CN111455336A - Electromagnetic field enhanced magnetron sputtering device and method for preparing diamond-like carbon coating - Google Patents
Electromagnetic field enhanced magnetron sputtering device and method for preparing diamond-like carbon coating Download PDFInfo
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- CN111455336A CN111455336A CN202010362213.4A CN202010362213A CN111455336A CN 111455336 A CN111455336 A CN 111455336A CN 202010362213 A CN202010362213 A CN 202010362213A CN 111455336 A CN111455336 A CN 111455336A
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- 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
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Abstract
An orthogonal composite electromagnetic field enhanced magnetron sputtering device and a method for preparing a diamond-like coating thereof are disclosed, wherein an orthogonal composite electromagnetic field is formed by utilizing an annular closed magnetic field formed by a plurality of groups of electromagnetically enhanced magnetron sputtering cathodes and a strong magnetic ion source or a bunching magnetic field formed by a longitudinal electromagnetic coil and an electric field formed by applying positive voltage to a central anode of an assembly; meanwhile, the back of the magnetron sputtering cathode is provided with more than one group of electromagnetic coils, the sputtering area can be enlarged by overlapping the magnetic field of the cathode body, the sputtering channel is widened, the magnetic field intensity of the closed magnetic field can be increased, and the orthogonal electromagnetic field formed by the magnetron sputtering cathode and the central anode is favorable for improving the ionization rate of sputtered particles; the orthogonal composite electromagnetic field not only increases the free path of electrons, improves the plasma density, and improves the cleaning efficiency and effect, but also can greatly improve the ionization rate of sputtered particles, thereby realizing auxiliary deposition, improving the binding force of the coating, and obtaining the high-quality diamond-like coating.
Description
Technical Field
The invention belongs to the technical field of vacuum coating, and relates to a magnetron sputtering device with enhanced electromagnetic field and a method for preparing a diamond-like coating; in particular to a magnetron sputtering device enhanced by orthogonal composite electromagnetic field and a method for preparing a diamond-like coating.
Background
Diamond-like carbon films (Diamond-like carbon films) have many excellent physical and chemical properties, such as high hardness, low friction coefficient, excellent wear resistance, high dielectric constant, high breakdown voltage, wide band gap, chemical inertness, biocompatibility, etc. after years of development, D L C films have been used in many fields in practical and industrial production.
The existing D L C deposition technology mainly comprises Physical Vapor Deposition (PVD) and Chemical Vapor Deposition (CVD), wherein the PVD mainly comprises Ion Beam Deposition (IBD), magnetron sputtering, multi-arc ion plating, pulse laser deposition and the like, the CVD comprises hot wire chemical vapor deposition and plasma chemical enhanced vapor deposition (PECVD), and the several technologies have problems which are mainly shown in the following aspects that 1, the ion beam deposition is low in deposition rate due to low graphite sputtering rate, 2, the magnetron sputtering deposition is low in sputtering rate on one hand, and low in atomic energy on the other hand, so that the structure is loose and low in hardness, 3, a large number of carbon particles are generated in the multi-arc ion plating deposition process, 4, the pulse laser deposition energy consumption is high, the coating uniformity is poor, the effective deposition area is small, 5, the hot wire vapor deposition technology is high in deposition temperature, the range of a base material is greatly limited, and 6, the PECVD effectively reduces the reaction temperature, but the deposition efficiency is low in the deposition process, the carbon atom ionization rate is low, and the film-forming quality structure is not enough.
The existing diamond-like coating Physical Vapor Deposition (PVD) equipment mainly combines a single magnetron sputtering technology with plasma ionized hydrocarbon gas and utilizes a PECVD (plasma-enhanced chemical vapor deposition) technology to deposit and obtain the diamond-like coating.
The main reason that the structure of the diamond-like coating of the existing device for preparing the diamond-like coating by using the magnetron sputtering cathode cannot achieve good effect is that the ionization rate of particles in the magnetron sputtering process is low, meanwhile, the sputtering process is influenced by a magnetic field, the service life of a target material is influenced by a target surface etching channel, and the preparation cost of the diamond-like coating is increased.
Therefore, how to solve the above problems is an important research content for those skilled in the art.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a magnetron sputtering device with enhanced orthogonal composite electromagnetic field and a method for preparing a diamond-like coating, which are beneficial to improving the film forming quality and the production efficiency of the diamond-like coating.
In order to achieve the above objects and other related objects, the present invention provides an orthogonal composite electromagnetic field enhanced magnetron sputtering apparatus, including a cavity, a central anode, a magnetron sputtering cathode, an electromagnetic enhancement coil, a pair of strong magnetic ion sources, an upper longitudinal coil and a lower longitudinal coil, wherein the cavity is a polyhedral cavity shell; the central anode is longitudinally arranged at the central position in the vacuum chamber; the upper longitudinal coil and the lower longitudinal coil are symmetrically assembled at the central position of the vacuum chamber and are respectively arranged on the upper top cover and the lower top cover; the magnetron sputtering cathodes are distributed on the cavity in a circumferential direction, an air pumping hole 18 is formed in the side face of the cavity, the electromagnetic enhancement coil is assembled on the magnetron sputtering cathodes, and the magnetron sputtering cathodes and the pair of strong magnetic ion sources form a circumferential closed annular magnetic field; the upper longitudinal coil and the lower longitudinal coil form a longitudinal bunching magnetic field, and the circumferential closed annular magnetic field or the longitudinal bunching magnetic field and the central anode electric field form an orthogonal composite electromagnetic field.
