CN101081557A - Metallic carbide/adamantine (MeC/DLC) nanometer multi-layer film material and method for preparing the same - Google Patents
Metallic carbide/adamantine (MeC/DLC) nanometer multi-layer film material and method for preparing the same Download PDFInfo
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- CN101081557A CN101081557A CN 200710028834 CN200710028834A CN101081557A CN 101081557 A CN101081557 A CN 101081557A CN 200710028834 CN200710028834 CN 200710028834 CN 200710028834 A CN200710028834 A CN 200710028834A CN 101081557 A CN101081557 A CN 101081557A
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title description 13
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 title 1
- 229910001573 adamantine Inorganic materials 0.000 title 1
- 229910052751 metal Inorganic materials 0.000 claims abstract description 49
- 239000002184 metal Substances 0.000 claims abstract description 49
- 230000007704 transition Effects 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 150000004767 nitrides Chemical class 0.000 claims abstract description 9
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 8
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 150000001247 metal acetylides Chemical class 0.000 claims description 13
- 239000012528 membrane Substances 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000000151 deposition Methods 0.000 abstract description 19
- 239000010408 film Substances 0.000 description 48
- 239000010410 layer Substances 0.000 description 28
- 150000002500 ions Chemical class 0.000 description 20
- 230000008021 deposition Effects 0.000 description 15
- 235000019589 hardness Nutrition 0.000 description 14
- 238000001755 magnetron sputter deposition Methods 0.000 description 12
- 239000007789 gas Substances 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 7
- 238000010884 ion-beam technique Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 1
- 229910019580 Cr Zr Inorganic materials 0.000 description 1
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 1
- 229910010037 TiAlN Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001659 ion-beam spectroscopy Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
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- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/341—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one carbide layer
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- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/343—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one DLC or an amorphous carbon based layer, the layer being doped or not
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- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
- C23C28/42—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by the composition of the alternating layers
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention is nanometer multilayer metal carbide/diamond-like film material and its preparation process. The nanometer multilayer film material includes one base material layer, one transition layer and one nanometer multilayer film layer arranged successively. The transition layer consists of one metal layer, one metal nitride layer and one metal carbonitride layer; and the nanometer multilayer film layer consists of metal carbide layers and diamond-like film layers arranged alternately. The preparation process includes: bombarding with Ti, Cr, and Zr or W targets successively to clean the base material; depositing one metal layer, one metal nitride layer and one metal carbonitride layer successively; and depositing metal carbide layers and diamond-like film layers alternately. The nanometer multilayer film material has high micro hardness, low friction coefficient and high adhesion, and may be applied in improving the surface performance of metal parts.
Description
Technical field
The present invention relates to a kind of multi-layer film material and preparation method thereof, particularly a kind of metal carbides/DLC (MeC/DLC) multi-layer film material and preparation method thereof.
Background technology
Along with the requirement of progress of science and technology and production development, nanometer new material and surface engineering technology have obtained using widely in manufacturing industry.Since the last century the eighties, adopt gas phase deposition technology to prepare TiN, TiCN, contour hard, the wear-resistant coating of TiAlN at tool and mould, component surface, can significantly improve its serviceability and life-span, obtained successful commerce and used.But these signal layer coatings still exist, and hardness is not high enough, the big weak points such as (0.4～0.8) of coefficient of friction, still can not satisfy the needs of tool and mould and parts operating mode high request in some applications.
