CN111455311A - 一种多层纳米复合四面体非晶碳膜制备工艺 - Google Patents

一种多层纳米复合四面体非晶碳膜制备工艺 Download PDF

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CN111455311A
CN111455311A CN202010282444.4A CN202010282444A CN111455311A CN 111455311 A CN111455311 A CN 111455311A CN 202010282444 A CN202010282444 A CN 202010282444A CN 111455311 A CN111455311 A CN 111455311A
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朱汉钰
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Jiangsu Liyu Razor Co ltd
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Abstract

本发明公开了一种多层纳米复合四面体非晶碳膜制备工艺,本发明包含五个工艺步骤,并且多层纳米复合四面体非晶碳膜的膜层结构分为注入钉扎层、金属过渡层、金属氮化物过渡层和非晶碳膜层(ta‑c),本发明的有益效果是:本发明能够有效的提高剃须刀表面沉积的非晶碳膜的硬度,膜基结合力和耐摩擦磨损性,能够制备出具有润滑效果的非晶碳膜涂层,制备过程中,设备操作简单,工艺成熟,可实现批量生产,本发明不仅仅可以应用于手动剃须刀领域,也适合所有其它刀具轴承等零件中高硬耐磨涂层沉积。

Description

一种多层纳米复合四面体非晶碳膜制备工艺
技术领域
本发明涉及离子束相关技术领域,具体为一种多层纳米复合四面体非晶碳膜制备工艺。
背景技术
剃须刀是日常生活中不可缺少的用品,市场需求量极其庞大。在高端品牌中,剃须刀刀片表面均有耐磨防护涂层,用于提高剃须刀品质,四面体非晶碳是一种类金刚石结构,其碳碳杂化建中sp3键含量超过50%且不含氢,具有高的硬度、弹性模量、热导率和电阻率,优异的耐磨性和抗蚀性,以及良好的化学惰性和生物相容性等性质,被广泛用于应用于机械、电子与微电子、生物医学及航空航天等各个领域。
目前,非晶碳膜的制备技术很多,大体分为化学气相沉积和物理气相沉积,具体包含PECVD法、溅射法、离子镀、激光脉冲沉积和真空电弧沉积等。其中CVD法制备需要高温不合适不锈钢材质的剃须刀表面处理;溅射法制备的碳膜SP2(石墨键)成份过高,碳膜硬度较低,无法提升剃须刀品质;电弧技术可以实现低温沉积ta-C膜,但结构疏松,膜基结合力不足。
发明内容
本发明的目的是针对现有的问题,提供一种多层纳米复合四面体非晶碳膜制备工艺,本发明利用真空弧离子镀结合离子注入技术制备的多层纳米复合非晶碳膜有助于大幅增加膜基结合力,有效地提高剃须刀耐用性,提升剃须刀品质。本发明使用的金属靶材阴极弧源,离化率理论上可达100%,弧流大小可控,负偏压及脉冲幅宽频率可调。本发明提供的离子镀技术制备多层纳米复合ta-C膜技术,沉积效率高,涂层具有高硬度、耐磨损,低摩擦系数、高结合力等特点,不仅适合用于生产涂层剃须刀,同样适用于其他加工刀具及轴承等工件领域。
本发明为实现上述技术目的所采用的技术方案为:一种多层纳米复合四面体非晶碳膜制备工艺,包含五个工艺步骤:基材抛光清洗、注入钉扎层的制备、金属过渡层的制备、金属氮化物过渡层的制备、非晶碳膜层的制备。并且多层纳米复合四面体非晶碳膜的膜层结构分为四层结构:注入钉扎层、金属过渡层、金属氮化物过渡层、非晶碳膜层。
进一步的,所述基材抛光清洗依次使用漂洗、清洗、烘干,漂洗使用金属去污液漂洗和混合油超声漂洗,第一步先使用金属去污液漂洗,第二步使用混合油超声漂洗,漂洗的时间为5-20min,清洗过程中使用的是清水进行清洗,清洗时间为5-10min,烘干的温度为70-100℃,完成上述一系列操作后静置备用。
进一步的,所述注入钉扎层的制备包括:注入1、Ti沉积、注入2,其中注入1:将基材钢样固定于样品台,并转动至注入靶位开始注入,注入离子源为纯度99.9%的纯Ti离子源,注入条件为:真空度:1×10-3~6×10-3Pa,注入弧压为:50~70V,高压为:5~8kV,弧流为:3~6mA,注入剂量为:1×1014~1×1015Ti/cm2;Ti沉积:转动样品至沉积靶位开始沉积,沉积弧源为纯度99%的Ti弧源,沉积条件为:真空度:1×10-3~6×10-3Pa,沉积弧流:70~130A,负偏压:-50V~-300V,占空比:50%~100%,沉积时间:3~60秒;注入2:将样品再次转动至注入靶位开始注入,注入离子源为纯度99.9%的纯Ti离子源,注入条件为:真空度1×10-3~6×10-3Pa,注入弧压:60~80V,高压:10~15kV,弧流:3~6mA,注入剂量1×1014~1×1015Ti/cm2。