Furthermore, the central anode is arranged at the central position in the vacuum chamber and structurally comprises a spiral pipe internally provided with an inlet and outlet water cooling pipe or a cylindrical anode welded with an inlet and outlet water channel.
Furthermore, the electromagnetic enhancement coil can be a single electromagnetic coil sleeved on the magnetron sputtering cathode flange and the magnetron sputtering cathode magnetic shoe, or two electromagnetic coils respectively sleeved on the magnetron sputtering cathode flange and the magnetron sputtering cathode magnetic shoe.
Furthermore, when two electromagnetic coils are sleeved on a single magnetron sputtering cathode magnetic shoe and a magnetron sputtering cathode flange, the two electromagnetic coils are connected in series or independently connected with power, wherein the electromagnetic coil on the magnetron sputtering cathode flange is a direct current power supply, and the electromagnetic coil on the magnetron sputtering cathode magnetic shoe is a pulse power supply.
Further, the pair of strong magnetic ion sources themselves form a radially closed magnetic field.
The invention also provides a method for preparing the diamond-like coating by the magnetron sputtering device with the enhanced orthogonal composite electromagnetic field, which comprises the following steps:
⑴, putting the substrate to be plated into an orthogonal composite electromagnetic field enhanced magnetron sputtering device, wherein the device is provided with four groups of electromagnetic enhanced magnetron sputtering cathodes, two groups of which are Cr targets and two groups of which are WC targets, a pair of strong magnetic ion sources, an upper longitudinal coil, a lower longitudinal coil and a central anode;
⑵, after the vacuum chamber of the film plating machine is vacuumized, when the vacuum degree is below 5E-3pa, argon is introduced when the vacuum degree is 1-10pa, 200-800V negative bias is applied to the rotating stand, 1-25V positive voltage is applied to the central anode, the current of the electromagnetic enhancement coil assembled on the magnetron sputtering cathode is 1-5A, the current of the upper longitudinal coil and the current of the lower longitudinal coil are 1-5A, glow discharge is generated on the rotating stand, the plasma density of the glow discharge is increased under the influence of the orthogonal composite electromagnetic field, the workpiece to be plated on the rotating stand can be efficiently cleaned, and the cleaning time is 30-60 min;
⑶, starting a metal Cr target, adjusting the power of the metal Cr target to 5-20kw, applying 0-100V negative bias on a rotating stand, applying 1-25V positive voltage on a central anode, setting the current of an electromagnetic enhancement coil assembled on a magnetron sputtering cathode to be 1-5A, setting the current of an upper longitudinal coil and a lower longitudinal coil to be 1-5A, and depositing a metal substrate Cr layer with the thickness of 0-2um under the action of an orthogonal composite electromagnetic field;
⑷, after the process of the metal substrate layer is finished, starting a WC target, adjusting the target power to realize a composite gradient layer of metal Cr and WC, wherein the Cr target power is reduced to 1-5Kw from 5-20Kw, the WC target power is increased to 5-20Kw from 1-5Kw, 0-100V negative bias is applied on a rotating frame, 1-25V positive voltage is applied on a central anode, the current of an electromagnetic enhancement coil assembled on a magnetron sputtering cathode is 1-5A, the current of an upper longitudinal coil and the current of a lower longitudinal coil are both 1-5A, a gradient composite layer with the thickness of 0-2um is deposited under the action of an orthogonal composite electromagnetic field, and then a composite layer with the thickness of 0-2um is deposited, wherein the WC target power is 5-20Kw, and the Cr target power is 1-5 Kw;
⑸, then introducing acetylene with the flow of 0-300sccm, closing the Cr target, wherein the WC target power is 5-20Kw, applying 0-100V negative bias on the rotating stand, applying 1-25V positive voltage on the central anode, the current of the electromagnetic enhancement coil assembled on the magnetron sputtering cathode is 1-5A, the current of the upper longitudinal coil and the lower longitudinal coil is 1-5A, and depositing a gradient WC-H layer with the thickness of 0-1um under the action of the orthogonal composite electromagnetic field, and then depositing a WC-H layer with the thickness of 0-2um, wherein the WC target power is 5-20Kw, and the acetylene flow is 50-300 sccm;
⑹, after finishing the deposition of the WC-H layer, applying 400-1200V negative bias voltage on the rotating frame, applying 1-25V positive voltage on the central anode, setting the current of the electromagnetic enhancement coil assembled on the magnetron sputtering cathode to be 1-5A, setting the current of the upper longitudinal coil and the lower longitudinal coil to be 1-5A, introducing 200-1000sccm acetylene gas, and depositing the diamond-like coating with the thickness of 1-5um by glow discharge.
