Environment-friendly quartz surface carbon coating device and method

By preheating under vacuum environment, carbon source rotary sputtering and high-temperature calcining on the quartz surface, the problem of insufficient binding force of the quartz surface coating in the prior art is solved, and the long-term stable use of quartz containers and high purity and quality stability of synthetic materials are achieved.

CN119569353APending Publication Date: 2025-03-07DONGFANG ELECTRIC (LESHAN) EBAN HIGH-PURITY MATERIALS CO LTD
View PDF 1 Cites 0 Cited by

Patent Information

Application Number
CN202411757415.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-03
Publication Date
2025-03-07

AI Technical Summary

Technical Problem

In the prior art, the bonding force of the quartz surface coating cannot meet the requirements of long-term use, resulting in the quartz container being prone to rupture and material flow out, affecting the synthesis quality and increasing environmental pollution and economic losses.

Method used

Environmentally friendly quartz surface coating devices and methods are adopted, including surface treatment of quartz containers, preheating under vacuum, rotary sputtering of carbon sources and high-temperature calcination, forming a uniform and dense carbon layer, enhancing adhesion and reducing impurity pollution.

Benefits of technology

The uniform density and high adhesion of the carbon layer are achieved, which reduces the risk of rupture of quartz containers, extends the service life of quartz containers, reduces production costs, and improves the purity and quality stability of synthetic materials.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119569353A_ABST
    Figure CN119569353A_ABST
Patent Text Reader

Abstract

The invention relates to the technical field of quartz carbon coating, in particular to an environment-friendly quartz surface carbon coating device and method, and the method comprises the following steps: S1, quartz container surface treatment; s2, removing air in the quartz container, and placing the quartz container in a vacuum environment; s3, preheating in a vacuum state; s4, carrying out rotary sputtering on the carbon source; and S5, high-temperature calcination is carried out, after calcination is completed, rapid cooling is carried out in a normal-temperature environment, and carbon coating is completed. According to the device and the method, a vacuum carbon source sputtering method is adopted, a carbon source is uniformly sputtered to the surface of quartz, and a formed carbon layer is uniform, compact, high in adhesive force and not prone to falling off. The carbon layer isolates the sample from quartz, the risk of bursting during synthesis is reduced, the quartz container can be repeatedly used, and the cost is reduced.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the technical field of quartz carbon coating, and in particular to an environmentally friendly quartz surface carbon coating device and method. Background Art

[0002] In the process of preparing high-purity materials, quartz containers are prone to adhesion with the purified or synthesized materials under certain conditions, which ultimately makes it impossible to directly take out the purified or synthesized materials from the quartz containers; at the same time, it will also cause the quartz containers to break and the materials to flow out. For example, in the preparation and single crystal growth of high-purity cadmium zinc telluride and cadmium telluride, quartz tubes are often used as synthesis containers or growth containers. Under high temperatures, quartz tends to change into silicon dioxide crystals, and crystallization forms on the surface of quartz. This phenomenon introduces impurities in quartz into the sample, which seriously affects the quality of cadmium zinc telluride and cadmium telluride; and the raw materials cadmium and zinc are easy to adhere to quartz, making it difficult for the material to separate from the quartz container, and even causing the quartz container to crack. Once the quartz container cracks, the sample will flow out, causing environmental pollution and economic losses. Similarly, in the process of cadmium direct pulling, quartz crucibles are used as containers, and there is also the problem that the material is difficult to separate from the quartz or cracks, resulting in a short service life of the quartz container and high production costs.