Diamond-film-like (Diamond-like Carbon, be abbreviated as DLC) be a kind of amorphous carbon-film that contains diamond lattic structure, because it has a series of excellent properties similar to diamond film, as higher hardness, extremely low coefficient of friction, good thermal conductivity, wear-resisting, corrosion resistance, and can realize low temperature large tracts of land deposition, and be with a wide range of applications in fields such as optics, electronics, acoustics, medical science, machineries, become the focus of Recent study.DLC depositing of thin film method mainly contains ion beam, magnetron sputtering, arc ion plating etc. at present.With the DLC film of ion gun ionization hydrocarbon (as methane, acetylene gas etc.) preparation, rete exquisiteness, hardness height, but poor with basal body binding force, internal stress is big, sedimentation rate was slow after thickness surpassed 500nm, and easily peeled off.With the DLC film of magnetron sputtering (graphitic source) technology preparation, film surface is bright and clean, fine and smooth, and sedimentation rate is moderate, but film hardness is on the low side.With the DLC film of cathodic arc ion plating (graphitic source) preparation, film hardness height, sedimentation rate is fast, but there is larger particles in the bright and clean inadequately exquisiteness of film surface, and internal stress is big, is difficult to obtain to use on tool and mould and parts.These studies show that, improve the adhesion of DLC film and matrix, reduce the rete internal stress, and low temperature, the large tracts of land uniform deposition of realizing the DLC film is to realize the commercial key in application of DLC film place.
Summary of the invention
The objective of the invention is to overcome the shortcoming and defect that existing DLC membrane technology exists, a kind of MeC/DLC nanometer multilayer membrane material is provided, this multi-layer film material has higher microhardness, low coefficient of friction, firm performances such as adhesive force.
Another object of the present invention provides a kind of MeC/DLC nanometer multilayer preparation method of film material, and this method satisfies the requirement of low temperature and large-area preparation, has the production efficiency height, low cost and other advantages.
The present invention is achieved by the following technical solutions: metal carbides/DLC nanometer multilayer membrane material is made of base material 1, transition zone I and nanometer multilayer rete II successively, transition zone I is made of metal level 2, metal nitride layer 3, metal carbonitride layer 4, and nanometer multilayer rete II is made of metal carbide layer 5 that replaces and DLC layer 6.
The base material 1 of described metal carbides/DLC nanometer multilayer membrane material is iron and steel, titanium alloy or carbide alloy.
The metal of described metal carbides/DLC nanometer multilayer membrane material is Ti, Cr, Zr or W.
Metal carbides/DLC nanometer multilayer preparation method of film material is to adopt Ti, Cr, Zr or W target, at base vacuum: 5.0 * 10
-3Pa, temperature: 150 ℃, work rest rotating speed: under 2～10rpm condition, may further comprise the steps successively:
1. base material is cleaned in the ion gun bombardment: pressure: 0.2～1.0Pa in the stove, Ar throughput: 150sccm, ion gun: 2Kw, bias voltage: 50～1000V, time: 30min;
2. prepare metal level: pressure: 0.2～0.4Pa in the stove, Ar throughput: 150sccm, magnetic control power: 2.0～10Kw, ion gun: 0.5Kw, bias voltage: 50～150V, time: 5～15min;
3. prepare metal nitride layer: pressure: 0.3～0.6Pa in the stove, Ar throughput: 120～150sccm, N2:40～50sccm, magnetic control power: 5.0～10Kw, ion gun: 0.5Kw, bias voltage: 50～150V, time: 15～30min;
4. prepare metal carbonitride layer: pressure: 0.4～0.8Pa in the stove, Ar throughput: 100～150sccm, CH
4Or C
2H
2Throughput: 30～50sccm, N
2: 5～30sccm, magnetic control power: 5.0～6.0Kw, ion gun: 0.5Kw, bias voltage: 50～150V, time: 15～30min;
5. prepare metal carbides and DLC layer: pressure: 0.6～1.0Pa in the stove, Ar throughput: 100sccm, CH
4Or C
2H
2Throughput: 50～150sccm, magnetic control power: 1.0～3.0Kw, ion gun: 2Kw, bias voltage: 50～150V, time: 100～150min.
The present invention at first adopts gas ion source ionization argon gas under high bias voltage material surface to be carried out icon bombardment cleaning.The advantage that ion beam sputtering is cleaned is that the Energy Controllable scope is wide, having solved conventional glow discharge bias voltage cleans a little less than the energy, and the too high material surface that easily causes of arc ions cleaning energy " is beaten arc " and shortcomings such as " getting confused ", can keep under the enough low situation of material temperature, thoroughly remove surface impurity foreign matter layer.Polished surface improves the material surface microroughness simultaneously, significantly improves the interface binding power of subsequent film and matrix material.
