CN115110033A - 一种超硬膜层制造方法 - Google Patents
一种超硬膜层制造方法 Download PDFInfo
- Publication number
- CN115110033A CN115110033A CN202210891402.XA CN202210891402A CN115110033A CN 115110033 A CN115110033 A CN 115110033A CN 202210891402 A CN202210891402 A CN 202210891402A CN 115110033 A CN115110033 A CN 115110033A
- Authority
- CN
- China
- Prior art keywords
- target
- film
- arc
- preparing
- cleaning
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000000151 deposition Methods 0.000 claims abstract description 22
- 230000008021 deposition Effects 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims description 47
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 37
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 37
- 239000007789 gas Substances 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 230000037452 priming Effects 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 239000013077 target material Substances 0.000 abstract description 2
- 238000007747 plating Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001771 vacuum deposition Methods 0.000 description 5
- 230000006872 improvement Effects 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 206010040844 Skin exfoliation Diseases 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
本发明公开了一种超硬膜层制造方法。本发明采用Cr靶、Ti靶、W靶作为靶材制备膜层,按不同的膜层硬度进行交替成膜。使用多弧沉积膜层和磁控溅射沉积交替制备超硬膜,形成软硬膜层交替生长,有利于形成高密度位错,有效阻止晶面滑移,有利于膜层组成元素扩散,改善了内应力集中现象,提高了超硬膜的总体强度,硬度。通过改良膜层组织结构达到提高显微硬度的效果,避免单纯依靠膜厚提高性能,节省生产时间与资源,有较好的经济与社会效益。
Description
技术领域
本发明涉及真空镀膜技术领域,具体为一种超硬膜层制造方法。
背景技术
真空镀膜是关于材料表面处理,运用于材料合成与加工的技术。真空镀膜可以运用于各种不同的领域,例如光学、集成电路、钟表、建筑、汽车、包装、机械生产等。真空镀膜运用的领不同,对材料表面的要求也会随之变化,因此也诞生了多种具备各种不同功能的膜层组合。随着设备制造和镀膜工艺技术的不断改善,真空镀膜技术迅速发展,镀膜不再仅起到了单纯的装饰效果,膜层性能指标也在不断进步提高。膜层性能指标中包括提高产品表面硬度,使得产品具有抗刮伤的性能,不仅仅优化了产品的外观品质,而且延长了膜层的使用寿命。
目前,提高膜层表面硬度通常依靠增加膜厚来实现,但是膜层厚度增加,会导致靶材成本上升,能耗增大,破坏表面的光亮度,甚至造成货件必须再进行二次抛光打磨。另外,膜厚增厚会造成膜层内应力加大,使得产品边角位膜层发生剥落的风险上升。
为了解决上述问题,本发明提供了一种超硬膜层制造方法。
发明内容
本发明的目的在于提供一种超硬膜层制造方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种超硬膜层制造方法,该方法包括以下步骤:
步骤一:弧靶轰击清洗:
S11:取基材,清洗,烘干,得到处理后的基材,通入氩气,气压为1.5×10-1Pa,开Cr弧靶,电流为55-70A,对处理后的基材进行轰击清洗;
S12:清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
S21:开Cr靶打底层,沉积6-8min;
S22:开Ti靶预启动,沉积2-3min;
