CN112522677A - Composite coating device - Google Patents
Composite coating device Download PDFInfo
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- CN112522677A CN112522677A CN202011334802.8A CN202011334802A CN112522677A CN 112522677 A CN112522677 A CN 112522677A CN 202011334802 A CN202011334802 A CN 202011334802A CN 112522677 A CN112522677 A CN 112522677A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/50—Substrate holders
- C23C14/505—Substrate holders for rotation of the substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
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Abstract
The invention discloses a composite coating device, which comprises a vacuum chamber and a workpiece rotating stand positioned in the vacuum chamber, wherein an ion beam source, a pulse arc ion source and a magnetic filtration arc ion source are integrated in the vacuum chamber; the ion beam source is used for cleaning a workpiece or assisting deposition; the pulsed arc ion source is used for exciting the graphite target to generate carbon ions and depositing the Ta-C carbon film; the magnetic filtering arc ion source is used for exciting the metal target material, generating metal ions and depositing a metal film, an alloy film or a compound film. The device integrates three technologies of ion beam technology, magnetic filtration ion plating and pulse ion plating into a vacuum chamber, provides various film coating modes, realizes multifunctional and structural advanced film preparation, has the characteristics of rich functions and strong expansibility, and is suitable for developing scientific research and diversified production in the industrial field. Particularly, the Ta-C carbon film with low stress, high bonding strength and adjustable structure and performance can be efficiently prepared by utilizing the device.
Description
Technical Field
The invention belongs to the technical field of vacuum coating, and particularly relates to a composite coating device.
Background
The tetrahedral amorphous carbon Ta-C carbon film has extremely high hardness and lower friction coefficient, and is an abrasion-resistant film widely applied in the fields of machinery, electronics, textile, automobile, aerospace and the like. However, the Ta-C carbon film has high residual stress, low toughness and high brittleness, so that the bonding strength between the film and the substrate is poor, the film is easy to fall off in the using process, and the deposition thickness and the application of the diamond-like carbon are limited. With the continuous development of film preparation technology, analysis and test means and nanotechnology, people continuously deepen the understanding of the structure and the performance of the traditional film, and the research on the Ta-C carbon film is also developed from single-layer and single-component to composite, gradient and multi-layer. The multilayer composite structure is prepared or element doping is carried out by adopting multiple technology integration, so that the residual stress of the Ta-C carbon film can be effectively reduced, the binding force between the Ta-C carbon film and a substrate is improved, and the application value of the Ta-C carbon film is improved.
The prior art has the following defects: the preparation method of the Ta-C coating has the following problems:
(1) the Ta-C carbon film is mainly prepared by a direct current arc ion plating technology, a magnetic filtration arc ion plating technology and a sputtering technology. Although the direct current arc ion plating technology has higher ionization rate and deposition rate, large particle pollution is brought, and the quality of the Ta-C carbon film is influenced; although large particles can be filtered by the magnetic filtration arc ion plating technology, the speed of the deposition process can be reduced, so that the target utilization rate and the film coating efficiency are lower; although the sputtering technology has less large particles, the utilization rate of the target material is low, the ionization rate is low and the coating rate is low; the three technologies can not accurately control the energy of carbon ions, and the structure and the performance of the Ta-C carbon film can be regulated and controlled.
(2) The transition layer is mainly prepared by sputtering or direct current arc technology, the target ionization rate of the sputtering technology is usually less than 40%, the deposition rate is low, and the direct current arc technology inevitably brings large particle pollution.
The technology for preparing the Ta-C carbon film and the transition layer is combined to prepare the Ta-C carbon film and the composite film thereof, the structure and the performance of the Ta-C carbon film cannot be accurately regulated, and the Ta-C carbon film often has low production efficiency, poor film quality and a complex equipment structure.
Disclosure of Invention
The purpose is as follows: in order to overcome the defects in the prior art, the invention provides a composite coating device.
