CN108966474A - A kind of high-power combination frequency ICP plasma generator - Google Patents
A kind of high-power combination frequency ICP plasma generator Download PDFInfo
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- CN108966474A CN108966474A CN201811163946.4A CN201811163946A CN108966474A CN 108966474 A CN108966474 A CN 108966474A CN 201811163946 A CN201811163946 A CN 201811163946A CN 108966474 A CN108966474 A CN 108966474A
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/46—Generating plasma using applied electromagnetic fields, e.g. high frequency or microwave energy
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/46—Generating plasma using applied electromagnetic fields, e.g. high frequency or microwave energy
- H05H1/4645—Radiofrequency discharges
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- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Electromagnetism (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Plasma Technology (AREA)
Abstract
This application discloses a kind of high-power combination frequency ICP plasma generators, comprising: radio-frequency power supply, frequency 3-27.12MHz, power 1-10KW；Intermediate frequency power supply, frequency 50-1000KHz, power 10-200KW；Plasmatron, inside are formed with plasma and inner cavity occur；Spiral induction coil is coaxially wrapped in the plasma pipe outer wall, and upper end is the radio-frequency power supply incoming end, and lower end is the intermediate frequency power supply incoming end, and tap is the radio-frequency power supply, intermediate frequency power supply common ground end below the radio-frequency power supply incoming end；Gas distribution head is sealed at the top of the plasmatron.The advantage of the invention is that the cost of power supply is low, high reliablity can substantially reduce the manufacture or purchase cost of induction power supply.
Description
Technical field
This application involves plasma generator, in particular to a kind of high-power combination frequency ICP plasma generator.
Background technique
High-power ICP plasma application technology is widely used in nano material preparation, powder spray, intermetallic composite coating etc.
Many technical fields.
ICP plasma generator has begun from the sixties in last century for equipment set industry, structure
It is improved by the optimization of many years, it is very perfect.Its basic structure includes the induction coil of 4-6 circle, high-frequency alternating current
It can be sent into plasma；The plasma chamber of one tubulose uses quartz material, usually for limiting plasma
Range；Gas is sent into plasma chamber with a kind of specific mode by one gas distribution head, stable to guarantee to generate
Plasma, and the centre of plasma chamber is confined a plasma in, make plasma chamber tube wall discord plasma
It directly contacts, to protect plasma chamber not damage because contacting the high temperature of plasma.For power at five kilowatts or more
Device, it is also necessary to be cooled down in cavity external application coolant liquid, usually use bimetallic tube, it is cooling to lead to deionized water between tube wall.It is high
Frequency AC power source typically uses radio-frequency power supply, and frequency is at 3 megahertzs to tens megahertzs, and power is at several kilowatts to up to a hundred thousand
Watt differ.
The major defect of above-mentioned ICP plasma generator is must to use radio-frequency alternating current power supply, and frequency arrives several for 3 megahertzs
Ten megahertzs, in this frequency range, radio-frequency power supply is very sensitive to the variation of the impedance of load, once air-flow changes, draws
The internal resistance variation for playing plasma, is easy for causing plasma extinguishment；To solve this problem, it to be usually equipped with and radio frequency electrical
The comparable radio frequency adaptation of source power, to be automatically adjusted internal resistance matching when plasma internal resistance changes.In addition
One the disadvantage is that radio-frequency power supply generally uses solid state RF transistor as power amplifying device, by semiconductor devices manufacture work
The limitation of skill, the power of RF transistors can only accomplish 150 watts or so, therefore powerful radio-frequency power supply is needed with tens even
Up to a hundred such transistors, cause the Reliability comparotive of radio-frequency power supply poor, also, the medium frequency induction power supply with equal-wattage
(frequency is tens to several hundred kilohertzs) is compared, and the purchase cost of radio-frequency power supply wants 8-10 times high.And the radio frequency of equal-wattage
The purchase cost of distribution network also has 1/4 or so of the price of the radio-frequency power supply of same power.
