CN108411265A - 一种低应力致密涂层的制备方法 - Google Patents
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- 229910052786 argon Inorganic materials 0.000 claims abstract description 45
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- DGJPLFUDZQEBFH-UHFFFAOYSA-N argon xenon Chemical compound [Ar].[Xe] DGJPLFUDZQEBFH-UHFFFAOYSA-N 0.000 claims abstract description 4
- PDEXVOWZLSWEJB-UHFFFAOYSA-N krypton xenon Chemical compound [Kr].[Xe] PDEXVOWZLSWEJB-UHFFFAOYSA-N 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 229910052743 krypton Inorganic materials 0.000 claims description 24
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910052724 xenon Inorganic materials 0.000 claims description 24
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- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
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- 229910052713 technetium Inorganic materials 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
本发明公开了一种低应力致密涂层制备方法，步骤一.将工件清洗干净，放入真空室抽真空至6X10‑4Pa以上，通入惰性气体氩气，偏压为‑800V至‑1000V，刻蚀所述工件表面10分钟‑60分钟；步骤二.通入惰性气体氩气，溅射中间层Ti或Cr，厚度100nm‑500nm；步骤三.通入氩氪、氩氙、氪氙或氩氪氙惰性气体的混合气体，溅射所需沉积涂层。在溅射沉积过程，工作气体为氩氪、氩氙或氩氪氙的混合气体，同时控制合理沉积偏压，从而控制涂层应力水平。相对传统的涂层，在获得致密结构条件下，压应力更低，适用于涂层结合性能要求高，涂层厚度大的应用领域。
Description
技术领域
本发明属于真空沉积涂层制备工艺领域，具体涉及低应力致密涂层的制备方法，可用于厚/超厚涂层的制备。
背景技术
目前，磁控溅射法制备的致密硬质涂层厚度一般不超过10um，其主要原因是过高的压应力使厚涂层/基底结合性能劣化，也导致涂层本身在承载条件下断裂失效。沉积过程中离子轰击涂层，诱发涂层产生间隙插入型缺陷，这是压应力产生的主要原因。涂层厚度增加可以大幅提高使基体表面承载能力，同时显著提高抗磨损寿命，因此厚硬质涂层(厚度大于10um)具有更广泛的工业应用前景。为了获得厚涂层甚至超厚涂层(厚度大于50um)，主要可以通过以下几种手段实现：(1)通过超低负偏压(小于20V)或正偏压来减小或抑制离子轰击涂层表面，从而抑制压应力产生；(2)通过退火方式消除应力，包括沉积过程中用低能离子轰击退火或热辐射退火，以及沉积后热处理等手段；(3)通过梯度成分或结构设计以及多层设计来减小压应力。然而，对于超低负偏压，离子轰击不足会导致涂层疏松，退火方式可能无法将应力及时消除或由于退火过高导致基体性能劣化，通过梯度或多层设计往往导致涂层力学性能不佳。
发明内容
技术问题：本发明的目的在于提供一种磁控溅射法来制备低应力致密硬质涂层的方法，该制备方法简单，能同时兼顾低应力和涂层致密的要求，适用于涂层结合性能要求高，涂层厚度大的应用领域。
技术方案：为实现上述发明目的，本发明的一种低应力致密涂层制备方法采用如下技术方案：
