CN110306153A - 一种掺杂Cr的DLC涂层的制备方法 - Google Patents

一种掺杂Cr的DLC涂层的制备方法 Download PDF

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CN110306153A
CN110306153A CN201910662656.2A CN201910662656A CN110306153A CN 110306153 A CN110306153 A CN 110306153A CN 201910662656 A CN201910662656 A CN 201910662656A CN 110306153 A CN110306153 A CN 110306153A
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唐坤
王广欣
朱宇杰
孙浩亮
海茵茨罗尔夫斯托克
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Henan University of Science and Technology
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Abstract

本发明公开了一种掺杂Cr的DLC涂层的制备方法，充分利用了高功率脉冲磁控溅射膜层光洁度、均匀度、致密度高的优点，为改善DLC涂层结合力和膜层韧性差的缺点，采用了底层和过渡层设计方法。这一独特的膜系设计和参杂工艺既保证了涂层结合力的提高，又保证了涂层沉积速率、涂层致密性和耐磨减摩性能的提高。采用本发明的方法制备的掺Cr的DLC涂层外观呈灰黑色，表面光滑致密，涂层的硬度32GPa，膜基结合力达到72N，涂层厚度为1.45μm。涂层的干摩擦系数为0.2。表明掺Cr的DLC涂层具有良好的耐磨和减摩性能。