The ion beam technology, the magnetic filtration arc ion plating technology and the pulse arc ion plating technology are invented by the preschool university, and the ion beam technology is mainly used for auxiliary coating, can carry out ion cleaning and etching, and improves the surface quality of a matrix and the film-substrate binding force. The magnetic filtration arc ion plating has the characteristics of high evaporation rate, strong ion energy, few large particles and the like, and can be used for preparing common metal films (Ti, Cr, Cu, Al and the like), alloy films (Ti/Al, Ti/Cr and the like) or compound films (TiN, CrN, TiCN and the like). The pulse arc ion plating technology can prepare the Ta-C carbon film, the ionization rate of the graphite target material is high, negative bias is not needed, the deposition temperature is low, and the structure and the performance of the prepared Ta-C carbon film can be regulated and controlled.
By combining the three technologies, the Ta-C carbon film with a multilayer composite structure can be prepared or element doping is carried out, the application value of the Ta-C carbon film is improved, an alloy film or a multilayer composite film with certain periodicity can be prepared, and the advanced film preparation with multiple functions and structure is realized.
The technical scheme adopted by the invention is as follows:
a composite coating device comprises a vacuum chamber and a workpiece rotating stand positioned in the vacuum chamber, wherein an ion beam source, a pulse arc ion source and a magnetic filtration arc ion source are integrated in the vacuum chamber;
the ion beam source is used for cleaning a workpiece or assisting deposition;
the pulsed arc ion source is used for exciting the graphite target to generate carbon ions and depositing a Ta-C carbon film;
the magnetic filtering arc ion source is used for exciting the metal target material, generating metal ions and depositing a metal film, an alloy film or a compound film.
In some embodiments, the ion beam source is mounted on the side wall of the vacuum chamber, the central axis of the ion beam source passes right above the center of the workpiece rotating stand, and a tungsten wire is mounted right above the ion source and used for generating a thermionic neutralizing ion flow;
the pulse arc ion source is arranged on the side wall of the vacuum chamber, and the central axis of the pulse arc ion source passes through the position right above the circle center of the workpiece rotating stand;
the magnetic filtering arc ion source is arranged on the side wall of the vacuum chamber and is positioned at the same height with the pulse arc ion source, and the axis of the magnetic filtering arc ion source is parallel or vertical to the axis of the pulse arc ion source.
Furthermore, the second movement direction of the ion current generated by the magnetic filtering arc ion source is finally crossed or overlapped with the first movement direction of the carbon ion current generated by the pulse arc ion source.
In some embodiments, the ion beam source is a hall ion source, an anode layer ion source;
the electric arc discharge of the pulse electric arc ion source is pulse electric arc, and circulating cooling water is introduced into the target material.
In some embodiments, the deflection coil of the magnetic filtering arc ion source can change the magnetic field intensity by adjusting the working current to be 0-3A, so that the deflection angle of the ion flow can be adjusted to be 60-90 degrees.
In some embodiments, the composite coating device further comprises:
the filament current is adjustable from 0mA to 500mA, and the filament current is adjustable;
the pulse arc ion source power supply is used for supplying power to the pulse arc ion source, the pulse width is 10-500 ms adjustable, the frequency is 1-30 Hz adjustable, the working voltage is 100-350V adjustable, the energy of carbon ions can be adjusted to be changed in the range of 25eV-100eV by adjusting the working voltage, the pulse frequency and the pulse width, and the proportion of a diamond phase in the Ta-C carbon film is changed to be 75-88%;
the arc power supply is used for supplying power to the magnetic filtering arc ion source, and the arc current is adjustable from 50 to 150A.
In some embodiments, the composite coating apparatus further comprises a pulsed bias power supply; the positive pole of the pulse bias power supply is connected with the vacuum chamber, the vacuum chamber is grounded, the negative pole of the pulse bias power supply is connected with the workpiece rotating frame, and the workpiece rotating frame is insulated from the vacuum chamber.
Furthermore, the frequency of the pulse bias power supply is 40kHz, the voltage is adjustable from 0V to 1500V, the duty ratio is adjustable from 10% to 90%, and the bias is used for improving the energy of ions and enhancing the film-substrate binding force.
