CN108707868B - Vacuum ion plating Ag nano composite coating fastener and preparation method thereof - Google Patents
Vacuum ion plating Ag nano composite coating fastener and preparation method thereof Download PDFInfo
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- 238000007733 ion plating Methods 0.000 title claims abstract description 30
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 28
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 65
- 229910052709 silver Inorganic materials 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000010410 layer Substances 0.000 claims description 155
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- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 19
- 239000002131 composite material Substances 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 10
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- 238000001020 plasma etching Methods 0.000 claims description 8
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- 238000001816 cooling Methods 0.000 claims description 7
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 47
- 239000004332 silver Substances 0.000 abstract description 47
- 238000007747 plating Methods 0.000 abstract description 37
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- MXZVHYUSLJAVOE-UHFFFAOYSA-N gold(3+);tricyanide Chemical compound [Au+3].N#[C-].N#[C-].N#[C-] MXZVHYUSLJAVOE-UHFFFAOYSA-N 0.000 description 1
- 229920006262 high density polyethylene film Polymers 0.000 description 1
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- HKSGQTYSSZOJOA-UHFFFAOYSA-N potassium argentocyanide Chemical compound [K+].[Ag+].N#[C-].N#[C-] HKSGQTYSSZOJOA-UHFFFAOYSA-N 0.000 description 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 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
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- 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
- C23C14/06—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
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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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
- 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
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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
- 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
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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
- C23C28/02—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 only coatings only including layers of metallic material
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
- F16B1/00—Devices for securing together, or preventing relative movement between, constructional elements or machine parts
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Abstract
The invention provides a vacuum ion plating Ag nano composite coating fastener and a preparation method thereof, aiming at the defects of pollution and poor performance of the silver high-temperature self-lubricating coating of the fastener, the invention develops a silver nano composite coating material and a preparation method thereof by combining an arc ion plating technology and a magnetron sputtering technology and adopting an advanced ion etching auxiliary process so as to solve the problems of silver plating pollution and poor performance of the fastener. Developing a fastener Ag nano composite coating material and a preparation technology. The invention belongs to the field of new material technology research and preparation.
Description
Technical Field
The invention relates to a fastener with a vacuum ion plating Ag nano composite coating and a preparation method thereof, belonging to the technical field of new materials.
Background
High strength fasteners used in aerospace and other specialty applications are typically made from stainless steel, titanium alloys, and superalloys, and require not only superior wear resistance, but also good lubrication and corrosion resistance on their surfaces. The silver and the silver-based coating have good lubricating property in high-low temperature and vacuum environment, and are widely applied coating materials in fasteners. Silver plating includes electroplating, electroless plating, vapor deposition, and the like, and among them, electroplating is most widely used. The first patent to silver plating was proposed in 1838 by Elkington brother of birmingham, england, and the plating solution used was an alkaline cyanide plating solution, much like the alkaline cyanide gold plating system they invented. For over a century, the basic formulation of the silver plating solution is not much different from the original formulation, and only the concentration of silver complex ions is increased to achieve the purpose of rapid silver plating. Silver coatings were first applied for decoration inIn the electronic industry, the communication equipment and the instrument manufacturing industry, silver plating is used for reducing the contact resistance of the surface of metal parts and improving the welding capacity of the metal. Among various plating solution systems, the cyanogen plating solution is widely applied, the main defect in the past is that the used current density is small, and the current density can reach 10A/dm by efficiently plating silver at present2. The bright silver plating is generally 1.5-3A/dm2The plating surface is smooth without polishing, and can also be plated thickly. In recent years, high-speed selective silver plating of electronic components, such as selective silver plating of lead frames, has been rapidly developed, and a spray plating method is adopted. The current density used is as high as 300-3000A/dm2The concentration of the silver potassium cyanide in the plating solution is also as high as 40-75 g/L, and the anode adopts a platinum or platinized titanium anode, so that a silver layer with the thickness of about 4-5 mu m can be plated within 1s, and the silver layer can meet the requirement of bonding between a silicon chip and a silver soldering pad by using an aluminum wire. The industries of electric appliances, instruments and the like also adopt cyanide-free silver plating. Thiosulfate, sulfite, thiocyanate, ferrocyanide, and the like are used for the plating solution. In order to prevent the silver plating from discoloring, it is usually subjected to post-plating treatments, mainly brightening, chemical and electrochemical passivation, plating with noble or rare metals or coating with capping layers, etc.
