CN112391591B - 一种WCrSiN超硬涂层及其制备方法 - Google Patents

一种WCrSiN超硬涂层及其制备方法 Download PDF

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CN112391591B
CN112391591B CN202011252080.1A CN202011252080A CN112391591B CN 112391591 B CN112391591 B CN 112391591B CN 202011252080 A CN202011252080 A CN 202011252080A CN 112391591 B CN112391591 B CN 112391591B
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杨俊峰
杨红艳
杨瑞芳
张临超
谢卓明
王坤
刘瑞
王先平
吴学邦
方前锋
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Hefei Institutes of Physical Science of CAS
Nuclear Power Institute of China
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    • C23C14/02—Pretreatment of the material to be coated
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Abstract

本发明公开了一种WCrSiN超硬涂层及其制备方法，涉及表面涂层技术领域，包括依次沉积在基体表面的WCrSi打底层和WCrSiN主体层。本发明提出了一种WCrSiN超硬涂层，该四元纳米复合超硬薄膜涂层中，(W，Cr)2N、(W，Cr)N、SiNx三相复合，基于固溶强化、多相强化以及纳米复合结构的组合，实现不同尺度的协同强化作用，从而最大程度上提高了薄膜的硬度，其硬度可达45GPa以上。此外，在溅射WCrSiN主体层前先在基体表面溅射一层WCrSi打底层，能够提高薄膜涂层与基体之间的结合力，改善膜裂等缺陷。本发明制备方法操作简单、沉积速率快、易于批量生产，有很好的推广价值。

Description

一种WCrSiN超硬涂层及其制备方法
技术领域
本发明涉及表面涂层技术领域，尤其涉及一种WCrSiN超硬涂层及其制备方法。
背景技术
绿色和智能是我国制造业发展的两大主题。但是，我国制造业还存在精度低、能耗大等问题。因此，如何提高材料加工精度、降低能耗已经成为急需解决的问题，甚至成为一些产业发展的瓶颈。例如，能源探测时如何提高钻头的使用寿命、加深探测深度；航空、航天等行业如何减少摩擦，提高服役时间等。
表面改性技术和表面涂层工艺应运而生并受到了越来越多的关注和重视。涂层刀具的出现，被认为是金属切削刀具技术发展史上的一次革命。硬质薄膜尤其是超硬薄膜倍受青睐。用PVD法将超硬薄膜材料镀于金属切削刀具表面，既适应现代制造业对金属切削刀具的高技术要求，又符合绿色制造理念。表面镀有超硬薄膜的金属切削刀具既保持了其基体较高的强度，又能发挥其表面涂层“超硬、强韧、耐磨、自润滑”的优势，从而大大提高了金属切削刀具在现代加工过程中的耐用度和适应性。因此硬质薄膜材料可以广泛应用于机械制造，汽车工业，纺织工业，地质钻探，模具工业，航空航天等领域。目前，国内外研究者关注在超硬耐磨涂层成分优化设计上，以开发出更多性能优异的多元超硬涂层。
发明内容
基于背景技术存在的技术问题，本发明提出了一种WCrSiN超硬涂层及其制备方法，该涂层硬度高，且制备方法操作简单、沉积速率快。
本发明提出的一种WCrSiN超硬涂层，包括依次沉积在基体表面的WCrSi打底层和WCrSiN主体层。
优选地，所述WCrSiN主体层的成分为：W39at％、Cr8at％、Si8at％、N45at％。
优选地，所述WCrSi打底层的厚度为0.01-0.02μm。
本发明还提出了上述WCrSiN超硬涂层的制备方法，是采用多弧离子镀技术在基体表面依次溅射WCrSi打底层和WCrSiN主体层。
优选地，包括以下步骤：
S1、安装：将W-Cr-Si靶安装在直流阴极上，基体装入样品台，固定靶材和基体的距离为150mm；
S2、中频偏压清洗：将真空室抽真空至1x10-3pa，然后加热基片至430℃，向真空室通入Ar，控制Ar流量为60sccm，工作气压为2.5Pa；开启中频电源，设定电压为1200V，对基体表面进行清洗；
S3、溅射打底层WCrSi：调节Ar流量为40-60sccm，工作气压为0.40-0.76Pa；设定中频偏压电源电压为600-900V、占空比50％，同时开启W-Cr-Si靶溅射电源，设定电流为40-60A、溅射时间8-15min，在基体上溅射WCrSi打底层；
S4、溅射主体层WCrSiN：同时向真空室通入Ar和N2，调节Ar流量为5-15sccm，N2流量为20-100sccm，工作气压为0.30-0.76Pa；设定中频偏压电源电压为200-500V、占空比50％，设定溅射电源电流为90-120A、溅射时间30min，在WCrSi打底层上溅射WCrSiN主体层。
优选地，S2中，清洗15-20min。
有益效果：本发明提出了一种WCrSiN超硬涂层，该四元纳米复合超硬薄膜涂层中，(W，Cr)2N、(W，Cr)N、SiNx三相复合，基于固溶强化、多相强化以及纳米复合结构的组合，实现不同尺度的协同强化作用，从而最大程度上提高了薄膜的硬度，其硬度可达45GPa以上。此外，在溅射WCrSiN主体层前先在基体表面溅射一层WCrSi打底层，能够提高薄膜涂层与基体之间的结合力，改善膜裂等缺陷。本发明制备方法操作简单、沉积速率快、易于批量生产，有很好的推广价值。
附图说明
图1为本发明实施例中所得WCrSiN超硬涂层纵截面的SEM图；
图2为本发明实施例中所得WCrSiN超硬涂层表面的SEM图；
图3为本发明实施例中所得WCrSiN超硬涂层在不同偏压下的XRD图；
图4为本发明实施例中所得WCrSiN超硬涂层的硬度曲线图。
具体实施方式
下面，通过具体实施例对本发明的技术方案进行详细说明。
实施例
一种WCrSiN超硬涂层的制备方法，包括以下步骤：
S1、安装：将W-Cr-Si复合靶安装在直流阴极上，将清洗干净的金属基体装入样品台，固定靶材和基体的距离为150mm；
S2、中频偏压清洗：将真空室抽真空至1x10-3pa，然后加热基片至430℃，向真空室通入Ar，控制Ar流量为60sccm，工作气压为2.5Pa；开启中频电源，设定电压为1200V，对基体表面进行清洗，清洗时间为15-20min；
S3、溅射打底层WCrSi：调节Ar流量为50sccm，工作气压为0.60Pa；设定中频偏压电源电压为800V、占空比50％，同时开启W-Cr-Si靶溅射电源，设定电流为60A、溅射时间10min，在基体上溅射WCrSi打底层；
S4、溅射主体层WCrSiN：同时向真空室通入Ar和N2，调节Ar流量为15sccm，N2流量为60sccm，工作气压为0.50Pa；设定中频偏压电源电压为500V、占空比50％，设定溅射电源电流为120A、溅射时间30min，在WCrSi打底层上溅射WCrSiN主体层。
对本实施例中制得的涂层进行表征和性能检测。图1为所得涂层截面的SEM图，可以看出涂层由由致密的柱状晶组成，涂层厚度约为3μm。图2为所得涂层表面的SEM图，可以看出涂层表面致密、光滑，有非常少的大颗粒出现。图3为涂层在不同偏压条件下的XRD图，可以看出在200V偏压下，薄膜出现明显的(111)择优取向。利用纳米压痕仪NanoindenterG200测试薄膜涂层的硬度和深度关系，结果见图4，可以看出薄膜的硬度达到45GPa以上。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (2)