Transition zone of the present invention has comprised the metal level Me of adhesive attraction, plays the metal nitride layer MeN and the metal carbonitride layer MeCN of hardness gradient transitional function.Depositing metal layers adopts Cr, Ti, Zr etc., is because the adhesion of materials such as they and iron and steel, titanium alloy, carbide alloy is good; Plated metal nitride layer TiN, CrN, ZrN etc. and metal carbonitride layer TiCN, CrCN, ZrCN etc. are in order to set up the hardness gradient transition between base material and MeC/DLC multilayer film, to reduce the rete internal stress, improving the toughness of film/basic adhesion and rete.
MeC/DLC nano-multilayer film of the present invention is to have utilized magnetron sputtering technique and the ion beam technology in the physical vapour deposition (PVD) respectively, utilize rectangle gas ion source ionization hydrocarbon (methane, acetylene etc.) preparation DLC film, under carbon-containing atmosphere, open the magnetron sputtering metallic target simultaneously and prepare the MeC film, before making base material rest on ion gun and magnetic controlled sputtering target successively by workpiece rotation, alternating deposit goes out the MeC film and the DLC film of nanoscale, alternately is formed by stacking to several thousand MeC and DLC by hundreds of.Control thickness in monolayer and modulation period in the MeC/DLC multilayer film by control gas flow, workpiece rotational frequency, ion gun and magnetic control target power, MeC film thickness in monolayer is 1～5nm, and DLC film thickness in monolayer is 2～10nm.Nanometer size effect by means of material, it is big that the MeC/DLC nano-multilayer film that obtains has overcome individual layer DLC film internal stress, is difficult in the thicker shortcoming of material surface deposition, and its hardness is higher, film/basic adhesion is good, and impact resistance, mar proof all have significantly raising than individual layer DLC film.
Fig. 1 is a MeC/DLC nano-multilayer film structural representation of the present invention.Base material 1 among the figure; Transition zone I comprises metal level 2, metal nitride layer 3, metal carbonitride layer 4; Metal carbides/DLC multilayer film II comprise metal carbide layer 5 and DLC layer 6.
The specific embodiment
Adopt double T i target, gas is high-purity Ar, N
2And CH
4, base material is a Cr12MoV mould steel.
Operate successively by listed technological process of table 1 and parameter.The thickness of magnetron sputtering deposition transition zone Ti/TiN/TiCN is respectively 0.2,0.4,0.3 μ m; The TiC monofilm thickness of magnetron sputtering and ion beam alternating deposit is 1nm, and the DLC monofilm thickness is 3nm, and multilayer film thickness is 3.0 μ m.The rete gross thickness is 3.9 μ m, and hardness number is HV2500, and film/basic adhesion is 60N, and the coefficient of friction of rete is 0.12.
Table 1 embodiment 1 concrete technological process table
| Step | Base vacuum: 5.0 * 10 -3Pa, temperature: 150 ℃, work rest rotating speed: 5rpm | |||||||||
| Pressure (Pa) in the stove | Throughput (sccm) | Magnetic control power (Kw) | Ion gun (Kw) | Bias voltage (V) | Time (min) | |||||
| Ar | N 2 | CH 4 | Ti | |||||||
| The ion gun bombardment | 0.2 | 150 | 2 | 1000 | 30 | |||||
| The rete deposition | Transition zone | Ti | 0.3 | 150 | 10 | 0.5 | 100 | 10 | ||
| TiN | 0.4 | 120 | 50 | 10 | 0.5 | 100 | 20 | |||
| TiCN | 0.6 | 100 | 15 | 30 | 6 | 0.5 | 100 | 20 | ||
| Alternating layer | TiC/ DLC | 0.8 | 100 | 150 | 3 | 2 | 100 | 150 | ||
Adopt two Cr targets, gas is high-purity Ar, N
2And C
2H
2, base material is the Ti6Al4V titanium alloy.