Summary of the invention
It is an object of the invention to be 10-200KW with power, frequency be tens to several hundred kHz Medium frequency induction electricity
Source replaces power to be 10-200KW, the radio-frequency power supply that frequency is 3 to tens megahertzs, occurs for high-power ICP plasma
Device.Medium frequency induction power supply uses high-power IGBT module, the output power of each module up to ten thousands of to one, 200 kilowatt,
The cost of power supply is low, high reliablity, can substantially reduce the manufacture or purchase cost of induction power supply.
To achieve the above object, the present invention provides the following technical solutions.
The embodiment of the present application discloses a kind of high-power combination frequency ICP plasma generator, comprising:
Radio-frequency power supply, frequency 3-27.12MHz, power 1-10KW；
Intermediate frequency power supply, frequency 50-1000KHz, power 10-200KW；
Plasmatron, inside are formed with plasma and inner cavity occur；
Spiral induction coil, is coaxially wrapped in the plasma pipe outer wall, and upper end is the radio-frequency power supply incoming end, lower end
For the intermediate frequency power supply incoming end, the radio-frequency power supply incoming end lower section tap, which is the radio-frequency power supply, intermediate frequency power supply is public is connect
Ground terminal；
Gas distribution head is sealed at the top of the plasmatron.
It preferably, further include high-tension ignition electrode in above-mentioned high-power combination frequency ICP plasma generator, from
The gas distribution head is introduced to the plasma and inner cavity occurs.
Preferably, in above-mentioned high-power combination frequency ICP plasma generator, the spiral induction coil is 8-20mm
Diameter copper pipes are rolled into tubulose by ceramic material or insulation fibre material, and the spiral induction coil circle number is that 6-7 is enclosed, and adjacent two
Circle spacing is 5-10mm, and the common ground end position is that 1-2 is enclosed at tap below the radio-frequency power supply incoming end.
Preferably, in above-mentioned high-power combination frequency ICP plasma generator, the spiral induction coil and described etc.
It is coaxially arranged with cooling tube between gas ions pipe, flows and is provided between the cooling inside pipe wall and the plasma pipe outer wall
Coolant liquid.
Preferably, close at the gas distribution head axle center in above-mentioned high-power combination frequency ICP plasma generator
Envelope, which is provided with, is connected to the center tracheae that inner cavity occurs for the plasma.
Preferably, in above-mentioned high-power combination frequency ICP plasma generator, the gas distribution head offers company
Lead to the rotary pneumatic air inlet pipe that inner cavity occurs for the plasma, the rotary pneumatic air inlet pipe is connected in the plasma generation
The entrance of chamber is located at the plasma and inner cavity top side occurs, the gas distribution head is coaxially connected be provided with rotation conductance to
Pipe, the rotation gas guide pipe are located at the plasma and inner cavity top occur.
It is furthermore preferred that in above-mentioned high-power combination frequency ICP plasma generator, the gas distribution head with it is described
Sealed set has water-output flange between cooling tube, and water outlet is provided at the top of the water-output flange, and the coolant liquid goes out described in
Mouth of a river outflow, the water-output flange bottom is provided with sealing flange.
It is furthermore preferred that the plasma bottom of the tube is same in above-mentioned high-power combination frequency ICP plasma generator
Sealing is provided with and communicated with inlet flange, and the inlet flange side offers the inlet chamber for being connected to its inner cavity.
It is furthermore preferred that in above-mentioned high-power combination frequency ICP plasma generator, the inlet flange with it is described cold
But co-axial seal is provided with water ring flange between pipe, and the water ring flange inner wall is formed with the ring being connected to inside the cooling tube
Chamber, inlet flange bottom co-axial seal are provided with water-in flange, and the water-in flange side offers water inlet, it is described into
Water law is blue, inlet flange successively offers the feed pathway for being connected to the ring cavity, and the coolant liquid flows into institute from the water inlet
The ring cavity is flowed into after stating feed pathway, then is flowed into inside the cooling tube.
Preferably, in above-mentioned high-power combination frequency ICP plasma generator, the radio-frequency power supply passes through coaxial electrical
Cable is connected to radio frequency matching network, and the radio frequency matching network passes through coaxial cable again and radio-frequency power is connected to the radio-frequency power supply
Incoming end, the intermediate frequency power supply are connected to the intermediate frequency power supply incoming end by water-cooled cable.
