CN107130213A - Multicomponent alloy laminated film Preparation equipment and preparation method - Google Patents

Multicomponent alloy laminated film Preparation equipment and preparation method Download PDF

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Publication number
CN107130213A
CN107130213A CN201710305293.8A CN201710305293A CN107130213A CN 107130213 A CN107130213 A CN 107130213A CN 201710305293 A CN201710305293 A CN 201710305293A CN 107130213 A CN107130213 A CN 107130213A
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China
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source
multicomponent alloy
laminated film
vacuum chamber
cathode arc
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CN201710305293.8A
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CN107130213B (en
Inventor
赵海波
梁红樱
董骐
杜建
鲜广
但秦
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Chengdu Rui Rui Technology Coating Technology Co Ltd
Sichuan University
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Chengdu Rui Rui Technology Coating Technology Co Ltd
Sichuan University
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Priority to CN201710305293.8A priority Critical patent/CN107130213B/en
Publication of CN107130213A publication Critical patent/CN107130213A/en
Priority to RU2017133149A priority patent/RU2678492C1/en
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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
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • 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
    • C23C14/24Vacuum evaporation
    • C23C14/26Vacuum evaporation by resistance or inductive heating of the source
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82BNANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B1/00Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • 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
    • C23C14/0641Nitrides
    • 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
    • C23C14/14Metallic material, boron or silicon
    • C23C14/18Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • 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
    • C23C14/24Vacuum evaporation
    • C23C14/32Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325Electric arc evaporation
    • 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
    • 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
    • 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
    • C23C14/54Controlling or regulating the coating process
    • 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
    • C23C28/00Coating 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
    • C23C28/30Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322Coatings 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
    • 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
    • C23C28/00Coating 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
    • C23C28/30Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34Coatings 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
    • 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
    • C23C28/00Coating 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
    • C23C28/30Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34Coatings 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
    • C23C28/347Coatings 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 layers adapted for cutting tools or wear applications

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nanotechnology (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention discloses a kind of multicomponent alloy laminated film Preparation equipment and preparation method, especially a kind of multicomponent alloy laminated film Preparation equipment and preparation method for being related to nano coating technical field.The present invention provides a kind of multicomponent alloy laminated film Preparation equipment for the cutting tool combination property for being remarkably improved institute's plated film, including heating system, air supply system, cooling system, vacuum system, vacuum chamber, luggage carrier, elevating mechanism, crucible evaporation source, controlled sputtering source, cathode arc source and electric control system.The equipment of the application can realize the group technology of cathodic arc ion plating and magnetron sputtering, and the binary evaporation source technique that vacuum evaporation coating is combined with magnetron sputtering, carry out the preparation of multicomponent alloy laminated film, accurately control the institutional framework of all kinds of films, so as to obtain the comprehensive excellent multi-element film such as high hardness, low internal stress, high adhesion, low roughness, good wearability, and with high sedimentation rate in preparation process.

Description

Multicomponent alloy laminated film Preparation equipment and preparation method
Technical field
It is related to nanometer the present invention relates to a kind of multicomponent alloy laminated film Preparation equipment and preparation method, especially one kind to apply The multicomponent alloy laminated film Preparation equipment and preparation method of layer technical field.
Background technology
Manufacturing development be unable to do without cutting tool, and modern cutting tools have become the pass of lifting manufacturing industry technical merit One of key factor.At a high speed, efficiently, intelligence and environmental protection as machining pursue target, high intensity, high-toughness material and height Updating for the difficult-to-machine material performance such as temperature alloy, titanium alloy, requirements at the higher level are proposed to cutting tool.Modern cutting technology It is related to ambit extensively, wherein tool surface is modified the modern cutting technology that (coating) technology is in response to the market demand and grown up One of.It is widely used to the industries such as Aero-Space, automobile, the energy, ship, generating at present, it has also become manufacturing crucial skill One of art.
Cutting tool is except that should have a good ambient temperature mechanical properties, such as intensity, toughness, outside hardness, for high-speed cutting, For dry cutting, hard machining etc., should also possess excellent hot property, such as anti-chemical affinity, diffusion, dissolving, thermal shock resistance properties, Mechanical behavior under high temperature etc..
Coating is as one kind of modern cutting tools process for modifying surface, and it is by method chemically or physically in cutter table Micro-, nano level film is obtained on face, and with the features such as hardness is high, lubricity is good, high-temperature behavior is excellent.Table is carried out to cutter Finishing coat processing, is important channel and the means for improving cutting tool combination property, can tool life, raising processing Efficiency and machining accuracy, contribute to high-speed cutting, dry cutting, hard machining, the realization of precision cutting process.
During High-speed machining or DRY CUTTING, cutting temperature turns into the main original of influence coated cutting tool service life Cause, therefore improve the high-temperature behavior of film, ensure that the red hardness of coated cutting tool turns into PVD (Physical Vapor in recent years Deposition) the exploitation focus of technology.The content for improving Al in TiAlN films is to improve the effective method of coating performance One of, with the increase of Al content, the hardness and high-temperature behavior of film are all being improved, but bring therewith is stress in thin films Increase, the decline of toughness and the increase with iron-based material compatibility, so as to cause the generation of built-up edge.Therefore in practical application In, the combination property of such coated cutting tool does not obtain the change of essence.From the point of view of the latest development, development multicomponent alloy is answered It is very necessary to close thin film technique.The Basic Ways of ganoine thin film improved combination properties are the diversification of thin film composition, profit The characteristics of with different elements each, realize that the matched well of integrated performance index is always polynary, the main think of of superhard film development One of road.Solved by changing thin-film material composition at a high speed, high-temperature machining processing problems, such as routine TiN, TiAlN, Cr and Y is added in AlCrN can improve inoxidizability;Abrasion resistance can be improved by adding Zr, V, B and Hf;Hardness can be improved by adding Si With anti-chemical diffusivity.