In some embodiments, the composite coating device further comprises a heating system and a vacuum-pumping system;
the heating system is arranged in the vacuum chamber, comprises a heating pipe, a thermocouple and a temperature control module and is used for adjusting the temperature of the vacuum chamber to be 0-500 ℃, and the temperature control precision is +/-5 ℃;
the vacuum pumping system is a secondary vacuum pump set and comprises a turbo molecular pump and a mechanical rotary vane pump.
In some embodiments, the workpiece rotating frame is a planetary gear frame, a plurality of stations are arranged on the workpiece rotating frame, the workpiece rotating frame is driven by a servo motor, and the rotating speed is adjustable from 0 r/min to 3 r/min.
In other embodiments, the magnetically filtered arc ion source is replaced with a dc arc ion source.
Has the advantages that: compared with the prior art, the composite coating device provided by the invention has the following advantages:
(1) the invention integrates the three technologies of ion beam technology, magnetic filtration arc ion plating technology and pulse arc ion plating technology into a vacuum chamber, can prepare a plurality of simple substance films, compound films and element doped films and composite films thereof by selecting different gases and solid target materials, has strong universality and wide application range, and has higher scientific research and industrial popularization values;
(2) the pulsed arc ion source configured by the composite coating equipment can efficiently prepare the Ta-C carbon film, and the magnetic filtration arc ion source is used for preparing the transition layer or doping elements, so that the residual stress in the deposition process of the Ta-C carbon film can be effectively reduced, the bonding force of the Ta-C carbon film is improved, the toughness of the film is improved, and the application value of the Ta-C carbon film is improved;
(3) a plurality of magnetic filtration arc ion sources, a plurality of ion beam sources and a plurality of pulse arc ion sources can be installed according to requirements, the effective coating area is enlarged, and large-area and batch production of the Ta-C carbon film is realized.
Drawings
FIG. 1 is a schematic structural diagram of a composite coating apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an exemplary pulsed arc ion source;
FIG. 3 is a schematic diagram of a magnetic filtering arc ion source according to an embodiment;
FIG. 4 is an XPS spectrum of a Ta-C carbon film prepared by a composite coating apparatus according to an embodiment of the present invention;
in the figure: the device comprises a vacuum chamber 1, an ion beam source 2, an ion beam source power supply 3, a pulse arc ion source 4, a pulse arc ion source power supply 5, a magnetic filtering arc ion source 6, an arc power supply 7, a pulse bias power supply 8, a heating system 9, a workpiece rotating frame 10, a vacuum pumping system 11, a graphite target 12, a pulse type arc 13, circulating cooling water 14, a first movement direction 15, a metal target 16, a deflection coil 17, a second movement direction 18 and a deflection angle 19.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
As shown in fig. 1 to 3, a composite coating apparatus comprises a vacuum chamber 1, an ion beam source 2, an ion beam source power source 3, a pulsed arc ion source 4, a pulsed arc ion source power source 5, a magnetic filtration arc ion source 6, an arc power source 7, a pulse bias power source 8, a heating system 9, a workpiece rotating stand 10, and a vacuum pumping system 11; the ion beam source 2, the pulsed arc ion source 4 and the magnetic filtering arc ion source 6 are combined in one vacuum chamber 1, so that various films and composite films thereof can be prepared, and particularly Ta-C carbon films with adjustable structures and properties can be prepared.
As a further explanation of the above scheme, the ion beam source 2 is a hall ion source, and is installed on the sidewall of the vacuum chamber 1, the central axis of the ion beam source 2 passes through the position right above the center of the circle of the workpiece turret 10, and a tungsten filament is installed right above the ion source for generating a hot electron neutralizing ion flow. The ion beam source 2 is used for cleaning the workpiece or assisting deposition, and the common gas is nitrogen or argon.
The ion beam source power supply 3 is used for supplying power to the ion beam source 2, and filament current is adjustable from 0mA to 500 mA.
The pulse arc ion source 4 is arranged on the side wall of the vacuum chamber 1, the central axis of the pulse arc ion source passes through the position right above the circle center of the workpiece rotating stand 10 and is used for exciting the graphite target material 12, generating carbon ions and depositing a Ta-C carbon film.
