CN109295414B - Technology and equipment for coating film in deep hole - Google Patents

Technology and equipment for coating film in deep hole Download PDF

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Publication number
CN109295414B
CN109295414B CN201811507016.6A CN201811507016A CN109295414B CN 109295414 B CN109295414 B CN 109295414B CN 201811507016 A CN201811507016 A CN 201811507016A CN 109295414 B CN109295414 B CN 109295414B
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cylinder
magnetic field
vacuum chamber
current
deep hole
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CN109295414A (en
Inventor
廖斌
欧阳晓平
罗军
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Guangdong Guangxin Ion Beam Technology Co Ltd
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Beijing Normal University
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/04Coating on selected surface areas, e.g. using masks
    • C23C14/046Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/32Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325Electric arc evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/50Substrate holders
    • C23C14/505Substrate holders for rotation of the substrates

Abstract

The invention discloses a technology and equipment for coating a film in a deep hole, which comprises two cathode target systems, two magnetic filtration systems, a vacuum chamber, a turnover system, a ceramic solenoid, a workpiece system, an auxiliary anode and the like. The bent pipe is a direct current magnetic field, the cylindrical vacuum chamber is a strong pulse focusing magnetic field, and the ceramic pipe wound in the vacuum chamber is also a pulse focusing magnetic field. The cathode target is a target material which can be pushed when in work, inert gas Ar and hydrogen are introduced into the vacuum chamber before the coating of the inner wall of the cylinder, the surface is cleaned through corona discharge between the auxiliary anode and the inner wall of the coated part, and arc deposition coating is carried out after the cleaning. The length-diameter ratio of the cylinder capable of being coated by the method can be more than 20: 1, the diameter of the hole is not less than 20mm, the thickness uniformity of the film layer is better than +/-15%, and the key technical bottlenecks of poor uniformity of coating on the inner wall and limited length-diameter ratio at home and abroad are overcome.

