CN114411098A - 一种TiNb涂层的镀膜方法 - Google Patents
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- 238000000576 coating method Methods 0.000 title claims abstract description 39
- 239000011248 coating agent Substances 0.000 title claims description 29
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 20
- 239000000956 alloy Substances 0.000 claims abstract description 20
- 238000007747 plating Methods 0.000 claims abstract description 18
- 239000013077 target material Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 13
- 229910052786 argon Inorganic materials 0.000 claims abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 9
- 238000010849 ion bombardment Methods 0.000 claims description 9
- 238000010884 ion-beam technique Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 230000002035 prolonged effect Effects 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical group [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 claims description 3
- 238000005488 sandblasting Methods 0.000 claims description 3
- 238000000992 sputter etching Methods 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 6
- 239000010936 titanium Substances 0.000 description 24
- 239000010955 niobium Substances 0.000 description 23
- 238000007733 ion plating Methods 0.000 description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000007888 film coating Substances 0.000 description 3
- 238000009501 film coating Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 229910000997 High-speed steel Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
一种TiNb涂层的镀膜方法,所述TiNb涂层的镀膜方法的TiNb合金靶材的配比为Nb=55~65%,其余为Ti,事先设置好了靶材中Nb和Ti的配比,因此在TiNb合金靶材蒸发产生相应离子,沉积到被镀工件表面形成TiNb膜层时,能精准控制Nb和Ti蒸发比例。并且TiNb合金靶材的该配比为最佳比例,使得在最佳配比下形成的TiNb膜层的成分配比为Nb=60%~63%,其余为Ti、N、以及Ar,使所述TiNb膜层具有更好的强度。相较于两种单质靶材混合镀,操作更简单,并使TiNb膜层的比例更精准,提高TiNb膜层的强度和被镀件的耐用性。
Description
技术领域
本发明涉及电弧离子镀技术领域,特别涉及一种TiNb涂层的镀膜方法。
背景技术
电弧离子镀在工业上主要用于在高速钢刀具上镀制TiN膜作为耐磨硬质膜,以及在不锈钢制品上镀制膜作为仿金装饰膜。氮化钛薄膜镀覆在刀具或模具表面上会使寿命成倍提高,但随着机加工行业的发展,单纯的氮化钛薄膜已经不能满足刀具切削的需要,添加其他合金元素可以改善并提高氮化钛薄膜的性能。