[0003] Commonly used high-purity quartz is mainly 99.99% to 99.999% pure. It is inevitable that quartz contains a very small amount of metal atoms. During the synthesis process, these metal atoms are freed to the quartz surface, contaminating the sample and affecting the yield rate. At present, the relevant patent CN11188159A of quartz surface coating technology discloses a method for carbon coating of quartz crucible / tube. The quartz tube is placed in a furnace at a certain temperature. Acetone gas is introduced into the quartz tube under normal pressure with nitrogen as the carbon source carrier, so that the acetone is decomposed and deposited on the surface of the quartz tube to achieve carbon coating. Patent CN113755817A discloses a method for preparing a carbon coating on the surface of quartz and a quartz material. Using C1-C3 gaseous hydrocarbons as the gas source, a uniform carbon layer is coated on the quartz surface by chemical vapor deposition process at a certain temperature and vacuum. However, the bonding strength of the coating cannot meet the requirements of long-term use. Summary of the invention

[0004] The purpose of the present invention is to provide an environmentally friendly quartz surface carbon coating device and method to solve the technical problem in the prior art that the bonding force of the coating cannot meet the requirements of long-term use.

[0005] The invention discloses an environmentally friendly quartz surface carbon coating method, comprising the following steps:

[0006] S1. Quartz container surface treatment;

[0007] S2. Remove the air in the quartz container and place the quartz container in a vacuum environment;

[0008] S3. Preheating under vacuum;

[0009] S4. Carbon source rotation sputtering;

[0010] S5. High temperature calcination. After calcination, the temperature is rapidly lowered in a room temperature environment to complete carbonization.

[0011] Furthermore, the surface treatment of the quartz container is specifically performed by using sodium hydroxide alkaline washing - ultrapure water washing - aqua regia acid washing - ultrapure water washing, and then drying for standby use.

[0012] Furthermore, the quartz container is ultrapure water quartz with an electrical conductivity of not less than 12 MΩ·CM.

[0013] Furthermore, in step S2, the vacuum degree in the quartz container tube is lower than 10Pa.

[0014] Furthermore, the quartz container is a quartz tube or a quartz crucible.

[0015] Furthermore, the preheating in step S3 is to heat the material to 950-1050° C. in a vacuum state to complete the preheating.

[0016] Furthermore, the step S4 is to perform carbon source rotation sputtering at 950-1050°C.

[0017] Furthermore, the high temperature calcination temperature is 950-1050°C and the vacuum degree is 10 -3 Pa—10 -4 Pa, calcination time is 30-40min.

[0018] An environmentally friendly quartz surface carbon coating device comprises a control system, a vacuum system, a rotary carbon coating mechanism, a heating system, a pneumatic system and a carbon source supply system. The vacuum system, the rotary carbon coating mechanism, the heating system, the pneumatic system and the carbon source supply system are all controlled by the control system to realize automatic operation of the carbon coating device.

[0019] Furthermore, the vacuum system includes a vacuum pump, and the vacuum pump is connected to a vacuum gauge, a vacuum solenoid valve, an electromagnetic air-breaking valve and the rotary carbon coating mechanism;

[0020] The vacuum pump provides vacuuming power, the vacuum gauge detects the vacuum degree in the quartz container to be coated, the vacuum solenoid valve is used to open and close the connection between the vacuum pump and the quartz container to be coated, and the electromagnetic air-breaking valve is used to break the vacuum in the quartz container to be coated.

[0021] Furthermore, the heating system includes a heating furnace body, the heating furnace body is connected to a temperature-controlling thermocouple, and the temperature-controlling thermocouple is connected to a temperature controller.

[0022] When in use, the temperature control thermocouple is used to measure the temperature of the furnace body, and the temperature controller cooperates with the control system to control the heating rate and temperature of the heating furnace body.

[0023] Furthermore, the heating furnace body is a vertical resistance furnace, which provides a temperature field for carbon coating.

[0024] Furthermore, the pneumatic system includes a pneumatic vertical slide rail and a pneumatic horizontal slide rail. The pneumatic horizontal slide rail is provided with a horizontal limit switch, and the pneumatic vertical slide rail is provided with a vertical limit switch and a slider. The horizontal limit switch and the vertical limit switch are used to detect the moving position of the slide rail slide.

[0025] The slider is located on a pneumatic vertical slide rail, and the control system controls the on and off of the air source of the pneumatic vertical / horizontal slide rail to make the slider move vertically up and down and stop;

[0026] The pneumatic vertical slide rail is located on the pneumatic horizontal slide rail, so that the pneumatic vertical slide rail can move horizontally left and right.