Furthermore, the cleaning process can also use a strong magnetic ion source to clean the workpiece to be plated on the rotating frame, and the cleaning process comprises the following steps: after a vacuum chamber of a film plating machine is vacuumized, when the vacuum degree is below 5E-3pa, argon is introduced when the vacuum degree is 1-10pa, a negative bias of 50V is applied to a rotating frame, the current of an electromagnetic enhancement coil assembled on a magnetron sputtering cathode is 1-5A, the current of an ion source is in a constant current mode and is 3-8A, wherein the bias setting of 50V to 200-300V is carried out in the cleaning process, and the cleaning time is 30-60 min.
Furthermore, when two electromagnetic coils are sleeved on a single magnetron sputtering cathode magnetic shoe and a magnetron sputtering cathode flange, the two electromagnetic coils are connected in series or independently connected with power, wherein the electromagnetic coil on the magnetron sputtering cathode flange is a direct current power supply, and the electromagnetic coil on the magnetron sputtering cathode magnetic shoe is a pulse power supply.
Furthermore, the electromagnetic coil on the magnetron sputtering cathode magnetic shoe is an electromagnetic coil with adjustable frequency and voltage in various waveforms of sine, cosine, triangle and rectangle.
Furthermore, the central anode, the upper longitudinal coil and the lower longitudinal coil can be replaced by a spiral copper pipe with a sealing assembly, and compared with a cylindrical central anode (1-25V) and a central anode and bunching magnetic field spiral copper pipe formed by the upper longitudinal coil (1-5A) and the lower longitudinal coil (1-25V), the function of bunching magnetic field and the central anode can be realized by applying large current (30-120A) and superposing an anode power supply (1-25V).
The invention enhances the annular closed magnetic field formed by the magnetron sputtering cathode and the electromagnetic ion source through the optimally designed electromagnetic field, and the radial magnetic field formed by the pair of strong magnetic ion sources, the beam-forming magnetic field formed by the central anode or the upper and lower longitudinal coils of the spiral tube interacts with the positive electricity applied on the central anode to form an orthogonal composite electromagnetic field around the workpiece rotating stand, thereby greatly prolonging the movement stroke of electrons, increasing the collision probability of the electrons with gas atoms and sputtering particles, increasing the concentration of plasma, and improving the ionization rate of the sputtering particles, so that more gas ions bombard the surface of the workpiece to be plated, and increasing the binding force and compactness of a gradient layer and the deposition rate and quality of a diamond-like coating.
Compared with the prior art, the device for preparing the composite magnetic field diamond-like coating provided by the invention has the following substantial differences and remarkable progress:
1) the movement stroke of electrons is improved by utilizing the orthogonal composite electromagnetic field, and the ionization rate of particles can be greatly improved.
2) The strength of the annular closed magnetic field can be effectively increased by enhancing the magnetron sputtering cathode through the electromagnetic field, and meanwhile, the utilization rate of the target material can be effectively improved through the interaction of the electromagnetic coil and the magnetic shoe, and the production cost is reduced.
3) The beam-bunching magnetic field generated by the spiral coil of the central anode of the spiral tube is utilized, and positive voltage is applied to form the central anode of the self-generated orthogonal electromagnetic field, so that the structure is simple, the cost is low, and the effect is obvious.
4) The electromagnetic field enhanced magnetron sputtering cathode is used for preparing the diamond-like coating, and the gradient coating prepared by the orthogonal composite electromagnetic field enhanced magnetron sputtering technology has compact structure and fine surface.
5) The plasma formed by the orthogonal composite electromagnetic field is used for preparing the diamond-like coating, the deposition rate can be improved by 2-5 times, and the surface smoothness, the structure compactness and the Sp3 content are greatly improved.
In a word, the orthogonal composite electromagnetic field enhanced magnetron sputtering device provided by the invention not only improves the cleaning beam current in the cleaning process, but also reduces the glow cleaning voltage, effectively inhibits the rotating stand of the workpiece to be plated from sparking and improves the yield; meanwhile, the particle deposition rate of the diamond-like coating substrate layer can be improved, so that the production efficiency is improved, the sputtering process of a magnetron sputtering cathode can be improved, the etching area is enlarged, and the utilization rate of the target material is improved; not only improves the ionization rate of the diamond-like coating acetylene gas and the deposition efficiency, but also improves the compactness and the binding force of the coating by bombarding the workpiece to be plated with high-energy cations.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a schematic structural diagram of an orthogonal composite electromagnetic field enhanced magnetron sputtering apparatus provided by the present invention;
FIG. 2 is a side view of an orthogonal composite electromagnetic field enhanced magnetron sputtering apparatus of the present invention (cylindrical central anode);
FIG. 3 is a schematic plane view of an orthogonal complex electromagnetic field enhanced magnetron sputtering apparatus of the present invention (cylindrical central anode);
FIG. 4 is a side view of an orthogonal composite electromagnetic field enhanced magnetron sputtering apparatus of the present invention (helical tube center anode);
FIG. 5 is a schematic planar view of an orthogonal composite electromagnetic field enhanced magnetron sputtering apparatus of the present invention (central anode of a spiral tube);
FIG. 6 is a schematic diagram of the orthogonal complex electromagnetic field toroidal closed magnetic field of the present invention;
FIG. 7 is a schematic diagram of the quadrature complex electromagnetic field (solenoid) bunching magnetic field of the present invention;
FIG. 8 is a schematic diagram of the magnetic field bunching of the orthogonal complex electromagnetic field (solenoid) of the present invention.