Technology the most frequently used PVD can be divided into three major types:Vacuum evaporation coating VE (Vacuum Evaporating), magnetic control splash Penetrate MS (Magnetron Sputtering), cathodic arc ion plating AIP (Arc Ion Plating).
In vacuum evaporation coating evaporation process, evaporation rate and its influence factor of membrane material etc. and the close phase of its saturated vapour pressure Close.Therefore it is evaporated in vacuo coating technology to be restricted by material character, the evaporation for alloy material can cause the segregation of composition.
Magnetron sputtering technique is compared with cathodic arc ion plating technology, and deposition efficiency is relatively low, and the ionization level of atom also compares Low, stress present in the Thin Film Tissue of preparation is also larger, and magnetron sputtering around plating property and adhesion it is poor.
Cathodic arc ion plating, in membrane-film preparation process, some metallic particles, the big molten drop produced by cathode arc source is easy The surface of film is pressed from both sides in the film or deposited to, the compactness of film on the one hand can be influenceed, the service life of film is reduced, it is another Aspect can cause film surface coarse;Thin film composition is relatively single.
Therefore, the single equipment technology of prior art is difficult to meet a variety of requirements, its bad adaptability, prepared film Combination property is not high, it is impossible to realize the preparation of the multicomponent alloy laminated film of high-quality.
The content of the invention
It is comprehensive that the technical problems to be solved by the invention are to provide a kind of cutting tool that can significantly improve institute's plated film The multicomponent alloy laminated film Preparation equipment of energy.
The present invention solves the multicomponent alloy laminated film Preparation equipment that its technical problem is used, including heating system, confession Gas system, cooling system, vacuum system, vacuum chamber, luggage carrier, elevating mechanism, crucible evaporation source, controlled sputtering source, negative electrode electricity Arc source, electromagnetic field generator and electric control system, the vacuum system and vacuum chamber, the elevating mechanism and loading Frame is connected, the air supply system and vacuum chamber, the electric control system and crucible evaporation source, controlled sputtering source, Cathode arc source, electromagnetic field generator, heating system electrical connection, the crucible evaporation source, controlled sputtering source, cathode arc source In vacuum chamber, the target-substrate distance of the cathode arc source is 160mm to 230mm, and the target-substrate distance of the controlled sputtering source is 50mm to 75mm.
It is further, in addition to heated filament ion gun that the heated filament ion gun is set in a vacuum chamber, the heated filament ion Source is electrically connected with electric control system.
It is further that the electric control system includes ion source current, argon-arc plasma field and maintains power supply, sputtering source electricity Source, cathode arc power supply, grid bias power supply, the argon-arc plasma field maintain power supply and ion source current to be connected with heated filament ion gun, institute State sputtering source current to be connected with controlled sputtering source, the cathode arc power supply is connected with cathode arc source.
It is further that the heating system is including the heating system inside the electron beam in the middle part of vacuum chamber and positioned at true The external radiation heating system of empty room furnace wall surrounding.
It is further that the controlled sputtering source is symmetrically distributed in the inwall of vacuum chamber, and the cathode arc source is with vacuum The centre of gyration of room is symmetry axis, and the inwall of vacuum chamber is distributed in the shape of a spiral.
Further that the vacuum system includes molecular pump, lobe pump, mechanical pump, maintains pump, the molecular pump with it is true Empty room is connected, and the maintenance pump is connected with the exhaust outlet that molecular pump is connected, the exhaust outlet connection of the lobe pump and molecular pump, institute The exhaust outlet for stating mechanical pump and lobe pump is connected.
It is further, in addition to protective case, the protective case is installed in side of the cathode arc source towards luggage carrier, institute State side of the protective case away from cathode arc source and be additionally provided with baffle plate.
It is comprehensive that another technical problem solved by the invention is to provide a kind of cutting tool that can significantly improve institute's plated film Close method prepared by the multicomponent alloy laminated film of performance.
The present invention solves the preparation method for the multicomponent alloy laminated film that its technical problem is used, and utilizes cathode arc source While carrying out multicomponent alloy material ions deposition, single metallic elements are mixed using controlled sputtering source, multicomponent alloy is formed and is combined Film layer.
It is further, by crucible evaporation source evaporated metal element, to deposit to form metallic compound in workpiece surface Other elements are implanted into by controlled sputtering source simultaneously, in workpiece surface formation multicomponent alloy laminated film.
The beneficial effects of the invention are as follows:It can realize that AIP is (cloudy using the multicomponent alloy laminated film Preparation equipment of the application Pole electrical arc ion plating) with MS (magnetron sputtering) group technology, and VE (vacuum evaporation coating) and MS (magnetic controlled sputtering ion plating) The binary evaporation source technique being combined, carries out the preparation of multicomponent alloy laminated film, flexibly realizes the in good time change of coating composition, The institutional framework of all kinds of films is accurately controlled, by while AIP ion depositions, mixing single metallic elements, significantly improving thin The performance of film, so as to obtain high rigidity, the combination property such as low internal stress, high-bond, low roughness, good wearability is excellent Different multiple elements design film, and with very high sedimentation rate in preparation process.
