CN105025649A - Device and method for generating inductive coupling hot plasma under low air pressure - Google Patents
Device and method for generating inductive coupling hot plasma under low air pressure Download PDFInfo
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- CN105025649A CN105025649A CN201510385291.5A CN201510385291A CN105025649A CN 105025649 A CN105025649 A CN 105025649A CN 201510385291 A CN201510385291 A CN 201510385291A CN 105025649 A CN105025649 A CN 105025649A
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Abstract
The invention provides a device and method for generating inductive coupling hot plasma under a low air pressure, and belongs to the technical field of low-temperature plasma generation. A radio-frequency power supply serves as an excitation source under the low air pressure, and argon gas serves as plasma generation gas. The breakdown of the argon gas is achieved in a double-layer ceramic tube. The argon gas after breakdown absorbs electromagnetic field energy coupled thereto to generate the hot plasma, and ejects the hot plasma along a spraying mouth of the inner ceramic tube, thereby forming an inductive coupling hot plasma flow. The hot plasma generated through the invention can effectively prevent particles from being oxidized and nitrided in a process of hot plasma processing, thereby providing technical basis for the processing of materials in a sealed cavity.
Description
Technical field
The present invention relates to a kind of generation device and production method of hot plasma; more specifically; the present invention relates at low pressure; argon gas is adopted to be that plasma generates gas; argon gas/nitrogen/oxygen is as protection gas; adopt radio-frequency power supply as drive source, produce and maintain the apparatus and method of inductively hot plasma.
Background technology
Inductively hot plasma prepares nano particle and the desirable thermal source of micron spherical powder and chemical reaction source.It has and can keep high temperature (3000 K-10000 K) on the one hand; It contains high energy electron, ion, excited atom, free radical isoreactivity particle on the other hand; In addition, be different from arc heat plasma, it by electrode fouling, is not very clean hot plasma.
Inductively hot plasma normally under atmospheric pressure produces.Generation device is adopt the quartz ampoule of individual layer or bilayer as the confinement tube of confined plasma, and pipe is outer places the coaxial inductive coil that passes to radio-frequency stage electric current, and induction coil is connected with radio-frequency power supply.The generation of plasma can be described below, and argon gas is passed into confinement tube, and starts power supply and apply electric current to induction coil, at this moment, is placed in by tesla's spark generator in pipe or is affixed on tube wall face, adding high pressure simultaneously on coil.The seed electrons that sparkover produces is subject to the acceleration of electric field, collide with gas molecule, the energy of electromagnetic field that these molecule simultaneously stability induction coils obtaining energy produce, continue accelerate and collide with the molecule of surrounding, this process occurs at short notice rapidly, finally all gas is ionized, thus produce plasma.The design of this plasma device and producing method can only under atmospheric pressure be carried out.
The inductively hot plasma produced under atmospheric pressure is in synthesis new material or nodularization metal dust process; particle inevitably reacts with remaining oxygen, nitrogen in chamber; namely can there is oxidation or nitrogenize phenomenon in particle, and this is disadvantageous to the new material of synthesis high-quality.
Summary of the invention
The present invention is in order to overcome above-mentioned the deficiencies in the prior art, avoid the generation of oxidation and nitrogenize phenomenon, improve quality and the performance of synthesized material, the invention provides a kind of apparatus and method producing inductively hot plasma at low pressure, at low pressure, under low nitrogen oxygen content environment, stable inductively hot plasma can be produced.
The device producing inductively hot plasma under a kind of low pressure of the present invention realizes by the following technical solutions: the device producing inductively hot plasma under a kind of low pressure, comprises plasma producing apparatus and upper end open and sidewall is provided with the stainless steel chamber of observation window; Described plasma producing apparatus comprises one and is vertically arranged on the double-layer ceramic pipe of stainless steel chamber upper port and is looped around the induction coil of double-layer ceramic pipe outer wall, and the two ends of induction coil are connected with radio-frequency power supply; The upper port sealing of double-layer ceramic pipe is provided with end cap, and end cap is provided with the circulating cooling water inlet be connected with interlayer inside and outside double-layer ceramic pipe; A quartz ampoule be positioned among internal layer earthenware is fixed with below end cap; End cap is provided with the plasma be connected with quartz ampoule and generates gas entrance; End cap is also provided with the protection gas entrance communicated with the interlayer between internal layer earthenware and quartz ampoule; Inside and outside double-layer ceramic pipe, interlayer is in the sealing of lower port place, and internal layer earthenware lower port is then sealedly connected in the upper port of stainless steel chamber, and stainless steel chamber side is connected with vacuum-pumping equipment.