Description

一种掺杂Cr的DLC涂层的制备方法
技术领域
本发明属于涂层材料技术领域，具体涉及一种掺杂Cr的DLC涂层的制备方法。
背景技术
物理气相沉积技术表示在真空条件下，采用物理方法，将材料源——固体或液体表面气化成气态原子、分子或部分电离成离子，并通过低压气体(或等离子体)过程，在基体表面沉积具有某种特殊功能的薄膜的技术。申请号为“201210423173.5”，专利名称为“一种掺Ti的类金刚石涂层的制备方法”中公开了一种制备掺Ti的DLC涂层的方法，将预处理好的基体放入电弧与磁控溅射复合镀膜设备的转架杆上，以柱弧Ti靶作为Ti源，以平面C靶作为C的来源，平面C靶共三对，以均布的方式安置在炉体内壁上，采用高纯Ar作为主要离化气体，保证有效的辉光放电过程；采用高纯N2作为反应气体，使其离化并与Ti、C元素结合，在基体表面沉积形成掺Ti的DLC涂层。制备的该掺Ti的DLC涂层外观呈黑色，表面光滑致密，涂层的硬度28GPa，膜基结合力达到60N，涂层厚度为2.5μm，当摩擦副为Al2O3球时，涂层的干摩擦系数为0.2。表明掺Ti的DLC涂层具有良好的耐磨和减摩性能。
上述专利在制备工艺、膜系设计均取有一定的新颖性，性能上取得了一定的突破。然并不适用于钨钴硬质合金系列的膜层设计与制备工艺。针对硬质合金工具最常用的材料钨钴合金的DLC膜系设计和制备方法，鲜有报道。
发明内容
本发明为解决上述技术问题采用如下技术方案，一种掺杂Cr的DLC涂层的制备方法，具体步骤为：
步骤S1:将表面处理好的钨钴合金基体放入溅射设备腔体的转架杆上，该转架整体转动的同时，转架杆自转，以保证涂层的均匀性；
步骤S2:以长柱型Cr靶作为参杂源，以长住型石墨靶作为碳元素的来源，平面Cr靶为参杂Cr元素来源，均匀分布并安装在炉体内壁上，采用高纯Ar作为主要离化气体，保证有效的辉光放电过程；分别采用Cr层作为打底层、CrN、CrN2、Cr+C作为梯度过渡层，高纯N2作为过渡层反应气体，C2H2作为DLC层反应气体，形成Cr、CrN、CrN2、Cr+C、α-C：H的多层膜系涂层；
步骤S3:制备工艺条件：
A)等离子体洗靶：
靶体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续800s；
B)等离子体清洗基体：
基体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续1940s；
C)Cr底层制备：
腔体温度设定400度，调节Ar通量到200sccm、腔体气压设定为2Pa，然后开启柱弧Cr靶，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，打底层阶段时间设定为600秒；
D)CrN过渡层制备：
Cr底层制备完成后，腔体气压设定为0.5Pa，通入反应气体N2，N2通量设定为20sccm，Ar通量保持不变，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，在Cr底层上制备CrN过渡层，持续900s；
E)CrN2过渡层制备：
将N2通量设定为20sccm，溅射时间为840s，其余参数与CrN过渡层制备参数一致；
F)Cr+C过渡层制备：
关闭N2通道，启动双极脉冲电源，将功率设定为10KW，持续溅射900s，其余参数与CrN过渡层制备参数一致；
G)掺Cr的DLC涂层的制备：
在CrN过渡层制备完成后，关闭N2通道，通入C2N2作为反应气体，C2H2流量控制为60sccm；该溅射阶段膜系设计为三层，每层溅射时间为900s，溅射功率分别为10Kw、7Kw、4Kw，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A；
进一步的，所述钨钴合金基体通过超声波清洗、超声碱洗、酸洗，去离子水清洗后用吹风机吹干。
进一步的，所述掺杂Cr的DLC涂层的厚度为1.45μm。
本发明充分利用了高功率脉冲磁控溅射膜层光洁度、均匀度、致密度高的优点，为改善DLC涂层结合力和膜层韧性差的缺点，采用了底层和过渡层设计方法。这一独特的膜系设计和参杂工艺既保证了涂层结合力的提高，又保证了涂层沉积速率、涂层致密性和耐磨减摩性能的提高。采用本发明的方法制备的掺Cr的DLC涂层外观呈灰黑色，表面光滑致密，涂层的硬度32GPa，膜基结合力达到72N，涂层厚度为1.45μm。涂层的干摩擦系数为0.2。表明掺Cr的DLC涂层具有良好的耐磨和减摩性能。
附图说明
图1为纳米氧化锆粉体的微观形貌图；
图2为2000倍涂层断面SEM图；
图3为40000倍涂层表面微观结构图；
图4为Ballcrater测试下多层膜系结构设计截面图；
图5为本发明在刀具上的实施；
图6为本发明在钻头上的实施。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
本实施例的掺杂Cr的DLC涂层的制备方法，包括下列步骤：
步骤S1:将表面处理好的钨钴合金基体放入溅射设备腔体的转架杆上，该转架整体转动的同时，转架杆自转，以保证涂层的均匀性；
步骤S2:以长柱型Cr靶作为参杂源，以长住型石墨靶作为碳元素的来源，平面Cr靶为参杂Cr元素来源，均匀分布并安装在炉体内壁上，采用高纯Ar作为主要离化气体，保证有效的辉光放电过程；分别采用Cr层作为打底层、CrN、CrN2、Cr+C作为梯度过渡层，高纯N2作为过渡层反应气体，C2H2作为DLC层反应气体，形成Cr、CrN、CrN2、Cr+C、α-C：H的多层膜系涂层；
步骤S3:制备工艺条件：
A)等离子体洗靶：
靶体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续800s；
B)等离子体清洗基体：
基体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续1940s；
C)Cr底层制备：
腔体温度设定400度，调节Ar通量到200sccm、腔体气压设定为2Pa，然后开启柱弧Cr靶，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，打底层阶段时间设定为600秒；
D)CrN过渡层制备：
Cr底层制备完成后，腔体气压设定为0.5Pa，通入反应气体N2，N2通量设定为20sccm，Ar通量保持不变，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，在Cr底层上制备CrN过渡层，持续900s；
E)CrN2过渡层制备：
将N2通量设定为20sccm，溅射时间为840s，其余参数与CrN过渡层制备参数一致；
F)Cr+C过渡层制备：
关闭N2通道，启动双极脉冲电源，将功率设定为10KW，持续溅射900s，其余参数与CrN过渡层制备参数一致；
G)掺Cr的DLC涂层的制备：
在CrN过渡层制备完成后，关闭N2通道，通入C2N2作为反应气体，C2H2流量控制为60sccm；该溅射阶段膜系设计为三层，每层溅射时间为900s，溅射功率分别为10Kw、7Kw、4Kw，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A；
进一步的，所述钨钴合金基体通过超声波清洗、超声碱洗、酸洗，去离子水清洗后用吹风机吹干。
进一步的，所述掺杂Cr的DLC涂层的厚度为1.45μm。
涂层结合界面如图2所示，厚度为1.45μm，组织致密，与基体结合紧密。图3为放大40000倍后涂层表面的微观结构，涂层颗粒结合紧密，致密度高。Ballcrater测试下多层膜系结构设计截面图如图4所示，图中可看到多层膜系结构具有层次性，层间界面清晰。
以上实施例描述了本发明的主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。