Brief description of the drawings
Fig. 1 is the general assembly drawing of the application;
Fig. 2 is the structural representation of the vacuum chamber of the application;
Fig. 3 is the plane outspread drawing of vacuum chamber;
Fig. 4 is the structural representation of heated filament ion gun;
Fig. 5 is the structural representation of luggage carrier;
Fig. 6 is the XRD spectrum of the AlCrN films prepared using single cathode arc;
Fig. 7 is the equipment using the present invention, and the XRD spectrum of AlCrN films is prepared using AMS techniques;
Fig. 8 is the hardness image of the AlCrN films prepared using single cathode arc;
Fig. 9 is the equipment using the present invention, and the hardness image of AlCrN films is prepared using AMS techniques;
Figure 10 is the XRD spectrum of the TiAlN films prepared using single cathode arc;
Figure 11 is the equipment using the present invention, using AMS techniques by addition element, adjusts Al67Ti33After N structures The XRD spectrum of TiAlN films;
Figure 12 is the hardness image of the TiAlN films prepared using single cathode arc;
Figure 13 is the equipment using the present invention, using AMS techniques by addition element, adjusts Al67Ti33After N structures The hardness image of TiAlN films;
Figure 14 is the voice signal figure of the slight crack experiment of the AlCrN films prepared using prior art;
Figure 15 is used while AIP carries out AlCrN compound depositions for the present invention, is just passed through MS and is implanted into simple substance elements Mo The voice signal figure of the slight crack experiment of obtained film;
Figure 16 is the structural representation of cathode arc source of the present invention;
Figure 17 is individually using film microstructure figure made from AIP;
Figure 18 is film microstructure figure prepared by being implanted into Me elements using MS simultaneously using AIP.
Main parts size and numbering in figure:Loading vehicle motor 1, carrier 2, luggage carrier 3, vacuum chamber support 4, elevating screw 5th, coil 6, peep hole 7, cathode arc source 8, controlled sputtering source 9, heated filament ion gun 10, gas flow interface 11, vacuum cavity 12nd, high vacuum valve 13, molecular pump 14, forevacuum valve 15, pre- take out valve 16, by-passing valve 17, lobe pump 18, maintain pump 19, machinery Pump 20, vacuum system support 21, impressed current anode 22, crucible evaporation source 23, base material 24, protective case 25, baffle plate 26, workpiece 27, in Interbed 28, AlCrMeN compositions 29, MeNx compositions 30, AlCrN compositions 31.
Embodiment
The invention will be further described below in conjunction with the accompanying drawings.
As shown in Figures 1 and 2, multicomponent alloy laminated film Preparation equipment of the invention, including heating system, supply system System, cooling system, vacuum system, vacuum chamber, luggage carrier 3, elevating mechanism, crucible evaporation source 23, controlled sputtering source 9, negative electrode electricity Arc source (i.e. CAE sources), electromagnetic field generator and electric control system, the vacuum acquiring system and vacuum chamber, it is described Elevating mechanism is connected with luggage carrier 3, the air supply system and vacuum chamber, and the electric control system is evaporated with crucible Source 23, controlled sputtering source 9, cathode arc source 8, electromagnetic field generator, heating system electrical connection, the crucible evaporation source 23, Controlled sputtering source 9, cathode arc source 8 are located in vacuum chamber, and the target-substrate distance of the cathode arc source 8 is 160mm to 230mm, institute The target-substrate distance for stating controlled sputtering source 9 is 50mm to 75mm.
Vacuum chamber is evacuated by vacuum system, forms vacuum cavity 12, makes the preparation process of multicomponent alloy laminated film, Completed in the vacuum environment for meeting preparation technology standard.As shown in figure 5, wherein luggage carrier 3 needs the knife of plated film for fixation Has and realizes the two dimensional surface motion of cutter, elevating mechanism is used for moving luggage carrier 3.The wherein two dimensional surface motion of luggage carrier 3 Elevating movement with elevating mechanism can be by the way of mechanically wide variety of worm drive.Specific implementation is to add Load vehicle motor 1, carrier 2, elevating mechanism use elevating screw 5, and provide the vacuum chamber support 4 of support vacuum chambers, Coil 6 is additionally provided with above vacuum chamber.
Crucible evaporation source 23 is used in membrane-film preparation process the coating for completing composite Ti N, CrN, ZrN, and as auxiliary from The reception anode in change source, realizes that gas ion etches purpose.And crucible evaporation source 23 can be played by evaporating to vacuum chamber Cleaning effect, its operating cost is low, diffractive good, the uniformity continuously worked can be ensured, particularly with non-conductive film Prepare for a long time particularly critical.
Cathode arc source 8 is used in multicomponent alloy laminated film preparation process, is deposited with cathodic arc ion plating (AIP) Based on technique and for the technical process for the addition for carrying out the polynary element of multicomponent alloy material.
Controlled sputtering source 9 is used in the implantation technique of multicomponent alloy laminated film preparation process trace element.
Heating system is used to heat vacuum chamber in multicomponent alloy laminated film preparation process, to maintain polynary conjunction The environment temperature of stabilization required for golden composite film preparation technology.