步骤一.将工件清洗干净，放入真空室抽真空至6X10-4Pa以上，通入惰性气体氩气，偏压为-800V至-1000V，刻蚀所述工件表面10分钟-60分钟；
步骤二.通入惰性气体氩气，溅射中间层Ti或Cr，厚度100nm-500nm；
步骤三.通入氩氪、氩氙、氪氙或氩氪氙惰性气体的混合气体，溅射所需沉积涂层。
其中，
所述的所需沉积涂层是氧化物、氮化物或碳化物的陶瓷类涂层，还需相应通入反应类气体，如氧气、氮气、甲烷等；
所述的所需沉积涂层成分含有Ti、Zn、Y、Ca、Sc、Sr或稀土元素的涂层溅射，氩气含量范围为0％-20％，氪气含量范围为0％-20％，氙气含量范围为60％-100％。
所述的所需沉积涂层成分含有Mg、V、Cr、Mn、Nb、Tc或Sn的溅射沉积过程，氩气含量范围为0％-20％，氪气含量范围为20％-100％，氙气含量范围为1％-100％。
所述的所需沉积涂层中无Ti、Zn、Y、Ca、Sc、Sr、Mg、V、Cr、Mn、Nb、Tc、Sn或稀土元素的涂层，氩气含量范围为60％-99％，氪气含量范围为1％-20％，氙气含量范围为0％-20％。
所述的在溅射沉积涂层过程中，气体离化率应大于10％，偏压范围为-10V至-50V。
有益效果：(1)与现有技术相比，本发明获得的涂层兼有低应力、致密特性和厚度大等特点。(2)不需要高温退火处理，适宜在对温度敏感基体上沉积。(3)对设备要求低，工艺简单易行。
具体实施方式
以下结合具体实施方式对本发明做进一步的说明。
实施例1：制备低应力致密TiAlN涂层
将Ti6Al4V样品(工件)清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入惰性气体氩气，溅射中间层Ti等，厚度约200nm。通入氩气、氪气、氙气和氮气，氩气在惰性气体中的含量为1％，氪气在惰性气体中的含量为1％，氙气在惰性气体中的含量为98％，氮气在混合气体中的含量为7％，TiAl靶直流溅射功率密度为10W/cm2，电离率10％，偏压-50V，沉积时间10小时，所获TiAlN涂层厚度20um，致密度99％，应力-100MPa。
实施例2：制备低应力致密TiAlN涂层
将Ti6Al4V样品清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入惰性气体氩气，溅射中间层Ti等，厚度约200nm。融入氩气、氪气、氙气和氮气，氩气在惰性气体中的含量为1％，氪气在惰性气体中的含量为20％，氙气在惰性气体中的含量为69％，氮气在混合气体中的含量为7％，TiAl靶直流溅射功率密度为10W/cm2，电离率10％，偏压-50V，沉积时间10小时，所获TiAlN涂层厚度20um，致密度98％，应力-800MPa。
实施例3：制备低应力致密TiAlN涂层
将Ti6Al4V基体样品清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入惰性气体氩气，溅射中间层Ti等，厚度约200nm。融入氩气、氪气、氙气和氮气，氩气在惰性气体中的含量为20％，氪气在惰性气体中的含量为1％，氙气在惰性气体中的含量为69％，氮气在混合气体中的含量为7％，TiAl靶直流溅射功率密度为10W/cm2，电离率10％，偏压-50V，沉积时间10小时，所获TiAlN涂层厚度20um，致密度99％，应力-500MPa。
实施例4：制备低应力致密TiAlN涂层
将Ti6Al4V样品清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入惰性气体氩气，溅射中间层Ti等，厚度约200nm。融入氩气、氪气、氙气和氮气，氩气在惰性气体中的含量为20％，氪气在惰性气体中的含量为20％，氙气在惰性气体中的含量为60％，氮气在混合气体中的含量为7％，TiAl靶直流溅射功率密度为10W/cm2，电离率10％，偏压-50V，沉积时间10小时，所获TiAlN涂层厚度20um，致密度99％，应力-1GPa。
实施例5：制备低应力致密Cr涂层
将GCr15模具钢样品清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入氩气、氪气和氙气，氩气在惰性气体中的含量为1％，氪气在惰性气体中的含量为98％，氙气在惰性气体中的含量为1％，Cr靶直流溅射功率密度为10W/cm2，采用钨丝等离子增强工艺，电离率90％，偏压-10V，沉积时间10小时，所获Cr涂层厚度30um，致密度100％，应力-100MPa。
