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CN105430861A - A temperature-controllable low-temperature plasma generation method - Google Patents

A temperature-controllable low-temperature plasma generation method Download PDF

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Publication number
CN105430861A
CN105430861A CN201510938928.9A CN201510938928A CN105430861A CN 105430861 A CN105430861 A CN 105430861A CN 201510938928 A CN201510938928 A CN 201510938928A CN 105430861 A CN105430861 A CN 105430861A
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temperature
low
plasma
gas
power supply
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刘新
黄帅
宋金龙
陈发泽
杨晓龙
刘吉宇
刘子艾
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Dalian University of Technology
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Dalian University of Technology
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05HPLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00Generating plasma; Handling plasma
    • H05H1/24Generating plasma

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Abstract

The invention provides a temperature-controlled low-temperature plasma generation method, and belongs to the technical field of plasma discharge reactors. According to the method, a gas supply device supplies a gas with a certain pressure under the conditions of an atmospheric pressure and a room temperature; the gas is introduced into a gas control device and is transmitted to a vortex tube according to certain flow and pressure; the gas which is cooled in real time enters a plasma generator and discharges to generate a low-temperature plasma under the control of a high voltage power supply; and a temperature monitoring device can detect and display the temperature of the gas which is cooled by the vortex tube and the temperature of the generated low-temperature plasma. Through matched adjustment of the power supply voltage, the frequency and the gas pressure and flow, the controlled temperature of the low-temperature plasma from 200 DEG C to -4 DEG C is achieved; a working gas is cooled by a passive vortex tube in real time; the temperature-controlled plasma which is lower than a low temperature or even the room temperature can be obtained after the plasma generator discharges; and only the flow and the pressure of the working gas input into the vortex tube need to be adjusted in the control of the plasma temperature.

Description

一种温度可控的低温等离子体产生方法A temperature-controllable low-temperature plasma generation method

技术领域technical field

本发明涉及一种低温等离子体产生方法,属于等离子体放电反应器技术领域。The invention relates to a method for generating low-temperature plasma, which belongs to the technical field of plasma discharge reactors.

背景技术Background technique

大气压低温等离子体在材料表面改性、杀菌、生物医学等领域有广泛的应用。对聚合物和生物材料等进行表面改性时,等离子体的温度对材料的性能影响显著,特别的,对细胞、细菌、皮肤、组织等有生物活性的对象进行改性时,达到蛋白质凝固温度以上的等离子体温度会将生物体直接灭活,这将使改性过程难以控制;等离子体用于刻蚀半导体材料时,温度会直接影响刻蚀出的纳米结构和表面完整性。同时,材料表面改性用的冷等离子体的温度通常难以控制,其温度一般在室温以上,使得等离子体作用于材料表面时相当于叠加一个加热过程,这是等离子体应用于精密加工和生物医疗等领域亟待解决的问题。公开号为CN100394542C的发明专利介绍了一种气体温度可控的等离子体刻蚀装置,通过电热丝在进气端对气体加热以控制气体的温度来改变气体分子的运动速度,使得反应腔内的介质均匀分布。公开号为CN103165368A的发明专利提出了一种温度可调的等离子体约束装置,在气体通过的区域布置填充有热交换液的管道实现调控等离子体约束装置的温度,可将装置的温度恒定在50℃~90℃之间的数值。公开号为CN103906336A的发明专利介绍了一种压力温度可调的气体放电等离子体发生装置,采用泵稳定压力气罐中的压力在0~1.1Mpa范围内,采用加热片可将气体加热至最高100℃。上述发明均采用对气体进行加热或热交换的方式控制等离子体和装置的温度,无法得到和控制室温以及低于室温状态的低温等离子体。Atmospheric pressure low-temperature plasma has a wide range of applications in the fields of material surface modification, sterilization, and biomedicine. When modifying the surface of polymers and biological materials, the temperature of the plasma has a significant impact on the performance of the material. In particular, when modifying biologically active objects such as cells, bacteria, skin, and tissues, the protein coagulation temperature is reached. The above plasma temperature will directly inactivate the organism, which will make the modification process difficult to control; when the plasma is used to etch semiconductor materials, the temperature will directly affect the etched nanostructure and surface integrity. At the same time, the temperature of cold plasma used for material surface modification is usually difficult to control, and its temperature is generally above room temperature, so that when the plasma acts on the surface of the material, it is equivalent to superimposing a heating process. This is the application of plasma in precision processing and biomedicine. issues that need to be resolved urgently. The invention patent with the publication number CN100394542C introduces a plasma etching device with controllable gas temperature. The electric heating wire heats the gas at the inlet end to control the temperature of the gas to change the movement speed of the gas molecules, so that the gas in the reaction chamber The medium is evenly distributed. The invention patent with the publication number CN103165368A proposes a temperature-adjustable plasma confinement device. Pipelines filled with heat exchange fluid are arranged in the area where the gas passes through to regulate the temperature of the plasma confinement device. The temperature of the device can be kept constant at 50 The value between ℃~90℃. The invention patent with the publication number CN103906336A introduces a gas discharge plasma generating device with adjustable pressure and temperature. The pressure in the gas tank is stabilized by a pump in the range of 0-1.1Mpa, and the gas can be heated to a maximum of 100Mpa by using a heating plate. ℃. The above-mentioned inventions all adopt the method of heating or exchanging heat to control the temperature of the plasma and the device, and it is impossible to obtain and control the low-temperature plasma at or below room temperature.