[0027] Furthermore, the slider is connected to the rotary carbon coating mechanism, and the carbon source supply system is fixed above the rotary carbon coating mechanism. When the slider moves, the carbon source supply system and the rotary carbon coating mechanism move with the slider.

[0028] Furthermore, the carbon source supply system is connected to the rotary carbon coating mechanism, and includes a carbon source container, a vacuum metal pipeline and a carbon source solenoid valve;

[0029] The vacuum pipeline connects the carbon source container and the carbon source battery valve, and the vacuum metal pipeline is used to transport the carbon source liquid;

[0030] The carbon source solenoid valve controls the supply of carbon source to the rotary carbon coating mechanism.

[0031] Furthermore, a carbon source bottle is arranged in the carbon source container, and a cover is arranged below the carbon source container.

[0032] When in use, the carbon source bottle is placed into the carbon source container from the bottom, and the carbon source bottle is fixed after the lid is closed.

[0033] Furthermore, a throttle valve is provided at the connection between the vacuum metal pipeline and the carbon source container, and the throttle valve is used to adjust the inlet flow rate of the carbon source liquid.

[0034] Furthermore, the rotary carbon coating mechanism includes a cooling cover, on which a rotating motor is provided, the rotating motor is connected to a sputtering quartz tube, the sputtering quartz tube is connected to the carbon source supply system, and the cooling cover is connected to a vacuum system.

[0035] Furthermore, the cooling cover is connected to the vacuum system via a vacuum nozzle.

[0036] Furthermore, the cooling cover is made of stainless steel, a sealing gasket is provided at the bottom of the cooling cover, and the upper end surface of the quartz container to be coated is sealed with the cooling cover through the sealing gasket.

[0037] Furthermore, the cooling cover is connected to a circulating cooling water jacket.

[0038] By setting a cooling water jacket and circulating cooling water into the cooling cover, the sealing gasket is cooled down to avoid damage to the sealing gasket in a high temperature environment.

[0039] Furthermore, the sputtering quartz tube is connected to the carbon source supply system by a sealed rotating head. After the connection, the sputtering quartz tube rotates together with the sealed rotating head. The rotating motor is connected to the sealed rotating head by a belt.

[0040] Furthermore, a magnetic fluid sealing bearing is used to seal between the sputtering quartz tube and the cooling cover.

[0041] During the carbon coating process, the control system controls the rotation of the rotary motor, and the sealed rotary head rotates together with the sputtering quartz tube. During the carbon coating process, the sputtering quartz tube is rotated to make the sputtered carbon source more uniform.

[0042] When in use, the liquid outlet of the sputtering quartz tube extends into the quartz container to be coated, and the carbon source liquid passes through the sputtering quartz tube from the carbon source supply system and then enters the quartz container to be coated.

[0043] Furthermore, small holes are evenly distributed on the sputtering quartz tube.

[0044] When in use, the carbon source liquid is sputtered from the small hole to the inner wall of the quartz tube to be coated. The carbon source liquid is rapidly decomposed and gasified at high temperature, and is deposited on the inner wall of the quartz container to be coated to form a dense carbon layer.

[0045] Furthermore, the control system controls the temperature of the heating furnace body, controls the opening and closing of each valve, controls the movement and stopping of the slider on the pneumatic vertical slide rail and the pneumatic horizontal slide rail, controls the speed and start and stop of the rotating motor, controls the vacuum degree of the quartz container to be coated through vacuum gauge feedback, the switching of the vacuum solenoid valve and the electromagnetic air-breaking valve, and the start and stop of the vacuum pump, thereby realizing the automatic operation of the carbon coating device.