Description

Technology and equipment for coating film in deep hole
Technical Field
The invention solves the problem of coating in deep holes, and the specific technology is based on a magnetic filtration deposition technology.
Technical Field
With the rapid development of scientific technology, the requirements on the surface modification technology of materials are higher and higher, and the traditional single surface modification technology is more and more difficult to meet the technical requirements on industrial production; the surface coating of the special-shaped piece becomes one of the future development directions.
In recent years, several surface modification composite technologies have been developed and put into industry one after another, and have played an important role. For example, the composite technology of the magnetron sputtering technology and the arc ion plating technology is compatible with the advantages that the magnetron sputtering technology can deposit films with large area and high uniformity and the ion plating technology can prepare films with high bonding force, and the process practicability is improved. And like multi-arc ion plating, a plurality of arc sources act together, so that the deposition of the multi-element composite film is realized, the deposition efficiency is obviously improved, and the technology is widely applied to the machining industry of cutters and parts at present. The existing surface deposition technology such as multi-arc ion plating, magnetron sputtering, chemical vapor deposition and the like is a very important modification means. However, it has an important disadvantage that these techniques are not suitable for depositing films in the holes, especially the uniformity of deposition is worse with a large aperture ratio. The magnetic filtering cathode vacuum arc deposition technology is a novel ion beam film preparation method developed in recent years, large particles and neutral atoms generated by an arc source are filtered through the magnetic filtering technology to obtain pure plasma beams without large particles, the problem caused by the existence of the large particles in the common arc source deposition method is effectively solved, the prepared film has excellent performance, but the important defect of the existing magnetic filtering deposition technology is still that the deep hole coating capacity is limited, and the uniform coating of the inner surface of the surface of a workpiece with large size and high aperture ratio cannot be realized. Deep hole coating is a technical bottleneck restricting the development of the deep hole coating at home and abroad, and no related deep hole technology is reported at present.
Disclosure of Invention
Aiming at the problems, the invention provides a deep hole coating technology and equipment aiming at deconstruction of a vacuum chamber structure, an arc source target structure, a coated piece and a rotating mechanism thereof based on the original magnetic filtration deposition system.
One of the purposes of the embodiment of the invention is to effectively carry out deep hole regulation and control on ion beam current by designing deep hole coating equipment, realize the treatment of workpieces with larger length-diameter ratio, and simultaneously greatly reduce arcing current and greatly prolong the service life of a cathode.
Further speaking:
the technology is a magnetic filtration deposition technology;
the deposited cylinder can be a metal, nonmetal or non-temperature-resistant film inner wall, the diameter of the deposited cylinder is more than 20mm, the length of the deposited cylinder is 1.2-2m, and the uniformity of a film layer is +/-15%;
before coating the inner wall of the cylinder, the surface is cleaned by corona discharge between an auxiliary anode and a cathode cylinder, and Ar and H are introduced into the cylinder2The ratio of the mixed gas Ar to H210: 1, and the discharge voltage is 800V;
when the plating part cylinder is plated with a film, the arcing current of the two cathode targets is 20-90A; the magnetic field current of the magnetic filtration system is 1-5A;
the strong pulse focusing magnetic field on the cylindrical vacuum chamber is formed by mixing direct current and pulse current, the direct current is 1-2A, the pulse current is 1A-1KA, the frequency is 10Hz-1KHz, and the combination of the direct current and the pulse current can obviously improve the transport capacity of the plasma and improve the perforation capacity of the plasma;
the focusing magnetic field wound on the ceramic tube in the vacuum chamber is a pulse magnetic field with current of-1 KA-1KA alternating change and frequency of 10Hz-1KHz, and the magnetic field in the ceramic tube alternates;
the ceramic cylinder and the cylinder with the plating part are turned over in a vacuum chamber, the plating part is connected with a bias voltage through an electric brush, the bias voltage is-1000 and 1000V and is changed alternately, and the frequency is 10Hz-200 Hz;
the plated part and the ceramic cylinder are limited through ceramic, and in order to ensure the uniformity of the plated film and the beam intensity, the difference between the diameter of the plated part and the diameter of the ceramic cylinder is not more than 20 mm;
the length-diameter ratio of the film to be coated can be as high as 20: 1, the diameter of the hole is not less than 20mm, and the thickness uniformity of the film layer is better than +/-15%.
Compared with the prior art, the embodiments of the invention have the following advantages:
1. the embodiment of the invention provides a technology and equipment for coating a film in a deep hole, the length-diameter ratio of the cylinder capable of coating the film can be more than 20: 1, the diameter of the hole is not less than 20mm, the thickness uniformity of a film layer is better than +/-15 percent, and the industrialized application of inner plating of the cylinder is greatly facilitated;
2. compared with the existing magnetic filtration deposition device, the high-pulse magnetic field is arranged outside the vacuum chamber of the device, so that the plasma led out by magnetic filtration can be focused, the probability of the plasma entering a plated part tube is greatly improved, and the high-length-diameter-ratio plating capacity of the plasma is improved;
3. compared with the existing magnetic filtering device, the device has the advantages that the strong focusing ceramic tube is arranged in the vacuum chamber, and the uniform coating capacity of the inner surface of the coated part can be greatly improved by setting the current direction of the ceramic tube coil;
4. compared with the prior surface deposition technology, the patent adopts an electric brush conduction mode on the plating part, and the electric potential of the plating part is changed alternately in the film plating process, for example, when the inner wall of the plating part is at a positive electric potential, plasma is compressed for transmission; when the inner wall of the plated part is at a negative potential, ions in the plasma are attracted to the inner wall for plating; therefore, the uniform film coating can be realized through the potential conversion of the inner wall, which is greatly different from the traditional deposition mode;