The arc discharge of the pulse arc ion source 4 is a pulse arc 13, the circulating cooling water 14 is filled in the target material, the heat generated by the arc discharge can be taken away in the discharge gap, the temperature of the target surface is reduced, the generation of large particles is reduced under the condition of no filtration, the deposition rate is higher, and the film coating rate is not lower than 1 mu m/h.
The pulse arc ion source power supply 5 is used for supplying power to the pulse arc ion source 4, the pulse width is 10-500 ms adjustable, the frequency is 1-30 Hz adjustable, the working voltage is 100-350V adjustable, the energy of carbon ions can be regulated and controlled to change within 25eV-100eV by regulating the working voltage, the pulse frequency and the pulse width, the proportion of a diamond phase in the Ta-C carbon film is changed to be 75-88%, and the regulation and control of the structure and the performance of the Ta-C carbon film are realized.
The magnetic filtering arc ion source 6 is arranged on the side wall of the vacuum chamber 1, is positioned at the same height with the pulse arc ion source 4, has an axis parallel or vertical to the axis of the pulse arc ion source 4, and is used for exciting the metal target material 16 to generate metal ions, depositing metal films (Ti, Cr, Cu, Al and the like), alloy films (Ti/Al, Ti/Cr and the like) or compound films (TiN, CrN, TiCN and the like), and the film coating speed is not lower than 1.5 mu m/h.
The magnetic field generated by the deflection coil 17 of the magnetic filtering arc ion source 6 can deflect the movement direction of the metal ion flow generated by the magnetic filtering arc ion source, large particles which are not ionized are not deflected, and the pollution of the large particles in the film can be reduced.
The deflection coil of the magnetic filtering arc ion source 6 can change the magnetic field intensity by adjusting the working current between 0 and 3A, so that the deflection angle 19 of the ion flow can be adjusted between 60 and 90 degrees.
The second movement direction 18 of the ion current generated by the magnetic filtration arc ion source 6 is finally crossed or overlapped with the first movement direction 15 of the carbon ion current generated by the pulse arc ion source 4, so that the preparation of a multilayer composite Ta-C carbon film or an element-doped Ta-C carbon film can be realized.
The arc power supply 7 is used for supplying power to the magnetic filtering arc ion source 6, and the arc current 50-150A is adjustable.
The positive electrode of the pulse bias power supply 8 is connected with the vacuum chamber 1, the vacuum chamber 1 is grounded, the negative electrode of the pulse bias power supply is connected with the workpiece rotating frame 10, the workpiece rotating frame 10 is insulated from the vacuum chamber 1, the frequency of the pulse bias power supply is 40kHZ, the voltage is 0-1500V adjustable, the duty ratio is 10% -90% adjustable, the bias voltage is used for improving the energy of ions and enhancing the membrane-substrate binding force.
The heating system 9 is installed in the vacuum chamber 1, consists of a heating pipe, a thermocouple and a temperature control module, and is used for adjusting the temperature of the vacuum chamber to 0-500 ℃ with the temperature control precision of +/-5 ℃.
The workpiece rotating frame 10 is arranged in the vacuum chamber 1 and is a planetary gear carrier, a plurality of stations are arranged on the rotating frame, the rotating frame is driven by a servo motor, and the rotating speed is adjustable at 0-3 r/min.
The vacuum pumping system 11 is a secondary vacuum pump set and consists of a turbo molecular pump and a mechanical rotary vane pump.
Furthermore, the composite coating device also comprises a cooling system for taking away heat generated by each ion source in the coating process.
Through the technical scheme, the composite coating device can be provided with a plurality of magnetic filtering arc ion sources, a plurality of ion beam sources and a plurality of pulse arc ion sources according to needs, can realize the functions of ion beam cleaning, ion implantation, simple substance coating, compound coating, multilayer coating, composite coating and the like, and particularly can efficiently prepare the Ta-C carbon film with high quality and adjustable structure and performance.
In other embodiments, the magnetically filtered arc ion source may be replaced with a dc arc ion source.