S23:开W靶预启动,沉积2-3min;
步骤三:制备硬化层:
S31:通入乙炔,将乙炔气量由20-30sccm升至80-90sccm,保持10-12分钟,偏压为100-200V;降乙炔气量至20-30sccm;
S32:重复步骤S314-6次,降乙炔气量至30-40sccm,关Ti靶,Cr靶;
步骤四:制备加硬层:保持W靶开启,电流为10-20A,开Cr弧靶,沉积8-10min;
步骤五:制备颜色层:关Cr弧靶,保持W靶开启,沉积颜色层,偏压为100-200V。
较为优化地,步骤S11中,轰击清洗工艺参数为:偏压为400-600V,清洗时间为4-8min。
较为优化地,步骤一中,基材为铜、铁、锌、铝、合金中的一种或多种。
较为优化地,步骤二中,Cr靶、Ti靶、W靶的靶电流均为10-20A,沉积时维持气压为0.4-0.5Pa,偏压为100-120V。
较为优化地,步骤S31中,乙炔气量由20-30sccm升至80-90sccm的时间控制为10min以内。
较为优化地,步骤四中,开Cr弧靶,靶电流为60-70A。
较为优化地,步骤二中,制备纯金属底层时,将氩气气压升高至4.5×10-1Pa。
较为优化地,所述Cr靶的靶电流为10-20A,Ti靶的靶电流为10-18A、W靶的靶电流为10-20。
与现有技术相比,本发明所达到的有益效果是:
(1)本发明采用Cr靶、Ti靶、W靶作为靶材制备膜层,按不同的膜层硬度进行交替成膜,既能有效利用WC高硬度的材料性能,又减缓硬度梯度陡变状态,降低内应力集中风险。
(2)普通发明中的膜层由单纯磁控溅射膜层构成,本发明提出的新膜层组合由多弧沉积膜层和磁控溅射沉积组成,具体为按照阴极弧沉积膜层+溅射沉积膜层+阴极弧沉积膜层+溅射沉积膜层交替组成,有利于形成高密度位错,有效阻止晶面滑移,从微观结构层面提高膜层总体强度,硬度。
(3)本发明膜层在生长过程中,会形成软硬膜层交替生长,有利于膜层组成元素扩散,进一步改善内应力集中现象。
(4)本发明通过改良膜层组织结构达到提高显微硬度的效果,拓展了膜层性能,避免单纯依靠膜厚提高性能,节省了生产时间与资源,有较好的经济与社会效益。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
步骤一:弧靶轰击清洗:
(1)取基材,清洗,烘干,得到处理后的基材,通入氩气,气压为1.5×10-1Pa,开3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为70A,偏压为500V,时间为3min,关Cr弧靶;
(2)再次开另外3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为70A,偏压为500V,时间为3min;
(3)清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
(1)开Cr靶打底层,靶电流为15安培,成膜8分钟,气压保持在0.4Pa,偏压为100V;
(2)开Ti靶,靶电流为12安培,成膜3分钟,气压保持在0.4Pa,偏压为100V;
(3)开W靶,靶电流为15安培,成膜3分钟,气压保持在0.4Pa,偏压为100V;
步骤三:制备硬化层:
(1)通入乙炔,将乙炔气量由在10min中内由20sccm升至80sccm,保持10分钟,偏压为100V;降乙炔气量至20sccm;
(2)重复步骤三(1)4-6次,最后一次将乙炔气量降至30sccm,关Ti靶,关Cr靶;
步骤四:制备加硬层:保持W靶开启,电流为15A,氩气气压保持0.4Pa不变,开3只Cr弧靶,靶电流为60A,偏压为100V,时间为4min,关Cr弧靶;再次开另外3只Cr弧靶,靶电流为60A,偏压为100V,时间为4min;
步骤五:制备颜色层:关Cr弧靶,保持W靶开启,调整气压至0.5Pa,通入乙炔130sccm。40分钟,结束镀膜。
实施例2
步骤一:弧靶轰击清洗:
(1)取基材,清洗,烘干,得到处理后的基材,通入氩气,气压为1.5×10-1Pa,开2只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为60A,偏压为400V,时间为2min,关Cr弧靶;
(2)再次开另外2只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为60A,偏压为400V,时间为2min;
(3)清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
(1)开Cr靶打底层,靶电流为15安培,成膜6分钟,气压保持在0.45Pa,偏压为110V;
(2)开Ti靶,靶电流为12安培,成膜2分钟,气压保持在0.45Pa,偏压为110V;
(3)开W靶,靶电流为15安培,成膜2分钟,气压保持在0.45Pa,偏压为110V;
步骤三:制备硬化层:
(1)通入乙炔,将乙炔气量由在10min中内由25sccm升至85sccm,保持10分钟,偏压为150V;降乙炔气量至25sccm;
(2)重复步骤三(1)4-6次,最后一次将乙炔气量降至35sccm,关Ti靶,关Cr靶;