Compared with electroplating, chemical silver plating has the advantages of simple process, suitability for irregular matrix materials, lower cost and the like; the chemical plating layer has the performances of high density, uniform thickness, good corrosion resistance, good wear resistance and the like. In addition to conventional work piece processing, in recent years, there has been some progress in electroless silver plating of powder surfaces. The composite powder with silver-plated surface has wide application, such as: the silver plating on the surface of the copper powder can be used as electronic slurry, electrode material, catalyst, electromagnetic shielding material and the like; silver plating on the surface of hollow or solid microspheres (glass or ceramic) can be used as thick film circuit materials, capacitors, gaskets and sealing materials; the microcapsule surface made of the high-density polyethylene film is plated with silver, and the microcapsule can be used as a balloon electrode and the like for clinical interventional therapy. At present, many workers are engaged in the research of electroless silver plating, and are continuously exploring the preparation of excellent electroless plating layers by adopting simple processes and low cost. The inner container of the daily used hot water kettle is treated by chemical silvering. Because the silver plating layer is bright and reflective, the infrared radiation generated by heat can be well reflected back, so that a better heat preservation effect is achieved. Therefore, the silvered hot water kettle has better heat preservation effect.
The PVD ion plating technology is a hot technology of domestic and foreign research in the last two decades, and various prepared coatings have the defects of high hardness, good adhesive force, good substrate adaptability, no pollution and the like, are successfully applied to the field of parts, and are the fields with the most active development of surface treatment technology. The PVD coating techniques for silver and silver-based coatings include evaporation, sputtering, ion plating, and the like. The most common method for vacuum evaporation silver plating is resistance heating, which has the advantages of simple structure of the heating source, low cost and convenient operation; the disadvantages of resistance heating can be overcome by electron beam heating and laser heating silver plating. In electron beam heating, the bombarded material is directly heated by using a focused electron beam, and the kinetic energy of the electron beam is changed into heat energy to evaporate the material. Laser heating utilizes high-power laser as a heating source, but because of high-power electron beam evaporation and high manufacturing cost of the laser, the laser can only be used in a few research laboratories at present. The most obvious advantage of evaporation silver plating is that the deposition rate is fast, and the preparation of silver coating with dozens of microns and hundreds of microns is easy to realize. However, the disadvantage is that the uniformity is poor, a uniform coating cannot be obtained on a workpiece with a complex shape, and the adhesion is poor due to mechanical bonding. With the further development of the PVD coating technology, the bonding strength between the coating and the substrate is further improved, and the preparation of the silver coating with high adhesion on the surface of the fastener by using the PVD coating technology is the first choice of the surface coating technology of the parts.
Because of the contact and deformation of the fastener during use, the coating adhesion is highly required compared with that of a common workpiece. The magnetron sputtering technique in the PVD coating technique can provide good surface quality but cannot improve the adhesion of the surface coating well. Arc ion plating can provide better adhesion, but the corrosion resistance of the coating is problematic due to greater particle contamination. Therefore, the method comprehensively utilizes the advantages of the arc ion plating and magnetron sputtering technology to deposit the silver coating on the surface of the fastener, and has better application prospect. .
Disclosure of Invention
The invention aims to: aiming at the defects of pollution and poor performance of the silver high-temperature self-lubricating coating of the fastener, the silver nano composite coating material and the preparation method thereof are developed by combining an arc ion plating technology and a magnetron sputtering technology and adopting an advanced ion etching auxiliary process so as to solve the problems of silver plating pollution and poor performance of the fastener. Developing a fastener Ag nano composite coating material and a preparation technology.
In order to solve the problems, the fastener with the vacuum ion plating Ag nano composite coating is adopted, the surface of the fastener is provided with the Ag nano composite coating, the Ag nano composite coating is of a gradient layer structure and consists of a diffusion layer, a binding layer, a transition layer and an Ag high-temperature self-lubricating composite coating, the diffusion layer is a pure Ti diffusion layer prepared by adopting an arc ion plating method through high-energy bombardment, the binding layer is a pure Ti layer prepared by adopting an ion plating method through low energy, the transition layer is a Ti-Ag nano multilayer film formed by Ti evaporated by the arc ion plating method and Ag prepared under the high-voltage condition of an intermediate frequency magnetron sputtering method, and the self-lubricating layer is an Ag nano composite coating prepared by an intermediate frequency methodIAnd Ag prepared by direct current magnetron sputtering methodIIFormed of AgI/AgIIA nano-multilayer film.
