CN114592169B - Self-supporting carbon stripping film without target frame and preparation method thereof - Google Patents
Self-supporting carbon stripping film without target frame and preparation method thereof Download PDFInfo
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- CN114592169B CN114592169B CN202210183675.9A CN202210183675A CN114592169B CN 114592169 B CN114592169 B CN 114592169B CN 202210183675 A CN202210183675 A CN 202210183675A CN 114592169 B CN114592169 B CN 114592169B
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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
- C23C14/0005—Separation of the coating from the substrate
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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
- C23C14/58—After-treatment
- C23C14/5826—Treatment with charged particles
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
- G21K5/00—Irradiation devices
- G21K5/08—Holders for targets or for other objects to be irradiated
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Physical Vapour Deposition (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for preparing a self-supporting carbon stripping film without a target frame. The method comprises the following steps: 1) Taking a glass sheet and spin-coating betaine solution; 2) Placing the carbon-coated film in a vacuum chamber of a carbon arc method carbon-coated film preparation device, and vacuumizing until the vacuum degree is less than 1.5 x 10 ‑ 3 Pa; 3) The carbon arc current is regulated to 100A-160A to perform carbon arc discharge, and a carbon stripping film is plated to the target thickness; 4) Placing the glass sheet coated with the carbon stripping film in water, and separating the carbon stripping film from the glass sheet until the whole carbon stripping film floats on the water surface; 5) Taking out the carbon stripping film from the water surface by using a hollow metal target frame, and standing until the water is completely evaporated; 6) Placing the carbon film with the target frame in a vacuum chamber of plasma equipment, and vacuumizing; 7) Performing stress change on the carbon peeling film by utilizing carbon plasma; 8) And taking out the carbon stripping film from the vacuum chamber, and taking the carbon stripping film out of the hollow metal target frame to obtain the self-supporting carbon stripping film without the target frame.
Description
Technical Field
The invention belongs to the technical field of target preparation for nuclear physics experiments, and particularly relates to a self-supporting carbon stripping film without a target frame and a preparation method thereof.
Background
Most of the time in nuclear physics experiments require that the target film be a self-supporting film, i.e., no substrate is self-supporting to form a film. Because the melting point of carbon is highest in the simple substance materials, the chemical stability is good, the limit thickness of the self-supporting carbon stripping film is one order of magnitude lower than that of self-supporting films made of other materials, and the prepared carbon stripping film has high mechanical strength and is easy to obtain a large-area self-supporting film. Accelerators typically employ a self-supporting carbon release film as a release body for the heavy ionic extra-nuclear charge to achieve a higher charge state. The current self-supporting carbon stripping film has a thickness of less than 200 micrograms per square centimeter (about 1 micrometer) and an effective area of more than phi 30mm because of thinner thickness and larger effective area, and the self-supporting carbon stripping film prepared in the current preparation process cannot realize self-supporting under the action of no external force due to the stress of the film, but has to adopt a target frame to apply an additional external force to the film so as to realize self-supporting, namely the carbon stripping film is fixed on a special hollow metal target frame so as to realize self-supporting. The self-supporting carbon release film would automatically curl due to the stress of the film itself and be unusable without the additional external force of the target frame. The target frame is brought in, so that the beam in the accelerator is beaten on the target frame to influence the emission of ions in the beam of the accelerator, thereby causing the quality reduction of the beam such as the beam intensity, the size and the like, and influencing the operation efficiency of the accelerator, and particularly, the problem is particularly remarkable when the beam spot diameter of the beam in the accelerator is larger. In order to solve the problem of target frame carry-in, it is important to develop a self-supporting carbon release film without a target frame.
Disclosure of Invention
In order to solve the problem that the self-supporting carbon release film has to be introduced by a target frame by adopting the target frame, the invention provides a method for preparing the self-supporting carbon release film without the target frame. According to the method, the stress of the carbon plasma on the carbon stripping film is changed on the basis of the traditional process for preparing the self-supporting carbon stripping film, and the self-supporting of the carbon stripping film can still be realized when the target frame is removed through the stress change, so that the phenomenon that the self-supporting cannot be realized due to curling of the carbon stripping film prepared by the traditional process is avoided.