After gas enters plasma generation inner cavity, ionization, the ion of generation are generated under 10KV electrion of short duration
Under the excitation of radio-frequency power, stable initial plasma is formed；This plasma is in powerful intermediate frequency alternating electromagnetism
Under the excitation of field, the high-temperature plasma that power is dozens or even hundreds of kilowatt is generated.The cost of power supply is low, and high reliablity can
To substantially reduce the manufacture or purchase cost of induction power supply.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The some embodiments recorded in application, for those of ordinary skill in the art, without creative efforts,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 is shown in the specific embodiment of the invention with the signal of liquid or the equipment of gaseous precursor production nano material
Figure；
Fig. 2 show the structural schematic diagram of specific embodiment of the invention plasma pipe；
Fig. 3 show the structural schematic diagram of high-power combination frequency ICP plasma generator in the specific embodiment of the invention；
Fig. 4 is shown in the specific embodiment of the invention with the ICP plasma of liquid or gaseous precursor production nano material
The structural schematic diagram of gas-phase reactor；
Fig. 5 is shown in the specific embodiment of the invention with the ICP plasma of liquid or gaseous precursor production nano material
The structural schematic diagram of gas phase cooler；
Fig. 6 show the structural schematic diagram of bubbler in the specific embodiment of the invention；
Fig. 7 show the top view of air inlet ring in the specific embodiment of the invention；
Fig. 8 show the top view of heat exchanger in the specific embodiment of the invention；
Fig. 9 show in the specific embodiment of the invention the axial distribution map of gas temperature in reaction chamber.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out detailed retouch
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, those of ordinary skill in the art's every other implementation obtained without making creative work
Example, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation,
It is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
It as shown in connection with fig. 1, successively include that co-axial seal connects with liquid or the equipment of gaseous precursor production nano material
Plasma generator 100, reaction chamber 200, cooling chamber 300.
In conjunction with shown in Fig. 1-3, high-power combination frequency ICP plasma generator 100 includes:
Radio-frequency power supply 110, frequency 3-27.12MHz, power 1-10KW；
Intermediate frequency power supply 120, frequency 50-1000KHz, power 10-200KW；
Plasmatron 130, inside are formed with plasma and inner cavity 131 occur；
Spiral induction coil 140 is coaxially wrapped in 130 outer wall of plasmatron, and upper end is radio-frequency power supply incoming end 141, under
End is intermediate frequency power supply incoming end 142, and 141 lower section tap of radio-frequency power supply incoming end is radio-frequency power supply, intermediate frequency power supply common ground end
143；
Gas distribution head 150 is sealed at 130 top of plasmatron.With quartz, ceramics or other insulating materials systems
At for gas needed for inner cavity provides plasma occurs to plasma.
By taking 30KW combination frequency induction power supply ICP plasma generator as an example, radio-frequency power supply power source selects 2500W,
12.56 megahertzs of water cooling radio-frequency power supply；Radio frequency matching network selects 3000W π type water cooling matching network, intermediate frequency power supply power source
15KW is selected, the water cooling intermediate frequency power supply of 50 kHz, other power and the power supply of frequency also may be implemented in certain Application Range,
Scope of the present application all should belong to.
Plasma generator is connected and fixed by connecting rod and upper connecting plate, screw etc., forms an entirety.
Further, further include high-tension ignition electrode (figure does not regard), be introduced to plasma from gas distribution head 150
Inner cavity 131.
High-tension ignition electrode high voltage power supply 500 selects 10KV, 20 milliamperes of ac high-voltage transformers.
Further, 130 material of plasmatron be one of silicon nitride, boron nitride, aluminium nitride ceramics or a variety of, etc.
130 internal diameter of gas ions pipe is 30 to 160 millimeters, 200-400 millimeters high, 3-5 millimeters of wall thickness.
In the technical solution, the material mixed in various proportions, is subject to various additives and packing material is made, and has height
Thermal conductivity, high resistivity, low thermal expansion, the characteristic of heat shock resistance.Plasma generates in plasmatron.