Detailed Description
Other advantages and capabilities of the present invention will be readily apparent to those skilled in the art from the following description of the present invention, the description of which is provided in connection with the accompanying drawings.
The terms of direction and position of the present invention, such as "up", "down", "front", "back", "left", "right", "inside", "outside", "top", "bottom", "side", etc., refer to the direction and position of the attached drawings. Accordingly, the use of directional and positional terms is intended to illustrate and understand the present invention and is not intended to limit the scope of the present invention.
For convenience of description, the internal structures of the rough pumping system and part of the fine pumping system, the magnetron sputtering system, the strong magnetic ion source and other discharge devices used in the invention are simplified, and some bearings, electromagnetic coils of longitudinal coils, part of sealing rings and the like in the transmission process are not shown.
Referring to fig. 1, 2 and 3: the invention provides an orthogonal composite electromagnetic field enhanced magnetron sputtering device which comprises an internal tangent right octagonal machine cavity, a rotating frame component 10, an electromagnetic enhanced outer coil 11, an upper longitudinal coil 12, a cylindrical central anode 13, magnetron sputtering cathodes 14, strong magnetic ion sources 15, electromagnetic enhanced inner coils 16 and a lower longitudinal coil 17, wherein the cylindrical central anode 13, the upper longitudinal coil 12 and the lower longitudinal coil 17 are respectively assembled on the upper top cover and the lower top cover of the internal tangent right octagonal machine cavity, four groups of magnetron sputtering cathodes 14 are uniformly assembled on four surfaces of the internal tangent right octagonal machine cavity, the strong magnetic ion sources 15 are assembled between the two groups of magnetron sputtering cathodes 14, the electromagnetic enhanced inner coils 16 can be sleeved on magnetic shoes of the magnetron sputtering cathodes 14, and the electromagnetic enhanced outer coils 11 can be sleeved on mounting flanges of the magnetron sputtering cathodes 14.
See fig. 6 for an illustration: the octahedral vacuum cavity comprises a vacuum cavity and a door, wherein eight inscribed circular surfaces are respectively provided with an air exhaust port 18, a magnetron sputtering cathode 001(N), a strong magnetic ion source 001(S), a magnetron sputtering cathode 002(N), an observation window, a magnetron sputtering cathode 003(S), a strong magnetic ion source 002(N) and a magnetron sputtering cathode 004(S), the polarity of a magnetic field between the two strong magnetic ion sources is opposite, and an annular closed magnetic field can be formed between the magnetron sputtering cathode 001, the strong magnetic ion source 001, the magnetron sputtering 002, the magnetron sputtering 003, the strong magnetic ion source 002 and the magnetron sputtering cathode 004.
Referring to FIG. 7: the upper center and the lower center of the regular octahedron vacuum cavity are sleeved with a longitudinal coil 12 and a lower longitudinal coil 17, the current directions of the upper longitudinal coil and the lower longitudinal coil are consistent, an upper magnetic field (N) and a lower magnetic field (S) of the vacuum cavity can be formed in the cavity, a central bunching longitudinal magnetic field can be formed, and meanwhile, the cylindrical anode is internally provided with a water inlet pipe which is directly communicated with the bottom and a water return port which is communicated with the end part, so that the cooling of the cylindrical.
Referring to fig. 4 and 5: the bunching magnetic field and the central anode can be formed by a spiral copper pipe, can be water-cooled and can form the central bunching magnetic field by using large current, and can be superposed with a central anode power supply; the electromagnetic reinforcing external coil comprises an internally tangent right-angle machine cavity, a rotating frame component 20, an electromagnetic reinforcing external coil 21, a spiral tube central anode 22, magnetron sputtering cathodes 23, a strong magnetic ion source 24 and an electromagnetic reinforcing internal coil 25, wherein the spiral tube central anode 22 is assembled on an upper top cover of the internally tangent right-angle machine cavity, four groups of magnetron sputtering cathodes 23 are uniformly assembled on four surfaces of the internally tangent right-angle machine cavity, the strong magnetic ion source 24 is assembled between the two groups of magnetron sputtering cathodes 23, the electromagnetic reinforcing internal coil 25 can be sleeved on a magnetic shoe of the magnetron sputtering cathodes 23, and the electromagnetic reinforcing external coil 21 can be sleeved on a mounting flange of the magnetron sputtering cathodes 23.
Referring to FIG. 8: spiral pipe center anode 22 carries out spiral coil processing for single copper pipe and forms to and be equipped with mounting flange and vacuum seal subassembly, and its copper intraduct can lead to the cooling water, cools off the spiral pipe in the vacuum chamber, and outside the vacuum chamber, the big beam current can be applyed at the business turn over water both ends of spiral pipe simultaneously, makes it form the bunch magnetic field in the vacuum chamber, and is the same also can be at a center anode positive pole of the tip stack of spiral pipe, negative pole ground connection. Thus, the cylindrical central anode 13 can be superposed with the central anode formed by the longitudinal coil 12 and the lower longitudinal coil 17 and the bunching magnetic field can be realized by one spiral pipe.