The present invention adopts double-layer ceramic pipe as producing and the agent set of confined plasma, and its benefit can effectively increase thermal endurance and resistance to impact.According to Paschen's law, the puncture voltage Vs of gas is the function of air pressure p and electrode spacing d.D is certain, and Vs is only relevant with air pressure, and namely minimum break-down voltage depends on suitable air pressure.Accordingly, under stainless steel chamber is in certain air pressure, passes into inert gas argon gas by plasma generation gas entrance and generate gas as plasma, utilize the high pressure being applied to induction coil to be punctured by argon gas, the argon gas of conduction absorbs energy of electromagnetic field makes region of discharge expand, and forms plasma.Under the effect of air-flow, plasma is injected into stainless steel chamber along the lower port (namely retraining the mouth of pipe) of internal layer earthenware.
At once add protection gas by protection gas entrance after lighting plasma, between plasma and internal layer earthenware, form one deck air film in order to protect internal layer earthenware from thermal shock.Now, plasma does not reach stable state.Adding increases power supply power output while appropriate plasma generates gas argon gas guarantees that plasma operates in stable state.Finally adjustment vacuum-pumping equipment reaches the stainless steel chamber pressure needed for application.
The method producing inductively hot plasma under a kind of low pressure of the present invention adopts following technical scheme to realize: a kind of method producing inductively hot plasma under low pressure, comprises the following steps: first utilize vacuum-pumping equipment that the air pressure in stainless steel chamber is maintained 32-40 kPa; Secondly pass into argon gas by gas ions generation gas entrance and generate gas as plasma, throughput is 2.0 m
3/ h; Raise the anode voltage of radio-frequency power supply gradually, when anode voltage reaches 6-7 kV, anode current suddenlys change, and represents when being greater than 5A and light plasma; By protecting gas entrance to add protection gas while increasing the power output of power supply, described protection gas is the wherein one in argon gas, nitrogen, oxygen; Plasma is regulated to generate throughput and stainless steel chamber pressure, to maintain stable plasma.Here adjustment is realized by the stability of the plasma in observation window stainless steel chamber.
Compared with prior art, the invention has the beneficial effects as follows the drawback overcoming and can only light inductively hot plasma at atmospheric pressure, achieve and produce inductively hot plasma in low pressure confined space, effectively avoid the oxidation of particle in hot plasma processing procedure and nitrogenize phenomenon, for the material processed of hot plasma in airtight chamber provides technical foundation.Another advantage of the present invention is that generation plasma flow process is simple and easy, and the plasma of generation is very stable, and is controlled.
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram producing inductively hot plasma under low pressure of the present invention.
101 is radio-frequency power supplies, adopts electron tube radio-frequency power supply.
102 is induction coils, passes into radio-frequency current wherein, in order to excite fast-changing electromagnetic field.
103 is protection gas entrances, in order to pass into protection gas (argon gas/nitrogen/oxygen).
104 is that plasma generates gas entrance.
105 is circulating cooling water inlets, in order to cool ceramic confinement tube.
106 is quartz ampoules, generates gas in order to pass into plasma, and insulation blocking gas.
107 is double-layer ceramic pipes, and it is the agent set of confined plasma.
108 is stainless steel chambers.
109 is vacuum-pumping equipments.
110 is inductively hot plasmas.
Fig. 2 is that inductively hot plasma produces and maintains flow chart.