Further, spiral induction coil 140 is that 8-20mm diameter copper pipes are wrapped by ceramic material or insulation fibre material 144
Tubulose is wrapped up in into, spiral induction coil 140 encloses number as 6-7 circle, and space between the adjacent coils 5-10mm, 143 position of common ground end is to penetrate
141 lower section 1-2 of frequency power incoming end is enclosed at tap.
Spiral incudes snare on cooling tube, close to gas distribution head, away from 10-100 millimeters of gas distribution head.
Further, cooling tube 160, cooling tube are coaxially arranged between spiral induction coil 140 and plasmatron 130
Flowing is provided with coolant liquid between 130 outer wall of 160 inner walls and plasmatron.
Cooling effective quartz or ceramic material are made, 50 to 200 millimeters of internal diameter, 250-450 millimeters long, and 3-5 millimeters of wall thickness.
Further, the central gas that sealed set has connection plasma that inner cavity 131 occurs at 150 axle center of gas distribution head
Pipe 151.The mixed gas of pure argon or pure argon and nitrogen, hydrogen is passed through in center tracheae 151.
In the technical solution, the effective quartz of central gas, ceramics or other insulating materials are made, and 8 to 16 millimeters of internal diameter, wall thickness
It is 1 to 2 millimeters, 150 to 200 millimeters long, for injecting one or more process gas.
Further, gas distribution head 150 offers one or more rotary pneumatics that inner cavity 131 occurs for connection plasma
Air inlet pipe 152, the entrance that rotary pneumatic air inlet pipe 152 is connected to plasma generation inner cavity 131 are located at plasma and inner cavity occur
131 top-sides, gas distribution head 150 is coaxially connected to be provided with rotation gas guide pipe 153, and rotation gas guide pipe 153 is located at plasma
131 top of inner cavity occurs for body.Pure argon is passed through in rotary pneumatic air inlet pipe 152.
Rotary pneumatic air inlet pipe and cavity are tangent, for argon gas or other gases needed for injecting plasma, rotation conductance to
Effective quartz, ceramics or other insulating materials are made, 35 to 140 millimeters of internal diameter, 50 to 100 millimeters, 2 to 3 millimeters of wall thickness long；From
The gas that rotary pneumatic air inlet pipe enters spirally is flowed to other end in pipe under the guidance of rotation gas guide pipe.
Further, sealed set has water-output flange 170, water-output flange between gas distribution head 150 and cooling tube 160
170 tops are provided with water outlet 171, and coolant liquid is flowed out from water outlet 171, and 170 bottom of water-output flange is provided with sealing flange
172。
In the technical solution, water-output flange, sealing flange are made of quartz or ceramics or metal, are fixed with bolt, with poly-
Tetrafluoroethene, rubber or other flexible material sealing ring/gaskets are sealed.
Further, 130 bottom co-axial seal of plasmatron is provided with and communicated with inlet flange 180,180 side of inlet flange
Face offers the inlet chamber 181 for being connected to its inner cavity.Nitrogen or hydrogen or other process gas are passed through in inlet chamber 181.
Further, co-axial seal is provided with water ring flange 190, water ring flange between inlet flange 180 and cooling tube 160
190 inner walls are formed with the ring cavity 191 inside connection cooling tube 160, and 180 bottom co-axial seal of inlet flange is provided with water-in flange
182,182 side of water-in flange offers water inlet 183, and water-in flange 182, inlet flange 180 successively offer connection ring cavity
191 feed pathway 184, coolant liquid flows into ring cavity 191 after flowing into feed pathway 184 from water inlet 183, then flows into cooling tube
Inside 160.
In the technical solution, water ring flange, inlet flange and water-in flange respectively by by quartz ceramics or metal constitute,
Junction high-temperature agglomerant adhering and sealing.
Further, radio-frequency power supply 110 is connected to radio frequency matching network 111, radio frequency matching network 111 by coaxial cable
Radio-frequency power is connected to by coaxial cable by radio-frequency power supply incoming end 141 again, during intermediate frequency power supply 120 is connected to by water-cooled cable
Frequency power incoming end 142.
