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CN108505001A - A kind of composite wear-resistant layer and preparation method thereof - Google Patents

A kind of composite wear-resistant layer and preparation method thereof Download PDF

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Publication number
CN108505001A
CN108505001A CN201810308825.8A CN201810308825A CN108505001A CN 108505001 A CN108505001 A CN 108505001A CN 201810308825 A CN201810308825 A CN 201810308825A CN 108505001 A CN108505001 A CN 108505001A
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CN
China
Prior art keywords
film layer
composite wear
magnetron sputtering
resistant layer
thin film
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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.)
Pending
Application number
CN201810308825.8A
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Chinese (zh)
Inventor
周少波
刘春雨
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou Color Coating Vacuum Coating Co Ltd
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Suzhou Color Coating Vacuum Coating Co Ltd
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Publication date
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Priority to CN201810308825.8A priority Critical patent/CN108505001A/en
Publication of CN108505001A publication Critical patent/CN108505001A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021Reactive sputtering or evaporation
    • C23C14/0036Reactive sputtering
    • C23C14/0057Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0635Carbides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/083Oxides of refractory metals or yttrium

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  • 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

The present invention provides a kind of composite wear-resistant layer and preparation method thereof, wherein the composite wear-resistant layer includes:Titanium carbide nanometer thin film layer and zirconia nanopowder film layer;The titanium carbide nanometer thin film layer is set to the surface of the metal base, and the zirconia nanopowder film layer is set to the surface of the titanium carbide nanometer thin film layer.The composite wear-resistant layer of the present invention can be compound in the surface of tableware, can not only play the role of beautifying tableware, while improve the scratch resistance of tableware, wearability, corrosion resistance, full of the use demand for meeting modernized society people.