The method for preparing the self-supporting carbon release film without the target frame provided by the invention comprises the following steps:
1) Taking a glass sheet, and spin-coating a layer of betaine solution on the glass sheet;
2) Placing the glass sheet coated with betaine solution into a vacuum chamber of a carbon stripping film preparation device by a carbon arc method, and vacuumizing until the vacuum degree is less than 1.5×10 -3 Pa；
3) The current of the carbon arc is adjusted to 100A-160A, the distance of the carbon rod is adjusted to 4-7mm, carbon arc discharge is carried out, and a carbon stripping film is plated to the target thickness;
4) Placing the glass sheet coated with the carbon stripping film in water, and separating the carbon stripping film from the glass sheet until the whole carbon stripping film floats on the water surface;
5) Taking out the carbon stripping film from the water surface by using a hollow metal target frame, taking out the carbon stripping film, standing the metal target frame on which the carbon stripping film is taken out on a table top until the water on the surfaces of the carbon stripping film and the target frame is completely evaporated;
6) Placing the carbon stripping film with the target frame in a vacuum chamber of plasma equipment, and vacuumizing to 5 x 10 -4 Pa or less;
7) Performing stress change on the carbon peeling film by utilizing carbon plasma;
8) And taking the carbon stripping film with the target frame, which is changed by the plasma stress, out of the vacuum chamber, and taking the carbon stripping film out of the hollow metal target frame, thus obtaining the self-supporting carbon stripping film without the target frame.
In the method step 1), the glass sheet is washed and dried before use.
In the above method step 3), the thickness of the carbon release film may be 85 micrograms per square centimeter to 95 micrograms per square centimeter.
In the above method step 7), when the carbon plasma is used for treating the carbon peeling film, parameters of the plasma equipment are as follows: the voltage is 400V-500V, the current is 300mA-550mA, the argon pressure is 0.3Pa-0.6Pa (specifically, 0.45 Pa), and the time is 20min-55min.
The invention has the following beneficial effects:
the invention realizes the preparation of the self-supporting carbon stripping film without the target frame, solves the problem that the target frame is needed to be introduced by the target frame in the traditional process, adopts the carbon plasmas with the same components as the carbon stripping film to change the stress of the self-supporting carbon stripping film, and the prepared self-supporting carbon stripping film without the target frame can not introduce new impurities. Compared with the traditional self-supporting carbon stripping film with the target frame, the self-supporting carbon stripping film without the target frame can improve the quality of the beam current of the accelerator, and further improve the operation efficiency of the accelerator.
Drawings
FIG. 1 is a carbon release film prepared without stress modification;
FIG. 2 is a carbon release film prepared by stress modification in example 1 of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples, but the invention is not limited to the following examples. The methods are conventional methods unless otherwise specified. The starting materials are available from published commercial sources unless otherwise specified.
Example 1
A self-supporting carbon stripping film without a target frame and a preparation process thereof mainly comprise the following steps:
(1) Cleaning the glass sheet, and airing the cleaned glass sheet;
(2) Spin coating a layer of betaine solution on the dried and cleaned glass sheet;
(3) Placing the glass sheet coated with betaine solution into a vacuum chamber of a carbon stripping film preparation device by a carbon arc method, and vacuumizing until the vacuum degree is less than 1.5×10 -3 Pa；
(4) The distance between the carbon rods is adjusted to 5mm, the carbon arc current is adjusted to 140A, and carbon arc discharge plating is carried out to peel off the carbon film until the film thickness is 90 micrograms per square centimeter;
(5) Placing the glass sheet coated with the carbon stripping film in water, and separating the carbon stripping film from the glass sheet until the whole carbon stripping film floats on the water surface;
(6) Taking out the carbon stripping film from the water surface by using a hollow metal target frame, taking out the carbon stripping film, standing the metal target frame on which the carbon stripping film is taken out on a table top until the water on the surfaces of the carbon stripping film and the target frame is completely evaporated;
(7) Placing a self-supporting carbon stripping film with a target frame in a vacuum chamber of plasma equipment;
(8) Vacuum of plasma equipment to 5 x 10 -4 Pa, parameters of the regulated plasma device are as follows: the plasma type is carbon plasma, the voltage is 450V, the current is 400mA, the argon pressure is 0.45Pa, and the time is 35min. Thin film using carbon plasmaStress changes;
(9) And taking the carbon stripping film with the target frame, which is changed by the plasma stress, out of the vacuum chamber, and taking the carbon stripping film out of the hollow target frame, wherein the carbon stripping film is not curled like the carbon stripping film prepared by the traditional process after the target frame is removed due to the stress change of the film, so that the self-supporting carbon stripping film without the target frame is obtained. (the physical diagram is shown in FIG. 2)
The self-supporting carbon release film without a target frame prepared in this example had a thickness of 100 micrograms per square centimeter and an area of 60mm by 25mm.
Example 2
Unlike example 1, the parameters of the plasma apparatus in step (9) are as follows: the voltage was 500V, the current was 500mA, the argon pressure was 0.45Pa, and the time was 25 minutes.
Comparative example 1
Unlike example 1, the carbon release film was prepared without carbon plasma treatment (i.e., without step (7) and step (8)).
The carbon release film prepared in this comparative example was automatically curled after the target frame was removed.
A physical diagram of the prepared carbon release film is shown in FIG. 1.
Comparative example 2
Unlike example 1, the parameters of the plasma apparatus in step (9) are as follows: the voltage was 450V, the current was 400mA, the argon pressure was 0.45Pa, and the time was 65 minutes.