The ion beam source may also be replaced by a hall ion source as the anode layer ion source.
EXAMPLE 1 preparation of Ti/Ta-C carbon film thin film by the above-described composite coating apparatus
(1) The target material of the pulse arc ion source is graphite, the target material of the magnetic filtration arc ion source is titanium, the gas source of the ion beam source is nitrogen, and the substrate is a silicon wafer.
(2) Cleaning before film coating: sequentially using acetone, ethanol and deionized water to ultrasonically clean the silicon wafer for 10-15 min, and removing pollutants on the surface of the substrate; and (3) putting the silicon wafer subjected to ultrasonic cleaning into a forced air drying oven for drying for 30-45 min, and taking out for later use.
(3) And (3) vacuum pumping: starting composite coating equipment, mounting a coating substrate on a workpiece rotating stand, closing a cabin door of a vacuum chamber, and starting a mechanical rotary vane pump to perform rough vacuum pumping; when the pressure in the vacuum chamber reaches 5Pa, starting the turbo molecular pump to further vacuumize the vacuum chamber until reaching the preset vacuum degree of 5E-3 Pa.
(4) Ion beam cleaning: opening a nitrogen valve, and introducing nitrogen into the vacuum chamber; when the air pressure of the vacuum chamber reaches 0.15Pa, sequentially starting a workpiece rotating frame, an ion beam source and a filament power supply, adjusting parameters to be 2000V and 60mA respectively, exciting an ion beam to bombard a coated substrate, and carrying out plasma cleaning for 3-5 min; and after the end, the filament power supply, the ion beam source and the argon gas valve are closed in sequence.
(5) The heating system was started and heated to 150 ℃ in a vacuum chamber.
(6) And (3) starting the magnetic filtration arc ion source and the pulse bias power supply in sequence, adjusting the cathode current to be 75-90A, the bias voltage to be 600-800V and the coil deflection current to be 2A, lasting for 10-20 min, depositing a Ti transition layer with the thickness of 0.25-0.5 mu m on the surface of the silicon wafer, and closing the magnetic filtration arc ion source, the pulse bias power supply and the heating system in sequence.
(7) After the silicon wafer to be coated is cooled to room temperature, a pulse arc ion source is started, the working voltage is set to be 250-350V, the frequency is set to be 3-10 Hz, 6000 pulses are worked, a Ta-C carbon film with the thickness of 0.3-0.5 mu m is prepared on the surface of the Ti transition layer, and the Ti/Ta-C composite film with the diamond phase proportion of 75-88% and high bonding force is formed.
EXAMPLE 2 preparation of Cr/Ta-C Cr composite film by the above-mentioned composite coating apparatus
(1) The target of the pulse arc ion source is graphite, the target of the magnetic filtration arc ion source is chromium, the gas source of the ion beam source is argon, and the substrate is 304 stainless steel.
(2) Cleaning before film coating: sequentially using a gasoline solvent, ethanol and deionized water to ultrasonically clean the coated substrate for 10-15 min, and removing pollutants on the surface of the substrate; and (3) putting the stainless steel sheet subjected to ultrasonic cleaning into a blast drying oven for drying for 30-45 min, and taking out for later use.
(3) And (3) vacuum pumping: starting composite coating equipment, mounting a coating substrate on a workpiece rotating stand, closing a cabin door of a vacuum chamber, and starting a mechanical rotary vane pump to perform rough vacuum pumping; when the pressure in the vacuum chamber reaches 5Pa, starting the turbo molecular pump to further vacuumize the vacuum chamber until reaching the preset vacuum degree of 1.5E-3 Pa.
(4) Ion beam cleaning: opening an argon valve, and introducing argon into the vacuum chamber; when the air pressure of the vacuum chamber reaches 0.1Pa, sequentially starting a workpiece rotating frame, an ion beam source and a filament power supply, adjusting parameters to respectively reach 3000V and 75mA, exciting an ion beam to bombard the surface of the stainless steel sheet, and carrying out plasma cleaning for 5-10 min; and after the end, the filament power supply, the ion beam source and the argon gas valve are closed in sequence.