发明内容Contents of the invention

本发明提供了一种温度可控的低温等离子体产生方法,采用将气体冷却后再进行放电的方式控制等离子体的温度。The invention provides a temperature-controllable low-temperature plasma generation method, which controls the temperature of the plasma by cooling the gas and then discharging it.

本发明在大气压室温条件下采用涡流管冷却气体,然后通过裸电极放电的形式产生低温等离子体。The invention uses a vortex tube to cool the gas under the condition of atmospheric pressure and room temperature, and then generates low-temperature plasma in the form of bare electrode discharge.

一种温度可控的低温等离子体产生方法,该方法所用的装置包括供气装置、气体控制装置、涡流管、高压电源、等离子体发生器和温度监测装置;供气装置提供具有一定压力的工作气体,工作气体通向气体控制装置,按照一定的流量和压力输向涡流管;工作气体经涡流管冷却后,进入等离子体发生器;高压电源控制等离子体发生器的放电过程,并产生低温等离子体;温度监测装置用于监测冷却后的工作气体温度和产生的低温等离子体的温度;通过调整输入涡流管的工作气体压力、流量和涡流管参数,控制输入等离子体发生器的工作气体温度,从而控制由等离子体发生器产生的低温等离子体的温度;通过电源电压、频率、气体压力和流量的配合调整,实现低温等离子体温度从200℃~-4℃范围内可控。A temperature-controllable low-temperature plasma generation method, the device used in the method includes a gas supply device, a gas control device, a vortex tube, a high-voltage power supply, a plasma generator and a temperature monitoring device; the gas supply device provides a working pressure with a certain pressure Gas, the working gas leads to the gas control device, and is transported to the vortex tube according to a certain flow rate and pressure; the working gas enters the plasma generator after being cooled by the vortex tube; the high-voltage power supply controls the discharge process of the plasma generator, and generates low-temperature plasma body; the temperature monitoring device is used to monitor the temperature of the cooled working gas and the temperature of the generated low-temperature plasma; by adjusting the working gas pressure, flow rate and parameters of the vortex tube input to the vortex tube, the temperature of the working gas input into the plasma generator is controlled, In order to control the temperature of the low-temperature plasma generated by the plasma generator; through the coordinated adjustment of power supply voltage, frequency, gas pressure and flow rate, the temperature of the low-temperature plasma can be controlled from 200°C to -4°C.

供气装置提供的工作气体为高纯的氮气、氩气、氦气、氯气、氧气、经过滤干燥的空气中的一种或两种以上混合。The working gas provided by the gas supply device is one or a mixture of two or more of high-purity nitrogen, argon, helium, chlorine, oxygen, and filtered and dried air.

所述的等离子体发生器放电形式是裸电极放电、介质阻挡放电或空心阴极放电。The discharge form of the plasma generator is bare electrode discharge, dielectric barrier discharge or hollow cathode discharge.

所述的高压电源是直流高压电源、低频高压电源、射频高压电源、微波高压电源或脉冲高压电源。The high-voltage power supply is a DC high-voltage power supply, a low-frequency high-voltage power supply, a radio frequency high-voltage power supply, a microwave high-voltage power supply or a pulse high-voltage power supply.

当输入涡流管的工作气体压力为0.5MPa,流量为18~25mL/min时,涡流管将工作气体冷却至7℃~1℃,采用低频正弦交流等离子体电源,放电电压3.0kV、频率60kHz时,经等离子体发生器产生的的低温等离子体的温度为15℃~4℃。When the pressure of the working gas input into the vortex tube is 0.5MPa and the flow rate is 18-25mL/min, the vortex tube cools the working gas to 7°C-1°C, using low-frequency sinusoidal AC plasma power supply, discharge voltage 3.0kV, frequency 60kHz , the temperature of the low-temperature plasma generated by the plasma generator is 15°C to 4°C.