TiNb(氮化钛铌)涂层是一种高硬度,高抗氧化温度且晶粒细腻的优良膜层,适用于大部分切削刀具。Nb作为用途广泛的单质金属材料,具有细晶强化和弥散强化的效果,同时也是单质材料中超导临界温度最高的材质之一,可以极大的提高强度。现有技术中TiNb涂层的镀膜方法如专利号为CN00108513.1所公开的专利名称为用电弧离子镀沉积氮化钛铌超硬质梯度薄膜的方法,该技术方案使通过将高速钢工件经过清洗干燥后放入设备真空室中,纯钛和纯铌靶材相间隔置于电弧离子镀的弧源位置上,然后进行镀膜。现有技术中是通过两种单质靶材即Ti靶材和Nb靶材在镀膜机中混合镀的方法实现,但是电弧镀靶材的电流密度大,使两种靶材很难按精准的比例蒸发,会导致电镀出来的涂层成分配比难以控制。而不同的涂层成分配比会使涂层的硬度,抗氧化性等等属性有所不同,难以制作出质量更好的TiNb涂层。
发明内容
有鉴于此,本发明提供了一种TiNb涂层的镀膜方法,以解决上述技术问题。
一种TiNb涂层的镀膜方法,包括以下步骤:
步骤S1:在镀膜机的阴极蒸发源上安装TiNb合金靶材,所述TiNb合金靶材的配比为Nb=55~65%,其余为Ti。
步骤S2:被镀工件经过去油处理和喷沙处理后,设置在所述镀膜机的偏置阴极转架上。
步骤S3:所述镀膜机开始真空抽气,使所述镀膜机的真空室内的极限真空度不低于1×10-3pa。
步骤S4:所述镀膜机开启加热程序,使温度提升,真空度会随温度的提升而下降,然后不断开断加热程序,直至真空度不再下降,在加热过程中真空室内的真空度应该保持在1×10-2pa以上。
步骤S5:通入氩气到0.3pa,开启离子束刻蚀对被镀工件进行离子刻蚀清洗15分钟,使被镀工件表面原子被移开或从表面上被除掉,以对被镀工件进行清洗。
步骤S6:向真空室内通入300sccm的氩气和600sccm的氮气,使真空室内的压强维持在0.4~0.6pa。
步骤S7:对被镀工件施加偏压,并顺序放出电弧,使TiNb合金靶材蒸发产生相应离子,然后带正电的离子在偏压的作用下会沉积到位于转架上的被镀工件表面,形成TiNb膜层,所述TiNb膜层的成分配比为Nb=60%~63%,其余为Ti、N、以及Ar。
步骤S8:关闭气体和电弧源,然后加热到300度维持30分钟。
步骤S9:开启速冷充气循环系统,直至真空室内的温度降低至120度以下,然后在真空室内充入大气,开门取出被镀工件。
进一步地,所述TiNb合金靶材通过熔铸的方式制成。
进一步地,在上述步骤S5中,离子束刻蚀的电弧电流在50A~70A,对于精密细小的被镀工件可以改为辉光离子轰击清洗或辉光离子轰击和离子束刻蚀相互叠加清洗,辉光离子轰击清洗需要先将偏压电源调到500~600V,1~2pa清洗10分钟,然后再将偏压电源调到600~800V,分两段3pa清洗5分钟。
进一步地,所述TiNb膜层的颜色为银白泛微黄色。
进一步地,在上述步骤S7中,工作偏压需要从大到小按顺序调整:1.工作偏压200V,5分钟;2.工作偏压150V,5分钟;3.工作偏压100V,70分钟;4.工作偏压80V,10分钟;5.工作偏压60V,10分钟,保证TiNb膜层厚度为3μm~3.5μm,如果厚度没达到则延长工作偏压为100V的工作时间。
与现有技术相比,本发明提供的TiNb涂层的镀膜方法的通过TiNb合金靶材来镀TiNb膜层,且所述TiNb合金靶材的配比为Nb=55~65%,其余为Ti。事先设置好了靶材中Nb和Ti的配比,因此在TiNb合金靶材蒸发产生相应离子时,能精准控制Nb和Ti蒸发比例。该配比为Nb和Ti的最佳配比,在该最佳配比下形成的TiNb膜层的成分配比为Nb=60%~63%,其余为Ti、N、以及Ar,使所述TiNb膜层具有更好的强度。相较于两种单质靶材混合镀,操作更简单,并使TiNb膜层的比例更精准,提高TiNb膜层的强度和被镀件的耐用性。
附图说明
图1为本发明提供的一种TiNb涂层的镀膜方法的流程图。
具体实施方式
以下对本发明的具体实施例进行进一步详细说明。应当理解的是,此处对本发明实施例的说明并不用于限定本发明的保护范围。
如图1所示,其为本发明提供的TiNb涂层的镀膜方法的流程图。所述TiNb涂层的镀膜方法,包括以下步骤:
步骤S1:在镀膜机的阴极蒸发源上安装TiNb合金靶材,所述TiNb合金靶材的配比为Nb=55~65%,其余为Ti。所述TiNb合金靶材通过熔铸的方式制成,所述镀膜机配备高性能的偏压电源。
步骤S2:被镀工件经过去油处理和喷沙处理后,设置在所述镀膜机的偏置阴极转架上。
步骤S3:所述镀膜机开始真空抽气,使所述镀膜机的真空室内的极限真空度不低于1×10-3pa。
步骤S4:所述镀膜机开启加热程序,使温度提升,真空度会随温度的提升而下降,然后不断开断加热程序,直至真空度不再下降。在加热过程中真空室内的真空度应该保持在1×10-2pa以上。在本实施中加热到450度,其温度可以根据被镀工件而设置。
步骤S5:通入氩气到0.3pa,开启离子束刻蚀对被镀工件进行离子刻蚀清洗15分钟,使被镀工件表面原子被移开或从表面上被除掉,以对被镀工件进行清洗。离子束刻蚀的电弧电流在50A~70A。对于精密细小的被镀工件可以改为辉光离子轰击清洗或辉光离子轰击和离子束刻蚀相互叠加清洗。辉光离子轰击清洗需要先将偏压电源调到500~600V,1~2pa清洗10分钟,然后再将偏压电源调到600~800V,分两段3pa清洗5分钟。