Description

A kind of composite wear-resistant layer and preparation method thereof
Technical field
The present invention relates to technology of thin film material preparation field more particularly to a kind of surfaces for being compound in metal base Composite wear-resistant layer and preparation method thereof.
Background technology
Tableware is the daily necessities often needed to use in people's daily life.With the development of society, people are for height The demand of shelves tableware is higher and higher.However, current top grade tableware is limited to the property of material itself, wearability and corrosion-resistant Property is poor, is unable to fully meet the use demand of people.Therefore, in view of the above-mentioned problems, it is necessary to propose further solution party Case.
Invention content
The purpose of the present invention is to provide a kind of composite wear-resistant layers and preparation method thereof, existing in the prior art to overcome It is insufficient.
For achieving the above object, the present invention provides a kind of composite wear-resistant layer, is used to be compound in the table of metal base Face, the composite wear-resistant layer include:Titanium carbide nanometer thin film layer and zirconia nanopowder film layer;The titanium carbide nano thin-film Layer is set to the surface of the metal base, and the zirconia nanopowder film layer is set to the table of the titanium carbide nanometer thin film layer Face.
The improvement of composite wear-resistant layer as the present invention, the titanium carbide nanometer thin film layer are deposited using medium frequency magnetron sputtering It forms.
As the improvement of composite wear-resistant layer of the invention, the gas being passed through in the medium frequency magnetron sputtering is acetylene.
The improvement of composite wear-resistant layer as the present invention, the zirconia nanopowder film layer are deposited using medium frequency reactive sputtering It forms.
As the present invention composite wear-resistant layer improvement, the metal base in stainless steel, carbon steel, aluminium alloy one Kind.
For achieving the above object, the present invention provides a kind of composite wear-resistant layer, is used to be compound in the table of metal base Face, the composite wear-resistant layer include at least two layers unit film layer being cascading, and any unit film layer includes carbonization Titanium nanometer thin film layer and zirconia nanopowder film layer, wherein the zirconia nanopowder film layer is set to the titanium carbide nanometer In film layer, the titanium carbide nanometer thin film layer is set to the surface of substrate layer or the zirconium oxide of unit film layer adjacent thereto In nanometer thin film layer.
For achieving the above object, the present invention provides a kind of preparation method of composite wear-resistant layer comprising following steps:
S1, metal base is placed in magnetron sputtering space, closing is placed with the magnetron sputtering space of metal base;
S2, closed magnetron sputtering space is vacuumized, it is made to meet the needs of magnetron sputtering;
S3, it is passed through argon gas into magnetron sputtering space, and is powered to titanium target, while high pressure is applied to target surface, under high pressure effect, The surface of the argon ion bombardment metal base of ionization;
S4, under vacuum conditions is passed through the mixed gas of argon gas and acetylene into magnetron sputtering space and is powered to titanium target, in institute It states deposition on metal base and forms titanium carbide nanometer thin film layer;
S5, stopping are passed through the mixed gas of argon gas and acetylene, while being powered to titanium target, be passed through into magnetron sputtering space argon gas and The mixed gas of oxygen simultaneously applies high pressure to zirconium target, deposits to form zirconia nanopowder on the surface of the titanium carbide nanometer thin film layer Film layer.
The improvement of the preparation method of composite wear-resistant layer as the present invention, in the step S2, to closed magnetron sputtering When space is vacuumized:
First time pumping is carried out to closed sputtering chamber using aspiration pump, the vacuum degree in magnetron sputtering space is made to reach 2Pa-5Pa, It is evacuated carrying out second to closed sputtering chamber using aspiration pump, the vacuum degree in magnetron sputtering space is made to reach 1 × 10-4Pa-2 ×10-4Pa。
The improvement of the preparation method of composite wear-resistant layer as the present invention, in the step S4, the volume of argon gas and acetylene Than being 5:2, the time that deposition forms titanium carbide nanometer thin film layer is 15 ~ 180 minutes.
The improvement of the preparation method of composite wear-resistant layer as the present invention, in the step S5, the volume of argon gas and oxygen Than being 5:1, the time that deposition forms zirconia nanopowder film layer is 2 ~ 20 minutes.
Compared with prior art, the beneficial effects of the invention are as follows:The composite wear-resistant layer of the present invention can be compound in the table of tableware Face can not only play the role of beautifying tableware, while improve the scratch resistance of tableware, wearability, corrosion resistance, be full of Meet the use demand of modernized society people.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments described in invention, for those of ordinary skill in the art, without creative efforts, Other drawings may also be obtained based on these drawings.
Fig. 1 is the schematic diagram of a layer structure of one technical solution of composite wear-resistant layer of the present invention;
Fig. 2 is the schematic diagram of a layer structure of another technical solution of composite wear-resistant layer of the present invention, wherein the quantity of unit film layer is two Layer.
Specific implementation mode
The present invention is described in detail for each embodiment shown in below in conjunction with the accompanying drawings, but it should explanation, these Embodiment is not limitation of the present invention, those of ordinary skill in the art according to function, method made by these embodiments, Or the equivalent transformation in structure or replacement, all belong to the scope of protection of the present invention within.
As shown in Figure 1, the composite wear-resistant layer of the present invention includes:Titanium carbide nanometer thin film layer 1 and zirconia nanopowder film Layer 2.Wherein, the titanium carbide nanometer thin film layer 1 is set to the surface of the metal base, the zirconia nanopowder film layer 2 It is set to the surface of the titanium carbide nanometer thin film layer 1.