(5) The heating system was started and heated to 300 ℃ in a vacuum chamber.
(6) And (3) starting the magnetic filtration arc ion source and the pulse bias power supply in sequence, adjusting the cathode current to be 90A and the bias voltage to be 800-1200V, depositing a Cr film on the surface of the substrate for 5-10 min, preparing the Cr film with the thickness of 0.12-0.25 mu m on the surface of the stainless steel sheet, and closing the magnetic filtration arc ion source, the pulse bias power supply and the heating system in sequence.
(7) After the substrate is cooled to room temperature, simultaneously starting the pulse arc ion source, the magnetic filtration arc ion source and the pulse bias power supply, setting the working voltage of the pulse arc ion source to be 250-300V, the frequency to be 5-15 Hz, the cathode current of the magnetic filtration arc ion source to be 70-90A and the substrate bias voltage to be 900-1200V, continuously working for 15-20 min, and preparing a Cr element doped Ta-C carbon film with the thickness of 0.4-0.6 mu m on the surface of the stainless steel, thereby forming the Cr/Ta-C/Cr composite film with high toughness and low friction.
EXAMPLE 3 preparation of ZrN thin film by the above composite coating apparatus
(1) The target material of the magnetic filtering arc ion source is zirconium, the gas source of the ion beam source is argon and nitrogen, and the matrix is TC4 titanium alloy.
(2) Cleaning before film coating: sequentially using acetone, ethanol and deionized water to ultrasonically clean the titanium alloy substrate for 5-10 min so as to remove pollutants on the surface of the substrate; and (4) putting the substrate cleaned by the ultrasonic wave into a blast drying oven for drying for 30min, and taking out for later use.
(3) And (3) vacuum pumping: starting composite coating equipment, mounting a coating substrate on a workpiece rotating stand, closing a cabin door of a vacuum chamber, and starting a mechanical rotary vane pump to perform rough vacuum pumping; when the pressure in the vacuum chamber reaches 5Pa, starting the turbo molecular pump to further vacuumize the vacuum chamber until reaching the preset vacuum degree of 1.5E-3 Pa.
(4) Ion beam cleaning: opening an argon valve, and introducing argon into the vacuum chamber; when the air pressure of the vacuum chamber reaches 0.15Pa, sequentially starting a workpiece rotating frame, an ion beam source and a filament power supply, adjusting parameters to make the values of the workpiece rotating frame, the ion beam source and the filament power supply respectively 2000V and 75mA, exciting an ion beam to bombard a coated substrate, and carrying out plasma cleaning for 3 min; and after the end, the filament power supply, the ion beam source and the argon gas valve are closed in sequence.
(5) The heating system was started and heated to 250 ℃ in a vacuum chamber.
(6) Opening a nitrogen valve, introducing nitrogen into the vacuum chamber until the air pressure of the vacuum chamber reaches 0.1 Pa; sequentially starting a magnetic filtration arc ion source and a pulse bias power supply, adjusting the cathode current to be 60-80A and the bias voltage to be 1000-1200V, exciting the Zr target, and depositing a ZrN film on the surface of the titanium alloy substrate; and simultaneously, sequentially starting an ion beam source and a filament power supply, adjusting parameters to be 2500V and 60mA respectively, exciting nitrogen ions to bombard the surface of the matrix, and assisting in depositing the ZrN film.
(7) The process lasts for 10min, the magnetic filtration arc ion source, the pulse bias power supply, the heating system, the ion beam source, the filament power supply and the nitrogen valve are closed in sequence, and the ZrN film with the thickness of 200nm is prepared on the surface of the substrate.
EXAMPLE 4 preparation of Ta-C film by the above-mentioned composite coating apparatus
(1) The target material of the pulse arc ion source is graphite, the gas source of the ion beam source is nitrogen, and the substrate is a nitrile rubber sheet.
(2) Cleaning before film coating: carrying out ultrasonic cleaning on an absolute ethyl alcohol substrate for 30-45 min to remove pollutants on the surface of the nitrile rubber; and (3) drying the nitrile rubber subjected to ultrasonic cleaning in a blast drying oven for 60-90 min, and taking out for later use.