[0046] Compared with the prior art, the present invention has the following beneficial effects:

[0047] 1. The device and method of the present invention adopts a vacuum carbon source sputtering method. The carbon source is evenly sputtered onto the quartz surface. The formed carbon layer is uniform and dense, has strong adhesion, and is not easy to fall off. The carbon layer isolates the sample from the quartz, reducing the risk of explosion during synthesis. The quartz container can be reused many times, reducing costs;

[0048] 2. The device and method of the present invention integrate quartz carbon coating and high-temperature calcination of the carbon layer. High-temperature vacuum calcination is conducive to further removing impurities in the coated carbon layer, improving the purity of the carbon layer, and effectively reducing the risk of contamination of the purity of the prepared material by the carbon-coated quartz container;

[0049] 3. The whole process of the device and method of the present invention is carried out in a closed environment, thus avoiding the safety problem of acetone vapor easily diffusing into the environment in the conventional method, and all controls are controlled according to the set program, with a high degree of automation, a short carbon coating cycle, and stable quality of the coated carbon layer. BRIEF DESCRIPTION OF THE DRAWINGS

[0050] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments are briefly introduced below. It should be understood that the following drawings only represent some embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without creative work.

[0051] Figure 1 It is a schematic diagram of the front view structure of the carbon coating device of the present invention.

[0052] Figure 2 It is a schematic diagram of the structure of the rotary carbon coating mechanism of the present invention.

[0053] Figure 3 It is a structural schematic diagram of the carbon source supply system of the present invention.

[0054] Figure 4 It is a left-side structural schematic diagram of the carbon coating device of the present invention.

[0055] In the above drawings, the meanings of the various marks are: 1-control system, 2-vacuum system, 3-rotary carbon coating mechanism, 4-heating system, 5-pneumatic system, 6-carbon source supply system, 7-vacuum pump, 8-vacuum gauge, 9-vacuum solenoid valve, 10-electromagnetic air-breaking valve, 11-heating furnace body, 12-temperature control thermocouple, 13-temperature controller, 14-pneumatic vertical slide rail, 15-pneumatic horizontal slide rail, 16-horizontal limit switch, 17-vertical limit switch, 18-slider, 19-carbon source container, 20-vacuum metal pipeline, 21-carbon source solenoid valve, 22-carbon source bottle, 23-lid, 24-throttle valve, 25-cooling cover, 26-rotating motor, 27-sputtering quartz tube, 28-vacuum nozzle, 29-sealing gasket, 30-circulating cooling water jacket, 31-sealed rotating head, 32-sealed bearing. DETAILED DESCRIPTION

[0056] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments.

[0057] An environmentally friendly quartz surface carbon coating device, such as Figure 1-Figure 4 As shown, it includes a control system 1, a vacuum system 2, a rotary carbon coating mechanism 3, a heating system 4, a pneumatic system 5 and a carbon source supply system 6. The vacuum system 2, the rotary carbon coating mechanism 3, the heating system 4, the pneumatic system 5 and the carbon source supply system 6 are all controlled by the control system 1 to realize the automatic operation of the carbon coating device.

[0058] In some embodiments, the vacuum system 2 includes a vacuum pump 7, and the vacuum pump 7 is connected to a vacuum gauge 8, a vacuum solenoid valve 9, an electromagnetic air-breaking valve 10 and the rotary carbon coating mechanism 3;

[0059] The vacuum pump 7 provides vacuuming power, the vacuum gauge 8 detects the vacuum degree in the quartz container to be coated, the vacuum solenoid valve 9 is used to open and close the connection between the vacuum pump 7 and the quartz container to be coated, and the electromagnetic air breaking valve 10 is used to break the vacuum in the quartz container to be coated.

[0060] In some embodiments, the heating system 4 includes a heating furnace body 11 , the heating furnace body 11 is connected to a temperature-controlling thermocouple 12 , and the temperature-controlling thermocouple 12 is connected to a temperature controller 13 .

[0061] When in use, the temperature control thermocouple 12 is used to measure the temperature of the furnace body, and the temperature controller 13 cooperates with the control system 1 to control the heating rate and heating temperature of the heating furnace body 11.

[0062] In some embodiments, the heating furnace body 11 is a vertical resistance furnace, which provides a temperature field for carbon coating.