步骤四:制备加硬层:保持W靶开启,电流为10-20A,氩气气压保持0.4Pa不变,开2只Cr弧靶,靶电流为65A,偏压为80V,时间为4.5min,关Cr弧靶;再次开另外2只Cr弧靶,靶电流为65A,偏压为80V,时间为4.5min;
步骤五:制备颜色层:关Cr弧靶,调整气压至0.5Pa,开W靶,通入乙炔130sccm。40分钟后,关W靶,结束镀膜。
实施例3
步骤一:弧靶轰击清洗:
(1)取基材,清洗,烘干,得到处理后的基材,通入氩气,气压为1.5×10-1Pa,开4只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为55A,偏压为600V,时间为4min,关Cr弧靶;
(2)再次开另外4只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为55A,偏压为600V,时间为4min;
(3)清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
(1)开Cr靶打底层,靶电流为20安培,成膜8分钟,气压保持在0.5Pa,偏压为120V;
(2)开Ti靶,靶电流为20安培,成膜3分钟,气压保持在0.5Pa,偏压为120V;
(3)开W靶,靶电流为20安培,成膜3分钟,气压保持在0.5Pa,偏压为120V;
步骤三:制备硬化层:
(1)通入乙炔,将乙炔气量由在10min中内由30sccm升至90sccm,保持10分钟,偏压为200V;降乙炔气量至30sccm;
(2)重复步骤三(1)4-6次,最后一次将乙炔气量降至40sccm,关Ti靶,关Cr靶;
步骤四:制备加硬层:保持W靶开启,电流为20A,氩气气压保持0.4Pa不变,开4只Cr弧靶,靶电流为70A,偏压为120V,时间为5min,关Cr弧靶;再次开另外4只Cr弧靶,靶电流为70A,偏压为120V,时间为5min;
步骤五:制备颜色层:关Cr弧靶,调整气压至0.5Pa,开W靶,通入乙炔130sccm。40分钟后,关W靶,结束镀膜。
对比例1:单纯磁控溅射膜层。
步骤一:弧靶轰击清洗:通入氩气,使炉内气压达到1.2×10-1Pa
(1)取基材,清洗,烘干,得到处理后的基材,开3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为70A,偏压为600V,时间为4min,关Cr弧靶;
(2)再次开另外3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为70A,偏压为600V,时间为4min;
(3)清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
开W靶打底层,靶电流为15安培,成膜8分钟,气压保持在0.5Pa,偏压为100V;
步骤三:制备硬化层:
通入乙炔,将乙炔气量由在10min中内由30sccm升至90sccm,保持130分钟,偏压为100V;
步骤四:制备颜色层:保持W靶运行,保持气压0.5Pa,通入乙炔130sccm。30分钟后,结束镀膜。
对比例2:单纯磁控溅射膜层
步骤一:弧靶轰击清洗:通入氩气,使炉内气压达到1.2×10-1Pa
(1)取基材,清洗,烘干,得到处理后的基材,开3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为65A,偏压为600V,时间为4min,关Cr弧靶;
(2)再次开另外3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为65A,偏压为600V,时间为4min;
(3)清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
开W靶打底层,靶电流为17安培,成膜8分钟,气压保持在0.5Pa,偏压为100V;
步骤三:制备硬化层:
保持W靶运行,通入乙炔,将乙炔气量由在10min中内由30sccm升至90sccm,保持130分钟,偏压为100V;
步骤四:制备颜色层:W靶继续运行,保持气压0.5Pa,通入乙炔130sccm。30分钟后,结束镀膜。
对比例3:单纯磁控溅射膜层
步骤一:弧靶轰击清洗:通入氩气,使炉内气压达到1.2×10-1Pa
(1)取基材,清洗,烘干,得到处理后的基材,开3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为65A,偏压为600V,时间为4min,关Cr弧靶;
(2)再次开另外3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为65A,偏压为600V,时间为4min;
(3)清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
开Ti靶,靶电流为15安培,成膜3分钟,气压保持在0.4Pa,偏压为100V;
开W靶,靶电流为17安培,成膜7分钟,气压保持在0.5Pa,偏压为100V;
步骤三:制备硬化层:
