CN108686597B - Gas discharge reactor, gas discharge system and preparation method of trichlorosilane - Google Patents
Gas discharge reactor, gas discharge system and preparation method of trichlorosilane Download PDFInfo
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- CN108686597B CN108686597B CN201810470531.5A CN201810470531A CN108686597B CN 108686597 B CN108686597 B CN 108686597B CN 201810470531 A CN201810470531 A CN 201810470531A CN 108686597 B CN108686597 B CN 108686597B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
Abstract
The invention provides a gas discharge reactor, a gas discharge system and a preparation method of trichlorosilane, and belongs to the technical field of polycrystalline silicon production. The gas discharge reactor comprises an inner electrode, an outer electrode, a first dielectric medium and a second dielectric medium, wherein the outer electrode is arranged outside the inner electrode, the second dielectric medium is arranged in the outer electrode, the first dielectric medium is arranged between the inner electrode and the outer electrode, a rare gas discharge cavity is formed between the inner electrode and the first dielectric medium, a material gas discharge cavity is formed between the first dielectric medium and the outer electrode, the gas discharge reactor is provided with a material gas inlet and a material gas outlet, and the material gas inlet and the material gas outlet are both arranged on the outer electrode and communicated with the material gas discharge cavity. The preparation method of the trichlorosilane uses the gas discharge reactor of the gas discharge system, and separates material gas and rare gas in the preparation process, so that the rare gas can be recycled, and the pollution of the trichlorosilane can be avoided.
Description
Technical Field
The invention relates to the technical field of polycrystalline silicon production, in particular to a gas discharge reactor, a gas discharge system and a preparation method of trichlorosilane.
Background
At present, the improved siemens method is the mainstream technology for producing polycrystalline silicon, and more than 95 percent of polycrystalline silicon on the market is produced by the improved siemens method. According to statistics, when the improved Siemens method is adopted to produce the polysilicon, about 16 tons of silicon tetrachloride can be produced every 1 ton of polysilicon is produced. The link of preparing trichlorosilane by hydrogenating silicon tetrachloride is the key for guaranteeing closed cycle of an improved Siemens method, so that low-pollution hydrogenation of silicon tetrachloride is realized, and further, high-purity trichlorosilane is prepared, which is the necessary requirement for producing high-purity polysilicon.
Currently, a cold hydrogenation method is mostly adopted in a polysilicon factory to treat silicon tetrachloride. The cold hydrogenation method is characterized in that silicon tetrachloride, hydrogen and metal-grade silicon powder react in a large fluidized bed reactor in a gas-solid fluidized state at the temperature of about 850K and the pressure of about 2.2MPa to generate trichlorosilane, dichlorosilane and other substances.
The ultra-low temperature hydrogenation method of silicon tetrachloride is an emerging silicon tetrachloride treatment technology. The ultralow-temperature hydrogenation method of the silicon tetrachloride is characterized in that the silicon tetrachloride and the hydrogen are in a mixed gas form in a gas discharge reactor and are subjected to discharge reaction under the excitation of an electromagnetic field, the products are trichlorosilane and hydrogen chloride, and the reaction temperature is 298K-373K.
The existing gas discharge reactor adopts a single-layer medium, metal particles can be sputtered from an exposed electrode in the discharge process, the discharge gas is polluted, the product quality is influenced, and the separation of products is difficult.
Disclosure of Invention
The invention aims to provide a gas discharge reactor, which improves the product quality and avoids product pollution.
A second object of the present invention is to provide a gas discharge system, which can recycle rare gas, improve product quality, and avoid product contamination.
The third purpose of the invention is to provide a method for preparing trichlorosilane, which enables rare gas to be recycled and can avoid pollution of trichlorosilane.