After gas enters plasma generation inner cavity, ionization, the ion of generation are generated under 10KV electrion of short duration
Under the excitation of radio-frequency power, stable initial plasma is formed；This plasma is in powerful intermediate frequency alternating electromagnetism
Under the excitation of field, the high-temperature plasma that power is dozens or even hundreds of kilowatt is generated.
After working gas enters plasma generation inner cavity, after steady air currents delay in 1-2 minutes, high-voltage electricity is opened
Radio-frequency power supply and intermediate frequency power supply are opened in source, and preferably positive 1500 watts of radio-frequency power, reverse radio-frequency power is lower than 50 watts；In starting
Frequency power adjustment is to 10-15KW, after 1-2 minutes stabilizations, with the rate of 2-5KW per minute, by the output of intermediate frequency power supply
Power is transferred to 30KW；Maintaining stable power supply and gas input, good chilled(cooling) water supply (CWS), this plasma generator energy
Enough continual and steady work ten a few houres to time a couple of days.The cost of power supply is low, high reliablity, greatly reduces the system of induction power supply
It makes or purchase cost.
In conjunction with shown in Fig. 1,4-7, the ICP plasma gas-phase reactor of nano material is produced with liquid or gaseous precursor,
Including reaction chamber 200, co-axial seal is connected to plasma generator 100 and cooling chamber 300 respectively at reaction chamber 200 both ends, reaction
200 side wall of chamber is tightly connected, air inlet ring at least provided with an air inlet ring 210 between 200 side wall of air inlet ring 210 and reaction chamber
Annular static pressure chamber 211 is formed with inside 210,200 side wall of reaction chamber offers multiple rotation gas nozzles for being connected to annular static pressure chamber 211
212, multiple rotation gas nozzles 212 are arranged successively setting along 200 circumferencial direction of reaction chamber, and it is anti-that one is coaxially arranged with inside cooling chamber 300
Chamber is answered to clear up ring 220, reaction chamber cleaning 220 diameter of ring is slightly less than 200 diameter of reaction chamber, and reaction chamber clears up the cleaning reaction of ring 220
200 inner wall of chamber.
The air inlet ring 210 of top brings liquid precursor 244 into reaction chamber 200, liquid by hydrogen or nitrogen or argon gas
Presoma 244 is the compound comprising element needed for nano material.The air inlet ring 210 of lower section is passed through cooling gas, cooling gas
For hydrogen or argon gas or nitrogen or helium or its mixed gas.For variety classes presoma, different cooling airs can choose
Body inhibits the generation of back reaction or reduces the degree that back reaction occurs while the temperature of cooling reaction cavity.
Gas enters reaction chamber in rotary manner, extends the reaction time.
Further, 210 side of air inlet ring is provided with the suction nozzle 213 for being connected to annular static pressure chamber 211, and rotation gas nozzle 212 prolongs
It stretches line and 200 axial line of reaction chamber is non-intersecting.
Further, 200 side wall of reaction chamber is the first double-layer tube wall 230,230 bottom of the first double-layer tube wall and top-side
It is respectively formed with the first double-layer tube wall inlet 231 and the first double-layer tube wall liquid outlet 232, is flowed between the first double-layer tube wall 230
It is connected with coolant liquid.
Further, 200 top and bottom of reaction chamber pass through respectively the first connecting flange 250 be sealedly attached to plasma hair
Raw device 100 and cooling chamber 300, the first double-layer tube wall inlet 231 and the first double-layer tube wall liquid outlet 232 are respectively arranged at first
250 side wall of connecting flange.
Further, 200 side wall of reaction chamber is provided at least two thermocouples 400 from top to bottom, anti-for monitoring the position
Answer 200 internal temperature of chamber.
For the temperature measurement and regulation in reaction chamber.
Further, reaction chamber cleaning ring 220 is driven by the drive rod 221 of a coaxial arrangement.