保持W靶运行,通入乙炔,将乙炔气量由在10min中内由30sccm升至90sccm,保持130分钟,偏压为100V;
步骤四:制备颜色层:W靶继续运行,保持气压0.5Pa,通入乙炔130sccm。30分钟后,结束镀膜。
对比例4:单纯磁控溅射膜层
步骤一:弧靶轰击清洗:通入氩气,使炉内气压达到1.2×10-1Pa
(1)取基材,清洗,烘干,得到处理后的基材,开3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为65A,偏压为600V,时间为4min,关Cr弧靶;
(2)再次开另外3只Cr弧靶,对处理后的基材进行轰击清洗,靶电流为65A,偏压为600V,时间为4min;
(3)清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
开Cr靶打底层,靶电流为17安培,成膜7分钟,气压保持在0.4Pa,偏压为100V;
开W靶,靶电流为17安培,成膜3分钟,气压保持在0.5Pa,偏压为100V;
步骤三:制备硬化层:
保持W靶运行,通入乙炔,将乙炔气量由在10min中内由30sccm升至90sccm,保持130分钟,偏压为100V;
步骤四:制备颜色层:W靶继续运行,保持气压0.5Pa,通入乙炔130sccm。30分钟后,结束镀膜。
实验
取实施例1至实施例3、对比例1至对比例2制备得到的镀膜基材进行性能测试,得到的结果如下表所示:使用球磨仪进行膜厚测量;使用划痕仪进行划痕仪测试,载荷为250g;使用震盘方法,对膜层进行耐磨测试。
结论:由表上数据对比可知,由本发明提供的方法,使用多弧沉积膜层和磁控溅射沉积交替制备超硬膜层,得到的超硬膜硬度更好,内应力集中现象得到改善。通过震盘方法,对膜层进行耐磨测试,由此表上数据对比可知,膜的内应力情况得到改善,使用寿命增长。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种超硬膜层制造方法,其特征在于:该方法包括以下步骤:
步骤一:弧靶轰击清洗:
S11:取基材,清洗,烘干,得到处理后的基材,通入氩气,气压为1.5×10-1Pa,开Cr弧靶,电流为55-70A,对处理后的基材进行轰击清洗;
S12:清洗结束,关Cr弧靶;
步骤二:制备纯金属底层:
S21:开Cr靶打底层,沉积6-8min;
S22:开Ti靶预启动,沉积2-3min;
S23:开W靶预启动,沉积2-3min;
步骤三:制备硬化层:
S31:通入乙炔,将乙炔气量由20-30sccm升至80-90sccm,保持10-12分钟,偏压为100-200V;降乙炔气量至20-30sccm;
S32:重复步骤S314-6次,降乙炔气量至30-40sccm,关Ti靶,Cr靶;
步骤四:制备加硬层:保持W靶开启,电流为10-20A,开Cr弧靶,沉积8-10min;
步骤五:制备颜色层:关Cr弧靶,保持W靶开启,沉积颜色层,偏压为100-200V。
2.根据权利要求1所述的一种超硬膜层制造方法,其特征在于:步骤S11中,轰击清洗工艺参数为:偏压为400-600V,清洗时间为4-8min。
3.根据权利要求1所述的一种超硬膜层制造方法,其特征在于:步骤一中,基材为铜、铁、锌、铝、合金中的一种或多种。
4.根据权利要求1所述的一种超硬膜层制造方法,其特征在于:步骤二中,Cr靶、Ti靶、W靶的靶电流均为10-20A,沉积时维持气压为0.4-0.5Pa,偏压为100-120V。
5.根据权利要求1所述的一种超硬膜层制造方法,其特征在于:步骤S31中,乙炔气量由20-30sccm升至80-90sccm的时间控制为10min以内。
6.根据权利要求1所述的一种超硬膜层制造方法,其特征在于:步骤四中,开Cr弧靶,靶电流为60-70A。
7.根据权利要求1所述的一种超硬膜层制造方法,其特征在于:步骤二中,制备纯金属底层时,将氩气气压升高至4.5×10-1Pa。
8.根据权利要求4所述的一种超硬膜层制造方法,其特征在于:所述Cr靶的靶电流为10-20A,Ti靶的靶电流为10-18A、W靶的靶电流为10-20A。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210891402.XA CN115110033B (zh) | 2022-07-27 | 2022-07-27 | 一种超硬膜层制造方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210891402.XA CN115110033B (zh) | 2022-07-27 | 2022-07-27 | 一种超硬膜层制造方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN115110033A true CN115110033A (zh) | 2022-09-27 |
CN115110033B CN115110033B (zh) | 2024-01-23 |
Family
ID=83335043