The Ti-Ag transition layer coating is of a nano multilayer structure formed by alternately forming Ti and Ag, the thickness of a single-layer Ti layer is 3-20 nanometers, the thickness of a single-layer Ag layer is 5-20 nanometers, and the thickness range of a modulation period formed by the two coatings is 8-40 nanometers;
AgI/AgIIthe nano multilayer film is Ag formed by medium-frequency magnetron sputteringIAnd Ag formed by DC magnetron sputteringIINano-alternating coating of layers, single layer of AgIThe thickness of the layer is 5-30 nm, and the layer is AgIIThe thickness of the layer is 10-50 nm, and the thickness range of the modulation period formed by the two coatings is 15-80 nm;
the thickness of the diffusion layer is 5-10 nanometers, the thickness of the bonding layer is 20-200 nanometers, the thickness of the transition layer is 100-200 nanometers, and the thickness of the high-temperature self-lubricating coating is 1-10 micrometers;
the invention also provides a preparation method of the vacuum ion plating Ag nano composite coating fastener, which comprises the following steps:
after the alloy steel fastener is subjected to plasma etching at the temperature of 100-450 ℃ in the argon and hydrogen environment, carrying out arc discharge on a target 2 in the argon environment by adopting an electric arc of a circular vacuum furnace, and preparing a 2-10 nanometer Ti diffusion layer under the conditions of 0.02-0.2Pa, minus 800V and minus 1000V; then, preparing a 20-200 nanometer Ti bonding layer by adopting medium-frequency magnetron sputtering under the conditions of 0.4-1Pa, 50V to 500V on the target 8 in an argon environment; after the preparation of the bonding layer is finished, under the condition of 0.4-1Pa, -50V to-200V, the intermediate frequency magnetron sputtering is adopted to prepare a 100-plus-200 nanometer Ti-Ag nanometer composite metal transition layer for the target 8 and the first direct current magnetron sputtering is adopted to prepare a target 4, the thickness of the single-layer Ti layer is 3-20 nanometers, the thickness of the single-layer Ag layer is 5-20 nanometers, and the thickness range of a modulation period formed by the two coatings is 8-40 nanometers; after the preparation of the transition layer is finished, carrying out 1-10 micron Ag in an argon environment at 0.4-1Pa by adopting a medium-frequency magnetron sputtering target 8, a first direct-current magnetron sputtering target 4 and a second direct-current magnetron sputtering target 5 under the condition of-50V to-250VI/AgIIPreparation of nano multilayer high-temperature self-lubricating coating, single-layer AgIThe thickness of the layer is 5-30 nm, and the layer is AgIIThe thickness of the layer is 10-50 nanometers, the modulation period thickness range formed by the two coatings is 15-80 nanometers, the total thickness of the coatings is controlled to be 1.125-10.41 micrometers, and the Ti-Ag nano composite metal coating fastener is obtained after the preparation is finished and natural cooling is carried out.
The invention adopts an ion source etching technology to clean oxides shown by a fastener, wherein the atmosphere adopts a mixed gas of argon and hydrogen, the argon mainly provides heavier argon ion etching, and the hydrogen mainly aims at damaging a high polymer material with poorer argon ion cleaning to achieve the purpose of cleaning. The purpose of adopting medium-frequency magnetron sputtering is mainly to improve the ionization rate and the density of the coating. The direct current magnetron sputtering is mainly used for improving the deposition rate. The vacuum ion silver plating technology belongs to a completely environment-friendly technology, so that the environment is not polluted, the pollution caused by silver plating is greatly reduced, and the vacuum ion silver plating technology has good social and economic benefits.