Embodiment
Produce a device for inductively hot plasma under low pressure, comprise plasma producing apparatus and upper end open and sidewall is provided with the stainless steel chamber 108 of observation window; Described plasma producing apparatus comprises one and is vertically arranged on the double-layer ceramic pipe 107 of stainless steel chamber 108 upper port and is looped around the induction coil 102 of double-layer ceramic pipe 107 outer wall, and the two ends of induction coil 102 are connected with radio-frequency power supply 101; The upper port sealing of double-layer ceramic pipe 107 is provided with end cap, and end cap is provided with the circulating cooling water inlet 105 be connected with interlayer inside and outside double-layer ceramic pipe 107; A quartz ampoule 106 be positioned among internal layer earthenware is fixed with below end cap; End cap is provided with the plasma be connected with quartz ampoule 106 and generates gas entrance 104; End cap is also provided with the protection gas entrance 103 communicated with the interlayer between internal layer earthenware and quartz ampoule 106; Inside and outside double-layer ceramic pipe 107, interlayer is in the sealing of lower port place, and internal layer earthenware lower port is then sealedly connected in the upper port of stainless steel chamber 108, and stainless steel chamber 108 side is connected with vacuum-pumping equipment 109.Double-layer ceramic pipe 107 is provided with the recirculated cooling water entrance and exit be connected with inside and outside interlayer simultaneously, and being connected with external refrigeration water feeder forms loop, realizes cooling.
Double-layer ceramic pipe 107 material is SiN, and wherein internal layer earthenware thickness is respectively 3mm, and outer earthenware thickness is 2mm, and length is 300mm; Curb pins layer thickness is 1mm, and internal layer earthenware internal diameter is 60mm.
Induction coil 102 is 8 mm by an internal diameter, and external diameter is that the copper tube coiling of 10mm forms; Induction coil is totally 4 circles, and turn-to-turn is apart from being 10 mm, and the internal diameter of every circle coil is 74 mm; Pass into the deionized water of circulation in induction coil 102, induction coil 102 outer wall is connected with radio-frequency power supply 101.Pass into circulation deionized water in induction coil 102, can ensure that induction coil is not burned under the effect of electric current.
Quartz ampoule 106 generates gas for passing into plasma, and its internal diameter is 30mm, and external diameter is 34mm, and length is 40mm.
Radio-frequency power supply 101 is a kind of electron tube power sources, and hunting power is 100 kW, and operating frequency is 3.0 ± 0.5MHz.
Stainless steel chamber 108 is Double water-cooled structures, and upper end seals with plasma producing apparatus and is connected, and lower end seals, and side is connected with vacuum-pumping equipment 109.
Adopt bipolar water ring pump, model be 2S-230 as vacuum-pumping equipment 109, its ultimate vacuum is 3.5kPa.
Produce a method for inductively hot plasma under low pressure, comprise the following steps: first utilize vacuum-pumping equipment 109 that the air pressure in stainless steel chamber 108 is maintained 32-40 kPa; Secondly pass into argon gas by gas ions generation gas entrance 104 and generate gas as plasma, throughput is 2.0 m
3/ h; Raise the anode voltage of radio-frequency power supply 101 gradually, when anode voltage reaches 6-7 kV, anode current suddenlys change, and represents when being greater than 5A and light plasma; By protecting gas entrance 103 to add protection gas while increasing the power output of power supply, described protection gas is the wherein one in argon gas, nitrogen, oxygen; Plasma is regulated to generate throughput and stainless steel chamber pressure, to maintain stable plasma.
Embodiment: the production method of argon gas inductively hot plasma under a kind of low pressure.Comprise following flow process:
(1) plasma generating device is installed by correct shown in Fig. 1 and check sealing;
(2) open vacuum-pumping equipment, make the air pressure of stainless steel chamber maintain 32-40 kPa;
(3) pass into plasma and generate gas argon gas, purity is 999.9%, and throughput is 2.0 m
3/ h;
(4) open rf power system, raise anode voltage gradually, when anode voltage is 6-7 kV, anode current suddenlys change to when being greater than 5 A can light plasma;
(5) add protection gas argon gas, add high-power, adjustable pressure and positive flow index is remained unchanged, plasma now can be made to reach stable state;
Described in step (5), after lighting plasma, increase input power to maintain stable plasma, now power anode voltage can be elevated to 7 kV, and anode current is about 6 A;
Described in step (5), after lighting plasma, while increasing input power, increase plasma and generate gas argon gas to 3.0m
3/ h, increases protection gas argon gas 6.0m
3/ h;
Described in step (5), after lighting plasma, chamber pressure is maintained 60 kPa.