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210891402.XA Active CN115110033B (zh) | 2022-07-27 | 2022-07-27 | 一种超硬膜层制造方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115110033B (zh) |
Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0875596A1 (en) * | 1997-04-30 | 1998-11-04 | Masco Corporation | Article having a decorative and protective coating |
WO1999055929A1 (de) * | 1998-04-29 | 1999-11-04 | Unaxis Trading Ag | Werkzeug oder maschinenbauteil und verfahren zur verschleissfestigkeitserhöhung eines solchen teiles |
US20030113590A1 (en) * | 2001-12-19 | 2003-06-19 | Guocun Chen | Low pressure coated article |
JP2004010923A (ja) * | 2002-06-04 | 2004-01-15 | Toyota Motor Corp | 摺動部材及びその製造方法 |
US20050170162A1 (en) * | 2004-02-02 | 2005-08-04 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) | Hard laminated film, method of manufacturing the same and film-forming device |
CN103009697A (zh) * | 2012-12-18 | 2013-04-03 | 安徽天一重工股份有限公司 | 一种自润滑梯度复合超硬膜及其制备方法 |
WO2017136970A1 (zh) * | 2016-02-11 | 2017-08-17 | 广东工业大学 | TiAlSiZrN基复合涂层、具有该复合涂层的梯度超细硬质合金刀具及其制备方法 |
CN208121182U (zh) * | 2018-04-11 | 2018-11-20 | 深圳市正和忠信股份有限公司 | 一种黑色导电pvd薄膜 |
WO2019043167A1 (en) * | 2017-08-31 | 2019-03-07 | Walter Ag | WEAR-RESISTANT PVD TOOL COATING CONTAINING TIALN NANOCOUCHE FILMS |
CN109913825A (zh) * | 2019-03-25 | 2019-06-21 | 伯恩高新科技(惠州)有限公司 | 一种高振动耐磨性能的pvd复合膜层制备工艺 |
JP2019157259A (ja) * | 2018-03-16 | 2019-09-19 | 世枝 麦 | 高硬度殺菌pvdフィルムの調製方法 |
CN112458417A (zh) * | 2020-11-24 | 2021-03-09 | 创隆实业(深圳)有限公司 | 一种多元层状加硬涂层生长工艺 |
-
2022
- 2022-07-27 CN CN202210891402.XA patent/CN115110033B/zh active Active
Patent Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0875596A1 (en) * | 1997-04-30 | 1998-11-04 | Masco Corporation | Article having a decorative and protective coating |
US5922478A (en) * | 1997-04-30 | 1999-07-13 | Masco Corporation | Article having a decorative and protective coating |
WO1999055929A1 (de) * | 1998-04-29 | 1999-11-04 | Unaxis Trading Ag | Werkzeug oder maschinenbauteil und verfahren zur verschleissfestigkeitserhöhung eines solchen teiles |
US20030113590A1 (en) * | 2001-12-19 | 2003-06-19 | Guocun Chen | Low pressure coated article |
JP2004010923A (ja) * | 2002-06-04 | 2004-01-15 | Toyota Motor Corp | 摺動部材及びその製造方法 |