[0063] In some embodiments, the pneumatic system 5 includes a pneumatic vertical slide 14 and a pneumatic horizontal slide 15, the pneumatic horizontal slide 15 is provided with a horizontal limit switch 16, the pneumatic vertical slide 14 is provided with a vertical limit switch 17 and a slider 18, and the horizontal limit switch 16 and the vertical limit switch 17 are used to detect the moving position of the slide table.

[0064] The slider 18 is located on the pneumatic vertical slide rail 14, and the control system 1 controls the on and off of the air source of the pneumatic vertical / horizontal slide rail to make the slider 18 move vertically up and down and stop;

[0065] The pneumatic vertical slide rail 14 is located on the pneumatic horizontal slide rail 15, so that the pneumatic vertical slide rail 14 can move horizontally left and right.

[0066] In some embodiments, the slider 18 is connected to the rotary carbon coating mechanism 3 , and the carbon source supply system 6 is fixed above the rotary carbon coating mechanism 3 . When the slider 18 moves, the carbon source supply system 6 and the rotary carbon coating mechanism 3 follow the movement of the slider 18 .

[0067] In some embodiments, the carbon source supply system 6 is connected to the rotary carbon coating mechanism 3 and includes a carbon source container 19, a vacuum metal pipeline 20 and a carbon source solenoid valve 21;

[0068] The vacuum pipeline connects the carbon source container 19 and the carbon source battery valve, and the vacuum metal pipeline 20 is used to transport the carbon source liquid;

[0069] The carbon source solenoid valve 21 controls the supply of the carbon source to the rotary carbon coating mechanism 3 .

[0070] In some embodiments, a carbon source bottle 22 is disposed in the carbon source container 19 , and a cover 23 is disposed below the carbon source container 19 .

[0071] When in use, the carbon source bottle 22 is placed into the carbon source container 19 from the bottom of the carbon source container 19 , and the carbon source bottle 22 is fixed after the lid 23 is closed.

[0072] In some embodiments, a throttle valve 24 is provided at the connection between the vacuum metal pipeline 20 and the carbon source container 19, and the throttle valve 24 is used to adjust the inlet flow rate of the carbon source liquid.

[0073] In some embodiments, the rotary carbon coating mechanism 3 includes a cooling cover 25 , on which a rotating motor 26 is disposed. The rotating motor 26 is connected to a sputtering quartz tube 27 , which is connected to the carbon source supply system 6 , and the cooling cover 25 is connected to the vacuum system 2 .

[0074] In some embodiments, the cooling cover 25 is connected to the vacuum system 2 via a vacuum nozzle 28 .

[0075] In some embodiments, the cooling cover 25 is made of stainless steel, a sealing gasket 29 is provided at the bottom of the cooling cover 25 , and the upper end surface of the quartz container to be coated is sealed with the cooling cover 25 through the sealing gasket 29 .

[0076] In some embodiments, the cooling cover 25 is connected to a circulating cooling water jacket 30 .

[0077] By providing a cooling water jacket, circulating cooling water is introduced into the cooling cover 25 to cool the sealing gasket 29, thereby preventing the sealing gasket 29 from being damaged in a high temperature environment.

[0078] In some embodiments, the sputtering quartz tube 27 is connected to the carbon source supply system 6 by a sealed rotating head 31. The connected sputtering quartz tube 27 rotates together with the sealed rotating head 31. The rotating motor 26 is connected to the sealed rotating head 31 by a belt.

[0079] In some embodiments, a magnetic fluid sealing bearing 32 is used to seal between the sputtering quartz tube 27 and the cooling cover 25 .

[0080] During the carbon coating process, the control system 1 controls the rotating motor 26 to rotate, and the sealed rotating head 31 rotates together with the sputtering quartz tube 27. During the carbon coating process, the sputtering quartz tube 27 is rotated to make the sputtered carbon source more uniform.

[0081] When in use, the liquid outlet of the sputtering quartz tube 27 extends into the quartz container to be coated, and the carbon source liquid flows from the carbon source supply system 6, passes through the sputtering quartz tube 27, and then enters the quartz container to be coated.