Cooling system is used for the requirement for meeting cooling technique in multicomponent alloy laminated film preparation process, and vacuum chamber is carried out Timely and effectively cool down.
Air supply system is mainly used in into vacuum chamber being passed through Ar, N2、H2、O2Deng gas, and the amount of the gas to being passed through is carried out Accurate regulation and control.The application is preferred to use six road mass flow control systems, and maximum stream flow is 300~1000sccm.
The electromagnetic field generator of this equipment, for producing variable electromagnetic, makes the drive in electric arc arc spot variable electromagnetic Under dynamic, not only along target surface annulus fast run, and radially move back and forth so that arc spot run faster, it is more; (under the driving of variable magnetic field, arc spot translational speed can be made compared to not using raising more than 30%, the number of arc spot during variable magnetic field Amount, which is compared not use, improves more than 30% during variable magnetic field) in addition, the plasma produced near evaporation material surface, passes through Variable electromagnetic can be pushed to coating film area (distance can be more than 300mm), greatly strengthen the plasma density in vacuum chamber, The environment and condition of reactive ion plated film are improved, so as to significantly improve reactive ion coating quality.
It can realize following coating process to strengthen by plated film using the multicomponent alloy laminated film Preparation equipment of the application The combination property of workpiece 27:
In the prior art employed in film preparation be vacuum evaporation coating, magnetron sputtering, cathodic arc ion plating its A kind of middle monotechnics, or bottom film is made first with cathodic arc ion plating, recycle magnetron sputtering to do top film, The method that i.e. cathodic arc ion plating and magnetron sputtering are carried out respectively.There is no phase using the material between the above method each film Mutually fusion, but layered coverage, on the surface of workpiece 27, the performance of each layer is single, it is impossible to fully realize to various material excellent properties Comprehensive utilization, make the combination property of final obtained film relatively low.
And the equipment of the present invention, in a vacuum chamber will be to cathode arc source 8, controlled sputtering source 9 is combined, and to its space bit Put and optimize arrangement, the target-substrate distance for making cathode arc source 8 is 160mm to 230mm, and the target-substrate distance of controlled sputtering source 9 is 50mm To 75mm.Wherein target-substrate distance refer to cathode arc source 8 or the grade target source of controlled sputtering source 9 to the surface of workpiece 27 to be coated away from From.So cathodic arc ion plating and magnetron sputtering can be realized using the equipment of the present invention while the technique carried out, enters in AIP While row deposition, trace element is implanted into by MS, final obtained film has closely been merged a variety of alloys within the same layer Material and single metallic elements, the performance of film are further improved by the incorporation of single metallic elements, so that using foregoing side Legal system obtains film while having high rigidity, low internal stress, high-bond, low roughness, the performance of high-wearing feature, and with very High deposition.
Based on being deposited using the equipment of the application with AIP, using multicomponent alloy material means, pass through cathode arc source 8 (CAE) synthesis of polynary element thin film, is realized;The implantation of trace element then uses MS technical schemes (AIP and MS combination abbreviation AMS), relative components content is less than 1%.The accurate control to film phase structure can be realized, can be reached most preferably with obtaining Mechanical property film phase structure.Figure 17 is when Me target currents are 0A, i.e., merely using film knot made from AIP methods Bottom is base material 24 in structure, figure, be close to base material 24 be intermediate layer 28 against intermediate layer 28 be AlCrN compositions 31.Figure 18 is When Me target currents are improved, i.e., obtained membrane structure when being implanted into Me elements using MS, the characteristics of it obtains film is:It is short Column structure form.Bottom is base material 24 in figure, be close to base material 24 be intermediate layer 28 against intermediate layer 28 be AlCrMeN into Divide 29 and MeNx compositions 30.It can be seen that coating is with typical post when Me target currents are 0A by Figure 17 and Figure 18 contrast Shape crystalline form state grows, when Me target currents are improved, and a part of Me atoms enter MeNx crystal lattice and replace Cr atoms, and coating is played Solution strengthening effect, another part Me formation Me is present forms tiny MeNx crystal grain suppression AlCrN crystal with AlCrN intergranulars Further growth, plays invigoration effect.
The binary evaporation source that vacuum evaporation coating is combined with magnetic controlled sputtering ion plating can be realized using the equipment of the present invention Technology;I.e. by crucible evaporation source evaporated metal element, while workpiece surface deposits to form metallic compound, pass through Controlled sputtering source is implanted into other elements, can be in N during specific implementation in workpiece surface formation multicomponent alloy laminated film2With Ar's Under mixed atmosphere, Ti elements are evaporated by electron beam evaporation source 23, traditional TiAlN thin film is formed, the same of TiN film is formed in deposition When by controlled sputtering source 9 be implanted into X element, be coated with (Ti on tool and mould surfaceX, Me1-X) N layers;The X is in Al, Cr, Si It is at least one.Because TiN is a kind of ideal thin film system, there are extensive preparation basis, such as AIP, MS, VE method Industrialization production requirements can all be met.TiN has excellent physics, chemical property, as hardness is high, coefficient of friction is low, it is good Chemical compatibility etc., is the desired coating material of slow cutting process tool, and it can mitigate cutting edge portion and processed material Adhesion, increase cutting-tool's used life and raising processing efficiency, are still at present using one of more thin-film material.But it is traditional TiN hardness is relatively low, wearability is short of, heat endurance is poor, limits its and widely applies.The improvement of TiAlN thin film is main It is embodied in new TiN based alloys and multiple elements design layer aspect.In addition, the binary nitride of magnesium-yttrium-transition metal, carbide are often It can each other dissolve each other, by adding some elements into TiN film, nitride type compound compound can be formed, and then can be from basic The upper performance for changing TiAlN thin film, improves its abrasion resistance and heat endurance.Using TiN as base, it is multi-element alloyed change control it is thin The phase structure of film, obtains so-called (TiX, Me1-X) N membrane systems.Polynary element can relate to C, Si, Cr, Al, Mo, W, V, Zr, Y, La etc..