(3) Ion beam cleaning: opening a nitrogen valve, and introducing nitrogen into the vacuum chamber; when the air pressure of the vacuum chamber reaches 0.15Pa, sequentially starting a workpiece rotating stand, an ion beam source and a filament power supply, adjusting parameters to be respectively 1500V and 45mA, exciting an ion beam to bombard nitrile butadiene rubber, and carrying out plasma cleaning for 10 min; and after the end, the filament power supply, the ion beam source and the argon gas valve are closed in sequence.
(4) Starting a pulse arc ion source, setting the working voltage of the pulse arc ion source to be 220-280V, the frequency to be 3-5 Hz, continuously working 3000-15000 pulses, and preparing the Ta-C carbon film with the thickness of 0.1-0.5 mu m and excellent wear resistance on the surface of the nitrile rubber.
In the description of the present application, it is to be understood that the terms "central," "longitudinal," "lateral," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings for the convenience of description and simplicity of description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be considered limiting of the claimed invention.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (10)
1. A composite coating device comprises a vacuum chamber and a workpiece rotating stand positioned in the vacuum chamber, and is characterized in that an ion beam source, a pulse arc ion source and a magnetic filtration arc ion source are integrated in the vacuum chamber;
the ion beam source is used for cleaning a workpiece or assisting deposition;
the pulsed arc ion source is used for exciting the graphite target to generate carbon ions and depositing a Ta-C carbon film;
the magnetic filtering arc ion source is used for exciting the metal target material, generating metal ions and depositing a metal film, an alloy film or a compound film.
2. The composite coating device according to claim 1, wherein the ion beam source is mounted on the side wall of the vacuum chamber, the central axis of the ion beam source passes right above the center of the workpiece turret, and a tungsten filament is mounted right above the ion beam source and used for generating a thermionic neutralizing ion flow;
the pulse arc ion source is arranged on the side wall of the vacuum chamber, and the central axis of the pulse arc ion source passes through the position right above the circle center of the workpiece rotating stand;
the magnetic filtering arc ion source is arranged on the side wall of the vacuum chamber and is positioned at the same height with the pulse arc ion source, and the axis of the magnetic filtering arc ion source is parallel or vertical to the axis of the pulse arc ion source.
3. The composite coating device according to claim 1, wherein the second moving direction of the ion current generated by the magnetic filtering arc ion source is finally crossed or overlapped with the first moving direction of the carbon ion current generated by the pulsed arc ion source.
4. The composite plating device according to claim 1, wherein the ion beam source is a Hall ion source or an anode layer ion source;
the electric arc discharge of the pulse electric arc ion source is pulse electric arc, and circulating cooling water is introduced into the target material.
5. The composite coating device according to claim 1, wherein the deflection coil of the magnetic filtering arc ion source can change the magnetic field intensity by adjusting the working current to 0-3A, so that the deflection angle of the ion flow can be adjusted to 60-90 °.
6. The composite plating device according to claim 1, further comprising:
the filament current is adjustable from 0mA to 500mA, and the filament current is adjustable;
the pulse arc ion source power supply is used for supplying power to the pulse arc ion source, the pulse width is 10-500 ms adjustable, the frequency is 1-30 Hz adjustable, the working voltage is 100-350V adjustable, the energy of carbon ions can be adjusted to be changed in the range of 25eV-100eV by adjusting the working voltage, the pulse frequency and the pulse width, and the proportion of a diamond phase in the Ta-C carbon film is changed to be 75-88%;
the arc power supply is used for supplying power to the magnetic filtering arc ion source, and the arc current is adjustable from 50 to 150A.
7. The composite plating device according to claim 1, further comprising a pulsed bias power supply; the positive pole of the pulse bias power supply is connected with the vacuum chamber, the vacuum chamber is grounded, the negative pole of the pulse bias power supply is connected with the workpiece rotating frame, and the workpiece rotating frame is insulated from the vacuum chamber.
