CN106835040A - 一种掺金属的类金刚石涂层的制备方法 - Google Patents

一种掺金属的类金刚石涂层的制备方法 Download PDF

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CN106835040A
CN106835040A CN201710005798.2A CN201710005798A CN106835040A CN 106835040 A CN106835040 A CN 106835040A CN 201710005798 A CN201710005798 A CN 201710005798A CN 106835040 A CN106835040 A CN 106835040A
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马胜利
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Abstract

本发明公开了一种掺金属的类金刚石涂层的方法,将预处理后的工件放入ISE‑MS镀膜设备真空室中的转架杆上,以安置在炉体左右内壁上的一对平面金属溅射靶作为相应掺金属的来源,通过调整中频脉冲电源的功率控制平面金属溅射靶的溅射率;将高纯Ar和CH4通过离子源进入真空室,其中,高纯Ar作为主要离化气体,CH4作为反应气体;采用了底层和过渡层设计方法,不但进一步提高涂层结合力,又保证了涂层耐磨和减摩性能的提高。所制备的掺金属的类金刚石涂层,外观呈灰色或黑色,表面光滑致密,掺金属的类金刚石涂层的硬度HV1800以上,膜基结合力达到50N以上,厚度为2.0μm~3.0μm,当摩擦副为Al2O3球时,掺金属的类金刚石涂层的干摩擦系数为0.1~0.25。

