CN115584492A - Method for generating high-density atmospheric pressure fluorocarbon plasma jet - Google Patents
Method for generating high-density atmospheric pressure fluorocarbon plasma jet Download PDFInfo
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- CN115584492A CN115584492A CN202211277678.5A CN202211277678A CN115584492A CN 115584492 A CN115584492 A CN 115584492A CN 202211277678 A CN202211277678 A CN 202211277678A CN 115584492 A CN115584492 A CN 115584492A
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- atmospheric pressure
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- fluorocarbon plasma
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/511—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/515—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using pulsed discharges
Abstract
The invention discloses a method for generating high-density atmospheric pressure fluorocarbon plasma jet, and belongs to the field of application of atmospheric pressure low-temperature plasma. The method adopts CF 4 Or Ar/CF 4 The mixed gas is used as working gas, a pulse modulation microwave power supply is used for exciting discharge, a discharge device is designed based on the principle of a coaxial resonant cavity, a local enhanced electric field is generated at the opening end of the device, the working gas is efficiently ionized, and atmospheric pressure fluorocarbon plasma jet flow with high density and controllable temperature is generated. The atmospheric pressure fluorocarbon plasma jet generated by the method is suitable for surface fluorination treatment of polymer insulating materials, and can make up for the defects of low density and insufficient fluorination degree of the material surface of the existing fluorocarbon plasma.
Description
Technical Field
The invention relates to the technical field of application of atmospheric pressure low-temperature plasma, in particular to a method for generating high-density atmospheric pressure fluorocarbon plasma jet.
Background
Solid insulation is commonly used in electrical engineering to achieve electrical isolation and mechanical fixation. Due to the existence of the surface flashover phenomenon, the interface of solid insulation and air is often a weak link of an insulation system, and the surface electric strength of the solid insulation and the air is far lower than that of a matrix of the solid insulation and the air. Therefore, the improvement of the surface resistance of the solid insulation has important significance. Fluorine-containing materials generally have high electrical insulation strength and chemical stability, and have wide application in insulation materials. Research shows that the surface fluorination treatment of the insulating material can effectively improve the electrical resistance of the edge surface without influencing the matrix performance. Surface fluorination of insulating materialsInitially through F 2 Or F 2 /N 2 The mixed gas treatment is directly carried out due to F 2 It is highly toxic and corrosive, requires the reaction to be carried out in a closed vacuum system, and is extremely hazardous. In recent years, researchers have proposed methods for surface fluorination of insulating materials using fluorocarbon plasmas to avoid F by generating activated fluorocarbon radicals by discharge of fluorocarbon gases to react with the surface of the material 2 The fluorocarbon plasma can be generated under atmospheric pressure, an expensive vacuum system is not needed, the cost can be reduced, and the fluorocarbon plasma is more efficient and convenient.
At present, atmospheric pressure fluorocarbon plasma is mainly generated based on a dielectric barrier discharge principle. Because fluorine has strong electron affinity, the breakdown field strength of the fluorocarbon gas under atmospheric pressure is high, and ionization is difficult, so that even if fluorocarbon plasma is generated under the excitation of a strong external electric field, the gas temperature is inevitably too high, and the application is difficult. To address this problem, researchers typically mix large amounts of inert gases (usually Ar and He) to reduce breakdown field strength and gas temperature. However, when a large amount of inert gas is added, the proportion of fluorocarbon gas is reduced, and the content of fluorocarbon groups in the generated plasma is greatly reduced, so that the degree of fluorination of the material surface is insufficient. The data show that application F 2 Or F 2 /N 2 The fluorine content on the surface of the material directly fluorinated by the mixed gas can reach 30-40%, while the fluorine content on the surface of the material treated by the atmospheric pressure fluorocarbon plasma generated by dielectric barrier discharge is usually 10-20%.
In view of the above, it is desirable to develop a method for generating a fluorocarbon plasma jet with high density and atmospheric pressure, so as to fluorinate the surface of an insulating material more sufficiently, and the high density plasma generally has a higher gas temperature, so that the gas temperature of the fluorocarbon plasma must be controlled to avoid thermal damage to the target, thereby being suitable for practical applications, and other problems to be solved (see below).