The invention is realized by adopting the following technical scheme:
a gas discharge reactor comprises an inner electrode, an outer electrode, a first dielectric medium and a second dielectric medium, wherein the outer electrode is arranged outside the inner electrode, the second dielectric medium is arranged in the outer electrode, the first dielectric medium is arranged between the inner electrode and the outer electrode, a rare gas discharge cavity is formed between the inner electrode and the first dielectric medium, a material gas discharge cavity is formed between the first dielectric medium and the outer electrode, the gas discharge reactor is provided with a material gas inlet and a material gas outlet, and the material gas inlet and the material gas outlet are both arranged on the outer electrode and communicated with the material gas discharge cavity.
Further, in a preferred embodiment of the present invention, the outer electrode and the first dielectric are both circular rings.
Further, in a preferred embodiment of the present invention, the inner electrode has a circular ring shape.
Further, in a preferred embodiment of the present invention, the distance between the inner electrode and the outer electrode is 1 mm-20 mm;
preferably, the distance between the inner electrode and the outer electrode is 3mm to 9 mm.
Further, in a preferred embodiment of the present invention, the distance between the inner electrode and the first dielectric is 0.5mm to 5 mm;
preferably, the distance between the inner electrode and the first dielectric is 1 mm-1.5 mm.
Furthermore, in a preferred embodiment of the present invention, the inner electrode and the outer electrode are made of metal materials;
preferably, both the inner and outer electrodes are Cu.
Further, in a preferred embodiment of the present invention, the first dielectric is a transparent insulating material, and the second dielectric is an opaque insulating material;
preferably, the first dielectric is quartz and the second dielectric is zirconia, alumina or silicon nitride.
Further, in a preferred embodiment of the present invention, a temperature measuring cavity is disposed at the material gas outlet, and a temperature measuring device is disposed on a cavity wall of the temperature measuring cavity.
The gas discharge system comprises a gas distribution device, a rare gas circulating device, a tail gas treatment device and the gas discharge reactor, wherein the gas distribution device comprises a hydrogen storage tank, a silicon tetrachloride storage tank, a gasifier and a buffer tank, the hydrogen storage tank and the silicon tetrachloride storage tank are communicated with the buffer tank, the buffer tank is communicated with the gasifier and a material gas inlet, the rare gas circulating device is communicated with two ends of a rare gas discharge chamber, and the tail gas treatment device is communicated with a material gas outlet.
A preparation method of trichlorosilane is suitable for the gas discharge system and comprises the following steps:
mixing silicon tetrachloride in a silicon tetrachloride storage tank and hydrogen in a hydrogen storage tank in a buffer tank to obtain material gas, introducing the material gas into a material gas discharge chamber through a material gas inlet, introducing mixed gas consisting of two rare gases into the rare gas discharge chamber, reacting under the conditions that the excitation voltage is 5-12 kV and the excitation frequency is 0.5 kHz-30 KHz, introducing the mixed gas consisting of the rare gases into a rare gas circulating device, and introducing the material gas into a tail gas treatment device through a material gas outlet.
The gas discharge reactor provided by the preferred embodiment of the invention has the beneficial effects that: when the rare gas discharge chamber is used, the rare gas passes through the rare gas discharge chamber, the material gas passes through the material gas discharge chamber, and the rare gas discharge chamber and the material gas discharge chamber are arranged separately, so that the rare gas and the material gas are separated, a product and the rare gas do not need to be separated, the rare gas can be recycled, and the loss is low. The inner electrode does not contain a dielectric medium, the energy consumption is low, the outer electrode contains a second dielectric medium, metal ions are prevented from being ionized when the outer electrode discharges, and material gas cannot be polluted.
The gas discharge system provided by the invention has the beneficial effects that: by using the gas discharge reactor, rare gas circulates in the rare gas discharge cavity through the rare gas circulating device, hydrogen in the hydrogen storage tank and silicon tetrachloride in the silicon tetrachloride storage tank are mixed in the buffer tank, are gasified through the gasifier and enter the material gas discharge cavity through the material gas inlet, and a product is obtained at the material gas outlet and is separated through the tail gas treatment device. The rare gas discharge chamber and the material gas discharge chamber are separately arranged, so that the rare gas and the material gas are separated, the product and the rare gas do not need to be separated, the rare gas can be recycled, and the loss is low. The inner electrode does not contain a dielectric medium, the energy consumption is low, the outer electrode contains a second dielectric medium, metal ions are prevented from being ionized when the outer electrode discharges, and material gas cannot be polluted.