Description

一种掺金属的类金刚石涂层的制备方法
技术领域
本发明属于表面涂层制备技术领域,具体涉及一种掺金属(Cr、Ti、W)的类金刚石涂层的方法。
背景技术
随着人们环保意识的增强,低碳生活已经成为社会的主旋律。CO2空调制冷压缩机因其环保、高效、节能备受制冷行业的重视和青睐,正成为当前技术研发的热点。但由于CO2冷媒自身的特点,制冷系统跨临界运行,且排气压力较高、压差远大于现有的氟利昂压缩机。现有的技术手段,无论是偏心轴材料优选,机械结构优化设计,还是表面处理工艺设计,均不能完全解决CO2压缩机中存在的偏心轴磨损、润滑和轴封泄漏等难题,因此需要对CO2旋转压缩机的关键部件如偏心轴、滑片等表面耐磨及减摩性能进行深入系统的研究,以寻求技术突破。
类金刚石涂层(Diamond-like Carbon,DLC)是碳基涂层的典型代表,它以其高硬度、低摩擦系数和良好的化学稳定性引起人们的广泛关注。DLC涂层是含有金刚石结构(sp3键)和石墨结构(sp2键)的亚稳非晶态物质,DLC涂层中的碳原子主要以sp3和sp2杂化键结合。因此,通过调控DLC涂层中的化学键成分比例,可有效优化涂层的耐磨、减摩性能,从而有望彻底解决CO2压缩机中存在的偏心轴磨损、润滑和轴封泄漏等长期技术难题。
然而,要想获得耐磨损性能优异的DLC涂层,仍面临巨大的技术挑战,因DLC涂层自身内应力大、韧性差,经常在使用过程中发生开裂和剥落,不能有效发挥它的功效。因此,目前世界范围正在研发各种掺金属的DLC涂层的制备方法,但由于DLC涂层掺杂成份及结构不同,DLC涂层性能及适用范围有着相当大的差别。
目前,制备DLC涂层主要采用磁控溅射沉积技术(MS),该方法具有DLC膜层致密和表面光洁度高等优点,但磁控溅射的主要缺点是涂层结合力不高,沉积速率较慢,难以满足严酷服役条件下的工件表面强化要求。
发明内容
本发明的目的在于,提供一种采用离子源增强磁控溅射技术(ISE-MS)制备掺金属的类金刚石涂层的方法,有望满足CO2旋转压缩机的偏心轴表面摩擦学性能应用上的严酷服役要求。
为了实现上述任务,本发明采取如下的解决方案:
一种掺金属的类金刚石涂层的方法,其特征在于,按下列步骤进行:
1)将预处理后的工件放入ISE-MS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)以安置在炉体左右内壁上的一对平面金属溅射靶作为相应掺金属的来源,通过调整中频脉冲电源的功率控制平面金属溅射靶的溅射率;将高纯Ar和CH4通过离子源进入真空室,其中,高纯Ar作为主要离化气体,保证有效的辉光放电过程,CH4作为反应气体,经过离子源使其离化成为DLC涂层中C元素的来源;
3)制备工艺条件:
A.工件等离子清洗:高纯Ar气体通过离子源通入真空室,流量为50sccm~100sccm,真空度为1.0~2.0×10-1Pa;逐渐增加离子源功率到1.5kW~1.8kW,工件负偏压到600V~850V,用高纯Ar离子轰击清洗工件表面,时间为20min~30min;
B.沉积金属底层:调节高纯Ar流量为50sccm~100sccm,真空度为1.0~2.0×10- 1Pa,离子源功率为0.3kW~0.8kW,工件负偏压为50V~80V,开启金属溅射靶,调整金属溅射靶功率为2.0kW~3.0kW,时间为5min~10min;
C.沉积金属碳化物过渡层:金属底层沉积完成后,将CH4通过离子源通入真空室,调节高纯Ar流量为80~120sccm,CH4流量为10sccm~20sccm,真空度为2.0~3.0×10-1Pa,离子源功率为0.8kW~1.0kW,工件负偏压为50-60V,调整金属溅射靶功率为2.0kW~3.0kW,时间为10min~20min;
D.沉积掺金属的DLC膜:金属碳化物过渡层沉积完成后,调节高纯Ar流量为100sccm~120sccm,CH4流量为50sccm~70sccm,真空度为3.0~3.5×10-1Pa,离子源功率为1.0kW~1.2kW,工件负偏压为30V~50V,在8min~12min内逐渐减小金属溅射靶功率到0.2kW~0.3kW,时间为150min~240min,得到掺金属的类金刚石涂层。
根据本发明,所述的金属溅射靶为平面Cr溅射靶、平面Ti溅射靶或平面W溅射靶。
本发明的掺金属的类金刚石涂层的方法,充分利用了磁控溅射膜层致密以及离子源增强膜层沉积速率和结合力高的优点。同时,采用了底层和过渡层设计方法,不但进一步提高涂层结合力,又保证了涂层耐磨和减摩性能的提高。
采用上述制备的掺金属的类金刚石涂层,外观呈灰色或黑色,表面光滑致密,掺金属的类金刚石涂层的硬度HV1800以上,膜基结合力达到50N以上,厚度为2.0μm~3.0μm,当摩擦副为Al2O3球时,掺金属的类金刚石涂层的干摩擦系数为0.1~0.25。具有耐磨和减摩性能,可显著改善偏心轴的负荷承载能力,提高其抗磨损和抗粘接性能,延长了偏心轴的使用寿命,是新型CO2空调压缩机偏心轴磨损、润滑和轴封泄漏等长期技术难题的突破。
附图说明
图1为本发明的ISE-MS镀膜设备结构示意图。
以下结合附图和发明人给出的具体实施例对本发明作进一步的详细说明。
具体实施方式
申请人在研究过程中发现,离子源增强磁控溅射沉积技术(ISE-MS),可显著提高沉积速率和结合力,是制备DLC涂层的优选方法,因此,研究开发了一种掺金属的DLC涂层的制备方法,该方法采用离子源增强磁控溅射技术(ISE-MS)在压缩机的偏心轴表面制备掺金属的DLC涂层,经申请人测试表明,所得到的掺金属的DLC涂层具有很强的结合力并兼具耐磨减摩的优异性能。
本实施例给出一种掺Cr的DLC涂层制备方法,具体制备过程是:
(1)采用YZH–F200RET2型压缩机上的偏心轴(高速钢W18Cr4V制成,硬度HRC60),以及硬度为HRC60的高速钢W18Cr4V试块作为样品,经表面除油、抛光后浸入丙酮中超声波清洗,酒精脱水。
(2)将预处理好的样品放入ISE-MS镀膜设备中。ISE-MS镀膜设备如图1所示,至少包括真空室1、转台架2、偏压3、转架杆4、金属溅射靶5、永磁体6、离子源7、加热器8、泵组9,样品置于真空室1中的转架杆4上,转架杆4可以随转台架2转动,保证镀膜过程的均匀性。
(3)离子源7采用阳极层型矩形气体离子源,高纯Ar和CH4通过离子源7进入真空室,其中,高纯Ar作为主要离化气体,保证有效的辉光放电过程,CH4作为反应气体,经过离子源7使其离化成为DLC涂层中C元素的来源;
金属溅射靶5采用尺寸为435×95×10mm的1对平面Cr溅射靶作为相应掺Cr的来源,如图1所示,以对称的方式将平面Cr溅射靶分别安置在炉体左右内壁上,并通过调整中频脉冲电源的功率控制平面Cr溅射靶的溅射率。
(4)制备掺Cr的DLC涂层的工艺条件为:
A.工件等离子清洗:高纯Ar气体通过离子源通入真空室,高纯Ar气体流量为70sccm,真空度为1.5×10-1Pa。逐渐增加离子源功率到1.6kW和工件负偏压到700V,用高纯Ar离子轰击清洗工件表面,时间为25min。
B.沉积Cr底层:调节高纯Ar气体流量为80sccm,真空度为1.5×10-1Pa,离子源功率为0.6kW,工件负偏压为70V,开启Cr溅射靶,靶功率为2.5kW,时间为8min。
C.沉积CrC过渡层:Cr底层沉积完成后,将CH4通过离子源通入真空室,调节高纯Ar气体流量为110sccm,CH4流量为15sccm,真空度为2.5×10-1Pa,离子源功率为0.9kW,工件负偏压为55V,调整Cr溅射靶功率为2.5kW,时间为15min。
D.沉积掺Cr的DLC膜:CrC过渡层沉积完成后,调节高纯Ar气体流量为80sccm,CH4流量为60sccm,真空度为3.0×10-1Pa。离子源功率为1.1kW,工件负偏压为40V,10min内逐渐减小Cr溅射靶功率到0.25kW,沉积时间为200min,即得掺Cr的DLC涂层。
在上述工艺参数下,本实施例制备的掺Cr的DLC涂层外观呈黑色,表面光滑致密,掺Cr的DLC涂层的硬度为HV2500,厚度为2.5μm,膜基结合力为60N。当摩擦副为Al2O3球时,涂层的干摩擦系数为0.2。
将上述实施例制备的掺Cr的DLC涂层的偏心轴安装在YZH-F200RET2型压缩机上进行寿命考核。通过10000次超负荷高湿度反复开停试验后,拆解机芯进行目测观察和实际测试,偏心轴磨损状态在正常范围,而没有掺Cr的DLC涂层的偏心轴正常工作100次后就粘着磨损失效。表明掺Cr的DLC涂层完全达到了新型CO2压缩机偏心轴的设计要求,满足了新型CO2旋转压缩机的偏心轴表面摩擦学性能应用上的严酷服役要求,可突破现有新型CO2旋转压缩机的偏心轴制造的技术瓶颈。
当然,上述实施例中的金属溅射靶还可以是平面Ti溅射靶或平面W溅射靶,同样可以在YZH–F200RET2型压缩机上的偏心轴表面制备掺Ti或W的类金刚石涂层。