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for generating high-density atmospheric pressure fluorocarbon plasma jet, which solves the following technical problems:
1. surface fluorination of conventional insulating materials initially by F 2 Or F 2 /N 2 The mixed gas treatment is directly carried out due to F 2 Strong toxicity and corrosiveness, the reaction needs to be carried out in a closed vacuum system, and the danger is extremely high;
2. fluorine has strong electron affinity, the breakdown field strength of the fluorocarbon gas under atmospheric pressure is high, and the fluorocarbon gas is difficult to ionize, and even if fluorocarbon plasma is generated under the excitation of a strong external electric field, the gas temperature is inevitably too high to be applied;
3. after a large amount of inert gas is added, the proportion of the fluorocarbon gas is reduced, the content of fluorocarbon groups in the generated plasma is greatly reduced, and the fluorination degree of the surface of the material is insufficient;
4. applications F 2 Or F 2 /N 2 The fluorine content on the surface of the material directly fluorinated by the mixed gas can reach 30-40%, and the fluorine content on the surface of the material treated by the atmospheric pressure fluorocarbon plasma generated by dielectric barrier discharge is usually 10-20%;
5. the electron density of the glow discharge is generally not more than 10 17 /m 3 And the electron density of microwave discharge can reach 10 20 /m 3 Active particle components in the high-density plasma are more abundant, and the fluorination effect of the surface of the insulating material is favorably improved;
6. in order to reduce the gas temperature, the gas flow is usually increased or a cooling gas flow is additionally arranged to reduce the temperature, but the excessive gas flow causes the working gas to be transited from a laminar flow to a turbulent flow state, so that the instability of discharge is increased, the density of active particles is reduced, and even the discharge is extinguished.
(II) technical scheme
In order to realize the purpose, the invention is realized by the following technical scheme: a method for generating high-density atmospheric pressure fluorocarbon plasma jet is used for generating fluorocarbon plasma by adopting a pulse modulation microwave power supply and a coaxial microwave power supplyThe average electron density of the fluorocarbon plasma is greater than or equal to 10 20 /m 3 The working gas of the coaxial resonant cavity device is ionized under the action of the local enhanced electric field at the opening end of the coaxial resonant cavity device to generate atmospheric pressure fluorocarbon plasma jet.
Preferably, the working gas of the coaxial resonant cavity device is CF 4 A gas.
Preferably, the working gas of the coaxial resonant cavity device is Ar/CF 4 And (4) mixing the gases.
Preferably, the pulsed microwave power supply is capable of regulating the gas temperature by adjusting the duty cycle.
Preferably, the coaxial resonant cavity device is capable of ionizing the CF at atmospheric pressure 4 A gas.
Preferably, the microwave frequency of the pulse modulation microwave power supply is 2.45GHz, the output power is in the range of 0-200W, the frequency of the modulation pulse is in the range of 10Hz-200kHz, and the duty ratio is in the range of 1% -99%.
Preferably, the length of the coaxial resonant cavity device is designed to be one quarter of the wavelength of the microwave 30.6mm, one end of the coaxial resonant cavity device is open-circuited, the other end of the coaxial resonant cavity device is short-circuited, the microwave power is fed into the coaxial resonant cavity through the SMA interface, and the position of the coaxial resonant cavity is 6.5mm away from the inner wall of the short-circuited end, so that the open-circuited end of the inner conductor is a resonant position, and the maximum field intensity is obtained.
(III) advantageous effects
The invention provides a method for generating high-density atmospheric pressure fluorocarbon plasma jet. The method has the following beneficial effects:
(1) The method for generating the high-density atmospheric pressure fluorocarbon plasma jet uses microwave discharge to generate fluorocarbon plasma, and the density of the fluorocarbon plasma is higher than that of the fluorocarbon plasma generated by dielectric barrier discharge (for example, the electron density of atmospheric pressure dielectric barrier glow discharge is generally not more than 10) 17 /m 3 )。
(2) The method for generating the high-density atmospheric pressure fluorocarbon plasma jet generates a local enhanced electric field by using the coaxial resonant cavity device, and can directly ionize pure CF under atmospheric pressure 4 A fluorocarbon plasma jet is generated.
(3) The generation method of the high-density atmospheric pressure fluorocarbon plasma jet reduces the gas temperature by adopting a pulse modulation technology, can adjust the gas temperature within the range of 50-500 ℃ by combining other parameters, and selects the gas temperature according to the heat resistance of an acting object.
Drawings
FIG. 1 is a schematic diagram of a method for generating a high-density atmospheric-pressure fluorocarbon plasma jet.
FIG. 2 is pure CF 4 Image of a microwave plasma jet.
FIG. 3 is Ar/CF 4 Image of a microwave plasma jet.
FIG. 4 shows He/CF 4 Image of a microwave plasma jet.