The magnetron sputtering device with the enhanced orthogonal composite electromagnetic field mainly utilizes a closed magnetic field formed by an electromagnetic enhanced magnetron sputtering cathode and a strong magnetic ion source and a bunching magnetic field formed by an upper longitudinal coil and a lower longitudinal coil (a spiral tube anode) to interact to form the orthogonal composite electromagnetic field, electrons generate spiral motion under the action of the magnetic field in the orthogonal composite electromagnetic field, and the motion stroke of the electrons is increased, so that the collision probability with sputtered particles and glow discharge gas particles is increased, the plasma intensity is increased, the ionization rate of the particles is improved, a workpiece to be plated can be better cleaned, the ionization rate of the sputtered particles is increased, the compactness and the bonding force of a glow-like diamond coating basal layer are improved, and the deposition efficiency and the quality of the glow-like diamond coating are improved.
The following will be described in detail with reference to a specific process for preparing a diamond-like coating.
The first embodiment is as follows:
referring to FIG. 1: the diamond-like coating composite magnetic field coating equipment is configured as follows, four groups of electromagnetic enhanced magnetron sputtering cathodes 14 are used, wherein two groups are provided with metal Cr targets, two groups are provided with WC targets, a strong magnetic ion source 15 is arranged at the interval position of four groups of magnetron sputtering cathodes, four groups of magnetron sputtering cathodes 14 are provided with electromagnetic enhancement coils 11 and 16, a cylindrical central anode 13 and upper and lower longitudinal electromagnetic coils 12 and 17 are respectively arranged at the upper and lower central positions, in the glow discharge process, electrons are attracted to the water-cooled anode under the action of the electric field under the action of the orthogonal composite electromagnetic field, in the process of electron movement, hydrocarbon gas collides, so that the gas is ionized, a diamond-like coating is efficiently generated, in the process, the orthogonal composite electromagnetic field greatly increases the free path of electrons to collide with more particles, so that a high-quality diamond-like coating is obtained.
The preparation method of the diamond-like coating mainly comprises the following steps:
in this example, the method of the invention will be described by taking a metal target Cr and an alloy target WC as examples.
A pretreatment process: and (3) carrying out ultrasonic surface cleaning on the substrate to be plated, namely putting the substrate to be plated into a cleaning tank with an ultrasonic cleaner for removing oil and wax, and drying for later use after rinsing. The substrate is made of materials such as high-speed steel, hard alloy, metal ceramic, die steel and the like.
Loading: and putting the cleaned substrate to be plated into a vacuum chamber, assembling an ion source and a magnetron sputtering metal target on the chamber at intervals, assembling a central anode on an upper top plate, and assembling a longitudinal electromagnetic coil at the upper and lower central positions.
The process is described in table 1:
TABLE 1
The process of table 1 is described in detail as follows:
putting a substrate to be plated into a vacuum chamber of an internally-tangent octagonal machine, wherein the film plating machine is provided with a pair of strong magnetic ion sources, 2 groups of metal Cr targets, 2 groups of hard alloy WC targets and six components which are arranged at intervals and can realize a closed annular magnetic field; the center of the vacuum cavity is provided with a cylindrical central anode and upper and lower longitudinal coils.
Vacuumizing a vacuum chamber of a film plating machine, introducing argon, starting an electromagnetic enhancement coil 2.5A, a central anode +15V and upper and lower longitudinal coils 2.5A on a magnetron sputtering cathode, introducing argon, controlling the pressure to be about 3pa, starting a bias voltage power supply 350V, cleaning the surface of a product to be plated by ions by utilizing glow discharge, and activating a substrate; after the cleaning is finished, 2 groups of magnetron sputtering Cr targets are started, the target power is 12Kw, the current regulation position of an electromagnetic enhancement coil is 3A, the bias voltage is reduced to 20V, other parameters are unchanged, a metal substrate layer with a certain thickness (0-2um) is deposited, after the process of the metal substrate layer is finished, the power of the metal Cr target and the power of a hard alloy WC target are regulated by a certain gradient (12-2 Kw of the Cr target and 2-12Kw of the WC target are stably deposited), a mixed gradient layer of metal Cr and WC with a certain thickness (0-2um) is deposited, when the metal Cr target is deposited to a certain thickness, the metal Cr target is closed, the composition of hydrocarbon gas (20-200 of hydrocarbon gas and then stable deposition) is regulated, a WC-H gradient layer with a certain thickness (0-2um) is deposited, when the metal Cr target is deposited to a certain thickness, the WC target is closed, the electromagnetic enhancement coil on the magnetron sputtering WC cathode is opened by 2.5A, the central anode is +15V, the upper and lower longitudinal coils are 2.5A, acetylene is introduced into the chamber at 600sccm, the pressure is controlled to be about 5pa, a bias power supply is started at 850V, and the high-energy plasma glow discharge under the orthogonal composite electromagnetic field is utilized to ionize the hydrocarbon gas to obtain the diamond-like coating with a certain thickness.
Unloading: and after the process is finished, closing the negative bias, the electromagnetic enhancement coil, the central anode and the upper and lower longitudinal coils, stopping introducing the hydrocarbon gas and the argon gas, cooling the coating, introducing air into the vacuum chamber, recovering the atmospheric pressure, opening the door of the vacuum chamber, and taking out the plated substrate.