Compared with the prior art, the invention also has the following advantages:
1. compared with the common glow discharge ion source, the arc discharge ion source is adopted for ion cleaning before coating, the surface quality of the surface of the fastener can be greatly improved, the adhesive force of the coating is improved, the non-cleaning adhesive force is generally lower than 30N, and the cleaning adhesive force can reach 60N;
2. the coating structure adopts a multilayer structure, and is provided with a diffusion layer, a bonding layer, a transition layer and a self-lubricating layer, so that the structure and the components are gradually changed, and the coating and the substrate are metallurgically bonded and have good adhesive force;
3. compared with the conventional arc ion plating coating structure, the invention adopts the multilayer structure technology to inhibit the growth of columnar crystals and improve the density of the coating, thereby not only improving the corrosion resistance of the coating, but also greatly improving the toughness;
4. the transition layer adopts a thicker Ti metal layer, so that the bonding effect is better, and the stress of the coating is reduced;
5. due to the adoption of a multilayer structure, the invention can prepare thicker coatings;
6. the invention combines the Ti layer and the Ag layer to form a multilayer structure which is a multilayer nano-structure material, is an attempt at home and abroad, is particularly applied to the surface of a fastener, and can greatly improve the self-lubricating and corrosion-resistant properties of the fastener; meanwhile, the coating equipment has simple structure, easy control and good industrial application prospect.
Drawings
FIG. 1 is a schematic view of a coating apparatus (circular vacuum furnace) used in the present invention;
FIG. 2 is a schematic view of a coating structure designed according to the present invention;
the reference numerals have the following meanings, 1. a vacuum chamber door; (cylindrical) arc-to-target; 3. an ion source; 4. a first direct current magnetron sputtering target pair; 5. a second direct current magnetron sputtering target pair; 6. an air extraction opening; 7. a fastener; 8. the method comprises the following steps of medium-frequency magnetron sputtering target alignment, 9 auxiliary anode, 10 vacuum furnace wall, 11 heating pipe, a substrate, b.Ti diffusion layer, c.Ti bonding layer, d.Ti/Ag nano multilayer transition layer and e.AgI/AgIIA nano-multilayer self-lubricating layer.
Detailed Description
To make the objects, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail with reference to the accompanying drawings, and it should be understood that the specific embodiments described herein are only for explaining the present invention and are not intended to limit the present invention.
Example 1:
referring to fig. 1 and 2, the present embodiment provides a vacuum ion-plated Ag nanocomposite coating fastener, wherein the vacuum ion-plated Ag nanocomposite coating adopts a gradient layer structure and is composed of a diffusion layer, a bonding layer, a transition layer and an Ag high-temperature self-lubricating composite coating. 5-10 nanometers of diffusion layer, 20-200 nanometers of bonding layer thickness, 100-200 nanometers of transition layer thickness and 1-10 micrometers of high-temperature self-lubricating coating thickness. The diffusion layer is a pure Ti diffusion layer prepared by adopting an electric arc ion plating method through high-energy bombardment, the bonding layer is a pure Ti layer prepared by adopting an ion plating method through low energy, the transition layer is a Ti-Ag nano multilayer film formed by Ti evaporated by the electric arc ion plating method and Ag prepared under the condition of high voltage by a medium-frequency magnetron sputtering method, the thickness of the single-layer Ti layer is 3-20 nanometers, the thickness of the single-layer Ag layer is 5-20 nanometers, and the thickness range of a modulation period formed by the two coatings is 8-40 nanometers. The self-lubricating layer is Ag prepared by a medium-frequency methodIAnd Ag prepared by direct current magnetron sputtering methodIIFormed of AgI/AgIIA nano-multilayer film. Single layer of AgIThe thickness of the layer is 5-30 nm, and the layer is AgIIThe thickness of the layer is 10-50 nm, and the thickness of the modulation period formed by the two coatings is 15-80 nm.
The vacuum ion plating Ag nano composite metal coating fastener and the preparation method thereof are characterized in that after the alloy steel fastener is subjected to plasma etching at the temperature of 100-450 ℃ in the argon and hydrogen environment, arc discharge is carried out on a target 2 in the argon environment by adopting electric arc, and the preparation of a 2-10 nano Ti diffusion layer is carried out under the condition of 0.02-0.2Pa, minus 800V and minus 1000V; then preparing a 20-200 nanometer Ti bonding layer by adopting a target 8 under the condition of 0.4-1Pa, 50V to 500V in an argon atmosphere; after the preparation of the bonding layer is finished, the thickness is from 0.4 to 1Pa, from-50V to-Under the condition of 200V, preparing a 100-200 nanometer Ti-Ag nanometer composite metal transition layer for the target 8 by adopting medium-frequency magnetron sputtering and the target 4 by adopting first direct-current magnetron sputtering, wherein the thickness of a single-layer Ti layer is 3-20 nanometers, the thickness of a single-layer Ag layer is 5-20 nanometers, and the thickness range of a modulation period formed by the two coatings is 8-40 nanometers; after the preparation of the transition layer is finished, carrying out 1-10 micron Ag in an argon environment under the conditions of-50V to-250V on the target 8 by adopting medium-frequency magnetron sputtering and the target 4 by adopting first direct-current magnetron sputtering at 0.4-1PaI/AgIIPreparation of nano multilayer high-temperature self-lubricating coating, single-layer AgIThe thickness of the layer is 5-30 nm, and the layer is AgIIThe thickness of the layer is 10-50 nanometers, the thickness range of the modulation period formed by the two coatings is 15-80 nanometers, the total thickness of the coatings is controlled to be 1.125-10.41 micrometers, and the Ti-Ag nano composite metal coating fastener is obtained after the preparation is finished and natural cooling is carried out.