FIG. 5 is pure CF 4 Emission spectrum of microwave plasma jet.
FIG. 6 is Ar/CF 4 Emission spectrum of microwave plasma jet.
FIG. 7 is Ar/CF 4 Electron density diagnostic plot of microwave plasma jet.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a method for generating a high density atmospheric pressure fluorocarbon plasma jet is illustrated in a detailed schematic diagram. The pulse modulation microwave power supply is adopted to excite discharge, the length of a cavity of the coaxial resonator is designed to be one-fourth of the wavelength of microwave, namely 30.6mm, one end of the cavity is open, the other end of the cavity is short-circuited, microwave energy is fed into the coaxial resonator through a microwave high-frequency connector (SMA interface) and is 6.5mm away from the inner wall of the short-circuited end, and a local enhanced electric field can be generated at the open end under the action of resonance reflection of the device. CF (compact flash) 4 Or Ar/CF 4 The mixed gas passes through the coaxial resonatorThe gas interface of the device is introduced into the device, the total flow of the gas is controlled within the range of 0.1-10L/min, and the working gas is ionized under the action of the local enhanced electric field at the opening end of the device to generate atmospheric pressure fluorocarbon plasma jet. By regulating and controlling gas proportioning parameters and power supply parameters, atmospheric pressure fluorocarbon plasma jet flows with different appearances and different particle components can be obtained.
Example 1:
using a CF 4 As a working gas, the method is applied to generate an atmospheric pressure fluorocarbon plasma jet. When the microwave incident power was 100W, the pulse modulation duty ratio was 60%, the modulation frequency was 30kHz, and the gas flow rate was 0.4L/min, the discharge pattern was as shown in FIG. 2. Form pure CF at the open end of the device 4 Plasma jet, which is difficult to achieve in atmospheric pressure dielectric barrier discharge. Referring to FIG. 5, it can be seen that the main active species component in the fluorocarbon plasma jet comprises CF 2 Radical, CF 2 + Ion, C 2 Groups and F atoms, and the like.
Example 2:
using Ar and CF 4 Mixed as working gas, and the method is applied to generate atmospheric pressure fluorocarbon plasma jet. When the microwave power is 80W, the pulse modulation duty ratio is 50 percent, the modulation frequency is 20kHz, the total gas flow is 2L/min and CF 4 When the volume fraction is 2%, the discharge image is shown in fig. 3. The morphology of the fluorocarbon plasma jet at this time and pure CF 4 Plasma jets differ. Referring to FIG. 6, it can be seen that the main active species component in the fluorocarbon plasma jet comprises CF 2 Radical, CF 2 + Ion, C 2 A group, a F atom, an Ar atom, and the like. Referring to FIG. 7, for Ar/CF 4 The electron density of the plasma jet is diagnosed, and the average electron density is 10 20 /m 3 An order of magnitude.
Example 3:
using He and CF 4 Mixed as working gas, and the method is applied to generate atmospheric pressure fluorocarbon plasma jet. When the microwave power is 100W, the pulse modulation duty ratio is 50 percent, the modulation frequency is 20kHz, the total gas flow is 2L/min and CF 4 When the volume fraction is 2%, it is putThe electrical image is referred to fig. 4. At the moment, the discharge is concentrated at the port of the discharge device and inside the device, and effective fluorocarbon plasma jet flow cannot be formed outside the device, so that the working gas of the method adopts pure CF 4 Or Ar/CF 4 。
Example 4:
the gas temperature can be effectively reduced through a pulse modulation technology, the gas temperature of the microwave plasma under different duty ratios is shown in a table below, and the microwave plasma gas temperature can be adjusted in a wider temperature range by being used together with the gas flow.
The following is the effect of adjusting duty cycle on temperature under fixed gas flow, gas ratio conditions
With Ar/CF 4 Gas, CF 4 The proportion is as follows: 2%, total flow rate: 2L/min, microwave input power: 60W, modulation frequency: 20kHz, unit: measurement was repeated 3 times at DEG C
The temperature adjusting range of a larger range can be achieved by matching with traditional airflow adjustment, power adjustment, gas proportion and modulation.
It should be noted that in the description of the present invention, the terms "upper", "lower", "left", "right", "front", "rear", and the like indicate orientations or positional relationships based on structures shown in the drawings, and are only used for convenience in describing the present invention, but do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the technical scheme, the terms "first" and "second" are only used for referring to the same or similar structures or corresponding structures with similar functions, and are not used for ranking the importance of the structures, or comparing the sizes or other meanings.