Wherein, the titanium carbide nanometer thin film layer 1 is deposited using medium frequency magnetron sputtering, it is preferable that the intermediate frequency magnetic The gas being passed through in control sputtering is acetylene.The zirconia nanopowder film layer 2 is deposited using medium frequency reactive sputtering.The gold Belonging to base material can be selected from one kind in stainless steel, carbon steel, aluminium alloy etc..
As shown in Fig. 2, based on the same technical idea, the present invention also provides a kind of composite wear-resistant layer, being used to be compound in The surface of metal base, the composite wear-resistant layer include at least two layers unit film layer being cascading.Any unit Film layer includes titanium carbide nanometer thin film layer 1 and zirconia nanopowder film layer 2, wherein the zirconia nanopowder film layer 2 is arranged In in the titanium carbide nanometer thin film layer 1, the titanium carbide nanometer thin film layer 1 is set to the surface or adjacent thereto of substrate layer Unit film layer zirconia nanopowder film layer 2 on.To, in the technical program, it can be achieved that tableware surface recombination multilayer Wearing layer.
The present invention also provides a kind of preparation methods of composite wear-resistant layer comprising following steps:
S1, metal base is placed in magnetron sputtering space, closing is placed with the magnetron sputtering space of metal base;
S2, closed magnetron sputtering space is vacuumized, it is made to meet the needs of magnetron sputtering;
S3, it is passed through argon gas into magnetron sputtering space, and is powered to titanium target, while high pressure is applied to target surface, under high pressure effect, The surface of the argon ion bombardment metal base of ionization;
S4, under vacuum conditions is passed through the mixed gas of argon gas and acetylene into magnetron sputtering space and is powered to titanium target, in institute It states deposition on metal base and forms titanium carbide nanometer thin film layer;
S5, stopping are passed through the mixed gas of argon gas and acetylene, while being powered to titanium target, be passed through into magnetron sputtering space argon gas and The mixed gas of oxygen simultaneously applies high pressure to zirconium target, deposits to form zirconia nanopowder on the surface of the titanium carbide nanometer thin film layer Film layer.
With reference to several specific embodiments, above-mentioned preparation method is illustrated.
Embodiment 1
In the present embodiment on the substrate of stainless steel the compound present invention composite wear-resistant layer.Metal base is set by the movements and postures of actors In magnetron sputtering space, closing is placed with the magnetron sputtering space of metal base.Closed magnetron sputtering space is taken out Vacuum is to 3 × 10-3Pa.It is passed through argon gas into magnetron sputtering space, and is powered to titanium target, while high pressure is applied to target surface, in height Under pressure effect, the surface of the argon ion bombardment metal base of ionization.3 × 10-3Under the vacuum environment of Pa, filled using carbonization titanium target Enter argon gas, until air pressure is 0.5Pa, adjusts bias 100V, duty ratio 20%% sputters 40min with the power of 400W.X-ray Film thickness gauge measures titanium carbide nano thin-film thickness 1.2um.Using zirconium target, vacuum cavity is evacuated down to 4 × 10-3Pa, is filled with The volume flow of argon gas is 300sccm, adjusts bias 100V, and duty ratio 20% sputters 10min with the power of 400W.X-ray Film thickness gauge measures zirconia nanopowder film thickness 0.6um.
Embodiment 2
In the present embodiment on the substrate of stainless steel the compound present invention composite wear-resistant layer.Metal base is set by the movements and postures of actors In magnetron sputtering space, closing is placed with the magnetron sputtering space of metal base.Closed magnetron sputtering space is taken out Vacuum is to 1 × 10-3Pa.It is passed through argon gas into magnetron sputtering space, and is powered to titanium target, while high pressure is applied to target surface, in height Under pressure effect, the surface of the argon ion bombardment metal base of ionization.1 × 10-3Under the vacuum environment of Pa, filled using carbonization titanium target Enter argon gas, until air pressure is 3Pa, adjusts bias 200V, duty ratio 50% sputters 100min with the power of 1000W.X-ray film Thick instrument measures titanium carbide nano thin-film thickness 3.6um.Vacuum cavity is evacuated down to 3 × 10-3Pa is filled with the volume flow of argon gas For 400sccm, reaction gas O2, until air pressure is 0.5Pa, bias 200V is adjusted, duty ratio 50% is splashed with the power of 1000W Penetrate 20min.X-ray film thickness gauge measures zirconia nanopowder film thickness 1.8um.
Embodiment 3
In the present embodiment on the substrate of carbon steel material the compound present invention composite wear-resistant layer.Metal base is placed in by the movements and postures of actors In magnetron sputtering space, closing is placed with the magnetron sputtering space of metal base.Closed magnetron sputtering space take out true Sky is to 2 × 10-3Pa.It is passed through argon gas into magnetron sputtering space, and is powered to titanium target, while high pressure is applied to target surface, in high pressure Under effect, the surface of the argon ion bombardment metal base of ionization.2 × 10-3Under the vacuum environment of Pa, it is filled with using carbonization titanium target Ar gas adjusts bias 550V until air pressure is 2Pa, and duty ratio 85% sputters 180min.X ray film thickness with the power of 800W Instrument measures titanium carbide nano thin-film thickness 1.2um.Vacuum cavity is evacuated down to 2 × 10-3Pa is filled with the volume flow of Ar gases For 200sccm, it is re-filled with reaction gas CF4, until air pressure is 0.5Pa, adjusts bias 550V, duty ratio 50%, with 400W's Power sputters 20min.X ray film thickness gauges and measures zirconia nanopowder film thickness 0.6um.
In conclusion the composite wear-resistant layer of the present invention can be compound in the surface of tableware, beautification tableware can be not only played Effect, while the scratch resistance of tableware, wearability, corrosion resistance are improved, full of meeting making for modernized society people Use demand.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art The other embodiment being appreciated that.