According to the preparation method of the diamond-like coating, the effective stroke of partial electrons in glow discharge is increased by utilizing an annular closed magnetic field formed by electromagnetic enhanced magnetron sputtering and a strong magnetic ion source and an orthogonal composite electromagnetic field formed by a radial magnetic field formed by the strong magnetic ion source and a bunching magnetic field formed by upper and lower longitudinal coils, so that the ionization rate of hydrocarbon gas is increased, and the compactness, the binding force and the SP3 content of the diamond-like coating are improved; meanwhile, the electromagnetically enhanced magnetron sputtering cathode enlarges a sputtering area on one hand, greatly improves the ionization rate of sputtering particles on the other hand, and effectively improves the quality of a substrate layer; the existence of center anode has improved the velocity of motion of electron on the one hand, has increased the effective collision number of times of electron, has promoted plasma's concentration, and on the other hand has reduced the discharge voltage in the glow discharge, has promoted the cleaning performance, and more importantly has promoted the ionization rate of carbon particle, has reduced the effect that carbon gathers, very big promotion in the diamond-like coating SP 3's content.
Description of the drawings: the gradient described in the present preparation method means that the process parameter is linearly changed from one value to another value over a certain period of time, followed by a period of stable deposition.
Example two:
the main difference between the embodiment and the first embodiment is that a strong magnetic ion source is used for cleaning a workpiece to be plated in the preparation process of the diamond coating, and the specific process is as follows:
in this example, the method of the invention will be described by taking a metal target Cr and an alloy target WC as examples.
A pretreatment process: and (3) carrying out ultrasonic surface cleaning on the substrate to be plated, namely putting the substrate to be plated into a cleaning tank with an ultrasonic cleaner for removing oil and wax, and drying for later use after rinsing. The substrate is made of materials such as high-speed steel, hard alloy, metal ceramic, die steel and the like.
Loading: and putting the cleaned substrate to be plated into a vacuum chamber, assembling an ion source and a magnetron sputtering metal target on the chamber at intervals, assembling a central anode on an upper top plate, and assembling a longitudinal electromagnetic coil at the upper and lower central positions.
The process is described in table 2:
TABLE 2
The main difference between the process of the second table and the first table is that the workpiece to be plated is cleaned by utilizing a strong magnetic ion source, and the cleaning process comprises the following steps: argon is introduced (the vacuum degree is 5pa), negative bias voltage (50V) is applied to the rotating frame, positive voltage (15V) is applied to the central anode, the current of an electromagnetic enhancement coil assembled on the magnetron sputtering cathode is (2.5A), the ion source is in a constant current mode, the current is 5A, wherein bias voltage setting with certain gradient is carried out in the cleaning process (50V is increased to 200-300V), and the cleaning time is 30min.
In the process of cleaning the workpiece to be plated by utilizing the strong magnetic ion source and the orthogonal composite electromagnetic field, the central anode and the upper and lower longitudinal coils are closed, and high-energy cations output by the ion source bombard the workpiece to be plated under the action of the electric field and the annular closed magnetic field.
According to the preparation method of the diamond-like coating, the effective stroke of partial electrons in glow discharge is increased by utilizing an annular closed magnetic field formed by electromagnetic enhanced magnetron sputtering and a strong magnetic ion source and an orthogonal composite electromagnetic field formed by a radial magnetic field formed by the strong magnetic ion source and a bunching magnetic field formed by upper and lower longitudinal coils, so that the ionization rate of hydrocarbon gas is increased, and the compactness, the binding force and the SP3 content of the diamond-like coating are improved; meanwhile, the electromagnetically enhanced magnetron sputtering cathode enlarges a sputtering area on one hand, greatly improves the ionization rate of sputtering particles on the other hand, and effectively improves the quality of a substrate layer; the existence of the central anode improves the movement speed of electrons, increases the effective collision times of the electrons, improves the concentration of plasma, reduces the discharge voltage in glow discharge, improves the ionization rate of carbon particles, reduces the effect of carbon aggregation and greatly improves the content of SP3 in the diamond-like coating.
Description of the drawings: the gradient described in the present preparation method means that the process parameter is linearly changed from one value to another value over a certain period of time, followed by a period of stable deposition.
Example three:
referring to FIG. 4: the compound magnetic field coating equipment of the diamond-like coating is configured as follows, the used electromagnetic enhanced magnetron sputtering cathodes 23 are four groups, wherein two groups are provided with metal Cr targets, two groups are provided with WC targets, the strong magnetic ion source 24 is arranged at the interval position of the four groups of magnetron sputtering cathodes, the four groups of magnetron sputtering cathodes 23 are provided with electromagnetic enhanced coils 21 and 25, the central anode 22 of the spiral tube is arranged at the central position of the upper end of the cavity, electrons can be attracted to a water-cooling anode by the left and right electric field under the action of an orthogonal compound electromagnetic field in the glow discharge process, hydrocarbon gas can collide in the electron movement process, so that the gas is ionized, the diamond-like coating is efficiently generated, and in the process, the orthogonal compound electromagnetic field can greatly increase the free path of the electrons and collide with more particles, and the high-quality diamond-like coating is obtained.
The preparation method of the diamond-like coating mainly comprises the following steps:
in this example, the method of the invention will be described by taking a metal target Cr and an alloy target WC as examples.