According to the technical scheme, the Ag nano multilayer composite coating material is prepared by utilizing the high ionization rate of arc ion plating and the high density characteristic of medium-frequency magnetron sputtering. In order to improve the adhesion of Ag coatings and fasteners, the method first utilizes high concentration argon ions and hydrogen ions generated in the arc discharge process to etch the surface oxide of the fastener, generally because the oxide can reduce the bonding force of the coating and a substrate, and therefore the removal of the oxide is a very critical technology in the coating. Conventional chemical cleaning removes the oxide layer during cleaning, but the oxide layer forms on the surface quickly after air contact. The conventional glow discharge ion source has low output power, and the surface oxide can be removed by adopting the conventional glow discharge cleaning method, but the cleaning effect is limited due to low density of discharge plasma. The cleaning effect on the surface of the workpiece is limited, and in order to improve the cleaning efficiency of the surface of the workpiece, the arc discharge plasma source used in the patent can greatly improve the cleaning efficiency of the fastener. The test proves that the adhesive force of the coating and the substrate can be greatly improved.
The equipment used in the invention is a circular vacuum furnace with the diameter of 1.2 meters and the height of 1.5 meters. The external molecular pump system of extraction opening 6 is bled to the vacuum furnace, and equipment heats through heating pipe 11, control the interior temperature of stove.The furnace body is provided with a pair of medium-frequency magnetron sputtering targets 8, the medium-frequency magnetron sputtering targets 8 are oppositely distributed and driven by a 40kW alternating current power supply to carry out alternating current glow discharge evaporation; the arc target pair 2 (arc discharge target pair) is two targets which are oppositely arranged and are respectively driven by two direct current power supplies to carry out arc discharge evaporation; the first direct current magnetron sputtering target 4 and the second direct current magnetron sputtering target 5 are driven by 4 independent direct current power supplies to carry out glow discharge sputtering, and the power of each direct current power supply is 40 Kw; the furnace door is provided with the ion source 3 (ion etching source), the ion source 3 is driven by a direct current arc power supply, when arc discharge occurs, strong plasma is generated between the target and the auxiliary anode 9, so that an oxide layer and pollutants on the surface of a workpiece are cleaned, the adhesive force of the coating can be improved, when the workpiece is coated, the workpiece is completely immersed in the plasma, the ion bombardment effect is very obvious, and the uniformity of the coating is well ensured. Plasma etching is typically performed at a negative bias of 800 to 1000V with a cleaning time of 30-60 minutes. After ion etching is finished, the surface of a fastener base body is in a relatively clean state, Ti ions are evaporated at high temperature from an electric arc pair target 2 by adopting an electric arc ion plating technology and are diffused to the surface of the fastener at high speed under the action of high bias voltage, negative high voltage of 800 plus 1200V is added on the surface of the fastener, the high voltage has an accelerating action on the ionized Ti ions, the accelerated Ti ions can impact the surface of the fastener at high speed to form a Ti metallurgical diffusion layer, then the bias voltage is reduced, the air pressure is increased, 20-200 nm Ti bonding layer preparation is carried out under the condition of 0.4-1Pa, -50V to-500V, after the bonding layer preparation is finished, a medium-frequency magnetron sputtering pair target 8 is started, the Ti subjected to electric arc ion plating and Ag sputtered from the medium-frequency magnetron sputtering pair target 8 form a nano multilayer film, and the purpose of the transition layer is to improve the bonding force of a surface silver coating and, after the transition layer is finished, keeping the medium-frequency magnetron sputtering target pair 8 on, closing the electric arc target pair 2, starting the first pair of direct-current magnetron sputtering targets 4 and the second pair of direct-current magnetron sputtering targets 5, and depositing AgI/AgIINano multilayer high temperature self-lubricating coating of AgISilver layer, Ag, prepared for medium frequency magnetron targetsIIThe ionization rate of the intermediate frequency magnetic control target and the direct current magnetic control target has larger difference for the silver layer prepared for the direct current magnetic control targetIn addition, the deposited silver coating has different structures, and the grain sizes of the two silver layers have certain difference, so that a multilayer film can be formed, and the compactness of the coating is greatly improved.