Claims (10)

1. a kind of composite wear-resistant layer is used to be compound in the surface of metal base, which is characterized in that the composite wear-resistant layer packet It includes:Titanium carbide nanometer thin film layer and zirconia nanopowder film layer;The titanium carbide nanometer thin film layer is set to the Metal Substrate The surface of material, the zirconia nanopowder film layer are set to the surface of the titanium carbide nanometer thin film layer.
2. composite wear-resistant layer according to claim 1, which is characterized in that the titanium carbide nanometer thin film layer uses intermediate frequency magnetic Control sputtering sedimentation forms.
3. composite wear-resistant layer according to claim 2, which is characterized in that the gas being passed through in the medium frequency magnetron sputtering is Acetylene.
4. composite wear-resistant layer according to claim 1, which is characterized in that the zirconia nanopowder film layer is anti-using intermediate frequency Sputtering sedimentation is answered to form.
5. composite wear-resistant layer according to claim 1, which is characterized in that the metal base is selected from stainless steel, carbon steel, aluminium One kind in alloy.
6. a kind of composite wear-resistant layer is used to be compound in the surface of metal base, which is characterized in that the composite wear-resistant layer includes At least two layers unit film layer being cascading, any unit film layer includes titanium carbide nanometer thin film layer and zirconium oxide Nanometer thin film layer, wherein the zirconia nanopowder film layer is set in the titanium carbide nanometer thin film layer, the titanium carbide is received Rice film layer is set in the surface of substrate layer or the zirconia nanopowder film layer of unit film layer adjacent thereto.
7. a kind of preparation method of composite wear-resistant layer, which is characterized in that the preparation method of the composite wear-resistant layer includes following step Suddenly:
S1, metal base is placed in magnetron sputtering space, closing is placed with the magnetron sputtering space of metal base;
S2, closed magnetron sputtering space is vacuumized, it is made to meet the needs of magnetron sputtering;
S3, it is passed through argon gas into magnetron sputtering space, and is powered to titanium target, while high pressure is applied to target surface, under high pressure effect, The surface of the argon ion bombardment metal base of ionization;
S4, under vacuum conditions is passed through the mixed gas of argon gas and acetylene into magnetron sputtering space and is powered to titanium target, in institute It states deposition on metal base and forms titanium carbide nanometer thin film layer;
S5, stopping are passed through the mixed gas of argon gas and acetylene, while being powered to titanium target, be passed through into magnetron sputtering space argon gas and The mixed gas of oxygen simultaneously applies high pressure to zirconium target, deposits to form zirconia nanopowder on the surface of the titanium carbide nanometer thin film layer Film layer.
8. the improvement of the preparation method of the composite wear-resistant layer as the present invention, in the step S2, to closed magnetron sputtering sky Between when being vacuumized:
First time pumping is carried out to closed sputtering chamber using aspiration pump, the vacuum degree in magnetron sputtering space is made to reach 2Pa-5Pa, It is evacuated carrying out second to closed sputtering chamber using aspiration pump, the vacuum degree in magnetron sputtering space is made to reach 1 × 10-4Pa-2 ×10-4Pa。
9. the improvement of the preparation method of the composite wear-resistant layer as the present invention, in the step S4, the volume ratio of argon gas and acetylene It is 5:2, the time that deposition forms titanium carbide nanometer thin film layer is 15 ~ 180 minutes.
10. the improvement of the preparation method of the composite wear-resistant layer as the present invention, in the step S5, the volume ratio of argon gas and oxygen It is 5:1, the time that deposition forms zirconia nanopowder film layer is 2 ~ 20 minutes.
CN201810308825.8A 2018-04-09 2018-04-09 A kind of composite wear-resistant layer and preparation method thereof Pending CN108505001A (en)

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Application Number Priority Date Filing Date Title
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2163456A (en) * 1984-07-13 1986-02-26 Katsuhiro Okubo Method of forming a coloured hard coating
CN101462386A (en) * 2007-12-21 2009-06-24 山特维克知识产权股份有限公司 Coated cutting tool and a method of making a coated cutting tool
CN102899622A (en) * 2011-07-29 2013-01-30 鸿富锦精密工业(深圳)有限公司 Film-coated component and preparation method thereof
CN103436843A (en) * 2013-09-18 2013-12-11 佛山市伟盛利得镀膜有限公司 PVD (physical vapor deposition) composite membrane layer as well as preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2163456A (en) * 1984-07-13 1986-02-26 Katsuhiro Okubo Method of forming a coloured hard coating
CN101462386A (en) * 2007-12-21 2009-06-24 山特维克知识产权股份有限公司 Coated cutting tool and a method of making a coated cutting tool
CN102899622A (en) * 2011-07-29 2013-01-30 鸿富锦精密工业(深圳)有限公司 Film-coated component and preparation method thereof
CN103436843A (en) * 2013-09-18 2013-12-11 佛山市伟盛利得镀膜有限公司 PVD (physical vapor deposition) composite membrane layer as well as preparation method thereof

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