5. compared with the prior surface deposition technology, the magnetic filtration cathode is provided with double auxiliary anodesThe cathode can stably and reliably work under the condition of lower arcing current under high vacuum, the minimum arcing current can be as low as 20A, and meanwhile, the cathode is free of auxiliary gas, and the vacuum degree is 1 multiplied by 10-3Pa。
It should be noted that the foregoing method embodiments are described as a series of acts or combinations for simplicity in explanation, but it should be understood by those skilled in the art that the present invention is not limited by the order of acts or acts described, as some steps may occur in other orders or concurrently in accordance with the invention. Further, those skilled in the art will appreciate that the embodiments described in the specification are presently preferred and that no particular act is required to implement the invention.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Further features and advantages of embodiments of the present invention will be described in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of embodiments of the invention, are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a front view of the apparatus for coating inside a deep hole according to the present invention;
FIG. 2 is a cross-sectional view of a vacuum chamber of the present invention;
FIG. 3 is a speckle pattern in example 1 of the present invention;
FIG. 4 is a speckle pattern in example 2 of the present invention;
FIG. 5 is a speckle pattern of example 3 of the present invention;
FIG. 6 is a speckle pattern of embodiment 4 of the present invention.
Description of the reference numerals
101 cathode base flange
102 magnetic conductive anode cylinder
103 magnetic filtering magnetic field
104 magnetic filter pipeline
105 strong pulse magnetic field
106 vacuum chamber low cabinet
107 strong pulse magnetic field
108 magnetic filtering magnetic field
109 magnetic conductive anode cylinder
110 cathode base flange
111 auxiliary electrode
112 ceramic insulating tube
113 ceramic fixing ring
114 plated part cylinder
115 strong pulse coil package
116 overturning clamp
117 auxiliary electrode support shaft
118 first auxiliary anode
119 second auxiliary anode
120 bias brush
201 auxiliary electrode
202 auxiliary electrode supporting shaft
203 overturning clamp
204 plated part cylinder
205 ceramic fixing ring
206 ceramic insulating tube
207 vacuum chamber
Examples
Example 1
The inner diameter of a cylinder of a plated part is 80mm, the outer diameter is 110mm, the length is 1100mm, the inner diameter of a selected external insulation ceramic cylinder is 120mm, the cleaning vacuum before film plating is 0.5-2Pa, Ar: H2The discharge voltage is 800V, and the cleaning time is 30-60 min; the arc starting current is 30A and the vacuum degree is 1 multiplied by 10 when the cylinder of the plating part is plated-3Pa, bias voltage of-800V-800V, frequency of 50Hz, magnetic field of each coil and other parameters are as follows:
103: direct current 3A;
105: direct current 2A, pulse current frequency 50Hz, current 50A;
107: direct current 2A, pulse current frequency 50Hz, current 50A;
108: direct current 3A;
115: strong pulse coil: -50A, frequency 100 Hz;
example 2
The inner diameter of a cylinder of a plated part is 60mm, the outer diameter is 90mm, the length is 1100mm, the inner diameter of a selected external insulation ceramic cylinder is 110mm, the cleaning vacuum before film plating is 0.5-2Pa, Ar: H2The discharge voltage is 800V, and the cleaning time is 30-60 min; the arc starting current is 30A and the vacuum degree is 1 multiplied by 10 when the cylinder of the plating part is plated-3Pa, bias voltage of-800V-800V, frequency of 50Hz, magnetic field of each coil and other parameters are as follows:
103: direct current 3A;
105: direct current 2A, pulse current frequency 50Hz, current 50A;
107: direct current 2A, pulse current frequency 50Hz, current 50A;
108: direct current 3A;
115: strong pulse coil: -300A, frequency 100 Hz;
example 3
The inner diameter of a cylinder of a plated part is 40mm, the outer diameter is 60mm, the length is 1100mm, the inner diameter of a selected external insulation ceramic cylinder is 80mm, the cleaning vacuum before film plating is 0.5-2Pa, Ar: H2The discharge voltage is 800V, and the cleaning time is 30-60 min; the arc starting current is 30A and the vacuum degree is 1 multiplied by 10 when the cylinder of the plating part is plated-3Pa, bias voltage of-800V-800V, frequency of 50Hz, magnetic field of each coil and other parameters are as follows:
103: direct current 3A;
105: direct current 2A, pulse current frequency 50Hz, current 50A;
107: direct current 2A, pulse current frequency 50Hz, current 50A;
108: direct current 3A;
115: strong pulse coil: 800A-800A, frequency 100 Hz;
example 4
The inner diameter of a cylinder of the plated part is 40mm, the outer diameter is 60mm, the length is 1100mm, and selected external insulation ceramicsThe inner diameter of the cylinder is 80mm, the cleaning vacuum before film coating is 0.5-2Pa, Ar: H2The discharge voltage is 800V, and the cleaning time is 30-60 min; the arc starting current is 30A and the vacuum degree is 1 multiplied by 10 when the cylinder of the plating part is plated-3Pa, bias voltage of-800V-800V, frequency of 50Hz, magnetic field of each coil and other parameters are as follows:
103: direct current 3A;
105: direct current 2A, pulse current frequency 50Hz, current 50A;
107: direct current 2A, pulse current frequency 50Hz, current 50A;
108: direct current 3A;
115: strong pulse coil: -500A, frequency 100 Hz;
FIGS. 3, 4, 5 and 6 are graphs of deposition results for plating cylinders of different sizes. It should be noted that, the uniformity of each cylindrical coating film is verified in the following manner: and uniformly pasting white printing paper on the inner wall of the cylinder, and drawing out the paper after deposition is finished to check the surface coating condition. It can be obviously found that the deposition effect of the film layer of the plating part cylinders with different length-diameter ratios is not consistent under different external parameters. The graph proves that the deep hole deposition area of the cylinder can be greatly improved by utilizing the technology, so that the equipment and the technology can greatly improve the deep hole deposition capability of magnetic filtration deposition, expand the application range of the magnetic filtration deposition and make up the blank of key technology in the industrialized large-scale production process of the inner wall coating of the magnetic filtration deposition.