Example 2: performing plasma etching on the alloy steel fastener under the environment of 100 ℃, argon and hydrogen, performing arc discharge on a target 2 in the argon environment by adopting an electric arc, and preparing a nano Ti diffusion layer under the conditions of 0.02Pa and-800V; then, preparing a 20-nanometer Ti bonding layer on the target 8 under the conditions of 0.4Pa and 50V by adopting medium-frequency magnetron sputtering in an argon environment; after the preparation of the bonding layer is finished, under the conditions of 0.4Pa and-50V, the preparation of a 100-nanometer Ti-Ag nanometer composite metal transition layer is carried out on a target 8 by adopting medium-frequency magnetron sputtering and a target 4 by adopting first direct-current magnetron sputtering, the thickness of a single-layer Ti layer is 3 nanometers, the thickness of a single-layer Ag layer is 5 nanometers, and the thickness range of a modulation period formed by the two coatings is 8 nanometers; after the preparation of the transition layer is finished, carrying out 1 micron Ag on a target 8 by adopting medium-frequency magnetron sputtering, a target 4 by adopting first direct-current magnetron sputtering and a target 5 by adopting second direct-current magnetron sputtering under the condition of-50V in an argon environment at 0.4PaI/AgIIPreparation of nano multilayer high-temperature self-lubricating coating, single-layer AgIThe thickness of the layer is 5 nm, single layer of AgIIThe thickness of the layer was 10 nm and the modulation period formed by both coatings ranged in thickness from 15 nm. And controlling the total thickness of the coating to be 1.125 micrometers, and naturally cooling after the preparation is finished to obtain the Ag nano composite metal coating fastener.
Example 3: performing plasma etching on the alloy steel fastener at the temperature of 450 ℃ in an argon and hydrogen environment, performing arc discharge on a target 2 in the argon environment by adopting an electric arc, and preparing a 10-nanometer Ti diffusion layer under the conditions of 0.2Pa and-1000V; then preparing a 200-nanometer Ti bonding layer under the conditions of 1Pa to-500V by adopting a target 8 in an argon atmosphere; after the preparation of the bonding layer is finished, under the conditions of 1Pa and-200V, preparing a 200-nanometer Ti-Ag nanometer composite metal transition layer on a target 2 by adopting electric arc pair and a first direct current magnetron sputtering pair 4, wherein the thickness of a single-layer Ti layer is 20 nanometers, the thickness of a single-layer Ag layer is 20 nanometers, and the thickness range of a modulation period formed by the two coatings is 40 nanometers; after the preparation of the transition layer is finished, at 1Pa, medium-frequency magnetism is adoptedThe controlled sputtering target 8, the first direct current magnetron sputtering target 4 and the second direct current magnetron sputtering target 5 are subjected to 10 microns of Ag in an argon environment under the condition of-250VI/AgIIPreparation of nano multilayer high-temperature self-lubricating coating, single-layer AgIThe thickness of the layer is 30 nm, and the layer is AgIIThe thickness of the layer was 50 nm and the modulation period formed by both coatings ranged in thickness from 80 nm. The total thickness is controlled to be 10.41 microns, and the fastener with the Ti-Ag nano composite metal coating is obtained after the preparation is finished and the natural cooling is carried out. .