A pretreatment process: and (3) carrying out ultrasonic surface cleaning on the substrate to be plated, namely putting the substrate to be plated into a cleaning tank with an ultrasonic cleaner for removing oil and wax, and drying for later use after rinsing. The substrate is made of materials such as high-speed steel, hard alloy, metal ceramic, die steel and the like.
Loading: and putting the cleaned substrate to be plated into a vacuum chamber, assembling an ion source and a magnetron sputtering metal target on the chamber at intervals, assembling a central anode on an upper top plate, and sleeving the central anode of a spiral pipe at the center of the upper end of the vacuum chamber.
The process is described in table 3:
TABLE 3
The third embodiment is different from the first embodiment in that the central anode of the spiral tube is used to replace the central anode of the cylinder and the upper and lower longitudinal coils. The beam-focusing magnetic field generated by the upper and lower longitudinal coils is replaced by the beam-focusing magnetic field generated by the large current applied to the spiral tube, and meanwhile, positive voltage can be superposed on the central anode of the spiral tube to realize the effect of the central anode; compared with a cylindrical central anode and an upper longitudinal coil and a lower longitudinal coil, the plasma processing device has the advantages that equipment cost and installation difficulty are reduced, most importantly, the effective area of the central anode is increased, more electrons are accelerated, and the plasma concentration is improved.
The process of table three is described in detail as follows:
putting a substrate to be plated into a vacuum chamber of an internally-tangent octagonal machine, wherein the film plating machine is provided with a pair of strong magnetic ion sources, 2 groups of metal Cr targets, 2 groups of hard alloy WC targets and six components which are arranged at intervals and can realize a closed annular magnetic field; the center of the vacuum cavity is provided with a spiral pipe center anode.
Vacuumizing a vacuum chamber of a film plating machine, introducing argon, starting an electromagnetic enhancement coil 2A on a magnetron sputtering cathode, enabling the superposed voltage of a central anode of a spiral tube to be +10V, enabling the heavy current on the spiral tube to be 50A, introducing argon, controlling the pressure to be about 3pa, starting a bias power supply to be 300V, cleaning the surface of a product to be plated through ions by utilizing glow discharge, and activating a substrate; after the cleaning is finished, 2 groups of magnetic control sputtering Cr targets are started, the target power is 10Kw, the current regulation position of an electromagnetic enhancement coil is 2.5A, the bias voltage is reduced to 20V, other parameters are unchanged, a metal substrate layer with a certain thickness (0-1um) is deposited, after the process of the metal substrate layer is finished, the power of the metal Cr target and the power of a hard alloy WC target are regulated by a certain gradient (the Cr target is 10-2Kw, the WC target is stably deposited after 2-10 Kw), a mixed gradient layer of metal Cr and WC with a certain thickness (0-2um) is deposited, when the metal Cr target is deposited to a certain thickness, the metal Cr target is closed, a WC-H gradient layer with a certain thickness (0-2um) is deposited by regulating the components of the hydrocarbon gas through gradient (the hydrocarbon gas is 20-200, and then stable deposition), when the hydrocarbon gas is deposited to a certain thickness, the WC-H gradient layer with a certain thickness is deposited, the hard alloy target is closed, the superposed voltage of the central anode of the spiral tube is +10V, the heavy current on the spiral tube is 50A, acetylene is introduced into the spiral tube at 600sccm, the pressure is controlled to be about 5pa, the bias power supply is turned on at 700V, and the high-energy plasma glow discharge under the orthogonal composite electromagnetic field is utilized to ionize the hydrocarbon gas, so that the diamond-like coating with a certain thickness is obtained.
Unloading: and after the process is finished, closing the negative bias, the electromagnetic enhancement coil, the central anode and the upper and lower longitudinal coils, stopping introducing the hydrocarbon gas and the argon gas, cooling the coating, introducing air into the vacuum chamber, recovering the atmospheric pressure, opening the door of the vacuum chamber, and taking out the plated substrate.
According to the preparation method of the diamond-like coating, the effective stroke of partial electrons in glow discharge is increased by utilizing an annular closed magnetic field formed by electromagnetic enhanced magnetron sputtering and a strong magnetic ion source and an orthogonal composite electromagnetic field formed by a radial magnetic field formed by the strong magnetic ion source and a bunching magnetic field formed by upper and lower longitudinal coils, so that the ionization rate of hydrocarbon gas is increased, and the compactness, the binding force and the SP3 content of the diamond-like coating are improved; meanwhile, the electromagnetically enhanced magnetron sputtering cathode enlarges a sputtering area on one hand, greatly improves the ionization rate of sputtering particles on the other hand, and effectively improves the quality of a substrate layer; the existence of center anode has improved the velocity of motion of electron on the one hand, has increased the effective collision number of times of electron, has promoted plasma's concentration, and on the other hand has reduced the discharge voltage in the glow discharge, has promoted the cleaning performance, and more importantly has promoted the ionization rate of carbon particle, has reduced the effect that carbon gathers, very big promotion in the diamond-like coating SP 3's content.
Description of the drawings: the gradient described in the present preparation method means that the process parameter is linearly changed from one value to another value over a certain period of time, followed by a period of stable deposition.