The preparation method of trichlorosilane provided by the embodiment of the invention has the beneficial effects that: under the conditions that the excitation voltage is 5-12 kV and the excitation frequency is 0.5 kHz-30 KHz, the rare gas in the rare gas discharge chamber discharges and generates uniform low-voltage discharge glow. Under the simultaneous action of low-voltage discharge glow and power supply excitation, the material gas positioned in the material gas discharge chamber is discharged, and silicon tetrachloride hydrogenation reaction is generated. The rare gas discharge chamber and the material gas discharge chamber are separately arranged, so that the rare gas and the material gas are separated, the product and the rare gas do not need to be separated, the rare gas can be recycled, and the loss is low. The inner electrode does not contain a dielectric medium, the energy consumption is low, the outer electrode contains a second dielectric medium, metal ions are prevented from being ionized when the outer electrode discharges, and material gas cannot be polluted.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments are briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without creative efforts, and the protection scope of the present invention also belongs to the protection scope of the present invention.
FIG. 1 is a cross-sectional view of a gas discharge reactor provided by an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a gas discharge system according to an embodiment of the present invention.
Icon: 100-a gas discharge reactor; 110-an inner electrode; 120-an outer electrode; 130-a first dielectric; 140-a second dielectric; 150-rare gas discharge chamber; 160-material gas discharge chamber; 161-material gas inlet; 162-material gas outlet; 163-temperature measuring chamber; 164-a temperature detector; 200-a gas discharge system; 210-a gas distribution device; 220-rare gas recycle; 230-a tail gas treatment device; 211-hydrogen storage tank; 212-a silicon tetrachloride storage tank; 213-a gasifier; 214-a buffer tank; 215-a power supply device; 216 — rare gas cooler.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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 some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. 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.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
Examples
Referring to fig. 1, a gas discharge reactor 100 includes an inner electrode 110, an outer electrode 120, a first dielectric 130 and a second dielectric 140, the outer electrode 120 is disposed outside the inner electrode 110, the second dielectric 140 is disposed inside the outer electrode 120, the first dielectric 130 is disposed between the inner electrode 110 and the outer electrode 120, a rare gas discharge chamber 150 is formed between the inner electrode 110 and the first dielectric 130, a material gas discharge chamber 160 is formed between the first dielectric 130 and the outer electrode 120, the gas discharge reactor 100 has a material gas inlet 161 and a material gas outlet 162, and the material gas inlet 161 and the material gas outlet 162 are disposed on the outer electrode 120 and are communicated with the material gas discharge chamber 160.
When the rare gas discharge chamber is used, the rare gas passes through the rare gas discharge chamber 150, the material gas passes through the material gas discharge chamber 160, the rare gas discharge chamber 150 and the material gas discharge chamber 160 are separately arranged, the rare gas and the material gas are separated, a product and the rare gas do not need to be separated, the rare gas can be recycled, and the loss is low. The inner electrode 110 does not contain a dielectric medium, so that the energy consumption is low, the outer electrode 120 contains the second dielectric medium 140, and metal ions are prevented from being ionized when the outer electrode 120 discharges, so that material gas is not polluted.
The gas discharge reactor 100 has a cylindrical structure and is provided with a housing, which may form the outer electrode 120, or may be a separate housing, and the outer electrode 120 and the first dielectric 130 are both circular rings. The gas discharge reactor 100 is formed in a cylindrical structure, so that it is convenient to manufacture, and the contact effect of the outer electrode 120 and the first dielectric 130 with the material gas and the rare gas is better.