进一步的,所述金属过渡层的制备是将工件转至离子镀工位,在注入钉扎层之上沉积Ti膜过渡层,沉积条件为:沉积弧源为纯度99%的Ti弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:80~130A,负偏压:-150V~-350V,占空比50%~100%,沉积时间5~15分钟。
进一步的,所述金属氮化物过渡层的制备是在Ti过渡层103之上沉积TiN膜过渡层104,沉积条件为:沉积弧源为纯度99%的Ti弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:70~130A,负偏压:-150V~-350V,占空比50%~100%,N2进气量10-100sccm,沉积时间5~15分钟。
进一步的,所述非晶碳膜层的制备是在TiN过渡层104之上沉积ta-C层105,沉积条件为:沉积弧源为纯度99%的C弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:70~120A,负偏压:-100V~-300V,占空比50%~100%,沉积时间10~30分钟。
进一步的,对于所述注入钉扎层、金属过渡层、非晶碳膜层,注入所用的金属离子源有Ti、Zr、Cr,沉积所用的弧源有C、Ti、Zr、Cr。
进一步的,所述非晶碳膜层是无氢无金属掺杂的四面体非晶结构,其碳杂化建SP3含量超过80%。
进一步的,所述金属过渡层、金属氮化物过渡层、非晶碳膜层的总厚度为100~400m,摩擦系数0.03~0.15,膜硬度超过60Gpa。
附图说明
图1为本发明剃须刀表面多层纳米复合非晶碳膜涂层膜层结构示意图;
1-剃须刀刀刃、2-注入钉扎层、3-金属过渡层、4-金属氮化物过渡层、5-非晶碳膜层。
具体实施方式
下面对本发明做进一步的阐述,以下步骤中所用的原料均为本领域常规的原料或者是从市面上能够购买得到。
一种多层纳米复合四面体非晶碳膜制备工艺,包含五个工艺步骤:基材抛光清洗、注入钉扎层的制备、金属过渡层的制备、金属氮化物过渡层的制备、非晶碳膜层的制备。并且多层纳米复合四面体非晶碳膜的膜层结构分为四层结构:注入钉扎层、金属过渡层、金属氮化物过渡层、非晶碳膜层。
具体步骤为:
a.基材抛光清洗依次使用漂洗、清洗、烘干,漂洗使用金属去污液漂洗和混合油超声漂洗,第一步先使用金属去污液漂洗,第二步使用混合油超声漂洗,漂洗的时间为5-20min,清洗过程中使用的是清水进行清洗,清洗时间为5-10min,烘干的温度为70-100℃,完成上述一系列操作后静置备用。
b.注入钉扎层的制备包括:注入1、Ti沉积、注入2,其中注入1:将基材钢样固定于样品台,并转动至注入靶位开始注入,注入离子源为纯度99.9%的纯Ti离子源,注入条件为:真空度:1×10-3~6×10-3Pa,注入弧压为:50~70V,高压为:5~8kV,弧流为:3~6mA,注入剂量为:1×1014~1×1015Ti/cm2;Ti沉积:转动样品至沉积靶位开始沉积,沉积弧源为纯度99%的Ti弧源,沉积条件为:真空度:1×10-3~6×10-3Pa,沉积弧流:70~130A,负偏压:-50V~-300V,占空比:50%~100%,沉积时间:3~60秒;注入2:将样品再次转动至注入靶位开始注入,注入离子源为纯度99.9%的纯Ti离子源,注入条件为:真空度1×10-3~6×10-3Pa,注入弧压:60~80V,高压:10~15kV,弧流:3~6mA,注入剂量1×1014~1×1015Ti/cm2。
c.金属过渡层的制备是将工件转至离子镀工位,在注入钉扎层之上沉积Ti膜过渡层,沉积条件为:沉积弧源为纯度99%的Ti弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:80~130A,负偏压:-150V~-350V,占空比50%~100%,沉积时间5~15分钟。
d.金属氮化物过渡层的制备是在Ti过渡层103之上沉积TiN膜过渡层104,沉积条件为:沉积弧源为纯度99%的Ti弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:70~130A,负偏压:-150V~-350V,占空比50%~100%,N2进气量10-100sccm,沉积时间5~15分钟。
e.非晶碳膜层的制备是在TiN过渡层104之上沉积ta-C层105,沉积条件为:沉积弧源为纯度99%的C弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:70~120A,负偏压:-100V~-300V,占空比50%~100%,沉积时间10~30分钟。
f.对于注入钉扎层、金属过渡层、非晶碳膜层,注入所用的金属离子源有Ti、Zr、Cr,沉积所用的弧源有C、Ti、Zr、Cr。
g.非晶碳膜层是无氢无金属掺杂的四面体非晶结构,其碳杂化建SP3含量超过80%。
h.金属过渡层、金属氮化物过渡层、非晶碳膜层的总厚度为100~400m,摩擦系数0.03~0.15,膜硬度超过60Gpa。
对于本领域的技术人员而言,可根据以上描述的技术方案以及构思做出其它各种相应的改变以及变形,而所有的这些改变以及变形都应该属于本发明权利要求的保护范围之内。