[0082] In some embodiments, small holes are evenly distributed on the sputtering quartz tube 27 .

[0083] When in use, the carbon source liquid is sputtered from the small hole to the inner wall of the quartz tube to be coated. The carbon source liquid is rapidly decomposed and gasified at high temperature, and is deposited on the inner wall of the quartz container to be coated to form a dense carbon layer.

[0084] In some embodiments, the control system 1 controls the temperature of the heating furnace body 11, controls the opening and closing of each valve, controls the movement and stopping of the slider 18 on the pneumatic vertical slide rail 14 and the pneumatic horizontal slide rail 15, controls the speed and start and stop of the rotating motor 26, and controls the vacuum degree of the quartz container to be coated through feedback from the vacuum gauge 8, the switching of the vacuum solenoid valve 9 and the electromagnetic air-breaking valve 10, and the start and stop of the vacuum pump 7, thereby realizing the automatic operation of the carbon coating device.

[0085] Example 1

[0086] An environmentally friendly quartz surface carbon coating method using the above device in this embodiment includes the following steps:

[0087] An environmentally friendly quartz surface carbon coating method comprises the following steps:

[0088] S1. Surface treatment of a quartz container, wherein the surface treatment of the quartz container is specifically washing with sodium hydroxide - washing with ultrapure water - washing with aqua regia - washing with ultrapure water, washing and drying for standby use, and the quartz container is a quartz tube;

[0089] S2. Remove the air in the quartz tube and place the quartz tube in a vacuum environment with a vacuum degree of less than 10Pa;

[0090] S3. Heating to 1000°C in vacuum and then maintaining the temperature constant to complete preheating;

[0091] S4. Rotary sputtering of carbon source was performed at 1000°C under vacuum, with the rotation speed controlled at 5r / s;

[0092] S5. After the carbon source sputtering is completed, the coating is calcined at high temperature in a vacuum state. The calcination temperature is 1000℃ and the vacuum degree is better than 10 -3 Pa, the calcination time is not less than 30min, which is used to improve the uniformity of the carbon layer and enhance the adhesion of the carbon layer. At the same time, high temperature and high vacuum are conducive to the volatilization of impurities in the carbon layer and improve the purity of the carbon layer. After calcination, it is immediately removed from the heating furnace body and rapidly cooled in a room temperature environment to complete the carbon coating.

[0093] The carbon-coated quartz container prepared in the above embodiment was used for verification in the synthesis of high-purity cadmium zinc telluride and the direct pulling purification of high-purity cadmium. The carbon-coated quartz tube was used for verification of the synthesis of cadmium zinc telluride with a purity of 99.99999%. The prepared cadmium zinc telluride was relatively easy to remove during the tube breaking operation. The cadmium zinc telluride material would not contact the quartz tube wall. The carbon layer on the inner wall of the quartz tube was intact after the material was removed. The purity of the prepared cadmium zinc telluride was tested. The product quality met the standard requirements of GB / T 41662-2022, and the carbon layer would not cause pollution to the product. The carbon-coated quartz crucible was used for direct pulling purification to prepare high-purity cadmium with a purity of 99.99999%. The quartz crucible can be reused at least 8 times, and the purity of the prepared high-purity cadmium meets the standard requirements of YS / T 1190-2017. The coating index thickness is ≥0.1mm, and the bonding force of the coating is ≥30N.

[0094] Comparative Example 1

[0095] In this embodiment, which is a comparative example of the present invention, the only difference between Example 1 and Steps S2-S5 is that they are not performed under vacuum. During the process, the carbon source (acetone) may overflow into the air, which may cause harm to the operator. At the same time, the carbon layer may be oxidized by contact with the air at high temperature to generate carbon dioxide, which may affect the thickness and uniformity of the carbon layer.

[0096] Comparative Example 2

[0097] In this embodiment, which is used as a comparison of the present invention, the only change on the basis of Example 1 is that the rotating motor 26 is not used for sputtering and its operation, and the other steps are the same. The carbon layer thickness of the prepared carbon-coated quartz tube is tested. The carbon layer thickness ranges from 0.05 to 0.15 mm at different parts. The carbon layer is uneven and is easy to fall off during use.