The inner electrode 110 is circular, the contact effect of the inner electrode 110 and the rare gas is better, the rare gas is favorably discharged, and uniform low-voltage discharge glow is generated.
The distance between the inner electrode 110 and the outer electrode 120 is 1 mm-20 mm; preferably, the distance between the inner electrode 110 and the outer electrode 120 is 3mm to 9 mm. The distance between the inner electrode 110 and the first dielectric 130 is 0.5 mm-5 mm; preferably, the distance between the internal electrode 110 and the first dielectric 130 is 1mm to 1.5 mm. The rare gas in the rare gas discharge chamber 150 is discharged, and uniform low-pressure discharge glow is generated, so that the material gas in the material gas discharge chamber 160 is discharged, and the silicon tetrachloride hydrogenation reaction is generated.
The inner electrode 110 and the outer electrode 120 are both made of metal materials, and optionally, the inner electrode 110 and the outer electrode 120 are both made of Cu. The copper material has small resistance, and when the copper material is used as an electrode, the electrode consumes less joule heat, so that the contribution of the joule heat of the electrode to the low temperature of a reaction system can be reduced.
In this embodiment, the inner electrode 110 has a continuous thread structure, and the surface of the thread electrode has a continuous convex structure, so that a distorted electric field can be generated, and gas discharge can be promoted under a low excitation condition.
The external electrode 120 is attached to the surface of the second dielectric 140, and there is no gap between the external electrode 120 and the surface of the second dielectric 140. Optionally, the outer electrode 120 is a mesh structure, the mesh electrode has a point formed by intersecting metal wires, and may form a point-line discharge form with the threaded inner electrode 110, which may enhance the strength of the micro discharge channel, may induce more electron avalanches, and further may enable the discharge gas to generate more active particles, and ensure that the reaction has a high conversion rate, and in addition, there is no gap between the discharge electrode and the surface of the second dielectric medium 140, which may eliminate the energy consumption of gas discharge caused by the electric field between the outer electrode 120 and the second dielectric medium 140.
The first dielectric 130 is a transparent insulating material, and the second dielectric 140 is an opaque insulating material; preferably, the first dielectric 130 is quartz and the second dielectric 140 is zirconia, alumina or silicon nitride. The first dielectric 130 is selected to be transparent material to allow the light radiation generated in the rare gas discharge chamber 150 to pass through, and the second dielectric 140 is selected to be opaque material to avoid the loss of the light radiation generated in the discharge chamber, so that the light radiation can be limited in the discharge chamber, and the maximum utilization of the light radiation is realized.
The material gas outlet 162 is provided with a temperature measuring cavity 163, and the cavity wall of the temperature measuring cavity 163 is provided with a temperature detector 164. The material gas outlet 162 is provided with a temperature measuring cavity 163, and the tail gas temperature is detected by a thermocouple, so that the thermodynamic state of the discharged gas in the discharge chamber can be obtained. When the temperature of the material gas outlet 162 is measured, the material gas loses the discharge ionization state and is in a thermal equilibrium state, so that the gas temperature can be rapidly and accurately obtained.
A gas discharge system 200 comprises a gas distribution device 210, a rare gas circulation device 220, a tail gas treatment device 230 and a gas discharge reactor 100, wherein the gas distribution device 210 comprises a hydrogen storage tank 211, a silicon tetrachloride storage tank 212, a gasifier 213 and a buffer tank 214, the hydrogen storage tank 211 and the silicon tetrachloride storage tank 212 are both communicated with the buffer tank 214, the buffer tank 214 is communicated with the gasifier 213 and a material gas inlet 161, the rare gas circulation device 220 is communicated with two ends of a rare gas discharge chamber 150, and the tail gas treatment device 230 is communicated with a material gas outlet 162.