8. The composite plating device according to claim 7, wherein the frequency of the pulse bias power supply is 40kHz, the voltage is adjustable from 0V to 1500V, the duty ratio is adjustable from 10% to 90%, and the bias voltage is used for improving the energy of ions and enhancing the film-substrate binding force.
9. The composite plating device according to claim 1, further comprising a heating system, a vacuum pumping system;
the heating system is arranged in the vacuum chamber, comprises a heating pipe, a thermocouple and a temperature control module and is used for adjusting the temperature of the vacuum chamber to be 0-500 ℃, and the temperature control precision is +/-5 ℃;
the vacuum pumping system is a secondary vacuum pump set and comprises a turbo molecular pump and a mechanical rotary vane pump.
10. The composite coating device according to any one of claims 1 to 9, wherein the workpiece rotating frame is a planetary gear frame, a plurality of stations are arranged on the workpiece rotating frame, the workpiece rotating frame is driven by a servo motor, and the rotating speed is adjustable from 0 r/min to 3 r/min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109576652A (en) * | 2018-12-20 | 2019-04-05 | 江苏徐工工程机械研究院有限公司 | A kind of electric arc ion plating device |
| CN113463041A (en) * | 2021-07-01 | 2021-10-01 | 安徽工业大学 | Arc cathode magnetic filtration coating device |
| CN113594541A (en) * | 2021-07-13 | 2021-11-02 | 南京邮电大学 | Method for preparing LAGP-based solid electrolyte by plasma magnetic filtration technology |
| CN113897582A (en) * | 2021-10-11 | 2022-01-07 | 南京亿浦先进材料研究院有限公司 | Preparation method of magnetic filtration cathode vacuum arc deposition conductive carbon film |
| CN114164404A (en) * | 2021-11-13 | 2022-03-11 | 东莞市华升真空镀膜科技有限公司 | Vacuum coating equipment and coating method |
| CN114481073A (en) * | 2022-02-21 | 2022-05-13 | 兰州交通大学 | Multifunctional foundation and application research composite physical vapor deposition system |
| CN115110031A (en) * | 2022-07-11 | 2022-09-27 | 超微中程纳米科技（苏州）有限公司 | Method for preparing superhard diamond coating |
| CN115233164A (en) * | 2022-07-22 | 2022-10-25 | 安徽工业大学 | Arc ion plating method of diamond reinforced composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109576652A (en) * | 2018-12-20 | 2019-04-05 | 江苏徐工工程机械研究院有限公司 | A kind of electric arc ion plating device |
| CN109576652B (en) * | 2018-12-20 | 2024-04-30 | 江苏徐工工程机械研究院有限公司 | Arc ion coating device |
| CN113463041A (en) * | 2021-07-01 | 2021-10-01 | 安徽工业大学 | Arc cathode magnetic filtration coating device |
| CN113463041B (en) * | 2021-07-01 | 2022-08-02 | 安徽工业大学 | Arc cathode magnetic filtration coating device |
| CN113594541A (en) * | 2021-07-13 | 2021-11-02 | 南京邮电大学 | Method for preparing LAGP-based solid electrolyte by plasma magnetic filtration technology |
| CN113897582A (en) * | 2021-10-11 | 2022-01-07 | 南京亿浦先进材料研究院有限公司 | Preparation method of magnetic filtration cathode vacuum arc deposition conductive carbon film |
| CN114164404A (en) * | 2021-11-13 | 2022-03-11 | 东莞市华升真空镀膜科技有限公司 | Vacuum coating equipment and coating method |
| CN114481073A (en) * | 2022-02-21 | 2022-05-13 | 兰州交通大学 | Multifunctional foundation and application research composite physical vapor deposition system |
| CN114481073B (en) * | 2022-02-21 | 2024-02-20 | 兰州交通大学 | Multifunctional basic and application research composite physical vapor deposition system |
| CN115110031A (en) * | 2022-07-11 | 2022-09-27 | 超微中程纳米科技（苏州）有限公司 | Method for preparing superhard diamond coating |
| CN115233164A (en) * | 2022-07-22 | 2022-10-25 | 安徽工业大学 | Arc ion plating method of diamond reinforced composite material |
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