Example 4: performing plasma etching on the alloy steel fastener at 350 ℃ in an argon and hydrogen environment, performing arc discharge on a target 2 in the argon environment by adopting an electric arc, and preparing a 5-nanometer Ti diffusion layer under the conditions of 0.1Pa and-800V; then preparing a 100-nanometer Ti bonding layer under the conditions of 1Pa and-50V by adopting a target 8 in an argon atmosphere; after the preparation of the bonding layer is finished, under the conditions of 0.4Pa and-200V, the electric arc is adopted to carry out the preparation of a 150-nanometer Ti-Ag nanometer composite metal transition layer on the target 2 and the medium frequency magnetron sputtering is adopted to carry out the preparation of a target 8, the thickness of a single-layer Ti layer is 10 nanometers, the thickness of a single-layer Ag layer is 10 nanometers, and the thickness range of a modulation period formed by the two coatings is 20 nanometers; after the preparation of the transition layer is finished, carrying out 5-micron Ag in an argon atmosphere at 0.4Pa by adopting a medium-frequency magnetron sputtering target 8, a first direct-current magnetron sputtering target 4 and a second direct-current magnetron sputtering target 5I/AgIIPreparation of nano multilayer high-temperature self-lubricating coating, single-layer AgIThe thickness of the layer is 10 nm, single layer of AgIIThe thickness of the layer is 10 nanometers, the modulation period thickness range formed by the two coatings is 20 nanometers, the total thickness of the coatings is controlled to be 5.255 micrometers, and the Ti-Ag nano composite metal coating fastener is obtained after the preparation is finished and natural cooling is carried out.
Example 5: performing plasma etching on the alloy steel fastener at 300 ℃ in an argon and hydrogen environment, performing arc discharge on a target 2 in the argon environment by adopting an electric arc, and preparing a 10-nanometer Ti diffusion layer under the conditions of 0.2Pa and-1000V; then, preparing a 200-nanometer Ti bonding layer on the target 8 under the condition of 0.4a to 50V by adopting medium-frequency magnetron sputtering in an argon environment; after the bonding layer was prepared, the bonding layer was heated at 0.4Pa,under the condition of-50V, preparing a 200-nanometer Ti-Ag nanometer composite metal transition layer on a target 8 by adopting electric arc to target 2 and medium-frequency magnetron sputtering, wherein the thickness of a single-layer Ti layer is 3 nanometers, the thickness of a single-layer Ag layer is 20 nanometers, and the thickness range of a modulation period formed by the two coatings is 23 nanometers; after the preparation of the transition layer is finished, carrying out 6-micron Ag in an argon environment under the condition of-50V by adopting a medium-frequency magnetron sputtering target 8, a first direct-current magnetron sputtering target 4 and a second direct-current magnetron sputtering target 5 at 0.4PaI/AgIIPreparation of nano multilayer high-temperature self-lubricating coating, single-layer AgIThe thickness of the layer is 5 nm, single layer of AgIIThe thickness of the layer is 50 nanometers, the modulation period thickness range formed by the two coatings is 55 nanometers, the total thickness of the coatings is controlled to be 6.41 micrometers, and the Ti-Ag nano composite metal coating fastener is obtained after the preparation is finished and natural cooling is carried out.
The device used in the above embodiment is shown in FIG. 1, wherein the vacuum chamber of the device is surrounded by furnace walls, the height of the vacuum chamber is 1-1.5 m, and the diameter is 800-1500 mm. 1 is a vacuum chamber door; 2, tubular electric arc targets arranged face to face; 3 is an ion source; 4 and 5 are two pairs of direct current magnetron sputtering targets respectively, and two arc targets are arranged in the whole device; 7, a fastener, wherein the fastener does not rotate but can revolve with the workpiece frame; 6 is an air extraction opening; the layout enables the plasma density of the front part of the target in the vacuum chamber to be greatly increased, and the workpiece is completely immersed in the plasma. The deposition rate, the hardness and the adhesive force of the coating are greatly improved. Because the target structure is optimized, the magnetic field distribution between the two magnetic control targets is more uniform, the target surface is uniformly sputtered, and the uniformity of the coating is improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. A vacuum ion plating Ag nanometer composite coating fastener is characterized in that: the surface of the fastener is provided with an Ag nano composite coating which is in a gradient layer structure and is composed of a diffusion layerThe composite coating comprises a diffusion layer, a bonding layer, a transition layer and an Ag high-temperature self-lubricating composite coating, wherein the diffusion layer is a pure Ti diffusion layer prepared by adopting an arc ion plating method through high-energy bombardment, the bonding layer is a pure Ti layer prepared by adopting an ion plating method through low energy, the transition layer is a Ti-Ag nano multilayer film formed by Ti evaporated by the arc ion plating method and Ag prepared under the condition of high voltage by an intermediate frequency magnetron sputtering method, and the self-lubricating layer is Ag prepared by an intermediate frequency methodIAnd Ag prepared by direct current magnetron sputtering methodIIFormed of AgI/AgIIA nano-multilayer film; the Ti-Ag nano multilayer film is a nano multilayer structure formed by Ti and Ag alternatelyI/AgIIThe nano multilayer film is AgIAnd AgIINano alternating coatings are formed alternately.