Further, further include bubbler 240, be connected to the bottle body inside bottle body 241 including a bottle body 241 and sealing
Air inlet pipe 242 and bottle body escape pipe 243 place liquid precursor 244 inside bottle body 241, and bottle body air inlet pipe 242 extends to liquid
Presoma 244, the sealing of bottle body escape pipe 243 are connected to suction nozzle 213.It further include heating evaporation device (figure does not regard), heating evaporation
Device heating liquid precursor 244 generates steam and is passed through suction nozzle 213.
Liquid precursor, by bubbler, can carry liquid precursor with hydrogen, nitrogen, argon gas is included, but are not limited to
The steam to evaporate is sent into reaction chamber by air inlet ring；
Liquid precursor can also be used, but be not limited to heating evaporation device, and heating liquid precursor liquid boiling generates steam,
Reaction chamber is sent by air inlet ring.
Liquid precursor is the compound comprising element required for nano material, and boiling point is lower, can be taken with gas sparging
Band or heating evaporation form steam.In general, it can be used for the liquefied compound of CVD, MOCVD etc., all can serve as the present invention
The presoma of ICP plasma gas-phase reactor.
Further, inserted with internal lining pipe in reaction chamber 200 (figure does not regard).
In the technical solution, internal lining pipe can be inserted, the preparation for different nano-powders；Reaction cavity internal lining pipe, can
With with metal, quartz, ceramic material is made.
Reaction chamber clears up the powder of ring cleaning reaction cavity wall and heat-exchanger surface accumulation, and air inlet circumferential direction reaction chamber provides
Presoma and reaction gas needed for reaction, structure is simple, easy to operate, low in cost, and the nano material purity prepared compared with
It is high, stability is good, pattern uniform particle sizes, can be widely applied to the various preparations suitable for a variety of high-end nano materials.It receives
The particle size of rice flour body, can be through but not limited to axial-temperature gradient in control reaction chamber, the concentration of presoma, cooling air
The flow etc. of body is controlled.The nano-powder of preparation can be silicon powder, singly be not limited to silicon powder, if it is silicon powder, gas
State or liquid precursor raw material, such as silane can be SiH4、Si2H6、Si3H8Deng；Chlorosilane can be SiH2Cl2、SiHCl3、
SiCl4、Si2Cl6Deng.
In conjunction with shown in Fig. 1,5,8, the ICP plasma gas phase cooler of nano material is produced with liquid or gaseous precursor,
Including cooling chamber 300,300 co-axial seal of cooling chamber is connected to 200 tail end of reaction chamber, is provided with heat exchange at the top of cooling chamber 300
Device 310, heat exchanger 310 include that the multiple cooling water cavities 311 circularized and the multiple cooling water cavity 311 of connection is arranged
Coolant line 312, cooling chamber 300 include co-axial seal setting cylindricality cooling chamber 320 and taper cooling chamber 330, cylindricality
Cooling chamber 320 is sealedly attached to 200 tail end of reaction chamber, and cooling chamber cleaning ring 321, cooling chamber are provided in cylindricality cooling chamber 320
Cleaning 321 diameter of ring is slightly less than 320 diameter of cylindricality cooling chamber, and cooling chamber clears up ring 321 and clears up 320 inner wall of cylindricality cooling chamber.
Further, there are two about 321 ring of cooling chamber cleaning is oppositely arranged, cooling chamber cleaning ring 321 passes through opposite set
Two telescopic rods 322 driving set, 322 hermetic penetrant taper cooling chamber of telescopic rod, 330 side wall.
Further, 311 section of cooling water cavity is trapezoidal, and trapezoidal short side is close to 300 axle center of cooling chamber.
Further, the movement mobile for reaction chamber cleaning ring 220 is formed among the multiple cooling water cavities 311 circularized
Space 313.
Further, 300 side wall of cooling chamber is the second double-layer tube wall 340,340 bottom of the second double-layer tube wall and top-side
It is respectively formed with the second double-layer tube wall inlet 341 and the second double-layer tube wall liquid outlet 342, is flowed between the second double-layer tube wall 340
It is connected with coolant liquid.
Further, coolant line 312 is connected to inside the second double-layer tube wall 340.