Using the equipment of the application with AIP deposit based on can realize the preparation of insulation oxide film.Although AIP is helped In the generation of ionization, the deposition of its plated film is higher, but in O2When excessive or original electric field changes, O2It is easier in the moon Reacted on the target surface of pole, oxide is generated, so as to cause the failure of cathodic discharge, it is impossible to the element required for normal output. Current PVD oxide is mainly aluminum oxide, and Al, AlTi material are relative to be more easy to and O2React, therefore conventional way exists The Cr of certain content is added in Al materials, the oxidation of target surface can be effectively prevented, but chromium oxide stability is relatively poor, can cause The change of film performance.Although therefore prior art thinks that AIP depositions are high, the insulation for meeting and requiring can not be prepared with it Sull.And the variable electromagnetic for using the device, method of the application to be produced by control system and electromagnetic field generator, It can guide and drive O2Moved towards the direction of workpiece 27 of plated film, so as to away from target body, effectively prevent O2On cathode target surface React, generate oxide, prepare high performance sull, overcoming can not be prepared using AIP in the prior art The technology prejudice of insulation oxide.
As shown in figure 4, also including heated filament ion gun, the heated filament ion gun is set in a vacuum chamber, the heated filament ion Source is electrically connected with electric control system.The heated filament ion gun that the application is set up can significantly increase gas etching effect.For knife Have for coating, vacuum etching, activation are most important.Give up traditional CAE metals height bias using the equipment of the present invention to bang Blow mode, and use gas ion low bias etching method, can be more uniformly distributed, overall clean effect, and be ensured The integrality of cutting edge.In addition the heated filament ion gun that the application is set up can also play internal heating, increase ionization intensity, auxiliary The effect of deposition is helped, plays a part of increasing plasma when being individually evaporated ion plating.
The electric control system includes ion source current, plasma and maintains power supply, sputtering source current, cathode arc electricity Source, grid bias power supply, the argon-arc plasma field maintain power supply and ion source current be connecteds with heated filament ion gun, it is described sputter source current and Controlled sputtering source 9 is connected, and the cathode arc power supply is connected with cathode arc source 8, grid bias power supply and workpiece to be plated 27 during work Connection.Wherein ion source current be heated filament ion gun by power supply, plasma maintains the offer arc that power supply is heated filament ion gun Power supply, sputtering source current be controlled sputtering source 9 by power supply, cathode arc power supply is that cathode arc source 8 provides power supply.Bias plasma Source provides the electric field of control charged ion motion.Electric control system is mainly that the electric component of this equipment provides corresponding parameter Adjustable power supply, wherein the parameter such as voltage and electric current of each foregoing power supply can use existing electric-controlled according to technological requirement Technology processed is controlled regulation, makes this equipment by controlling the parameter of each power supply to control technical process, to power parameter Adjustment can be realized using hardware circuit, it would however also be possible to employ the mode that software and hardware is combined.
The heating system is including the heating system inside the electron beam in the middle part of vacuum chamber and positioned at vacuum chamber furnace wall four The external radiation heating system in week.The structure that the application is combined using interior external heat makes the globality of heating more perfect, and And in AMS system runnings, can effectively maintain the uniformity in temperature field, meet depositing operation requirement.Specific implementation is this Equipment using heated filament ion gun as internal heat, then on the basis of heated filament ion source heating, increase external radiation heating System.
As shown in figure 3, the controlled sputtering source 9 is symmetrically distributed in the inwall of vacuum chamber, the cathode arc source 8 is with vacuum The centre of gyration of room is symmetry axis, and the inwall of vacuum chamber is distributed in the shape of a spiral.Using Spiral distribution scheme, sky is made full use of Between, the target source of such cathode arc can increase to more than eight, significantly enhance adjustment and control of this equipment to film composition Ability, producing this equipment, composition is more complicated, the more excellent film of combination property.
The vacuum system, which includes the vacuum system, includes molecular pump 14, lobe pump 18, mechanical pump 20, maintenance pump 19, The molecular pump 14 and vacuum chamber, the exhaust outlet that the maintenance pump 19 is connected with molecular pump 14 are connected, the lobe pump 18 It is connected with the exhaust outlet of molecular pump 14, the mechanical pump 20 is connected with the exhaust outlet of lobe pump 18.May be used also on vacuum system pipeline Forevacuum valve 15 is set, valve 16, by-passing valve 17 is taken out in advance.The limiting pressure of vacuum chamber, work pressure are wherein determined with molecular pump 14 Power, the pumpdown time of high vacuum plates the stability of film pressure, it is desirable to which it does not return oil, no switching on and shutting down non-cutting time.Mechanical pump 20 is used In vacuum chamber being extracted into the pressure value that meets the air inlet of molecular pump 14, exhaust outlet.Which determine the pumpdown time of low vacuum.Maintain Pump 19 is used to maintain the pressure at expulsion of the exhaust outlet of molecular pump 14, vacuum chamber main pump in opening is also run well work, dimension Hold pump 19 and can select sliding vane rotary pump.Vacuum system is fixedly mounted on vacuum system support 21.