Claims (3)

1.一种掺杂Cr的DLC涂层的制备方法，其特征在于，具体步骤为：
步骤S1:将表面处理好的钨钴合金基体放入溅射设备腔体的转架杆上，该转架整体转动的同时，转架杆自转，以保证涂层的均匀性；
步骤S2:以长柱型Cr靶作为参杂源，以长住型石墨靶作为碳元素的来源，平面Cr靶为参杂Cr元素来源，均匀分布并安装在炉体内壁上，采用高纯Ar作为主要离化气体，保证有效的辉光放电过程；分别采用Cr层作为打底层、CrN、CrN2、Cr+C作为梯度过渡层，高纯N2作为过渡层反应气体，C2H2作为DLC层反应气体，形成Cr、CrN、CrN2、Cr+C、α-C：H的多层膜系涂层；
步骤S3:制备工艺条件：
A)等离子体洗靶：
靶体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续800s；
B)等离子体清洗基体：
基体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续1940s；
C)Cr底层制备：
腔体温度设定400度，调节Ar通量到200sccm、腔体气压设定为2Pa，然后开启柱弧Cr靶，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，打底层阶段时间设定为600秒；
D)CrN过渡层制备：
Cr底层制备完成后，腔体气压设定为0.5Pa，通入反应气体N2，N2通量设定为20sccm，Ar通量保持不变，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，在Cr底层上制备CrN过渡层，持续900s；
E)CrN2过渡层制备：
将N2通量设定为20sccm，溅射时间为840s，其余参数与CrN过渡层制备参数一致；
F)Cr+C过渡层制备：
关闭N2通道，启动双极脉冲电源，将功率设定为10KW，持续溅射900s，其余参数与CrN过渡层制备参数一致；
G)掺Cr的DLC涂层的制备：
在CrN过渡层制备完成后，关闭N2通道，通入C2N2作为反应气体，C2H2流量控制为60sccm；该溅射阶段膜系设计为三层，每层溅射时间为900s，溅射功率分别为10Kw、7Kw、4Kw，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A。
2.根据权利要求1所述的一种掺杂Cr的DLC涂层的制备方法，其特征在于：所述钨钴合金基体通过超声波清洗、超声碱洗、酸洗，去离子水清洗后用吹风机吹干。
3.根据权利要求1所述的一种掺杂Cr的DLC涂层的制备方法，其特征在于：所述掺杂Cr的DLC涂层的厚度为1.45μm。
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CN102912298A (zh) * 2012-10-29 2013-02-06 西安浩元涂层技术有限公司 具有抗腐蚀和减摩性能的掺Cr的DLC涂层及制备方法
CN103874780A (zh) * 2011-10-21 2014-06-18 欧瑞康贸易股份公司(特吕巴赫) 具有涂层的钻头
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CN114686829A (zh) * 2020-12-29 2022-07-01 苏州吉恒纳米科技有限公司 一种耐磨耐疲劳和反复冲击的涂层及生产工艺

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