1.一种WCrSiN超硬涂层，其特征在于，包括依次沉积在基体表面的WCrSi打底层和WCrSiN主体层；所述WCrSi打底层的厚度为0.01-0.02μm；
所述WCrSiN主体层的成分为：W 39at%、Cr 8at%、Si 8at%、N 45at%；
所述的WCrSiN超硬涂层的制备方法，包括以下步骤：
S1、安装：将W-Cr-Si靶安装在直流阴极上，基体装入样品台，固定靶材和基体的距离为150mm；
S2、中频偏压清洗：将真空室抽真空至1x10-3pa，然后加热基片至430℃，向真空室通入Ar，控制Ar流量为60sccm，工作气压为2.5Pa；开启中频电源，设定电压为1200V，对基体表面进行清洗；
S3、溅射打底层WCrSi：调节Ar流量为40-60sccm，工作气压为0.40-0.76Pa；设定中频偏压电源电压为600-900V、占空比50%，同时开启W-Cr-Si靶溅射电源，设定电流为40-60A、溅射时间8-15 min，在基体上溅射WCrSi打底层；
S4、溅射主体层WCrSiN：同时向真空室通入Ar和N2，调节Ar流量为5-15sccm，N2流量为20-100sccm，工作气压为0.30-0.76Pa；设定中频偏压电源电压为200V、占空比50%，设定溅射电源电流为90-120A、溅射时间30min，在WCrSi打底层上溅射WCrSiN主体层；
是采用多弧离子镀技术在基体表面依次溅射WCrSi打底层和WCrSiN主体层。
2.根据权利要求1所述的WCrSiN超硬涂层的制备方法，其特征在于，S2中，清洗15-20min。
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103382548A (zh) * 2013-06-27 2013-11-06 中国科学院宁波材料技术与工程研究所 一种基体表面纳米复合Me-Si-N超硬涂层的制备方法
CN103789725A (zh) * 2014-01-29 2014-05-14 仪征亚新科双环活塞环有限公司 一种活塞环表面的多层多元复合硬质pvd镀层、活塞环及制备工艺
CN107190233A (zh) * 2016-05-25 2017-09-22 上海仟纳真空镀膜科技有限公司 一种具有超高硬度的Si掺杂纳米复合涂层的制备工艺

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JP5206167B2 (ja) * 2008-07-04 2013-06-12 日立ツール株式会社 硬質皮膜被覆切削工具

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103382548A (zh) * 2013-06-27 2013-11-06 中国科学院宁波材料技术与工程研究所 一种基体表面纳米复合Me-Si-N超硬涂层的制备方法
CN103789725A (zh) * 2014-01-29 2014-05-14 仪征亚新科双环活塞环有限公司 一种活塞环表面的多层多元复合硬质pvd镀层、活塞环及制备工艺
CN107190233A (zh) * 2016-05-25 2017-09-22 上海仟纳真空镀膜科技有限公司 一种具有超高硬度的Si掺杂纳米复合涂层的制备工艺

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