Description of the drawings: in the first to third embodiments, the number of the electromagnetic enhancement coils is two, and in practical application, the electromagnetic enhancement coils can be a single electromagnetic coil sleeved on the magnetron sputtering cathode flange and the magnetron sputtering cathode magnetic shoe, or two electromagnetic coils respectively sleeved on the magnetron sputtering cathode flange and the magnetron sputtering cathode magnetic shoe, and meanwhile, the electromagnetic coils on the magnetron sputtering cathode magnetic shoe can be loaded with a power supply with adjustable frequency and voltage in various waveforms of sine, cosine, triangle and rectangle.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. The utility model provides a magnetron sputtering device of compound electromagnetic field reinforcing of quadrature, includes cavity, central positive pole, magnetron sputtering negative pole, electromagnetism reinforcing coil, a pair of strong magnetic ion source, goes up longitudinal coil and lower longitudinal coil, its characterized in that: the cavity is a regular polyhedron shell; the central anode is longitudinally arranged at the central position in the vacuum chamber; the upper longitudinal coil and the lower longitudinal coil are symmetrically assembled at the central position of the vacuum chamber and are respectively arranged on the upper top cover and the lower top cover; the magnetron sputtering cathodes are distributed on the cavity in a circumferential direction, an air pumping hole 18 is formed in the side face of the cavity, the electromagnetic enhancement coil is assembled on the magnetron sputtering cathodes, and the magnetron sputtering cathodes and the pair of strong magnetic ion sources form a circumferential closed annular magnetic field; the upper longitudinal coil and the lower longitudinal coil form a longitudinal bunching magnetic field, and the circumferential closed annular magnetic field or the longitudinal bunching magnetic field and the central anode electric field form an orthogonal composite electromagnetic field.
2. The magnetron sputtering apparatus with enhanced orthogonal composite electromagnetic field according to claim 1, wherein: the central anode is arranged at the central position in the vacuum chamber and structurally comprises a spiral pipe internally provided with an inlet and outlet water cooling pipe or a cylindrical anode welded with an inlet and outlet water channel.
3. The magnetron sputtering apparatus with enhanced orthogonal composite electromagnetic field according to claim 1, wherein: the electromagnetic enhancement coil can be a single electromagnetic coil sleeved on the magnetron sputtering cathode flange and the magnetron sputtering cathode magnetic shoe, or two electromagnetic coils respectively sleeved on the magnetron sputtering cathode flange and the magnetron sputtering cathode magnetic shoe.
4. The magnetron sputtering apparatus with enhanced orthogonal composite electromagnetic field according to claim 3, wherein: when two electromagnetic coils are sleeved on a single magnetron sputtering cathode magnetic shoe and a magnetron sputtering cathode flange, the two electromagnetic coils are connected in series or independently connected with electricity, wherein the electromagnetic coil on the magnetron sputtering cathode flange is a direct current power supply, and the electromagnetic coil on the magnetron sputtering cathode magnetic shoe is a pulse power supply.
5. The magnetron sputtering apparatus with enhanced orthogonal composite electromagnetic field according to claim 1, wherein: the pair of strong magnetic ion sources themselves form a radial closed magnetic field.
6. A method for preparing a diamond-like coating by using an orthogonal composite electromagnetic field enhanced magnetron sputtering device is characterized by comprising the following steps of: the method comprises the following steps:
7. A method of preparing a diamond-like coating according to claim 6, characterized in that: the cleaning process can also use a strong magnetic ion source to clean the workpiece to be plated on the rotating frame, and the cleaning process comprises the following steps: after a vacuum chamber of a film plating machine is vacuumized, when the vacuum degree is below 5E-3pa, argon is introduced when the vacuum degree is 1-10pa, a negative bias of 50V is applied to a rotating frame, the current of an electromagnetic enhancement coil assembled on a magnetron sputtering cathode is 1-5A, the current of an ion source is in a constant current mode and is 3-8A, wherein the bias setting of 50V to 200-300V is carried out in the cleaning process, and the cleaning time is 30-60 min.
8. A method of preparing a diamond-like coating according to claim 6, characterized in that: when two electromagnetic coils are sleeved on a single magnetron sputtering cathode magnetic shoe and a magnetron sputtering cathode flange, the two electromagnetic coils are connected in series or independently connected with electricity, wherein the electromagnetic coil on the magnetron sputtering cathode flange is a direct current power supply, and the electromagnetic coil on the magnetron sputtering cathode magnetic shoe is a pulse power supply.
9. A method of preparing a diamond-like coating according to claim 8, characterized in that: the electromagnetic coil on the magnetron sputtering cathode magnetic shoe is an electromagnetic coil with adjustable frequency and voltage in various waveforms of sine, cosine, triangle and rectangle.
10. A method of preparing a diamond-like coating according to claim 6, characterized in that: compared with a cylindrical central anode with 1-25V and a central anode and a beam-bunching magnetic field spiral copper pipe formed by the upper longitudinal coil and the lower longitudinal coil with 1-5A, the central anode, the upper longitudinal coil and the lower longitudinal coil can be used for realizing the functions of a beam-bunching magnetic field and the central anode by applying a large current of 30-120A and superposing an anode power supply with 1-25V.
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