[0098] Comparative Example 3

[0099] In this embodiment, which is used as a comparison of the present invention, the only change on the basis of Example 1 is that the calcination in S5 is followed by natural cooling at high temperature, and the other steps are the same. The carbon layer adhesion test is performed on the prepared carbon-coated quartz tube, and the carbon layer adhesion is <20N. During use, the carbon layer is easy to fall off.

[0100] The above are the implementation methods listed in this embodiment, but this embodiment is not limited to the above optional implementation methods. Those skilled in the art can arbitrarily combine the above methods to obtain other various implementation methods. Anyone can derive other various forms of implementation methods under the inspiration of this embodiment. The above specific implementation methods should not be understood as limiting the scope of protection of this embodiment. The scope of protection of this embodiment shall be based on the definition in the claims, and the description can be used to interpret the claims.

Claims

1. An environmentally friendly quartz surface carbon coating method, characterized in that: The following steps are involved: S1. Quartz container surface treatment; S2. Remove the air in the quartz container and place the quartz container in a vacuum environment; S3. Preheating under vacuum; S4. Carbon source rotation sputtering; S5. High temperature calcination. After calcination, the temperature is rapidly lowered in a room temperature environment to complete carbonization.

2. The environmentally friendly quartz surface carbon coating method according to claim 1, characterized in that: The surface treatment of the quartz container is specifically performed by using sodium hydroxide alkaline washing - ultrapure water washing - aqua regia acid washing - ultrapure water washing, and then drying for standby use.

3. The environmentally friendly quartz surface carbon coating method according to claim 1, characterized in that: The quartz container is ultrapure water quartz with an electrical conductivity of not less than 12 MΩ·CM.

4. The environmentally friendly quartz surface carbon coating method according to claim 1, characterized in that: In step S2, the vacuum degree in the quartz container tube is lower than 10Pa.

5. The environmentally friendly quartz surface carbon coating method according to claim 1, characterized in that: The preheating in step S3 is completed by heating the temperature to 950-1050° C. in a vacuum state.

6. The environmentally friendly quartz surface carbon coating method according to claim 1, characterized in that: The step S4 is to perform carbon source rotation sputtering at 950-1050°C.

7. The environmentally friendly quartz surface carbon coating method according to claim 1, characterized in that: The high temperature calcination temperature is 950-1050°C and the vacuum degree is 10 -3 Pa—10 -4 Pa, calcination time is 30-40min.

8. An environmentally friendly quartz surface carbon coating device, characterized in that: The invention comprises a control system (1), a vacuum system (2), a rotary carbon coating mechanism (3), a heating system (4), a pneumatic system (5) and a carbon source supply system (6); the vacuum system (2), the rotary carbon coating mechanism (3), the heating system (4), the pneumatic system (5) and the carbon source supply system (6) are all controlled by the control system (1), thereby realizing automatic operation of the carbon coating device.

9. The environmentally friendly quartz surface carbon coating device according to claim 8, characterized in that: The heating system (4) comprises a heating furnace body (11), the heating furnace body (11) is connected to a temperature control thermocouple (12), and the temperature control thermocouple (12) is connected to a temperature controller (13); When in use, the temperature control thermocouple (12) is used to measure the temperature of the furnace body, and the temperature controller (13) cooperates with the control system (1) to control the heating rate and heating temperature of the heating furnace body (11).

10. The environmentally friendly quartz surface carbon coating device according to claim 8, characterized in that: The rotary carbon coating mechanism (3) comprises a cooling cover (25), a rotating motor (26) is arranged on the cooling cover (25), the rotating motor (26) is connected to a sputtering quartz tube (27), the sputtering quartz tube (27) is connected to the carbon source supply system (6), and the cooling cover (25) is connected to a vacuum system (2).

Citation Information

Patent Citations

  • Preparation method of quartz surface carbon coating and quartz material

    CN113755817A