Peep hole 7 is provided with the vacuum chamber.Setting up peep hole 7 is easy to operating personnel to understand vacuum chamber inside information in real time Condition.Gas flow interface 11 is additionally provided with vacuum chamber, to be passed through associated gas in the course of the work.
As shown in figure 16, in addition to protective case 25, the protective case 25 is arranged on cathode arc source 8 towards luggage carrier (3) Side, the side of the protective case 25 away from cathode arc source 8 is additionally provided with baffle plate 26.Although AIP contributes to the hair of ionization Raw, the deposition of its plated film is higher, but in O2When excessive or original electric field changes, O2It is easier to send out on cathode target surface Raw reaction, generates oxide, so as to cause the failure of cathodic discharge, it is impossible to the element required for normal output.Current PVD oxygen Compound is mainly aluminum oxide, and Al, AlTi material are relative to be more easy to and O2React, therefore conventional way is added in Al materials The Cr of certain content, can effectively prevent the oxidation of target surface, but chromium oxide stability is relatively poor, can cause changing for film performance Become.Although therefore prior art thinks that AIP depositions are high, the sull for meeting and requiring can not be prepared with it.This Shen Target surface please effectively be protected using aforementioned structure, prevent O2Into cathode target surface, it is possible to which guiding is flowed through around target surface O2, moved towards the direction of film-coating workpiece 27, so as to away from target surface, effectively prevent O2Reacted on cathode target surface, generate institute The oxide of meaning, prepares high performance sull, and the skill of oxide can not be prepared using AIP in the prior art by overcoming Art prejudice.
Temperature measuring equipment and vacuum measuring device are provided with the vacuum chamber.By the temperature measuring equipment set up and Vacuum measuring device, can measure the temperature and vacuum in vacuum chamber, to enter in coating process to both the above parameter The accurate control of row.
The cooling system is multichannel water circulation type cooling system.Using multichannel water circulation type cooling system, cooling effect It is good, it is possible to save resource and cost.
The method of the multicomponent alloy laminated film of the present invention, carries out multicomponent alloy material ions using cathode arc source 8 and sinks While product, single metallic elements are mixed using controlled sputtering source 9, multicomponent alloy composite film layer is formed.Due in the prior art Coating process uses the technique that cathodic arc ion plating or magnetron sputtering are carried out respectively, therefore can not effectively combine two kinds of techniques Advantage, prevent obtained film from being provided simultaneously with a variety of excellent performances.And the application carried out with cathode arc source 8 it is polynary While alloy material ion deposition, single metallic elements are mixed using controlled sputtering source 9, multicomponent alloy composite film layer is formed, The metallurgical structure of film so can be accurately controlled, according to using needing the performance to film coating to optimize adjustment, And higher deposition can be ensured in preparation process, so that performance is higher compared with prior art for obtained film.
The technical process of multicomponent alloy laminated film is prepared using the multicomponent alloy laminated film Preparation equipment of the present invention:
A, AIP and MS
(1) pre-treatment:
Before plated film, cutter is dried after being cleaned through conventional alkalescent cleaning agent and absolute alcohol ultrasonic wave, is placed in coating chamber;
(2) preparation before coating:
1. vacuum chamber is inflated, and opens fire door;
2. electric arc, sputter target material are changed as needed, change sight glass;
3. each position of body of heater, pressure 0.6MPa are cleaned with high pressure air rifle;
4. appropriate fixture is selected, loads workpiece 27 (cutter), confirms that clamp movement is reliably errorless;
5. heated filament ion gun, cathode arc source 8, controlled sputtering source, impressed current anode 22, the insulation shape of the fixture of workpiece 27 are confirmed Condition, its resistance should be greater than 100K Ω;
6. close deposited chamber, close vent valve.
(3) vacuumize (to 5 × 10-2Pa) and preheating
1. handpiece Water Chilling Units are started;
2. mechanical pump (20), lobe pump (18), opening take out valve 16 in advance;
3. start compound vacuum gauge, open thermocouple rule 1, test fore line vacuum, vacuum is less than 5Pa
4. molecular pump 14 is started;
5. when molecular pump 14 enters normal operating conditions, and vacuum degree in vacuum chamber meets and is less than after 5Pa, and closing takes out valve in advance 16th, step valve 15, high vacuum valve 13 before opening;
6. when vacuum values are less than 5 × 10-2During Pa, 40~60sccm Ar gas is sent into, and opens auxiliary heating (5KW);
7. open workpiece 27 to rotate, frequency modulation 15Hz;
8. the composite heating stage is prepared to enter into after 40min.
(4) electron beam is heated
1. pressure in vacuum tank is adjusted to 2.5 × 10-190~120sccm of Pa, Ar throughput;
2. heated filament ion source current is opened, the slow electric current that rises is to 170~230A;
3. open field supply and be adjusted to 12~20A;
4. open argon-arc plasma field and maintain power supply, switch goes to heating gear;
5. electric arc is caused, electric current is gradually added in 180A;
6. 40~70min of composite heating period.