Operate successively by listed technological process of table 2 and parameter.Magnetron sputtering deposition transition zone Cr/CrN/CrCN, thickness are respectively 0.1,0.3,0.3 μ m; Magnetron sputtering and ion beam alternating deposit multilayer film CrC/DLC, the CrC monofilm thickness of deposition is 1nm, and the DLC monofilm thickness is 2nm, and multilayer film thickness is 2.4 μ m.The rete gross thickness is 3.1 μ m, and hardness number is HV2700, and film/basic adhesion is 80N, and the coefficient of friction of rete is 0.1.
Table 2 embodiment 2 concrete technological process tables
| Step | Base vacuum: 5.0 * 10 -3Pa, temperature: 150 ℃, work rest rotating speed: 8rpm | |||||||||
| Pressure (Pa) in the stove | Throughput (sccm) | Magnetic control power (Kw) | Ion gun (Kw) | Bias voltage (V) | Time (min) | |||||
| Ar | N 2 | C 2H 2 | Cr | |||||||
| The ion gun bombardment | 0.5 | 150 | 2 | 1000 | 30 | |||||
| The rete deposition | Transition zone | Cr | 0.4 | 150 | 6 | 0.5 | 100 | 5 | ||
| CrN | 0.6 | 140 | 50 | 6 | 0.5 | 100 | 15 | |||
| CrCN | 0.6 | 120 | 20 | 30 | 6 | 0.5 | 100 | 20 | ||
| Alternating layer | CrC/ DLC | 0.6 | 100 | 100 | 2 | 2 | 100 | 100 | ||
Adopt Cr and W target, gas is high-purity Ar, N
2And C
2H
2, base material is a YT 5 carbide.
Operate successively by listed technological process of table 3 and parameter.Magnetron sputtering deposition transition zone Cr/CrN/CrCN, thickness are respectively 0.2,0.3,0.3 μ m; Magnetron sputtering and ion beam alternating deposit multilayer film WC/DLC, the WC monofilm thickness of deposition is 1.5nm, and the DLC monofilm thickness is 3nm, and multilayer film thickness is 2.7 μ m.The rete gross thickness is 3.5 μ m, and hardness number is HV4300, and film/basic adhesion is 65N, and the coefficient of friction of rete is 0.12.
Table 3 embodiment 3 concrete technological process tables
| Step | Base vacuum: 5.0 * 10 -3Pa, temperature: 150 ℃, work rest rotating speed: 4rpm | ||||||||||
| Pressure (Pa) in the stove | Throughput (sccm) | Magnetic control power (Kw) | Ion gun (Kw) | Bias voltage (V) | Time (min) | ||||||
| Ar | N 2 | C 2H 2 | Cr | W | |||||||
| The ion gun bombardment | 0.7 | 150 | 2 | 1000 | 30 | ||||||
| The rete deposition | Transition zone | Cr | 0.2 | 150 | 5 | 0.5 | 100 | 15 | |||
| CrN | 0.4 | 150 | 50 | 5 | 0.5 | 100 | 25 | ||||
| CrCN | 0.6 | 120 | 20 | 30 | 6 | 0.5 | 100 | 20 | |||
| Alternating layer | WC/ DLC | 0.9 | 100 | 60 | 1 | 2 | 100 | 150 | |||
Adopt Cr and Zr target, gas is high-purity Ar, N
2And CH
4, base material is the YG6 carbide alloy.
Operate successively by listed technological process of table 4 and parameter.Magnetron sputtering deposition transition zone Cr/ZrN/ZrCN, thickness are respectively 0.1,0.3,0.2 μ m; Magnetron sputtering and ion beam alternating deposit multilayer film ZrC/DLC, the ZrC monofilm thickness of deposition is 2nm, and the DLC monofilm thickness is 3nm, and multilayer film thickness is 2.5 μ m.The rete gross thickness is 3.1 μ m, and hardness number is HV2400, and film/basic adhesion is 65N, and the coefficient of friction of rete is 0.14.