2. The vacuum ion plating Ag nanocomposite coating fastener according to claim 1, wherein: the Ti-Ag transition layer coating is a nano multilayer structure formed by alternately Ti and Ag, the thickness of a single-layer Ti layer is 3-20 nanometers, the thickness of a single-layer Ag layer is 5-20 nanometers, and the thickness range of a modulation period formed by the two coatings is 8-40 nanometers.
3. The vacuum ion-plated Ag nanocomposite coating fastener according to claim 2, wherein: agI/AgIIThe nano multilayer film is Ag formed by medium-frequency magnetron sputteringIAnd Ag formed by DC magnetron sputteringIINano-alternating coating of layers, single layer of AgIThe thickness of the layer is 5-30 nm, and the layer is AgIIThe thickness of the layer is 10-50 nm, and the thickness of the modulation period formed by the two coatings is 15-80 nm.
4. The vacuum ion plating Ag nanocomposite coating fastener according to claim 1, wherein: the thickness of the diffusion layer is 5-10 nanometers, the thickness of the bonding layer is 20-200 nanometers, the thickness of the transition layer is 100-200 nanometers, and the thickness of the high-temperature self-lubricating coating is 1-10 micrometers.
5. Vacuum ion plating Ag nano composite coating fastenerThe preparation method is characterized by comprising the following steps: performing plasma etching on the alloy steel fastener at the temperature of 100-450 ℃ in an argon and hydrogen environment, performing arc discharge on a target in the argon environment by adopting an electric arc of a circular vacuum furnace, and preparing a 2-10 nanometer Ti diffusion layer under the conditions of 0.02-0.2Pa, minus 800V to minus 1000V; then preparing a 20-200 nanometer Ti bonding layer by adopting medium-frequency magnetron sputtering in an argon environment under the conditions of 0.4-1Pa, -50V to-500V for a target; after the preparation of the bonding layer is finished, under the condition of 0.4-1Pa, -50V to-200V, preparing a 100-plus-200 nanometer Ti-Ag nanometer composite metal transition layer by adopting a medium-frequency magnetron sputtering target pair, a first direct-current magnetron sputtering target pair and a second direct-current magnetron sputtering target pair, wherein the thickness of a single-layer Ti layer is 3-20 nanometers, the thickness of a single-layer Ag layer is 5-20 nanometers, and the thickness range of a modulation period formed by the two coatings is 8-40 nanometers; after the preparation of the transition layer is finished, performing 1-10 micron Ag in argon atmosphere at 0.4-1Pa by adopting a medium-frequency magnetron sputtering target pair, a first direct-current magnetron sputtering target pair and a second direct-current magnetron sputtering target pair under the condition of-50V to-250VI/AgIIPreparation of nano multilayer high-temperature self-lubricating coating, single-layer AgIThe thickness of the layer is 5-30 nm, and the layer is AgIIThe thickness of the layer is 10-50 nanometers, the modulation period thickness range formed by the two coatings is 15-80 nanometers, the total thickness of the coatings is controlled to be 1.125-10.41 micrometers, and the Ti-Ag nano composite metal coating fastener is obtained after the preparation is finished and natural cooling is carried out.
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| CN110144477B (en) * | 2019-05-23 | 2020-12-01 | 西安建筑科技大学 | Ag/Ti2Preparation method of AlNb self-lubricating gradient composite material |
| CN111155066B (en) * | 2020-01-20 | 2021-03-16 | 西安交通大学 | Silver-plated microneedle array and preparation method thereof |
| CN113106399B (en) * | 2020-12-29 | 2022-07-26 | 阳江市新辉科技有限公司 | Multicolor antibacterial film layer and preparation method and application thereof |
| CN114807881A (en) * | 2022-04-24 | 2022-07-29 | 贵州航天精工制造有限公司 | Magnetron sputtering silver coating method for improving iron-based high-temperature alloy fastener |
| CN115094373B (en) * | 2022-08-23 | 2022-11-22 | 北京辰融科技有限责任公司 | Surface deposition process method for blade disc and blade tip |
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