(5) gas plasma is etched
1. heater current maintains 170~230A;
2. argon-arc plasma field maintains source current to reduce to 100~120A;
3. field supply reduces to 6~8A;
4. pressure in vacuum tank is adjusted to 2 × 10-1Pa, Ar throughput 50~65sccm, H212~20sccm of throughput;
5. breakdown grid bias power supply, gradually powers up and is depressed into 0~200V of DC voltage, 300~500V of pulse voltage;
6. the ion etching period is about 80~150min.
(6) coating
1. Ti, Cr, Zr layers:Nitrogen (Ar) 80~140sccm of flow, bias is adjusted to 800~1000V, opens 2 negative electrode electricity Arc source 8 (Ti, Cr, Zr), arc 70~100A of target current, 180~600sec of cycle;
2. TiN, CrN, ZrN layers:480~680sccm of nitrogen flow, bias is adjusted to 150V, opens 2 cathode arc sources 8 Source (Ti, Cr, Zr), arc 100~120A of target current, 180~600sec of cycle;
3. TiAl layers:540~900sccm of nitrogen flow, bias is adjusted to 100~120V, opens 4 cathode arc sources 8 (TiAl), 100~120A of arc target current, 3600~7200sec of cycle;
4. 2 controlled sputtering sources 9,1~3A of sputtering current, 3600~7200sec of cycle are opened:Nitrogen flow 540~ 900sccm, bias is adjusted to 80~100V;
5. close 4 sources of cathode arc source 8 (TiAl), open (2) individual cathode arc source 8 (AlTi), arc target current 100~ 120A, 1800~3600sec of cycle, nitrogen flow 540~900sccm, O230~100sccm of flow;
6. cathode arc, magnetic controlled sputtering target source, grid bias power supply are closed;
7. heating source, N are closed2、O2Source, the closing startup power supply of molecular pump 14, open and maintain pump (19);Send nitrogen 80~ 120sccm;
8. argon gas is sent to 30Pa;
(7) cool down:60~120min of process time.
B, VE and MS
(1) pre-treatment:
Before plated film, high-speed steel or hard alloy cutter (without special polishing) are through conventional alkalescent cleaning agent and anhydrous Dry, be placed in coating chamber after the cleaning of alcohol ultrasonic wave;
(2) equipment inspection:
1. vacuum chamber is inflated, and opens fire door;
2. sputter target material is changed as needed, changes sight glass;
3. vapor deposition source return, and add new 20~30g of evaporation material (Ti);
4. each position of body of heater, pressure 0.6MPa are cleaned with high pressure air rifle;
5. appropriate fixture is selected, loads workpiece 27 (cutter), confirms that clamp movement is reliably errorless;
6. electron gun, evaporation source 23, sputtering source, impressed current anode 22, the insulation status of the fixture of workpiece 27 are confirmed, its resistance should More than 100K Ω;
7. chassis is risen, deposited chamber is closed, closes vent valve.
(3) vacuumize and preheat
1. handpiece Water Chilling Units are started;
2. mechanical pump (20), lobe pump (18), opening take out valve 16 in advance;
3. start compound vacuum gauge, open thermocouple rule 1, test fore line vacuum, vacuum is less than 5Pa
4. molecular pump 14 is started;
5. when molecular pump 14 enters normal operating conditions, and vacuum degree in vacuum chamber meets and is less than after 5Pa, and closing takes out valve in advance 16th, step valve, high vacuum valve 13 before opening;
6. when vacuum values are less than 1 × 10-1During Pa, the Ar gas for the 40~60sccm that makes a gift to someone, and open auxiliary heating;
7. open workpiece 27 to rotate, frequency modulation 20Hz;
8. the composite heating stage is prepared to enter into after 40min.
(4) electron beam is heated
1. pressure in vacuum tank is adjusted to 2.5 × 10-190~110sccm of Pa, Ar throughput;
2. heated filament ion source current is opened, the slow electric current that rises is to 170~230A;
3. open field supply and be adjusted to 12~20A;
4. open argon-arc plasma field and maintain power supply, switch goes to heating gear;
5. electric arc is caused, electric current is gradually added in 180A;
6. 40~100min of composite heating period.
(5) gas plasma is etched
1. heated filament ion ource electric current maintains 170~230A;
2. argon-arc plasma field maintains source current to reduce to 100~120A;
3. field supply reduces to 6~8A;
4. pressure in vacuum tank is adjusted to 2 × 10-150~65sccm of Pa, Ar throughput;
5. breakdown grid bias power supply, gradually powers up and is depressed into 0~200V of DC voltage, 300~500V of pulse voltage;
6. the ion etching period is about 50~90min.
(6) coating
1. heated filament ion ource electric current maintains 170~230A;
2. argon gas is adjusted to 23~35sccm,
3. field supply is adjusted to 25~35A;
4. bias is adjusted to 0~200V of voltage DC, 300~500V of pulse;
Plus argon-arc plasma field maintains source current to 200A (5min) 5.;
6. 5~20min of Ti intermediate metals is coated;
7. send nitrogen 80~120sccm;
8. bias is adjusted to 180V (10min);
9. magnetic controlled sputtering target source, 1.0~2.0A (AlTiCr, C, Cr, Zr, Si etc.) are opened
10. bias is adjusted to 100~150V (10min);
(11) 20~50min of plated film period;
(12) magnetic controlled sputtering target source is closed;
(13) close argon-arc plasma field and maintain power supply, filament supply, magnetic field power supply, heating source, N2Source, closing molecular pump 14 start Power supply, opens and maintains pump (19);
(14) argon gas is sent to 30Pa;
(7) cool down:60~120min of process time.
Measured data is contrasted:
As shown in Figure 6 and Figure 7, AlCrN coatings and the equipment profit using the present invention are prepared using single cathode arc AlCrN coatings are prepared with AMS techniques to compare.Both have differences in (111), (200) diffraction maximum, are added by micro Mo, Cause the enhancing of AlCrN (200) diffracted intensity.As shown in Figure 8 and Figure 9, prepared using the equipment utilization AMS techniques of the present invention AlCrN coatings are after addition Mo, and film hardness improves about 10% or so.
As shown in fig. 10 and fig. 12, the TiAlN coatings prepared using single cathode arc, TiN (200) diffracted intensities compared with By force, TiAlN (200) diffracted intensity is relatively weak, and film hardness is about 2400~3000HV.
As illustrated in figures 11 and 13, Al is adjusted by addition element using the equipment utilization AMS techniques of the present invention67Ti33N Structure, TiAlN (200) diffracted intensity significantly changes, and film hardness is promoted to 3500~4000HV.
As shown in FIG. 14 and 15, to using film made from prior art and using the present invention in the same of AIP ion depositions When incorporation single metallic elements method made from film carry out scratch experiment, to cut produce during acoustic energy carry out detect To voice signal figure.As can be seen from the figure the acoustic energy during being produced using film cut produced by the present invention compares existing skill Art is substantially reduced, and is indicated above the film hardness prepared by the present invention and is increased significantly compared with prior art.

Claims (9)

1. multicomponent alloy laminated film Preparation equipment, it is characterised in that:Including heating system, air supply system, cooling system, vacuum System, vacuum chamber, luggage carrier (3), elevating mechanism, crucible evaporation source (23), controlled sputtering source (9), cathode arc source (8), electricity Field generator for magnetic and electric control system, the vacuum system and vacuum chamber, the elevating mechanism are passed with luggage carrier (3) Dynamic connection, the air supply system and vacuum chamber, the electric control system and crucible evaporation source (23), controlled sputtering source (9), cathode arc source (8), electromagnetic field generator, heating system electrical connection, the crucible evaporation source (23), controlled sputtering source (9), cathode arc source (8) is located in vacuum chamber, and the target-substrate distance of the cathode arc source (8) is 160mm to 230mm, the magnetic The target-substrate distance for controlling sputtering source (9) is 50mm to 75mm.
2. multicomponent alloy laminated film Preparation equipment as claimed in claim 1, it is characterised in that:Also include heated filament ion gun (10), the heated filament ion gun (10) is set in a vacuum chamber, and the heated filament ion gun (10) electrically connects with electric control system.
3. multicomponent alloy laminated film Preparation equipment as claimed in claim 2, it is characterised in that:The electric control system is also Power supply, sputtering source current, cathode arc power supply, grid bias power supply, the plasma are maintained including ion source current, plasma Power supply and ion source current is maintained to be connected with heated filament ion gun (10), the sputtering source current is connected with controlled sputtering source (9), institute Cathode arc power supply is stated to be connected with cathode arc source (8).
4. multicomponent alloy laminated film Preparation equipment as claimed in claim 1, it is characterised in that:The heating system includes position Heating system and the external radiation heating system positioned at vacuum chamber furnace wall surrounding inside electron beam in the middle part of vacuum chamber.
5. multicomponent alloy laminated film Preparation equipment as claimed in claim 1, it is characterised in that:The controlled sputtering source (9) The inwall of vacuum chamber is symmetrically distributed in, the cathode arc source (8) is divided in the shape of a spiral using the centre of gyration of vacuum chamber as symmetry axis Inwall of the cloth in vacuum chamber.
6. multicomponent alloy laminated film Preparation equipment as claimed in claim 1, it is characterised in that:The vacuum system includes dividing Sub- pump (14), lobe pump (18), mechanical pump (20), maintenance pump (19), the molecular pump (14) and vacuum chamber, the maintenance The exhaust outlet that pump (19) is connected with molecular pump (14) is connected, and institute's lobe pump (18) is connected with the exhaust outlet of molecular pump (14), described Mechanical pump (20) is connected with the exhaust outlet of lobe pump (18).
7. multicomponent alloy laminated film Preparation equipment as claimed in claim 1, it is characterised in that:Also include protective case, it is described Protective case be arranged on side of the cathode arc source (8) towards luggage carrier (3), the protective case away from cathode arc source (8) one Side is additionally provided with baffle plate (26).
8. the method that multicomponent alloy laminated film is prepared using the multicomponent alloy laminated film Preparation equipment described in claim 1, It is characterized in that:While carrying out multicomponent alloy material ions deposition using cathode arc source (8), utilize controlled sputtering source (9) Single metallic elements are mixed, multicomponent alloy composite film layer is formed.
9. multicomponent alloy preparation method of composite film as claimed in claim 8, it is characterised in that:Evaporated by crucible evaporation source Metallic element, is implanted into other elements, in workpiece while workpiece surface deposits to form metallic compound by controlled sputtering source Surface forms multicomponent alloy laminated film.
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