Claims (8)
1. produce a device for inductively hot plasma under low pressure, it is characterized in that: comprise plasma producing apparatus and upper end open and sidewall is provided with the stainless steel chamber (108) of observation window; Described plasma producing apparatus comprises one and is vertically arranged on the double-layer ceramic pipe (107) of stainless steel chamber (108) upper port and is looped around the induction coil (102) of double-layer ceramic pipe (107) outer wall, and the two ends of induction coil (102) are connected with radio-frequency power supply (101); The upper port sealing of double-layer ceramic pipe (107) is provided with end cap, and end cap is provided with the circulating cooling water inlet (105) be connected with the inside and outside interlayer of double-layer ceramic pipe (107); A quartz ampoule (106) be positioned among internal layer earthenware is fixed with below end cap; End cap is provided with the plasma be connected with quartz ampoule (106) and generates gas entrance (104); End cap is also provided with the protection gas entrance (103) communicated with the interlayer between internal layer earthenware and quartz ampoule (106); The inside and outside interlayer of double-layer ceramic pipe (107) is in the sealing of lower port place, and internal layer earthenware lower port is then sealedly connected in the upper port of stainless steel chamber (108), and stainless steel chamber (108) side is connected with vacuum-pumping equipment (109).
2. under a kind of low pressure according to claim 1, produce the device of inductively hot plasma, it is characterized in that: double-layer ceramic pipe (107) material is SiN, wherein internal layer earthenware thickness is 3mm, and outer earthenware thickness is 2mm, and length is 300mm; Curb pins layer thickness is 1mm, and internal layer earthenware internal diameter is 60mm.
3. produce the device of inductively hot plasma under a kind of low pressure according to claim 1 and 2, it is characterized in that: induction coil (102) is 8mm by an internal diameter, external diameter is that the copper tube coiling of 10mm forms; Induction coil is totally 4 circles, and turn-to-turn is apart from being 10mm, and the internal diameter of every circle coil is 74mm; Pass into the deionized water of circulation in induction coil (102), induction coil (102) outer wall is connected with radio-frequency power supply (101).
4. produce the device of inductively hot plasma under a kind of low pressure according to claim 2, it is characterized in that: quartz ampoule (106) generates gas for passing into plasma, and its internal diameter is 30mm, and external diameter is 34mm, and length is 40mm.
5. produce the device of inductively hot plasma under a kind of low pressure according to claim 1 and 2, it is characterized in that: radio-frequency power supply (101) is a kind of electron tube power source, and hunting power is 100 kW, and operating frequency is 3.0 ± 0.5MHz.
6. under a kind of low pressure according to claim 1 and 2, produce the device of inductively hot plasma, it is characterized in that: stainless steel chamber (108) is Double water-cooled structure, and upper end seals with plasma producing apparatus and is connected, lower end seals, and side is connected with vacuum-pumping equipment (109).
7. produce the device of inductively hot plasma under a kind of low pressure according to claim 1 and 2, it is characterized in that: adopt bipolar water ring pump, model be 2S-230 as vacuum-pumping equipment (109), its ultimate vacuum is 3.5kPa.
8. under a low pressure, produce the method for inductively hot plasma, adopt device as claimed in claim 1, it is characterized in that: comprise the following steps: first utilize vacuum-pumping equipment (109) that the air pressure in stainless steel chamber (108) is maintained 32-40 kPa; Secondly pass into argon gas by gas ions generation gas entrance (104) and generate gas as plasma, throughput is 2.0 m
3/ h; Raise the anode voltage of radio-frequency power supply (101) gradually, when anode voltage reaches 6-7kV, anode current suddenlys change, and represents when being greater than 5A and light plasma; By protecting gas entrance (103) to add protection gas while increasing the power output of power supply, described protection gas is the wherein one in argon gas, nitrogen, oxygen; Plasma is regulated to generate throughput and stainless steel chamber (108) air pressure, to maintain stable plasma.
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| CN108601193A (en) * | 2018-03-21 | 2018-09-28 | 中国科学院合肥物质科学研究院 | A kind of long scale uniform heat plasma arcs production method and device |
| CN108684129A (en) * | 2018-08-02 | 2018-10-19 | 王诗君 | Cold-plasma jet system and method based on piezoelectric ceramic transformer |
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