In addition, unless expressly stated or limited otherwise, the terms "mounted" and "connected" are to be construed broadly, e.g., the connection may be a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; the two structures can be directly connected or indirectly connected through an intermediate medium, and the two structures can be communicated with each other. To those skilled in the art, the specific meanings of the above terms in the present invention can be understood in light of the present general concepts, in connection with the specific context of the scheme.
Claims (7)
1. A method for generating high-density atmospheric pressure fluorocarbon plasma jet is used for generating fluorocarbon plasma, and is characterized in that: the discharge is generated by adopting a pulse modulation microwave power supply and a coaxial resonant cavity device, and the average electron density of the fluorocarbon plasma is more than or equal to 10 20 /m 3 The working gas of the coaxial resonant cavity device is ionized under the action of the local enhanced electric field at the opening end of the coaxial resonant cavity device to generate atmospheric pressure fluorocarbon plasma jet.
2. The method of claim 1, wherein the high-density atmospheric pressure fluorocarbon plasma jet is generated by: the working gas of the coaxial resonant cavity device is CF 4 A gas.
3. The method of claim 1, wherein the high-density atmospheric pressure fluorocarbon plasma jet is generated by: the working gas of the coaxial resonant cavity device is Ar/CF 4 And (4) mixing the gases.
4. The method of claim 1, wherein the high-density atmospheric pressure fluorocarbon plasma jet is generated by: the pulsed microwave power supply is capable of regulating the gas temperature by adjusting the duty cycle.
5. A method for generating a high density atmospheric pressure fluorocarbon plasma jet as claimed in claim 2, wherein: the coaxial resonant cavity device is capable of ionizing CF at atmospheric pressure 4 A gas.
6. The method of claim 1, wherein the high-density atmospheric pressure fluorocarbon plasma jet is generated by: the microwave frequency of the pulse modulation microwave power supply is 2.45GHz, the output power is in the range of 0-200W, the frequency of the modulation pulse is in the range of 10Hz-200kHz, and the duty ratio is in the range of 1% -99%.
7. The method of claim 1, wherein the high-density atmospheric pressure fluorocarbon plasma jet is generated by: the length of the coaxial resonant cavity device is designed to be one quarter of the wavelength of the microwave 30.6mm, one end of the coaxial resonant cavity device is open-circuit, the other end of the coaxial resonant cavity device is short-circuit, the microwave power is fed into the coaxial resonant cavity through the SMA interface, and the position of the coaxial resonant cavity is 6.5mm away from the inner wall of the short-circuit end, so that the open-circuit end of the inner conductor is a resonant position, and the maximum field intensity is obtained.
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| CN202211277678.5A CN115584492A (en) | 2022-10-19 | 2022-10-19 | Method for generating high-density atmospheric pressure fluorocarbon plasma jet |
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| CN202211277678.5A CN115584492A (en) | 2022-10-19 | 2022-10-19 | Method for generating high-density atmospheric pressure fluorocarbon plasma jet |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1038673A (en) * | 1988-05-25 | 1990-01-10 | 佳能株式会社 | Microwave plasma processing apparatus |
| CN111203164A (en) * | 2020-02-23 | 2020-05-29 | 李容毅 | Gas phase reaction buffer chamber based on atmospheric pressure microwave plasma torch |
| CN112135409A (en) * | 2020-10-16 | 2020-12-25 | 安徽酷熠电磁科技有限公司 | Air microwave plasma jet surface treatment device |
| CN114867180A (en) * | 2022-05-23 | 2022-08-05 | 安徽工业大学 | Double-channel atmospheric pressure microwave plasma jet device |
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2022
- 2022-10-19 CN CN202211277678.5A patent/CN115584492A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1038673A (en) * | 1988-05-25 | 1990-01-10 | 佳能株式会社 | Microwave plasma processing apparatus |
| CN111203164A (en) * | 2020-02-23 | 2020-05-29 | 李容毅 | Gas phase reaction buffer chamber based on atmospheric pressure microwave plasma torch |
| CN112135409A (en) * | 2020-10-16 | 2020-12-25 | 安徽酷熠电磁科技有限公司 | Air microwave plasma jet surface treatment device |
| CN114867180A (en) * | 2022-05-23 | 2022-08-05 | 安徽工业大学 | Double-channel atmospheric pressure microwave plasma jet device |
Non-Patent Citations (1)
| Title |
|---|
| 张兆镗: "《磁控管与微波加热技术》", 电子科技大学出版社, pages: 680 - 682 * |
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