当输入涡流管的工作气体压力为0.7MPa,气体流量为18~30mL/min时,气体冷却器将工作气体冷却至-10℃~-20℃,采用低频正弦交流等离子体电源,放电电压3.5kV、频率70kHz时,经等离子体发生器产生的的低温等离子体的温度为5℃~-4℃。When the pressure of the working gas input into the vortex tube is 0.7MPa, and the gas flow rate is 18-30mL/min, the gas cooler will cool the working gas to -10℃~-20℃, using a low-frequency sinusoidal AC plasma power supply, and the discharge voltage is 3.5kV 1. When the frequency is 70kHz, the temperature of the low-temperature plasma generated by the plasma generator is 5℃~-4℃.

本发明的有益之处在于:采用无源的涡流管实时冷却工作气体,经等离子体发生器放电后可获得低温甚至低于室温的温度可控的等离子体,并且等离子体温度的控制仅需调整输入涡流管的工作气体的流量和压力。The benefit of the present invention lies in that the working gas is cooled in real time by using a passive vortex tube, and a temperature-controllable plasma at a low temperature or even lower than room temperature can be obtained after being discharged by the plasma generator, and the control of the plasma temperature only needs to be adjusted The flow and pressure of the working gas entering the vortex tube.

附图说明Description of drawings

附图是本发明温度可控的低温等离子体产生方法原理图。The accompanying drawing is a schematic diagram of the temperature-controllable low-temperature plasma generation method of the present invention.

图中:1供气装置;2输气管道;3气体控制装置;4涡流管;5等离子体发生器;6高压电源;7温度监测装置;8低温等离子体。In the figure: 1 gas supply device; 2 gas pipeline; 3 gas control device; 4 vortex tube; 5 plasma generator; 6 high voltage power supply; 7 temperature monitoring device; 8 low temperature plasma.

具体实施方式detailed description

下面结合附图和具体实施方式对本发明作进一步的详细说明。The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.

本发明提供了一种温度可控的低温等离子体产生方法,使用此方法的设备包括供气装置1、输气管道2、气体控制装置3、涡流管4、等离子体发生器5、高压电源6和温度监测装置7。The invention provides a temperature-controllable low-temperature plasma generation method, the equipment using this method includes a gas supply device 1, a gas transmission pipeline 2, a gas control device 3, a vortex tube 4, a plasma generator 5, and a high-voltage power supply 6 And temperature monitoring device 7.

由供气装置1提供具有一定压力的工作气体,经输气管道2输送至气体控制装置3,调节工作气体的流量和压力后输送至涡流管4。经涡流管4冷却后的工作气体输送至等离子体发生器5中,在高压电源6的激励下等离子体发生器5的前端即可产生低温等离子体8。温度监测装置7可检测并显示输入等离子体发生器的工作气体的温度和低温等离子体的温度。The working gas with a certain pressure is provided by the gas supply device 1, and is delivered to the gas control device 3 through the gas transmission pipeline 2, and then delivered to the vortex tube 4 after adjusting the flow and pressure of the working gas. The working gas cooled by the vortex tube 4 is sent to the plasma generator 5 , and the front end of the plasma generator 5 can generate low-temperature plasma 8 under the excitation of the high-voltage power supply 6 . The temperature monitoring device 7 can detect and display the temperature of the working gas input into the plasma generator and the temperature of the low-temperature plasma.

实施例1Example 1

在室温22℃时,由气瓶供应纯度为99.999%的高纯氮气,气体压力为0.5MPa。经气体控制装置调节流量为18mL/min后输送至涡流管,采用热电偶数字测温仪测得冷却后的气体温度为7℃。冷却后的工作气体输送至等离子体发生器。等离子体发生器由正弦交流低频高压电源供电,频率60kHz,电压3.0kV。此时等离子体发生器产生的低温等离子体的宏观温度为约15℃。将输入涡流管的工作气体流量增大至25mL/min时,涡流管可将气体冷却至1℃,产生的低温等离子体宏观温度为4℃。At a room temperature of 22°C, high-purity nitrogen gas with a purity of 99.999% is supplied from a cylinder, and the gas pressure is 0.5 MPa. After the gas control device adjusted the flow rate to 18mL/min, it was sent to the vortex tube, and the temperature of the cooled gas was measured at 7°C by using a thermocouple digital thermometer. The cooled working gas is delivered to the plasma generator. The plasma generator is powered by a sinusoidal AC low-frequency high-voltage power supply with a frequency of 60kHz and a voltage of 3.0kV. At this time, the macroscopic temperature of the low-temperature plasma generated by the plasma generator is about 15°C. When the flow rate of the working gas input into the vortex tube is increased to 25mL/min, the vortex tube can cool the gas to 1°C, and the macroscopic temperature of the generated low-temperature plasma is 4°C.