Table 4 embodiment 4 concrete technological process tables
| Step | Base vacuum: 5.0 * 10 -3Pa, temperature: 150 ℃, work rest rotating speed: 5rpm | ||||||||||
| Pressure (Pa) in the stove | Throughput (sccm) | Magnetic control power (Kw) | Ion gun (Kw) | Bias voltage (V) | Time (min) | ||||||
| Ar | N 2 | CH 4 | Cr | Zr | |||||||
| The ion gun bombardment | 0.6 | 150 | 2 | 1000 | 30 | ||||||
| The rete deposition | Transition zone | Cr | 0.2 | 150 | 5 | 0.5 | 100 | 8 | |||
| ZrN | 0.45 | 150 | 40 | 5 | 0.5 | 100 | 30 | ||||
| ZrCN | 0.6 | 150 | 5 | 25 | 5 | 0.5 | 100 | 30 | |||
| Alternating layer | ZrC/ DLC | 0.8 | 100 | 100 | 2.5 | 2 | 100 | 100 | |||
Annotate: 1. thicknesses of layers adopts the cross section metallographic method to measure;
2. film hardness adopts micro Vickers to measure: load 10g, 15 seconds load times, survey three point hardnesses and average;
3. film/basic adhesion adopts film bond strength scratch test instrument to measure: loading velocity is 100N/min, and the speed of paddling is 4mm/min, and the time of paddling is 1 minute;
4. the rete coefficient of friction adopts ball-disc type friction wear testing machine to measure, and is GCr15 to mill part material, and linear velocity is 0.5m/s, and load is 0.98N.
The microhardness of MeC/DLC nanometer multilayer membrane material provided by the invention is higher, reach HV2000～4500, coefficient of friction is low to moderate 0.05～0.25, adhesive force 〉=60N, has good performance, and (D600mm * 600mm) preparation has the production efficiency height, low cost and other advantages to be easy to low temperature and large tracts of land.The surface property of metal material tool and mould, parts be can significantly improve, its service life and machining accuracy improved.
Claims (4)
1, a kind of metal carbides/DLC nanometer multilayer membrane material, it is characterized in that constituting by base material (1), transition zone I and nanometer multilayer rete II according to this, transition zone I is made of metal level (2), metal nitride layer (3), metal carbonitride layer (4), and nanometer multilayer rete II is made of metal carbide layer that replaces (5) and DLC layer (6).
2, metal carbides according to claim 1/DLC nanometer multilayer membrane material is characterized in that described base material (1) is iron and steel, titanium alloy or carbide alloy.
3, metal carbides according to claim 1/DLC nanometer multilayer membrane material is characterized in that described metal is Ti, Cr, Zr or W.
4, the described metal carbides of a kind of claim 1/DLC nanometer multilayer preparation method of film material is characterized in that adopting Ti, Cr, Zr or W target, at base vacuum: 5.0 * 10
-3Pa, temperature: 150 ℃, work rest rotating speed: under 2～10rpm condition, may further comprise the steps successively:
1. base material is cleaned in the ion gun bombardment: pressure: 0.2～1.0Pa in the stove, Ar throughput: 150sccm, ion gun: 2Kw, bias voltage: 50～1000V, time: 30min;
2. prepare metal level: pressure: 0.2～0.4Pa in the stove, Ar throughput: 150sccm, magnetic control power: 2.0～10Kw, ion gun: 0.5Kw, bias voltage: 50～150V, time: 5～15min;
3. prepare metal nitride layer: pressure: 0.3～0.6Pa in the stove, Ar throughput: 120～150sccm, N
2: 40～50sccm, magnetic control power: 5.0～10Kw, ion gun: 0.5Kw, bias voltage: 50～150V, time: 15～30min;
4. prepare metal carbonitride layer: pressure: 0.4～0.8Pa in the stove, Ar throughput: 100～150sccm, CH
4Or C
2H
2Throughput: 30～50sccm, N
2: 5～30sccm, magnetic control power: 5.0～6.0Kw, ion gun: 0.5Kw, bias voltage: 50～150V, time: 15～30min;
5. prepare metal carbides and DLC layer: pressure: 0.6～1.0Pa in the stove, Ar throughput: 100sccm, CH
4Or C
2H
2Throughput: 50～150sccm, magnetic control power: 1.0～3.0Kw, ion gun: 2Kw, bias voltage: 50～150V, time: 100～150min.
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| CN100506527C CN100506527C (en) | 2009-07-01 |
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