Claims (9)

1.一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:本发明共包含五个工艺步骤:基材抛光清洗、注入钉扎层的制备、金属过渡层的制备、金属氮化物过渡层的制备、非晶碳膜层的制备。并且多层纳米复合四面体非晶碳膜的膜层结构分为四层结构:注入钉扎层、金属过渡层、金属氮化物过渡层、非晶碳膜层。
2.根据权利要求1所述的一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:所述基材抛光清洗依次使用漂洗、清洗、烘干,漂洗使用金属去污液漂洗和混合油超声漂洗,第一步先使用金属去污液漂洗,第二步使用混合油超声漂洗,漂洗的时间为5-20min,清洗过程中使用的是清水进行清洗,清洗时间为5-10min,烘干的温度为70-100℃,完成上述一系列操作后静置备用。
3.根据权利要求1所述的一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:所述注入钉扎层的制备包括:注入1、Ti沉积、注入2,其中注入1:将基材钢样固定于样品台,并转动至注入靶位开始注入,注入离子源为纯度99.9%的纯Ti离子源,注入条件为:真空度:1×10-3~6×10-3Pa,注入弧压为:50~70V,高压为:5~8kV,弧流为:3~6mA,注入剂量为:1×1014~1×1015Ti/cm2;Ti沉积:转动样品至沉积靶位开始沉积,沉积弧源为纯度99%的Ti弧源,沉积条件为:真空度:1×10-3~6×10-3Pa,沉积弧流:70~130A,负偏压:-50V~-300V,占空比:50%~100%,沉积时间:3~60秒;注入2:将样品再次转动至注入靶位开始注入,注入离子源为纯度99.9%的纯Ti离子源,注入条件为:真空度1×10-3~6×10-3Pa,注入弧压:60~80V,高压:10~15kV,弧流:3~6mA,注入剂量1×1014~1×1015Ti/cm2。
4.根据权利要求1所述的一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:所述金属过渡层的制备是将工件转至离子镀工位,在注入钉扎层之上沉积Ti膜过渡层,沉积条件为:沉积弧源为纯度99%的Ti弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:80~130A,负偏压:-150V~-350V,占空比50%~100%,沉积时间5~15分钟。
5.根据权利要求1所述的一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:所述金属氮化物过渡层的制备是在Ti过渡层103之上沉积TiN膜过渡层104,沉积条件为:沉积弧源为纯度99%的Ti弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:70~130A,负偏压:-150V~-350V,占空比50%~100%,N2进气量10-100sccm,沉积时间5~15分钟。
6.根据权利要求1所述的一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:所述非晶碳膜层的制备是在TiN过渡层104之上沉积ta-C层105,沉积条件为:沉积弧源为纯度99%的C弧源,真空度:1×10-3~6×10-3Pa,沉积弧流:70~120A,负偏压:-100V~-300V,占空比50%~100%,沉积时间10~30分钟。
7.根据权利要求1所述的一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:对于所述注入钉扎层、金属过渡层、非晶碳膜层,注入所用的金属离子源有Ti、Zr、Cr,沉积所用的弧源有C、Ti、Zr、Cr。
8.根据权利要求1所述的一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:所述非晶碳膜层是无氢无金属掺杂的四面体非晶结构,其碳杂化建SP3含量超过80%。
9.根据权利要求1所述的一种多层纳米复合四面体非晶碳膜制备工艺,其特征在于:所述金属过渡层、金属氮化物过渡层、非晶碳膜层的总厚度为100~400m,摩擦系数0.03~0.15,膜硬度超过60GPa。
CN202010282444.4A 2020-04-12 2020-04-12 一种多层纳米复合四面体非晶碳膜制备工艺 Pending CN111455311A (zh)

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