清洗：
Ar气体流量30sccm，真空度1.0×10-1Pa，离子源功率1.5kW，工件负偏压600V，用Ar离子轰击工件表面，时间60min；
B.沉积Si底层：
Ar流量50sccm，真空度1.5×10-1Pa，离子源功率0.5kW，工件负偏压60V，开启溅射靶，溅射靶功率1.2kW，沉积时间10min；
C.沉积SiC过渡层：
将CH4通过离子源通入真空室，CH4流量30sccm，Ar流量60sccm，真空度2.0×10-1Pa，离子源功率1.0kW，工件负偏压60V，溅射靶功率2.0kW，沉积时间20min；
D.沉积掺Si的DLC涂层：
Ar流量80sccm，CH4流量60sccm，真空度5×10-1Pa，离子源功率2.0kW，工件负偏压30V，Si溅射靶功率0.2kW，沉积时间150min，获得掺Si的DLC涂层；
所述的掺Si的DLC涂层的硬度为HV3500，膜基结合力80N，厚度2.5μm，当摩擦副为Al2O3时，干摩擦系数为0.1。
2.如权利要求1所述的方法，其特征在于，所述预处理为表面抛光后浸入丙酮中超声波清洗，酒精脱水。
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