Claims (7)

1. A deep hole inner plating system, comprising:
the device comprises an arc source system, a magnetic filtering system, a vacuum system, a magnetic field system, a ceramic tube in a vacuum chamber, a plated part cylinder, a turnover system and a bias system;
the plated part is the inner wall of a metal or nonmetal film, the diameter of a deposited cylinder is more than 20mm, the length is 1.2-2m, and the uniformity of the film layer is +/-15%;
before the inner wall of the cylinder of the plated part is plated, the surface is cleaned by corona discharge between an auxiliary anode and a cathode cylinder, and Ar and H are introduced into the cylinder2Mixed gas ofThe ratio of the resultant gases Ar to H210: 1, and the discharge voltage is 800V;
when the plating part cylinder is plated with a film, the arcing current of the two cathode targets is 20-90A; the magnetic field current of the magnetic filtration system is 1-5A;
the strong pulse focusing magnetic field on the cylindrical vacuum chamber is a mixture of direct current and pulse current, the direct current is 1-2A, the pulse current is 1A-1KA, and the frequency is 10Hz-1 KHz;
the focusing magnetic field wound on the ceramic tube in the vacuum chamber is a pulse magnetic field with current of-1 KA-1KA alternating change and frequency of 10Hz-1 KHz;
the ceramic cylinder and the cylinder with the plating part are turned over in a vacuum chamber, the plating part is connected with a bias voltage through an electric brush, the bias voltage is-1000 and 1000V and is changed alternately, and the frequency is 10Hz-200 Hz;
the plated part and the ceramic cylinder are limited through the ceramic ring, and in order to ensure the uniformity of the plated film and the beam intensity, the difference between the diameter of the plated part and the diameter of the outer ceramic cylinder is not more than 20 mm;
the length-diameter ratio of the film to be coated can be as high as 20: 1, the diameter of the hole is not less than 20mm, and the thickness uniformity of the film layer is +/-15%.
2. A deep hole inner plating film system according to claim 1, characterized in that: the particles extracted into the vacuum chamber were 100% ions.
3. A deep hole inner plating film system according to claim 1, characterized in that: the surface cleaning process comprises bombarding Ar ions at 20-500 deg.C and vacuum degree of 1 × 10-3-1×10-5Pa, H for reducing oxides2The flow rate of (A) is 50-100 sccm.
4. A deep hole inner plating film system according to claim 1, characterized in that: the double auxiliary anodes are arranged, the cathode target arcing current is as low as 15-20A, the stable and reliable work can be realized, and the inner wall coating temperature is controlled at 20-400 ℃.
5. A deep hole inner plating film system according to claim 1, characterized in that: the current of the focusing magnetic field on the ceramic tube in the vacuum chamber changes alternately, namely the direction of the magnetic field in the ceramic tube changes alternately, the transport performance of the plasma is improved by 80-120%, and the uniformity of the inner wall coating is not higher than +/-15%.
6. A deep hole inner plating film system according to claim 1, characterized in that: the set bias voltage is alternately changed in positive and negative relative to the auxiliary pole, the transport performance of the plasma is improved by 20-50% due to the alternate change of the auxiliary magnetic field, and the uniformity is improved by 10-20%.
7. A deep hole coating equipment is characterized in that: assembled using the system of any one of claims 1-6.
CN201811507016.6A 2018-12-11 2018-12-11 Technology and equipment for coating film in deep hole Active CN109295414B (en)

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CN109881160B (en) * 2019-03-08 2020-06-30 北京师范大学 Deposition device
CN110318023A (en) * 2019-07-30 2019-10-11 中国人民解放军陆军工程大学 A kind of thin film deposition device and method of controllable magnetic field screening laser plasma
CN111101104A (en) * 2020-01-10 2020-05-05 安徽纯源镀膜科技有限公司 Method for metalizing surface of insulating material
CN111041430A (en) * 2020-01-10 2020-04-21 安徽纯源镀膜科技有限公司 Production process of high-temperature-resistant diamond-like carbon film layer
CN113186504B (en) * 2021-04-25 2022-07-26 北京师范大学 Pulse ion source coating extraction device
CN113388807A (en) * 2021-06-11 2021-09-14 哈尔滨工业大学 Coating device for optimizing coating of inner wall of pipe and coating method based on coating device
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Effective date of registration: 20210506

Address after: 510663 101, building C, PepsiCo smart Park, 179 pupu East Road, Huangpu District, Guangzhou City, Guangdong Province

Patentee after: Guangdong Guangxin Ion Beam Technology Co.,Ltd.

Address before: 100875, 19, Xinjie street, Haidian District, Beijing

Patentee before: BEIJING NORMAL University

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Inventor after: Liao Bin

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Inventor before: Liao Bin

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