步骤S6:向真空室内通入300sccm的氩气和600sccm的氮气,使真空室内的压强维持在0.4~0.6pa。
步骤S7:对被镀工件施加偏压,并顺序放出电弧,使TiNb合金靶材蒸发产生相应离子,然后带正电的离子在偏压的作用下会沉积到位于转架上的被镀工件表面,形成TiNb膜层。所述TiNb膜层的颜色为银白泛微黄色。
由于TiNb合金靶材的配比为Nb=55~65%,其余为Ti,事先设置好了靶材中Nb和Ti的配比,因此当TiNb合金靶材蒸发产生相应离子时,能精准控制Nb和Ti蒸发比例,且该TiNb合金靶材的成分配比为最佳比例,使得在该最佳配比下形成的TiNb膜层的成分配比为Nb=60%~63%,其余为Ti、N、以及Ar。使所述TiNb膜层具有更好的强度和抗氧化性。另外由于Nb的溅射速率为0.6,Ti的溅射速率为0.51,因此在较高的偏压下Nb在被镀工件上的反溅射损失比Ti要大。因此工作偏压需要从大到小按顺序调整:1.工作偏压200V,5分钟;2.工作偏压150V,5分钟;3.工作偏压100V,70分钟;4.工作偏压80V,10分钟;5.工作偏压60V,10分钟。保证速度的同时避免Nb和Ti损失太多且膜层均匀,应保证TiNb膜层厚度为3μm~3.5μm,如果厚度没达到则延长工作偏压为100V的工作时间。
步骤S8:关闭气体和电弧源,然后加热到300度维持30分钟。
步骤S9:开启速冷充气循环系统,直至真空室内的温度降低至120度以下,然后在真空室内充入大气,开门取出被镀工件。
与现有技术相比,本发明提供的TiNb涂层的镀膜方法的通过TiNb合金靶材来镀TiNb膜层,且所述TiNb合金靶材的配比为Nb=55~65%,其余为Ti。事先设置好了靶材中Nb和Ti的配比,因此在TiNb合金靶材蒸发产生相应离子时,能精准控制Nb和Ti蒸发比例。该配比为Nb和Ti的最佳配比,在该最佳配比下形成的TiNb膜层的成分配比为Nb=60%~63%,其余为Ti、N、以及Ar,使所述TiNb膜层具有更好的强度。相较于两种单质靶材混合镀,操作更简单,并使TiNb膜层的比例更精准,提高TiNb膜层的强度和被镀件的耐用性。
以上仅为本发明的较佳实施例,并不用于局限本发明的保护范围,任何在本发明精神内的修改、等同替换或改进等,都涵盖在本发明的权利要求范围内。
Claims (5)
1.一种TiNb涂层的镀膜方法,其包括以下步骤:
步骤S1:在镀膜机的阴极蒸发源上安装TiNb合金靶材,所述TiNb合金靶材的配比为Nb=55~65%,其余为Ti;
步骤S2:被镀工件经过去油处理和喷沙处理后,设置在所述镀膜机的偏置阴极转架上;
步骤S3:所述镀膜机开始真空抽气,使所述镀膜机的真空室内的极限真空度不低于1×10-3pa;
步骤S4:所述镀膜机开启加热程序,使温度提升,真空度会随温度的提升而下降,然后不断开断加热程序,直至真空度不再下降,在加热过程中真空室内的真空度应该保持在1×10-2pa以上;
步骤S5:通入氩气到0.3pa,开启离子束刻蚀对被镀工件进行离子刻蚀清洗15分钟,使被镀工件表面原子被移开或从表面上被除掉,以对被镀工件进行清洗;
步骤S6:向真空室内通入300sccm的氩气和600sccm的氮气,使真空室内的压强维持在0.4~0.6pa;
步骤S7:对被镀工件施加偏压,并顺序放出电弧,使TiNb合金靶材蒸发产生相应离子,然后带正电的离子在偏压的作用下会沉积到位于转架上的被镀工件表面,形成TiNb膜层,所述TiNb膜层的成分配比为Nb=60%~63%,其余为Ti、N、以及Ar。
步骤S8:关闭气体和电弧源,然后加热到300度维持30分钟。
步骤S9:开启速冷充气循环系统,直至真空室内的温度降低至120度以下,然后在真空室内充入大气,开门取出被镀工件。
2.如权利要求1所述的TiNb涂层的镀膜方法,其特征在于:所述TiNb合金靶材通过熔铸的方式制成。
3.如权利要求1所述的TiNb涂层的镀膜方法,其特征在于:在上述步骤S5中,离子束刻蚀的电弧电流在50A~70A,对于精密细小的被镀工件可以改为辉光离子轰击清洗或辉光离子轰击和离子束刻蚀相互叠加清洗,辉光离子轰击清洗需要先将偏压电源调到500~600V,1~2pa清洗10分钟,然后再将偏压电源调到600~800V,分两段3pa清洗5分钟。
4.如权利要求1所述的TiNb涂层的镀膜方法,其特征在于:所述TiNb膜层的颜色为银白泛微黄色。
5.如权利要求1所述的TiNb涂层的镀膜方法,其特征在于:在上述步骤S7中,工作偏压需要从大到小按顺序调整:1.工作偏压200V,5分钟;2.工作偏压150V,5分钟;3.工作偏压100V,70分钟;4.工作偏压80V,10分钟;5.工作偏压60V,10分钟,保证TiNb膜层厚度为3μm~3.5μm,如果厚度没达到则延长工作偏压为100V的工作时间。
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