The method has the advantages that the plasma treatment time is too long, so that the stress of the film is changed too much, and the carbon stripping film is curled in the opposite direction of the original curling direction after the target frame is removed.
Comparative example 3
Unlike example 1, the parameters of the plasma apparatus in step (9) are as follows: the voltage was 450V, the current was 400mA, the argon pressure was 0.45Pa, and the time was 15 minutes.
The method has the advantages that the plasma treatment time is too short, the stress change of the film is insufficient, and the carbon stripping film is curled towards the original curling direction after the target frame is removed.
Comparative example 4
Unlike example 1, the parameters of the plasma apparatus in step (9) are as follows: the voltage was 500V, the current was 700mA, the argon pressure was 0.45Pa, and the time was 35 minutes.
The method has the advantages that the current for plasma treatment is too large, so that the energy of the plasma is too high, and a self-supporting film is broken.
Comparative example 5
Unlike example 1, the parameters of the plasma apparatus in step (9) are as follows: the voltage was 400V, the current was 150mA, the argon pressure was 0.45Pa, and the time was 190min.
The current of the plasma treatment is too low, which makes the efficiency too low, resulting in prolonged working time.
Claims (4)
1. A method of making a frameless self-supporting carbon release film comprising the steps of:
1) Taking a glass sheet, and spin-coating a layer of betaine solution on the glass sheet;
2) Placing the glass sheet coated with betaine solution into a vacuum chamber of a carbon stripping film preparation device by a carbon arc method, and vacuumizing until the vacuum degree is less than 1.5×10 -3 Pa；
3) The distance between the carbon rods is adjusted to 4-7mm, the carbon arc current is adjusted to 100A-160A for carbon arc discharge, and the carbon stripping film is plated to the target thickness;
4) Placing the glass sheet coated with the carbon stripping film in water, and separating the carbon stripping film from the glass sheet until the whole carbon stripping film floats on the water surface;
5) Taking out the carbon stripping film from the water surface by using a hollow metal target frame, and standing the metal target frame with the carbon stripping film taken out until the water on the surfaces of the carbon stripping film and the target frame is completely evaporated;
6) Placing the carbon stripping film with the target frame in a vacuum chamber of plasma equipment, and vacuumizing to 5 x 10 -4 Pa or less;
7) Performing stress change on the carbon peeling film by utilizing carbon plasma;
8) Taking the carbon stripping film with the target frame after the stress change out of the vacuum chamber, and taking the carbon stripping film out of the hollow metal target frame to obtain a self-supporting carbon stripping film without the target frame;
in the step 7), when the carbon plasma is used for treating the carbon peeling film, parameters of the plasma equipment are as follows: the voltage is 400V-500V, the current is 300mA-550mA, the argon pressure is 0.3Pa-0.6Pa, and the time is 20min-55min.
2. The method according to claim 1, characterized in that: in the step 1), the glass sheet is washed and dried before use.
3. The method according to claim 1 or 2, characterized in that: in the step 3), the thickness of the carbon release film is 85 micrograms per square centimeter to 95 micrograms per square centimeter.
4. A free-standing carbon release film without a target frame prepared by the method of any one of claims 1-3.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210183675.9A CN114592169B (en) | 2022-02-24 | 2022-02-24 | Self-supporting carbon stripping film without target frame and preparation method thereof |
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| CN202210183675.9A CN114592169B (en) | 2022-02-24 | 2022-02-24 | Self-supporting carbon stripping film without target frame and preparation method thereof |
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| CN114592169A CN114592169A (en) | 2022-06-07 |
| CN114592169B true CN114592169B (en) | 2023-09-01 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001179870A (en) * | 1999-12-27 | 2001-07-03 | Denki Kagaku Kogyo Kk | Easy peel film |
| CN101705478A (en) * | 2009-12-04 | 2010-05-12 | 北京科技大学 | Method for improving strength of free-standing diamond film |
| CN103589999A (en) * | 2013-11-06 | 2014-02-19 | 北京大学 | Free-standing diamond nano-film preparing device and method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009530493A (en) * | 2006-03-17 | 2009-08-27 | トライアンフ，オペレーティング アズ ア ジョイント ヴェンチャー バイ ザ ガバナーズ オブ ザ ユニバーシティ オブ アルバータ，ザ ユニバーシティ オブ ブリティッシュ コロンビア，カールトン | Self-supporting multilayer film with diamond-like carbon layer |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001179870A (en) * | 1999-12-27 | 2001-07-03 | Denki Kagaku Kogyo Kk | Easy peel film |
| CN101705478A (en) * | 2009-12-04 | 2010-05-12 | 北京科技大学 | Method for improving strength of free-standing diamond film |
| CN103589999A (en) * | 2013-11-06 | 2014-02-19 | 北京大学 | Free-standing diamond nano-film preparing device and method |
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| CN114592169A (en) | 2022-06-07 |
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