实施例2Example 2

在室温22℃时,采用空气压缩机供气,将产生的压缩空气干燥和过滤后输送至气体控制装置。气体控制装置控制输入涡流管的气体压力为0.7MPa,流量为18mL/min时,涡流管可将空气冷却至-10℃。等离子体发生器由正弦交流低频高压电源供电,频率70kHz,电压3.5kV时,可产生宏观温度为5℃的低温等离子体。输入涡流管的工作气体流量增加至30mL/min时,涡流管可将工作气体冷却至-20℃,可产生宏观温度为-4℃的低温等离子体。At a room temperature of 22°C, an air compressor is used to supply air, and the generated compressed air is dried and filtered and sent to the gas control device. The gas control device controls the gas pressure input into the vortex tube to be 0.7MPa, and when the flow rate is 18mL/min, the vortex tube can cool the air to -10°C. The plasma generator is powered by a sinusoidal AC low-frequency high-voltage power supply with a frequency of 70kHz and a voltage of 3.5kV, which can generate low-temperature plasma with a macroscopic temperature of 5°C. When the flow rate of the working gas input into the vortex tube is increased to 30mL/min, the vortex tube can cool the working gas to -20°C and generate a low-temperature plasma with a macroscopic temperature of -4°C.

Claims (10)

1.一种温度可控的低温等离子体产生方法,其特征在于,该方法所用的装置包括供气装置、气体控制装置、涡流管、高压电源、等离子体发生器和温度监测装置;供气装置提供具有一定压力的工作气体,工作气体通向气体控制装置,按照一定的流量和压力输向涡流管;工作气体经涡流管冷却后,进入等离子体发生器;高压电源控制等离子体发生器的放电过程,并产生低温等离子体;温度监测装置用于监测冷却后的工作气体温度和产生的低温等离子体的温度;通过调整输入涡流管的工作气体压力、流量和涡流管参数,控制输入等离子体发生器的工作气体温度,控制由等离子体发生器产生的低温等离子体的温度;通过电源电压、频率、气体压力和流量的配合调整,实现低温等离子体温度从200℃~-4℃范围内可控。1. A temperature-controllable low-temperature plasma generation method is characterized in that the device used in the method comprises a gas supply device, a gas control device, a vortex tube, a high-voltage power supply, a plasma generator and a temperature monitoring device; a gas supply device Provide working gas with a certain pressure, the working gas leads to the gas control device, and is transported to the vortex tube according to a certain flow rate and pressure; the working gas enters the plasma generator after being cooled by the vortex tube; the high-voltage power supply controls the discharge of the plasma generator process, and generate low-temperature plasma; the temperature monitoring device is used to monitor the temperature of the cooled working gas and the temperature of the generated low-temperature plasma; by adjusting the working gas pressure, flow rate and vortex tube parameters input to the vortex tube, the input plasma is controlled The working gas temperature of the plasma generator is used to control the temperature of the low-temperature plasma generated by the plasma generator; through the adjustment of the power supply voltage, frequency, gas pressure and flow rate, the temperature of the low-temperature plasma can be controlled from 200°C to -4°C . 2.根据权利要求1所述的低温等离子体产生方法,其特征在于,供气装置提供的工作气体为氮气、氩气、氦气、氯气、氧气、经过滤干燥的空气中的一种或两种以上混合。2. The low-temperature plasma generation method according to claim 1, wherein the working gas provided by the gas supply device is one or both of nitrogen, argon, helium, chlorine, oxygen, and filtered and dried air. A mixture of the above. 3.根据权利要求1或2所述的低温等离子体产生方法,其特征在于,所述的等离子体发生器放电形式是裸电极放电、介质阻挡放电或空心阴极放电。3. The low-temperature plasma generation method according to claim 1 or 2, characterized in that, the discharge form of the plasma generator is bare electrode discharge, dielectric barrier discharge or hollow cathode discharge. 4.根据权利要求1或2所述的低温等离子体产生方法,其特征在于,所述的高压电源是直流高压电源、低频高压电源、射频高压电源、微波高压电源或脉冲高压电源。4. The low-temperature plasma generation method according to claim 1 or 2, characterized in that the high-voltage power supply is a DC high-voltage power supply, a low-frequency high-voltage power supply, a radio frequency high-voltage power supply, a microwave high-voltage power supply or a pulsed high-voltage power supply. 