Further, 300 top and bottom of cooling chamber passes through the second connecting flange 350 respectively and is sealedly attached to reaction chamber
200 with powder collection system (figure do not regard), the second double-layer tube wall inlet 341 is set respectively with the second double-layer tube wall liquid outlet 342
It is placed in 350 side wall of the second connecting flange.
Further, 300 side wall of cooling chamber is provided at least one thermocouple 400 from top to bottom, cold for monitoring the position
But 300 internal temperature of chamber.
For the temperature measurement and regulation in cooling chamber.
Cooling chamber clears up the powder of the cooling cavity wall accumulation of ring cleaning cylindricality, and column construction is simple, easy to operate, at low cost
It is honest and clean, and the nano material purity prepared is higher, stability is good, pattern uniform particle sizes, can be widely applied to various be suitable for
The preparation of a variety of high-end nano materials.
Below for preparing nano-silicon powder, to illustrate preparation method of nano material of the invention.
Any of argon gas or hydrogen or nitrogen or argon gas and hydrogen, nitrogen and other gases is passed through in the tracheae of center
The mixed gas of ratio；It is passed through argon gas in rotary pneumatic air inlet pipe, in plasma under the excitation of the alternating electric field of combination frequency
High power plasma is generated in body generation cavity body, the high-temperature gas ionized through plasma heating is discharged into reaction chamber；
Any of argon gas or hydrogen or nitrogen or argon gas and hydrogen, nitrogen and other gases is passed through in inlet flange
The gas temperature for entering reaction cavity is adjusted to higher than the critical reaction temperature of selected presoma by the mixed gas of ratio
It 200-300 DEG C, is monitored with thermocouple；
The precursor gas of diluted silicon is passed into reaction chamber by the air inlet ring of top, reaction chamber is monitored by thermocouple
Interior gas temperature；This temperature should be 100-200 DEG C higher than the critical reaction temperature of selected presoma；It is next into
Compression ring is passed through the mixed gas of any ratio of argon gas or hydrogen or nitrogen or argon gas and hydrogen, nitrogen and other gases, leads to
Cross the gas temperature in thermocouple monitoring reaction chamber；By adjusting the gas flow of the air inlet ring, temperature is adjusted to than selected
Presoma critical reaction temperature it is 50-100 DEG C high；Continue next one air inlet ring and is passed through argon gas or hydrogen or nitrogen, or
The mixed gas of any ratio of argon gas and hydrogen, nitrogen and other gases monitors the gas temperature of cooling chamber entrance by thermocouple
Degree；Temperature is adjusted to 100- lower than prepared nano-powder and the byproduct of reaction generation critical reaction temperature of back reaction
200℃。
Fig. 9 is shown in the axial distribution of gas temperature in reaction chamber；Letter respectively indicates in figure: A be ion generator with react
Chamber junction temperature, B-F are followed successively by the temperature between the top air inlet ring, intermediate air inlet ring, bottom air inlet ring and three,
G is the temperature at the top of cooling chamber, and the axial distribution of gas temperature is divided into 5 regions, A or more is high-temperature plasma area；The area A-B
It is temperature adjustment area；The area B-D is main reaction region, and in this warm area, presoma, which completes, is cracked into nuclear reaction；The area D-E is
The particle in grain reunion area, presoma cracking nucleation is agglomerated into nano particle in this warm area；The area F-G is back reaction inhibition zone, instead
The temperature of product is answered to be dropped rapidly to side reaction critical-temperature hereinafter, inhibiting side reaction in this section；
The nano particle and reaction end gas for reacting synthesis are sent into nanometer after being discharged into cooling cavities cooling from reaction chamber bottom
Powder collection system collects nano particle, and tail gas discharges after being discharged into exhaust treatment system processing.
ICP plasma generator has selected the high-power ICP plasma generator of combination frequency, and purchase cost is that power is suitable
RFCO2 laser P plasma generator 10% to 15%, significantly reduce the manufacturing cost of equipment；The technique of rational design and
Structure improves persursor material utilization rate, reduces equipment manufacturing costs and nano material production cost, can produce partial size
30 nanometers of nano-powder materials below.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above is only the specific embodiment of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection scope of the application.