Claims (2)

1.一种掺金属的类金刚石涂层的方法,其特征在于,按下列步骤进行:
1)将预处理后的工件放入ISE-MS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)以安置在炉体左右内壁上的一对平面金属溅射靶作为相应掺金属的来源,通过调整中频脉冲电源的功率控制平面金属溅射靶的溅射率;将高纯Ar和CH4通过离子源进入真空室,其中,高纯Ar作为主要离化气体,保证有效的辉光放电过程,CH4作为反应气体,经过离子源使其离化成为DLC涂层中C元素的来源;
3)制备工艺条件:
A.工件等离子清洗:高纯Ar气体通过离子源通入真空室,流量为50sccm~100sccm,真空度为1.0~2.0×10-1Pa;逐渐增加离子源功率到1.5kW~1.8kW,工件负偏压到600V~850V,用高纯Ar离子轰击清洗工件表面,时间为20min~30min;
B.沉积金属底层:调节高纯Ar流量为50sccm~100sccm,真空度为1.0~2.0×10-1Pa,离子源功率为0.3kW~0.8kW,工件负偏压为50V~80V,开启金属溅射靶,调整金属溅射靶功率为2.0kW~3.0kW,时间为5min~10min;
C.沉积金属碳化物过渡层:金属底层沉积完成后,将CH4通过离子源通入真空室,调节高纯Ar流量为80~120sccm,CH4流量为10sccm~20sccm,真空度为2.0~3.0×10-1Pa,离子源功率为0.8kW~1.0kW,工件负偏压为50-60V,调整金属溅射靶功率为2.0kW~3.0kW,时间为10min~20min;
D.沉积掺金属的DLC膜:金属碳化物过渡层沉积完成后,调节高纯Ar流量为100sccm~120sccm,CH4流量为50sccm~70sccm,真空度为3.0~3.5×10-1Pa,离子源功率为1.0kW~1.2kW,工件负偏压为30V~50V,在8min~12min内逐渐减小金属溅射靶功率到0.2kW~0.3kW,时间为150min~240min,得到掺金属的类金刚石涂层。
2.如权利要求1所述的方法,其特征在于,所述的金属溅射靶为平面Cr溅射靶、平面Ti溅射靶或平面W溅射靶。
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