5.根据权利要求3所述的低温等离子体产生方法,其特征在于,所述的高压电源是直流高压电源、低频高压电源、射频高压电源、微波高压电源或脉冲高压电源。5. The low-temperature plasma generation method according to claim 3, wherein the high-voltage power supply is a DC high-voltage power supply, a low-frequency high-voltage power supply, a radio frequency high-voltage power supply, a microwave high-voltage power supply or a pulsed high-voltage power supply. 6.根据权利要求1、2或5所述的低温等离子体产生方法,其特征在于,当输入涡流管的工作气体压力为0.5MPa,流量为18~25mL/min时,涡流管将工作气体冷却至7℃~1℃,采用低频正弦交流等离子体电源,放电电压3.0kV、频率60kHz时,经等离子体发生器产生的的低温等离子体的温度为15℃~4℃。6. The low-temperature plasma generation method according to claim 1, 2 or 5, characterized in that, when the pressure of the working gas input into the vortex tube is 0.5 MPa and the flow rate is 18-25 mL/min, the vortex tube cools the working gas To 7 ℃ ~ 1 ℃, using low-frequency sinusoidal AC plasma power supply, discharge voltage 3.0kV, frequency 60kHz, the temperature of the low-temperature plasma generated by the plasma generator is 15 ℃ ~ 4 ℃. 7.根据权利要求3所述的低温等离子体产生方法,其特征在于,当输入涡流管的工作气体压力为0.5MPa,流量为18~25mL/min时,涡流管将工作气体冷却至7℃~1℃,采用低频正弦交流等离子体电源,放电电压3.0kV、频率60kHz时,经等离子体发生器产生的的低温等离子体的温度为15℃~4℃。7. The low-temperature plasma generation method according to claim 3, characterized in that, when the pressure of the working gas input into the vortex tube is 0.5 MPa, and the flow rate is 18-25 mL/min, the vortex tube cools the working gas to 7° C. 1°C, using a low-frequency sinusoidal AC plasma power supply, when the discharge voltage is 3.0kV and the frequency is 60kHz, the temperature of the low-temperature plasma generated by the plasma generator is 15°C to 4°C. 8.根据权利要求4所述的低温等离子体产生方法,其特征在于,当输入涡流管的工作气体压力为0.5MPa,流量为18~25mL/min时,涡流管将工作气体冷却至7℃~1℃,采用低频正弦交流等离子体电源,放电电压3.0kV、频率60kHz时,经等离子体发生器产生的的低温等离子体的温度为15℃~4℃。8. The low-temperature plasma generation method according to claim 4, characterized in that, when the pressure of the working gas input into the vortex tube is 0.5 MPa, and the flow rate is 18-25 mL/min, the vortex tube cools the working gas to 7° C. 1°C, using a low-frequency sinusoidal AC plasma power supply, when the discharge voltage is 3.0kV and the frequency is 60kHz, the temperature of the low-temperature plasma generated by the plasma generator is 15°C to 4°C. 9.根据权利要求1、2、5、7或8所述的低温等离子体产生方法,其特征在于,当输入涡流管的工作气体压力为0.7MPa,气体流量为18~30mL/min时,气体冷却器将工作气体冷却至-10℃~-20℃,采用低频正弦交流等离子体电源,放电电压3.5kV、频率70kHz时,经等离子体发生器产生的的低温等离子体的温度为5℃~-4℃。9. The low-temperature plasma generation method according to claim 1, 2, 5, 7 or 8, characterized in that, when the working gas pressure input into the vortex tube is 0.7MPa, and the gas flow rate is 18-30mL/min, the gas The cooler cools the working gas to -10℃~-20℃, adopts low-frequency sinusoidal AC plasma power supply, when the discharge voltage is 3.5kV and the frequency is 70kHz, the temperature of the low-temperature plasma generated by the plasma generator is 5℃~- 4°C. 10.根据权利要求6所述的低温等离子体产生方法,其特征在于,当输入涡流管的工作气体压力为0.7MPa,气体流量为18~30mL/min时,气体冷却器将工作气体冷却至-10℃~-20℃,采用低频正弦交流等离子体电源,放电电压3.5kV、频率70kHz时,经等离子体发生器产生的的低温等离子体的温度为5℃~-4℃。10. The low-temperature plasma generation method according to claim 6, characterized in that, when the pressure of the working gas input into the vortex tube is 0.7 MPa and the gas flow rate is 18-30 mL/min, the gas cooler cools the working gas to - 10 ℃ ~ -20 ℃, low frequency sinusoidal AC plasma power supply, discharge voltage 3.5kV, frequency 70kHz, the temperature of the low temperature plasma generated by the plasma generator is 5 ℃ ~ -4 ℃.
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