US20050170162A1 (en) * | 2004-02-02 | 2005-08-04 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) | Hard laminated film, method of manufacturing the same and film-forming device |
CN103009697A (zh) * | 2012-12-18 | 2013-04-03 | 安徽天一重工股份有限公司 | 一种自润滑梯度复合超硬膜及其制备方法 |
WO2017136970A1 (zh) * | 2016-02-11 | 2017-08-17 | 广东工业大学 | TiAlSiZrN基复合涂层、具有该复合涂层的梯度超细硬质合金刀具及其制备方法 |
WO2019043167A1 (en) * | 2017-08-31 | 2019-03-07 | Walter Ag | WEAR-RESISTANT PVD TOOL COATING CONTAINING TIALN NANOCOUCHE FILMS |
JP2019157259A (ja) * | 2018-03-16 | 2019-09-19 | 世枝 麦 | 高硬度殺菌pvdフィルムの調製方法 |
CN208121182U (zh) * | 2018-04-11 | 2018-11-20 | 深圳市正和忠信股份有限公司 | 一种黑色导电pvd薄膜 |
CN109913825A (zh) * | 2019-03-25 | 2019-06-21 | 伯恩高新科技(惠州)有限公司 | 一种高振动耐磨性能的pvd复合膜层制备工艺 |
CN112458417A (zh) * | 2020-11-24 | 2021-03-09 | 创隆实业(深圳)有限公司 | 一种多元层状加硬涂层生长工艺 |
Also Published As
Publication number | Publication date |
---|---|
CN115110033B (zh) | 2024-01-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102392246B (zh) | 一种金属表面处理工艺 | |
CN110777336A (zh) | 一种基于能量调控原理制备超厚硬质薄膜的方法 | |
CN111690898B (zh) | 改进的镀膜工艺 | |
CN107254662B (zh) | 蓝色复合薄膜及其制备方法 | |
CN106244986A (zh) | 功能梯度的类金刚石碳薄膜及其制备方法和制品 | |
CN108456843A (zh) | 一种高性能TiAlSiN纳米复合涂层及其制备方法和应用 | |
CN102676989A (zh) | 镀膜件及其制备方法 | |
CN108893712A (zh) | 表面带有镀层的贵金属制品及其制备方法 | |
CN106119783A (zh) | 功能梯度的类金刚石碳薄膜及其制备方法和制品 | |
CN112144063B (zh) | 一种带有黑色多层膜的镀膜器件及其制备方法 | |
CN115110033B (zh) | 一种超硬膜层制造方法 | |
CN108359938B (zh) | 一种活塞环表面超厚类金刚石薄膜涂层制备方法 | |
CN110684954B (zh) | 金属制品及其制备方法和手机后壳 | |
KR102168776B1 (ko) | 이중층 크롬 나이트라이드 코팅된 물품들 및 관련된 방법들 | |
CN110656313B (zh) | 一种与硬质合金结合牢固的氮化锆铝/氧化铝复合涂层及其制备方法 | |
CN112458417A (zh) | 一种多元层状加硬涂层生长工艺 | |
CN114411097A (zh) | 基于微弧离子镀的分梳辊针布表面镀层的制备方法、分梳辊针布 | |
CN114293148A (zh) | 一种钛合金表面修复与强化功能涂层一体化的涂层材料及其制备方法和应用 | |
CN112779493A (zh) | 一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法 | |
CN106917066B (zh) | 一种四元单层超硬薄膜材料及其制备方法 | |
CN112941461A (zh) | 一种复合超硬强韧涂层材料以及制备方法 | |
CN111850483A (zh) | 一种多层梯度硬质涂层及其制备工艺 | |
CN113862671B (zh) | Pvd-cvd联用制备类金刚石膜的方法、类金刚石膜、合金材料及汽车部件 | |
CN114540764B (zh) | 镀膜产品及其制备方法 | |
CN115261774B (zh) | 一种铝合金易拉罐盖高速冲裁模刃口梯度渐变超硬复合膜层及其制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |