RU2678492C1 - Device for producing a composite film of multi-element alloy - Google Patents

Abstract

FIELD: chemistry.SUBSTANCE: invention relates to a device for producing a composite film of a multielement alloy. Device comprises a heating system, an air supply system, a cooling system, a vacuum system, a vacuum chamber, a holder, a lifting mechanism, a crucible evaporation source, a magnetron sputtering source, a source of cathode arc and an electrical control system. Device provides a composite multi-element alloy film by combining ion deposition using a cathode arc and magnetron sputtering, and using a dual evaporation source combining vacuum evaporation and magnetron sputtering.EFFECT: device allows to control the internal structure of all types of films and to obtain multi-element film with outstanding common properties, such as high hardness, low internal stress, high adhesive strength, low roughness and favorable wear resistance, as well as obtaining a film with a high deposition rate.5 cl, 18 dwg

Description

FIELD OF TECHNOLOGY

The present invention relates to a device for producing a composite film of a multi-element alloy and, in particular, to a device for producing a composite film of a multi-element alloy in the field of nanocoating technology.

BACKGROUND OF THE INVENTION

Modern cutting tools, absolutely necessary for the development of the manufacturing industry, have become one of the key factors in raising the technological level of the manufacturing industry. Currently, they are making great efforts to achieve such goals of the metal cutting process as high speed, high productivity, the use of intelligent systems and environmental protection. Continuously improved performance characteristics of high-strength materials, highly plastic materials and difficult-to-process materials such as high-temperature alloys and titanium alloys impose higher demands on cutting tools. Modern metal cutting technology includes a wide range of subject areas, among which the surface modification (coating) technology of cutting tools is one of the modern metal cutting technologies developed to meet market demands. It is currently widely used in the aerospace, automotive, energy, shipbuilding and energy generating industries as one of the key technologies in the manufacturing industry.

Cutting tools should not only have good mechanical characteristics at room temperature, such as strength, toughness and hardness, but also outstanding thermal characteristics, such as chemical affinity, diffusion ability, solubility, thermal shock resistance and high temperature mechanical properties for high speed cutting , dry cutting and hard cutting.

As one of the surface modification technologies of modern cutting tools, the coating technology can chemically or physically provide micron or nanometer-thick films with properties such as high hardness, good lubricity and excellent high temperature performance. Coating processing, as an important approach to improving the overall performance of cutting tools, can extend the life of the cutting tools, increase productivity and accuracy of the machining, and help to achieve high speed cutting, dry cutting, hard cutting and precision cutting.

During high speed machining or dry cutting, the cutting temperature is a key factor affecting the life of coated cutting tools. Therefore, the development of the technology of physical vapor deposition (PVD; from the English: physical vapor deposition) for improving the high-temperature characteristics of films and ensuring the hardness of coated cutting tools at a red-hot temperature is becoming a “hot spot”. Increasing the Al content in TiAlN films is one of the effective ways to improve the performance of the coating. The hardness and high temperature characteristics of the films increase with increasing Al content. However, the internal stress also increases, the toughness of the films decreases and the affinity for iron-based materials increases, so that edges with influxes of material are formed. Therefore, in applied tasks, the general properties of such coated cutting tools are not fundamentally improved. Based on recent developments, it is necessary to develop the technology of composite films from multi-element alloys. The basic approach for improving the overall properties of solid films is to vary the composition of the films. One of the main ideas is always the development of multi-element and superhard films by ensuring maximum consistency in the overall quality indicators and characteristics of various elements. The problems that exist in high-speed and high-temperature cutting methods can be solved by changing the composition of the film materials, for example, adding Cr and Y to standard TiN, TiAlN and AlCrN alloys can improve oxidation; the addition of Zr, V, B and Hf can increase the abrasion resistance, and the addition of Si can increase the hardness and diffusion resistance of chemicals.

The most common PVD methods can be divided into three categories, such as vacuum evaporation (VE; from the English: vacuum evaporating), magnetron sputtering (MS; from the English: magnetron sputtering) and cathodic arc ion deposition (AIP; from the English: cathodic arc ion plating).

As for vacuum evaporation, the evaporation rate of the film materials and the factors influencing it are closely related to the pressure of their saturated vapor. Therefore, the method of vacuum evaporation depends on the characteristics of the material, and the evaporation of the alloy materials can lead to segregation of the composition.

Compared to the cathode-arc ion deposition method, magnetron sputtering has a low deposition efficiency, a low ionization rate of atoms, and a high voltage in the resulting film structure; at the same time during magnetron sputtering, the performance characteristics of spiral coating and adhesion are poor.

As for the cathode-arc ion deposition, some metal particles and large droplets generated by the sources of the cathode arc are easily incorporated into the films or deposited on the surfaces of the films, which, on the one hand, can adversely affect the compaction and reduce the service life of the films, and, on the other hand, it can roughen the surface of the films; the composition of the films is relatively simple.

Therefore, simple technical equipment in the prior art is not enough to meet various requirements due to its poor adaptability; since the general operational characteristics of the obtained films are poor, using existing methods it is impossible to obtain composite films from multi-element alloys.

SUMMARY OF THE INVENTION

The technical problem that needs to be solved in the present invention is to provide a device for producing a composite film of a multi-element alloy, which could significantly improve the overall performance of a cutting tool coated with this film.

A device for producing a composite film from a multielement alloy provided by the present invention to solve technical problems includes a heating system, an air supply system, a cooling system, a vacuum system, a vacuum chamber, a holder, a lifting mechanism, a crucible evaporation source 23, a magnetron sputtering source, a cathode source arcs, electromagnetic field generator and electrical control system; the vacuum system is connected to a vacuum chamber; the lifting mechanism is connected to the holder through the transmission; the air supply system is connected to a vacuum chamber; the electrical control system is electrically connected to a crucible evaporation source 23, a magnetron sputtering source, a cathode arc source, an electromagnetic field generator and a heating system; a crucible evaporation source 23, a magnetron sputtering source, and a cathode arc source are located in a vacuum chamber; the target-substrate distance of the cathode arc source lies in the range from 160 mm to 230 mm; the target-substrate distance of the magnetron sputtering source is in the range from 50 mm to 75 mm.

In addition, the device comprises an ion source in the form of a filament; this ion source in the form of a filament is located in a vacuum chamber; an ion source in the form of a filament is electrically connected to an electrical control system.

In addition, the electrical control system includes an ion source power source, a plasma field power source, a magnetron sputter power source, a cathode arc source power source and a grid bias voltage source; a plasma field power source is connected to an ion source power source and an ion source in the form of a filament; the power source of the magnetron sputtering source is connected to the magnetron sputtering source, and the power source of the cathode arc source is connected to the cathode arc source.

In addition, the heating system comprises an internal electron beam heating system located in the center of the vacuum chamber, and an external radiation heating system located around the wall of the vacuum chamber furnace.

In addition, the magnetron sputtering source is symmetrically placed on the inner wall of the vacuum chamber; the source of the cathode arc is helically placed on the inner wall of the vacuum chamber, if we take the center of rotation of the vacuum chamber as the axis of symmetry.

In addition, the vacuum chamber comprises a molecular pump, a Roots vacuum pump, a mechanical pump, and a pressure maintenance pump; a molecular pump is connected to a vacuum chamber; a pressure maintenance pump is connected to an air outlet that is connected to a molecular pump; The Roots vacuum pump is connected to the air outlet of the molecular pump, and the mechanical pump is connected to the air outlet of the Roots vacuum pump.

In addition, the device also includes a protective casing; a protective casing is mounted on the source side of the cathode arc facing the holder; in addition, on the side of the protective casing behind the cathode arc source there is a reflector (screening partition).

Another technical problem that needs to be solved in the present invention is to provide a method for producing a composite film from a multi-element alloy, which can significantly improve the overall performance of a cutting tool coated with such a film.

The method for producing a composite film from a multi-element alloy used in the present invention to solve this technical problem consists in turning on the monometallic elements using a magnetron sputtering source while simultaneously depositing ions of the materials of the multi-element alloy using a cathode arc source to obtain a composite film of a multi-element alloy.

In addition, there is the evaporation of metal elements from the crucible source of evaporation and the subsequent implantation of other elements from the magnetron source of atomization while depositing a metal compound on the surface of the workpiece; accordingly, a composite film of a multi-element alloy is formed on the surface of the workpiece.

The beneficial effects of the present invention are as follows: the device for producing a multi-alloy alloy composite film of the present invention can provide a multi-alloy alloy composite film by a combined method of cathodic arc ion deposition (AIP) and magnetron sputtering (MS) and a dual source method evaporation combining vacuum evaporation (VE) and magnetron sputtering (MS); accordingly, it is possible to precisely control the internal structure of all types of films due to timely changes in the coating composition; at the same time, it includes monometallic elements during ion deposition by means of cathodic arc deposition (AIP), due to which the film performance is significantly improved, and, accordingly, a multi-element film with outstanding general properties such as high hardness, low internal stress high adhesion strength, low roughness and good abrasion resistance; in addition, the deposition rate during film production is high.

BRIEF DESCRIPTION OF GRAPHIC MATERIALS

FIG. 1 is a drawing of a General view of the device of the present invention;

FIG. 2 is a structural diagram of a vacuum chamber of the present invention;

FIG. 3 is an expanded plan view of a vacuum chamber;

FIG. 4 is a structural diagram of an ion source in the form of a filament;

FIG. 5 is a block diagram of a holder;

FIG. 6 is an X-ray diffraction (XRD; from the English: X-ray diffraction) spectrum of an AlCrN film obtained using only a cathode arc;

FIG. 7 is an X-ray diffraction spectrum of an AlCrN film obtained by the AMS method using the apparatus of the present invention;

FIG. 8 is a diagram of the hardness of an AlCrN film obtained using only a cathode arc;

FIG. 9 is a diagram of the hardness of an AlCrN film obtained by the AMS method using the apparatus of the present invention;

FIG. 10 is an X-ray diffraction spectrum of a TiAlN film obtained using only a cathode arc;

FIG. 11 is an X-ray diffraction spectrum of a TiAlN film with incorporated elements and an Al ₆₇ Ti ₃₃ N structure adjusted by the AMS method using the apparatus of the present invention;

Fig is a diagram of the hardness of the TiAlN film obtained using only the cathode arc;

FIG. 13 is a diagram of the hardness of a TiAlN film with incorporated elements and an Al ₆₇ Ti ₃₃ N structure adjusted by the AMS method using the apparatus of the present invention;

FIG. 14 is a diagram of acoustic signals from an AlCrN cracking experiment of films prepared according to the prior art;

FIG. 15 is a diagram of acoustic signals from a film cracking experiment obtained by implanting a monoplasmic element Mo while depositing an AlCrN compound by AIP;

FIG. 16 is a block diagram of a cathode arc source of the present invention;

FIG. 17 is a diagram of a film microstructure obtained using only AIP;

FIG. 18 is a diagram of a film microstructure obtained by implanting an Me element by MS while using AIP.

The main details and the corresponding numbers on the graphic materials are as follows: motor 1 of the carrier trolley; carrier trolley 2; holder 3; bracket 4 of the vacuum chamber; lifting screw 5; coil 6; viewing window 7; source 8 of the cathode arc; magnetron sputtering source 9; a source of 10 ions in the form of a filament; gas flow interface 11; vacuum space 12; high vacuum valve 13; molecular pump 14; fore-vacuum valve 15; pre-pump valve 16; bypass (bypass) valve 17; Roots pump 18; pressure maintenance pump 19; mechanical pump 20; bracket 21 of the vacuum system; auxiliary anode 22; crucible source 23 of evaporation; substrate 24; protective cover 25; reflector 26; workpiece 27; the intermediate layer 28; AlCrMeN 29 composition; MeNx 30 composition; AlCrN 31 composition.

DETAILED DESCRIPTION OF THE EMBODIMENTS OF THE INVENTION

Further, the present invention is described in combination with graphic materials as follows.

As shown in FIG. 1 and FIG. 2, a device for producing a multi-alloy alloy composite film of the present invention includes a heating system, an air supply system, a cooling system, a vacuum system, a vacuum chamber, a holder 3, a lifting mechanism, an evaporation crucible source 23, a magnetron sputtering source 9, a cathode arc source ( CAE source), electromagnetic field generator and electrical control system; the vacuum system is connected to a vacuum chamber; the lifting mechanism is connected to the holder 3 through the transmission; the air supply system is connected to a vacuum chamber; the electrical control system is electrically connected to a crucible evaporation source 23, a magnetron sputtering source 9, a cathode arc source 8, an electromagnetic field generator and a heating system; a crucible evaporation source 23, a magnetron sputtering source 9, and a cathode arc source 8 are located in a vacuum chamber; the target-substrate distance of the cathode arc source 8 lies in the range from 160 mm to 230 mm; the target-substrate distance of the magnetron sputtering source 9 lies in a range from 50 mm to 75 mm.

The vacuum system pumps air from the vacuum chamber to form a vacuum space 12, so that a composite film of a multi-element alloy can be obtained in a vacuum medium that meets the technological standard. As shown in FIG. 5, the holder 3 is used to fix the cutting tool to be coated and to allow the cutting tool to move in a two-dimensional plane, and the lifting mechanism is used to move the holder 3. In this case, the two-dimensional movement of the holder 3 and the upward movement of the lifting mechanism can be carried out with using a helical gear, which is widely used in the field of mechanical machinery. In a particular embodiment of the present invention, it is also possible to add a carrier carriage motor 1 and a carrier carriage 2; a lifting screw 5 is used as a lifting mechanism; the bracket 4 of the vacuum chamber is used as a support for the vacuum chamber, and a coil 6 is located above the vacuum chamber.

An evaporation crucible source 23 is used to coat TiN, CrN, and ZrN composites during film production and to provide gas ion etching as the receiving anode of the auxiliary ionization source. In addition, the crucible source of evaporation 23 can clean the vacuum chamber by evaporation with low operating costs and good diffraction and ensure the stability of continuous operation, which is especially important when obtaining a non-conductive film for a long time.

The cathode arc source 8 is used in an AIP-oriented process, during the preparation of a composite film from a multi-element alloy, and during the incorporation of many elements from materials of multi-element alloys.

The magnetron sputtering source 9 is used in the process of implantation of microelements during the production of a composite film from a multi-element alloy.

A heating system is used to heat a vacuum chamber during the production of a composite film of a multi-element alloy, so that a stable ambient temperature is maintained during the production.

The cooling system is used for timely cooling of the vacuum chamber to meet the requirements of the cooling process during the production of a composite film of a multi-element alloy.

The gas supply system is mainly used to pump gases, such as Ar, N ₂ , H ₂ and O ₂ , into a vacuum chamber with precise control of their quantity. In the present invention, it is preferable to use a 6-channel mass flow control system with a maximum flow rate ranging from 300 cm ³ / s to 1000 cm ³ / s.

The electromagnetic field generator of the device is used to generate an alternating electric field, providing not only the fast movement of the active spots of the arc along the circular ring, but also their movement back and forth along the radial direction under the influence of the alternating electromagnetic field, so that the speed of the active spots of the arc is higher, and their size is larger; (due to the alternating electromagnetic field, the speed and size of the active spots of the arc increase by more than 30% compared with active spots that are not driven by an alternating electromagnetic field); in addition, the plasma formed near the surface of the evaporated materials can be pushed by an alternating electromagnetic field into the coating region (by a distance exceeding 300 mm), which can significantly increase the plasma density in the vacuum chamber, improve the environment and conditions for the coating of the ions participating in the reaction and due to this, significantly improve the quality of the coating of the ions participating in the reaction.

Using the device for producing a multi-alloy alloy composite film of the present invention, the following coating methods can be implemented to improve the overall performance of the workpiece 27 to be coated.

In the prior art, only one of such technologies as VE, MS and AIP is usually used; or first use AIP to obtain the lower part of the film, and then MS to obtain the upper part of the film, that is, AIP and MS are used separately. When using this method, the materials of the individual films are not fused with each other, but cover the surface of the workpiece with 27 layers with separate characteristics; the outstanding performance properties of many materials cannot be used as a whole; accordingly, the general properties of the resulting film remain low.

Since in the device of the present invention, the cathode arc source and the magnetron sputtering source 9 are combined in a vacuum chamber and their spatial arrangement is optimized, the target-substrate distance of the cathode arc source 8 lies in the range from 160 mm to 230 mm, and the target is substrate "magnetron sputtering source 9 is in the range from 50 mm to 75 mm The distance "target substrate" means the distance from the source 8 of the cathode arc or magnetron source 9 of the spray to the surface of the workpiece 27, which must be coated. Accordingly, using the device of the present invention, a combined AIP and MS method can be implemented; due to the implantation of trace elements by means of MS and the simultaneous deposition of ions by means of AIP, it is possible to ultimately obtain a film with multi-element alloy materials and monometallic elements combined in one layer. Since the performance of the film is further improved by the inclusion of monometallic elements, the film obtained in this way can have such general performance as high hardness, low internal stress, high adhesion, low roughness, good abrasion resistance and high deposition rate.

The device of the present invention primarily uses AIP deposition and a multi-element alloy material to produce a composite multi-element film using a cathode arc source (CAE) 8, while the MS technical scheme (the combination of AIP and MS is briefly referred to as AMS) is used for implantation of trace elements, the relative whose content is less than 1%. In this case, it is possible to precisely control the physical structure of the film, and it is possible to obtain a physical structure with optimal mechanical characteristics. In FIG. 17 shows the film structure in the case where the current Me on the target is 0 A, that is, the film was obtained using only AIP; substrate 24 is shown at the bottom of the figure, intermediate layer 28 is located after substrate 24, and AlCrN composition 31 is located after intermediate layer 28. FIG. 18 shows the film structure with increasing current Me on the target, that is, the film that is obtained by MS and into which the Me element is implanted; such a structure is characterized by the shape of a short-columned structure. A substrate 24 is shown at the bottom of the figure, an intermediate layer 28 is located after the substrate 24, and the AlCrMeN composition 29 and the MeNx composition 30 are located after the intermediate layer 28. From a comparison of FIG. 7 and FIG. 8, it can be seen that if the current Me on the target is 0 A, then the coating grows in the form of a columnar crystal; if the Me current on the target increases, a part of Me atoms penetrates into the MeNx crystal, replacing Cr atoms for solid solution hardening of the coating; the other part of Me atoms forms small MeNx grains among AlCrN crystals, inhibiting the further growth of AlCrN crystals with the aim of hardening.

The dual vaporization method combining VE and MS can be carried out in the apparatus of the present invention, that is, the metal elements are vaporized in a crucible vapor source, and then other elements are implanted by the magnetron sputtering source during the deposition of metal compounds on the surface of the workpiece; thus, a composite film made of a multi-element alloy is formed on the surface of the workpiece; in a specific embodiment of the present invention, the Ti element is vaporized by an electron beam source 23 into a gas mixture of N ₂ and Ar to form a conventional TiN film; then element X is implanted using a magnetron sputtering source 9 during deposition of a TiN film to deposit a coating layer (Ti _X , Me _1-X ) N on the surface of the workpiece of the workpiece; element X is at least one or more of Al, Cr and Sr. TiN is an ideal film system with a broad base for production; for example, methods such as AIP, MS, and VE can satisfy industrial requirements. TiN, as an ideal coating material for low-speed cutting tools, has outstanding physical and chemical properties such as high hardness, low friction coefficient and favorable compatibility with chemicals. Due to the ability to reduce adhesion between the cutting edge and the material being processed and to increase the service life and technological efficiency of the cutting tool, TiN remains one of the film materials widely used at present. However, traditional TiN has low hardness and low wear resistance and thermal stability, which limits its wider use. The improvement of TiN films is mainly related to aspects of new TiN-based alloys and multi-element composite layers. In addition, binary nitrides and carbides of transition metals are always mutually soluble. The addition of certain elements to a TiN film can lead to the formation of a composite nitrogen compound, which can fundamentally change the performance of a TiN film and, consequently, increase wear resistance and thermal stability. A multi-element alloy, the basis of which is TiN, can change and regulate the physical structure of the film and make it possible to obtain the so-called (Ti _X , Me _1-X ) N film. Elements of a multi-element alloy include C, Si, Cr, Al, Mo, W, V, Zr, Y, and La, and the like.

Using an AIP deposition oriented device, it is possible to produce insulating oxide films. AIP promotes ionization, but the deposition rate of the coating is high; if there is an excess of O ₂ or the initial electric field changes, O _{2 is} more likely to react on the surface of the cathode target and generate oxides, which will lead to cessation of the cathode discharge and the inability to exit the necessary elements. Currently, the oxide in PVD is mainly alumina. Since Al and AITi-based materials are more likely to react with O ₂ , adding some Cr to Al-based materials can usually effectively stop the oxidation of the target surface. However, chromium oxide, which has low stability, will change the operational characteristics of the films. Therefore, it is characteristic of the prior art that, despite the high deposition rate by AIP, it is not possible to obtain a high-quality insulating oxide film using AIP. However, the alternating electromagnetic field that is generated by the electromagnetic field generator and control system when using the device of the present invention can cause O ₂ to shift to the workpiece 27 to be coated from the target, which prevents the formation of oxides due to the O ₂ reaction on the surface of the cathode target. Accordingly, it is possible to obtain an oxide film with high performance and overcome the disadvantages of the technology according to the prior art, consisting in the fact that AIP cannot be used to obtain oxide insulation.

As shown in FIG. 4, the device further comprises an ion source in the form of a filament; this ion source in the form of a filament is in a vacuum chamber; an ion source in the form of a filament is electrically connected to an electrical control system. An ion source in the form of a filament, new used in the present invention, can significantly enhance the effect of gas etching. For coating cutting tools, vacuum etching and activation are of great importance. The device of the present invention uses not a high threshold metal bombardment conventional for gas etching, but a low threshold etching by gas ions, which provides a more uniform and integrated cleaning effect and guarantees the integrity of the cutting tool blade. In addition, the ion source in the form of a filament, newly used in the present invention, can additionally play a role in internal heating, increasing the intensity of ionization and promoting deposition, as well as increasing the amount of plasma during ion deposition with separate evaporation.

The electrical control system includes an ion source power source, a plasma field power source, a magnetron sputtering power source, a cathode arc source power source and a grid bias voltage source; a plasma field power source is connected to an ion source power source and an ion source in the form of a filament; The power supply of the magnetron atomization source is connected to the magnetron atomization source, the power source of the cathode arc source is connected to the cathode arc source 8, and the grid bias voltage source is connected to the workpiece 27 to be coated during operation of the device. The power source of the ion source supplies power to the ion source in the form of a filament; the plasma field power source supplies arc power to the ion source in the form of a filament; the power source of the magnetron sputtering source supplies power to the magnetron sputtering source 9 and the cathode arc power supply supplies power to the cathode arc source 8. The grid bias voltage source provides an electric field for controlling the movement of charged ions. The electrical control system predominantly supplies power with adjustable parameters to the corresponding electrical components of the device; the voltage and current parameters of the above power sources can be adjusted using existing control methods in accordance with the requirements of the process; accordingly, the device can control the process by adjusting the parameters of each power source; in addition, power supply parameters can be adjusted using a hardware circuit or a combination of software and hardware.

The heating system comprises an internal electron beam heating system located in the center of the vacuum chamber, and an external radiation heating system located around the wall of the vacuum chamber furnace. The design, combining internal heating and external heating, according to the present invention increases the integrity of the heating and effectively maintains the uniformity of the temperature field during operation of the AMS system, which meets the requirements of the deposition process. In a specific embodiment of the present invention, the device uses an ion source in the form of a filament as an internal heating unit and an external radiation heating system based on heating an ion source in the form of a filament.

As shown in FIG. 3, the magnetron sputtering source 9 is symmetrically placed on the inner wall of the vacuum chamber; the source 8 of the cathode arc is helically placed on the inner wall of the vacuum chamber, if we take the center of rotation of the vacuum chamber as the axis of symmetry. The spiral arrangement can ensure full use of space, respectively, the number of sources (targets) of the cathode arc can be increased to 8 or more, significantly increasing the ability of the device to regulate and control film compositions, which allows using the device to obtain films with a more complex composition and outstanding overall operational characteristics.

The vacuum chamber comprises a molecular pump 14, a Roots vacuum pump 18, a mechanical pump 20, and a pressure maintenance pump 19; a molecular pump 14 is connected to a vacuum chamber; a pressure maintenance pump 19 is connected to an air outlet that is connected to a molecular pump 14; The Roots vacuum pump 18 is connected to the air outlet of the molecular pump 14, and the mechanical pump 20 is connected to the air outlet of the Roots vacuum pump 18. The fore-vacuum valve 15, the preliminary pumping valve 16 and the bypass valve 17 can be installed in the pipeline of the vacuum system. In this case, the molecular pump 14 is used to set the final pressure in the vacuum chamber, working pressure, the time of creating a high vacuum and ensuring the stability of the pressure when applying the coating without pumping oil or the need for additional time to start and stop. A mechanical pump 20 is used to pump air from the vacuum chamber to a pressure value that meets the requirements of the molecular pump with respect to the air inlet and air outlet. It determines the time required to create a low vacuum. The pressure maintaining pump 19 is used to maintain the outlet pressure in the air outlet of the molecular pump 14 and to maintain the normal operation of the vacuum chamber under conditions when the main pump is open. The pressure maintenance pump 19 may be a centrifugal vane pump. The vacuum system is rigidly mounted on the bracket 21 of the vacuum system.

An inspection window 7 is mounted on a vacuum chamber. The location of the viewing window 7 can help operators evaluate the situation in the vacuum chamber in real time. The gas flow separation surface 11 is also located on the vacuum chamber, so that the corresponding gas can be pumped into the chamber during operation of the device.

As shown in FIG. 16, the device also includes a protective casing 25; this protective casing 25 is mounted on the source side 8 of the cathode arc facing the holder 3; in addition, on the side of the protective casing 25, a reflector 26 is located behind the cathode source 8. AIP promotes ionization, but the coating deposition rate is high; if there is an excess of O ₂ or the initial electric field changes, O _{2 is} more likely to react on the surface of the cathode target and generate oxides, which will lead to cessation of the cathode discharge and the inability to exit the necessary elements. Currently, the oxide in PVD is mainly alumina. Since Al and AlTi-based materials are more likely to react with O ₂ , adding some Cr to Al-based materials can usually effectively stop the oxidation of the target surface. However, chromium oxide, which has low stability, will change the operational characteristics of the films. Therefore, it is characteristic of the prior art that, despite the high deposition rate by AIP, it is not possible to obtain high-quality insulating oxide films using AIP. In the present invention, the above structure is used to effectively protect the target surface, to prevent the penetration of O ₂ into the surface of the cathode target and can provide a bias of O ₂ that flows around the target surface to the workpiece 27 to be coated from the target surface, which prevents the formation of oxides due to the O ₂ reaction on the surface of the cathode target. Accordingly, it is possible to obtain an oxide film with high performance and overcome the disadvantages of the technology according to the prior art, consisting in the fact that AIP cannot be used to obtain oxides.

The vacuum chamber is equipped with a temperature measuring unit and a vacuum measuring unit. Thanks to the optional temperature measuring unit and the vacuum measuring unit, the temperature and vacuum level in the vacuum chamber can be measured, respectively, these two parameters can be precisely controlled during the coating process.

The cooling system is a multi-channel cooling system with water circulation. A multi-channel cooling system with water circulation can provide an acceptable cooling effect and thereby save resources and costs.

The method for producing a composite film from a multi-element alloy of the present invention is intended to include monometallic elements using a magnetron sputtering source 9 during the deposition of ions of materials of a multi-element alloy using a cathode arc source 8 to obtain a composite film from a multi-element alloy. In the prior art coating method, AIP or MS are used separately, therefore it is not possible to combine the advantages of the two methods, and the resulting films cannot simultaneously have many outstanding performance characteristics. In contrast, in the present invention, the monometallic elements are turned on using a magnetron sputtering source 9 during the deposition of ions of the materials of the multi-element alloy using the cathode arc source 8 to obtain a composite film of the multi-element alloy. Accordingly, it is possible to precisely control the metallurgical structure of the films, and the performance of the film coating can be optimized and adjusted according to needs; in addition, during the preparation of the film, a high deposition rate can be obtained, so that the resulting film has higher technical characteristics than films according to the prior art.

A method of producing a composite film from a multi-element alloy using the device of the present invention is as follows:

A. AIP and MS

(1) Pretreatment:

Place the cutting tool in the coating chamber after drying it after cleaning in a standard slightly alkaline detergent and dehydration with alcohol under the action of ultrasonic waves before coating;

(2) Preparations before coating:

- Aerate the vacuum chamber and open the oven door;

- If necessary, replace target materials of the cathode arc source and magnetron sputtering source and replace the glass of the viewing window;

- Clean all parts of the furnace body with a high-pressure pneumatic device at an air pressure of 0.6 MPa;

- Select the appropriate clamp for fixing the workpiece 27 (cutting tool); make sure that the clamp movement is correct;

- Check the insulation state of the ion source in the form of a filament, cathode arc source 8, magnetron sputtering source, auxiliary anode 22 and clamp 27 for the workpiece; resistance value should be more than 100 KOhm;

- Close the evaporation chamber and close the ventilation valve.

(3) Evacuation (up to 5 × 10 ^-2 Pa) and preheating

- Turn on the water cooling unit;

- Open the mechanical pump 20, the Roots vacuum pump 18 and the pre-pump valve 16;

- Turn on the composite vacuum gauge, turn on the thermocouple vacuum gauge 1 to measure the vacuum in the foreline; vacuum pressure should be less than 5 Pa;

- Turn on the molecular pump 14;

- If the molecular pump 14 is operating normally and the vacuum pressure in the vacuum chamber is less than 5 Pa, close the preliminary pumping valve 16 and open the fore-vacuum valve 15 and the high vacuum valve 13;

- If the vacuum value is less than 5 × 10 ^-2 Pa, pump 40-60 cm ³ / min Ar and turn on auxiliary heating (5 kW);

- Bring the workpiece 27 into rotational motion and adjust the frequency to 15 Hz;

- Enter the mixed heating phase after 40 minutes.

(4) Electron beam heating

- Adjust the pressure in the vacuum chamber to 2.5 × 10 ^-1 Pa, and the flow Ar to 90-120 cm ³ / min;

- Turn on the power source of the ion source in the form of a filament and slowly increase the current to 170-230 A;

- Turn on the magnetic field and adjust the current to 12-20 A;

- Turn on the power source of the plasma field and switch it to the position for heating;

- Light the arc and gradually increase the current to 180 A;

- Mixed heating time: 40-70 min.

(5) Gas plasma etching

- Maintain current through the filament at a level of 170-230 A;

- Reduce the current of the plasma field power source to 100-120 A;

- Reduce the magnetic field current to 6-8 A;

- Adjust the pressure in the vacuum chamber to 2 × 10 ^-1 Pa, the flow of Ar - up to 50-65 cm ³ / min and the flow of H ₂ - up to 12-20 cm ³ / min;

- Turn on the voltage source of the grid bias and gradually increase the voltage to 2-200V and the pulse voltage to 300-500V;

- The time of ion etching is approximately 80-150 minutes

(6) Coating

- Layer Ti, Cr and Zr: flow Ar: 80-140 cm ³ / min; bias voltage: 800-1000V; include 2 sources of cathode arcs (Ti, Cr, Zr); arc target current: 70-100A; period: 180-600 s;

- Layer TiN, CrN and ZrN: flow Ar: 480-680 cm ³ / min; bias voltage: 150V; include 2 sources of the cathode arc (Ti, Cr, Zr); arc target current: 100-100A; period: 180-600 s;

- TiAl layer: Ar flow: 540-900 cm ³ / min; bias voltage: 100-120V; include 4 sources of the cathode arc (TiAl); arc target current: 100-120A; period: 3600-7200 s;

- Turn on 2 magnetron sputtering sources 9; spray current: 1-3 A; period: 3600-7200 s; stream N ₂ : 540-900 cm ³ / min; bias voltage: 80-100V;

- Turn off 4 sources of the cathode arc (TiAl); turn on 2 sources of the cathode arc (TiAl); arc target current: 100-120 A; period: 1800-3600 s; stream N ₂ : 540-900 cm ³ / min; O ₂ stream: 30-100 cm ³ / min;

- Turn off the source of the cathode arc, the magnetron sputtering source and the voltage source of the grid bias;

- Turn off the heat source, sources N ₂ and O ₂ ; turn off the molecular pump 14; turn on the pressure maintenance pump 19 and pump 80-120 cm ³ / min N ₂ ;

- Download Ar to 30 Pa.

(7) Cooling: process time: 60-120 min.

B. VE and MS

(1) Pretreatment:

Place the cutting tool made of high-speed steel or hard alloy (no special polishing is required) in the coating chamber after cleaning in a standard weakly alkaline detergent and dehydration with alcohol under the action of ultrasonic waves before coating ;.

(2) Inspection device:

- Carry out aeration of the chamber and open the oven door;

- If necessary, replace the target materials of the magnetron sputtering source and replace the glass of the viewing window;

- Replace the source of evaporation and add new evaporating materials in an amount of 20-30 g (Ti);

- Clean all parts of the furnace body with a high-pressure pneumatic device at an air pressure of 0.6 MPa;

- Select the appropriate clamp for fixing the workpiece 27 (cutting tool); make sure that the clamp movement is correct;

- Check the insulation state of the electron gun, evaporation source 23, magnetron sputtering source, auxiliary anode 22 and clamp 27 for the workpiece; resistance value should be more than 100 KOhm;

- Lift the base plate, close the evaporation chamber and close the ventilation valve.

(3) Evacuation and preheating

- Turn on the water cooling unit;

- Open the mechanical pump 20, the Roots vacuum pump 18 and the pre-pump valve 16;

Turn on the composite vacuum gauge, turn on the thermocouple vacuum gauge 1 to measure the vacuum in the foreline; vacuum pressure should be less than 5 Pa;

- Turn on the molecular pump 14;

- If the molecular pump 14 is operating normally and the vacuum pressure in the vacuum chamber is less than 5 Pa, close the preliminary pumping valve 16 and open the fore-vacuum valve 15 and the high vacuum valve 13;

- If the vacuum value is less than 1 × 10 ^-2 Pa, pump 40-60 cm ³ / min Ar and turn on auxiliary heating (5 kW);

- Bring the workpiece 27 into rotational motion and adjust the frequency to 20 Hz;

- Enter the mixed heating phase after 40 minutes.

(4) Electron beam heating

- Adjust the pressure in the vacuum chamber to 2.5 × 10 ^-1 Pa, and the flow of Ar to 90-110 cm ³ / min;

- Turn on the power source of the ion source in the form of a filament and slowly increase the current to 170-230 A;

- Turn on the magnetic field and adjust the current to 12-20 A;

- Turn on the power source of the plasma field and switch it to the position for heating;

- Light the arc and gradually increase the current to 180 A;

- Mixed heating time: 40-100 min.

(5) Gas plasma etching

- Maintain the current of the ion source in the form of a filament at a level of 170-230 A;

- Reduce the current of the plasma field power source to 100-120 A;

- Reduce the magnetic field current to 6-8 A;

- Adjust the pressure in the vacuum chamber to 2 × 10 ^-1 Pa and the flow of Ar - up to 50-65 cm ³ / min;

- Turn on the voltage source of the grid bias and gradually increase the voltage to 2-200V and the pulse voltage to 300-500V;

- The time of ion etching is approximately 50-90 minutes.

(6) Coating

- Maintain the current of the ion source in the form of a filament at a level of 170-230 A;

- Adjust the flow of Ar to 23-35 cm ³ / min;

- Adjust the field current to 25-35 A;

- Adjust the mixing voltage to 0-200 V and the pulse voltage to 300-500V;

- Increase the plasma source current to 200 A (5 min);

- Apply a transition layer of metallic Ti for 5-20 minutes;

- Download N ₂ at a speed of 80-120 cm ³ / min;

- Adjust the bias voltage to 180V (10 min);

- Turn on the power source of the target magnetron sputtering source; 1.0-2.0 A (AlTiCr, C, Cr, Zr and Si, etc.);

- Adjust the bias voltage to 100-150V (10 min);

- Coating time: 20-50 min;

- Turn off the power source of the target magnetron sputtering source, the power source of the filament, the power source of the magnetic field, the heating source and the source of N ₂ ; turn off the molecular pump 14 and turn on the pressure maintenance pump 19;

- Download Ar to 30 Pa.

(7) Cooling: process time: 60-120 min.

Comparison of test results:

With regard to comparing AlCrN coatings obtained only by AIP and AlCrN coatings obtained by AMS using the device of the present invention, as shown in FIG. 6 and FIG. 7, the two coatings have a difference in diffraction peaks (111) and (200); the addition of the trace element Mo increases the diffraction intensity of AlCrN (200). As shown in FIG. 8 and FIG. 9, the hardness of the AlCrN coating film obtained by AMS using the device of the present invention increased by 10% with the addition of Mo.

As shown in FIG. 10 and FIG. 12, in the case of a TiAlN coating prepared by only AIP, the TiN (200) diffraction intensity is higher, the TiAlN (200) diffraction intensity is lower, and the film hardness is in the range of about 2400 to 3000 HV (Vickers hardness).

As shown in FIG. 11 and FIG. 13, in the case of a TiAlN coating obtained by AMS using the device of the present invention, after adding the elements and establishing the Al ₆₇ Ti ₃₃ N structure, the diffraction intensity of TiAlN (200) significantly changed, and the film hardness increased to about 3500-4000 HV.

FIG. 14 and FIG. 15 are diagrams of acoustic signals detected by acoustic energy during cracking caused by cracking experiments performed on films obtained by the prior art method and films obtained by the method of the present invention by implanting monometallic elements during AIP ion deposition. From graphical materials it can be seen that the acoustic energy during the formation of cracks caused in the films obtained according to the present invention is significantly lower compared to the films obtained according to the prior art, which indicates that the hardness of the film obtained according to the present invention significantly higher than the film obtained according to the prior art.

Claims (5)

1. A device for producing a composite film of a multi-element alloy containing a heating system, an air supply system, a cooling system, a vacuum system, a vacuum chamber, a workpiece holder (3), a lifting mechanism, an evaporation crucible source (23), a magnetron source (9) spraying, the source (8) of the cathode arc, a protective casing (25), an electromagnetic field generator and an electrical control system, while the vacuum system is connected to the vacuum chamber, the lifting mechanism is connected to the holder (3) of the processing of the workpiece through the transmission, the air supply system is connected to the vacuum chamber, the electrical control system is electrically connected to the crucible source (23) of evaporation, the magnetron source (9) of atomization, the source (8) of the cathode arc, the electromagnetic field generator and the heating system, while the crucible the evaporation source (23), the magnetron sputtering source (9) and the cathode arc source (8) are located in the vacuum chamber, and the distance from the cathode arc source (8) to the surface of the workpiece (27) is from 1 60 mm to 230 mm, the distance from the magnetron source (9) of sputtering to the surface of the workpiece (27) is from 50 mm to 75 mm, and the protective casing (25) is installed on the source side (8) of the cathode arc facing the holder (3) the workpiece, and on the side of the protective casing behind the source (8) of the cathode arc is a reflector (26). 2. The device according to p. 1, characterized in that it further comprises a source (10) of ions in the form of a filament, which is located in a vacuum chamber and is electrically connected to the electrical control system. 3. The device according to claim 2, characterized in that the electric control system comprises an ion source power source, a plasma field power source, a magnetron sputter power source, a cathode arc source power source and a grid bias voltage source, the plasma field power source being connected to the ion source power source and the ion source (10) in the form of a filament, the power supply of the magnetron sputtering source is connected to the magnetron sputtering source (9) and the power source I cathodic arc source connected to a source (8) cathodic arc. 4. The device according to claim 1, characterized in that the heating system comprises an internal electron beam heating system located in the center of the vacuum chamber, and an external radiation heating system located around the wall of the vacuum chamber furnace. 5. The device according to claim 1, characterized in that the vacuum chamber contains a molecular pump (14), a Roots vacuum pump (18), a mechanical pump (20) and a pressure maintaining pump (19), wherein the molecular pump (14) is connected to a vacuum chamber, a pressure maintaining pump (19) is connected to an air outlet that is connected to a molecular pump (14), a Roots vacuum pump (18) is connected to an air outlet of a molecular pump (14), and a mechanical pump (20) is connected to a vacuum outlet Roots pump (18).

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