Claims (10)
1. a kind of high-power combination frequency ICP plasma generator characterized by comprising
Radio-frequency power supply, frequency 3-27.12MHz, power 1-10KW；
Intermediate frequency power supply, frequency 50-1000KHz, power 10-200KW；
Plasmatron, inside are formed with plasma and inner cavity occur；
Spiral induction coil is coaxially wrapped in the plasma pipe outer wall, and upper end is the radio-frequency power supply incoming end, and lower end is institute
Intermediate frequency power supply incoming end is stated, tap is the radio-frequency power supply, intermediate frequency power supply common ground end below the radio-frequency power supply incoming end；
Gas distribution head is sealed at the top of the plasmatron.
2. high-power combination frequency ICP plasma generator according to claim 1, which is characterized in that further include high pressure
Ignitor is introduced to the plasma from the gas distribution head and inner cavity occurs.
3. high-power combination frequency ICP plasma generator according to claim 1, which is characterized in that the spiral sense
It should enclose and tubulose is rolled by ceramic material or insulation fibre material for 8-20mm diameter copper pipes, the spiral induction coil circle number is
6-7 circle, space between the adjacent coils 5-10mm, the common ground end position are that 1-2 circle is taken out below the radio-frequency power supply incoming end
At head.
4. high-power combination frequency ICP plasma generator according to claim 1, which is characterized in that the spiral sense
Should enclose between the plasmatron and be coaxially arranged with cooling tube, the cooling inside pipe wall and the plasma pipe outer wall it
Between flowing be provided with coolant liquid.
5. high-power combination frequency ICP plasma generator according to claim 1, which is characterized in that the gas point
There is sealed set at leftover of bolt of cloth axle center is connected to the center tracheae that inner cavity occurs for the plasma.
6. high-power combination frequency ICP plasma generator according to claim 1, which is characterized in that the gas point
The leftover of bolt of cloth, which offers, is connected to the rotary pneumatic air inlet pipe that inner cavity occurs for the plasma, and the rotary pneumatic air inlet pipe is connected to described etc.
The entrance that inner cavity occurs for gas ions is located at the plasma and inner cavity top side occurs, and the gas distribution head is coaxially connected to be set
It is equipped with rotation gas guide pipe, the rotation gas guide pipe is located at the plasma and inner cavity top occurs.
7. high-power combination frequency ICP plasma generator according to claim 4, which is characterized in that the gas point
Sealed set has water-output flange between the leftover of bolt of cloth and the cooling tube, is provided with water outlet, the cooling at the top of the water-output flange
Liquid is flowed out from the water outlet, and the water-output flange bottom is provided with sealing flange.
8. high-power combination frequency ICP plasma generator according to claim 4, which is characterized in that the plasma
Body bottom of the tube co-axial seal is provided with and communicated with inlet flange, and the inlet flange side offers the inlet chamber for being connected to its inner cavity.
9. high-power combination frequency ICP plasma generator according to claim 8, which is characterized in that the air inlet method
The blue co-axial seal between the cooling tube is provided with water ring flange, and the water ring flange inner wall is formed with the connection cooling tube
Internal ring cavity, inlet flange bottom co-axial seal are provided with water-in flange, and the water-in flange side is offered into water
Mouthful, the water-in flange, inlet flange successively offer the feed pathway for being connected to the ring cavity, and the coolant liquid is from the water inlet
Mouth flows into the ring cavity after flowing into the feed pathway, then flows into inside the cooling tube.
10. high-power combination frequency ICP plasma generator according to claim 1, which is characterized in that the radio frequency electrical
Source is connected to radio frequency matching network by coaxial cable, and the radio frequency matching network passes through coaxial cable again and radio-frequency power is connected to
The radio-frequency power supply incoming end, the intermediate frequency power supply are connected to the intermediate frequency power supply incoming end by water-cooled cable.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020118873A1 (en) * | 2018-12-13 | 2020-06-18 | 深圳市捷佳伟创新能源装备股份有限公司 | Reaction chamber structure of plasma deposition furnace |
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| CN108966474B (en) | 2024-10-22 |
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