实施例6：制备低应力致密Cr涂层
将GCr15模具钢样品清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入氩气、氪气和氙气，氩气在惰性气体中的含量为20％，氪气在惰性气体中的含量为78％，氙气在惰性气体中的含量为1％，Cr靶直流溅射功率密度为10W/cm2，采用钨丝等离子增强工艺，电离率90％，偏压-10V，沉积时间30小时，所获Cr涂层厚度100um，致密度100％，应力-200MPa。
实施例7：制备低应力致密Cr涂层
将GCr15模具钢样品清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入氩气、氪气和氙气，氩气在惰性气体中的含量为20％，氪气在惰性气体中的含量为60％，氙气在惰性气体中的含量为20％，Cr靶直流溅射功率密度为10W/cm2，采用钨丝等离子增强工艺，电离率90％，偏压-10V，沉积时间30小时，所获Cr涂层厚度30um，致密度100％，应力-500MPa。
实施例8：制备低应力致密TaN涂层
将GCr15模具钢样品清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入惰性气体氩气，溅射中间层Ti等，厚度约200nm。通入氩气、氪气、氙气和氮气，氩气在惰性气体中的含量为99％，氪气在惰性气体中的含量为1％，氙气在惰性气体中的含量为0％，氮气在混合气体中的含量为7％，Ta靶直流溅射功率密度为10W/cm2，电离率100％，偏压-50V，沉积时间10小时，所获TiAlN涂层厚度20um，致密度100％，应力-100MPa。
实施例9：制备低应力致密TaN涂层
将GCr15模具钢样品清洗干净，放入真空室抽真空至6X10-4Pa。通入惰性气体氩，偏压为-800V至-1000V，刻蚀样品表面20分钟。通入惰性气体氩气，溅射中间层Ti等，厚度约200nm。通入氩气、氪气、氙气和氮气，氩气在惰性气体中的含量为60％，氪气在惰性气体中的含量为20％，氙气在惰性气体中的含量为20％，氮气在混合气体中的含量为7％，Ta靶直流溅射功率密度为10W/cm2，电离率100％，偏压-50V，沉积时间10小时，所获TiAlN涂层厚度20um，致密度100％，应力-500MPa。
Claims (6)
1.一种低应力致密涂层制备方法，其特征在于，该制备方法包括以下步骤：
步骤一.将工件清洗干净，放入真空室抽真空至6X10-4Pa以上，通入惰性气体氩气，偏压为-800V至-1000V，刻蚀所述工件表面10分钟-60分钟；
步骤二.通入惰性气体氩气，溅射中间层Ti或Cr，厚度100nm-500nm；
步骤三.通入氩氪、氩氙、氪氙或氩氪氙惰性气体的混合气体，溅射所需沉积涂层。
2.根据权利要求1所述的一种低应力致密涂层制备方法，其特征在于，所述的所需沉积涂层是氧化物、氮化物或碳化物的陶瓷类涂层，还需相应通入反应类气体，如氧气、氮气、甲烷等。
3.根据权利要求1所述的一种低应力致密涂层制备方法，其特征在于，所述的所需沉积涂层成分含有Ti、Zn、Y、Ca、Sc、Sr或稀土元素的涂层溅射，氩气含量范围为0％-20％，氪气含量范围为0％-20％，氙气含量范围为60％-100％。
4.根据权利要求1所述的一种低应力致密涂层制备方法，其特征在于，所述的所需沉积涂层成分含有Mg、V、Cr、Mn、Nb、Tc或Sn的溅射沉积过程，氩气含量范围为0％-20％，氪气含量范围为20％-100％，氙气含量范围为1％-100％。
5.根据权利要求1所述的一种低应力致密涂层制备方法，其特征在于，所述的所需沉积涂层中无Ti、Zn、Y、Ca、Sc、Sr、Mg、V、Cr、Mn、Nb、Tc、Sn或稀土元素的涂层，氩气含量范围为60％-99％，氪气含量范围为1％-20％，氙气含量范围为0％-20％。
6.根据权利要求1所述的一种低应力致密涂层制备方法，其特征在于，所述的在溅射沉积涂层过程中，气体离化率应大于10％，偏压范围为-10V至-50V。
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