By using the gas discharge reactor 100, rare gas circulates in the rare gas discharge chamber 150 through the rare gas circulation device 220, after hydrogen in the hydrogen storage tank 211 and silicon tetrachloride in the silicon tetrachloride storage tank 212 are mixed in the buffer tank 214, the buffer tank 214 can play a role in further homogenizing gas and stabilizing gas pressure, the gas is gasified through the gasifier 213, enters the material gas discharge chamber 160 through the material gas inlet 161, and a product is obtained at the material gas outlet 162 and is separated through the tail gas treatment device 230. The rare gas discharge chamber 150 and the material gas discharge chamber 160 are separately arranged, so that the rare gas and the material gas are separated, the product and the rare gas do not need to be separated, the rare gas can be recycled, and the loss is low. The inner electrode 110 does not contain a dielectric medium, so that the energy consumption is low, the outer electrode 120 contains the second dielectric medium 140, and metal ions are prevented from being ionized when the outer electrode 120 discharges, so that material gas is not polluted.
Optionally, the gas discharge system 200 further comprises a power supply 215, the power supply 215 being electrically connected to the gas discharge reactor 100, the power supply 215 providing electrical energy to the inner electrode 110 and the outer electrode 120. Alternatively, the power source in the power supply device 215 is an alternating current power source, and the power source is a pulse power source. The pulse power supply is a positive and negative pulse power supply, the output frequency is 1 Hz-55 KHz, the positive pulse voltage is 1-50 KV, the negative pulse voltage is 1-20 KV, and the pulse width is 1-1000 muS.
Optionally, the gas discharge system 200 further includes a rare gas cooler 216, the rare gas cooler 216 is communicated with the rare gas discharge chamber 150, and the discharge tail gas in the rare gas discharge chamber 150 is processed by the rare gas cooler 216 and then is re-transported to the rare gas discharge chamber 150 for recycling during operation.
A preparation method of trichlorosilane is suitable for a gas discharge system 200 and comprises the following steps:
after the silicon tetrachloride in the silicon tetrachloride storage tank 212 and the hydrogen in the hydrogen storage tank 211 are mixed in the buffer tank 214, a material gas is obtained and is introduced into the material gas discharge chamber 160 through the material gas inlet 161, a mixed gas composed of two rare gases is introduced into the rare gas discharge chamber 150, after the reaction under the conditions that the excitation voltage is 5-12 kV and the excitation frequency is 0.5 kHz-30 KHz, the mixed gas composed of the rare gases enters the rare gas circulation device 220, and the material gas enters the tail gas treatment device 230 through the material gas outlet 162.
Under the conditions of the excitation voltage of 5-12 kV and the excitation frequency of 0.5 kHz-30 KHz, the rare gas in the rare gas discharge chamber 150 discharges and generates uniform low-voltage discharge glow. Under the simultaneous action of low-voltage discharge glow and power supply excitation, the material gas positioned in the material gas discharge chamber 160 is discharged, and silicon tetrachloride hydrogenation reaction is generated. The rare gas discharge chamber 150 and the material gas discharge chamber 160 are separately arranged, so that the rare gas and the material gas are separated, the product and the rare gas do not need to be separated, the rare gas can be recycled, and the loss is low. The inner electrode 110 does not contain a dielectric medium, so that the energy consumption is low, the outer electrode 120 contains the second dielectric medium 140, and metal ions are prevented from being ionized when the outer electrode 120 discharges, so that material gas is not polluted.
Optionally, the molar ratio of hydrogen to silicon tetrachloride is 6: 1-30: 1; the temperature of the material mixed gas entering the material discharge chamber is 300K-375K, and the pressure of the material mixed gas is 0.1 MPa-1 MPa. At low temperature, the pollution of the gas discharge reactor 100 to the material gas can be minimized, the material cost of the gas discharge reactor 100 can be reduced to the maximum extent, the generation of high-purity materials can be ensured, and the purification pressure can be reduced. The discharge gas is easier to discharge under low pressure, and can generate uniform discharge glow, thereby being beneficial to controlling discharge reaction.
Alternatively, the rare gas is selected from at least two of helium (He), neon (Ne), and argon (Ar), and preferably, the rare gas mixture gas is composed of neon and argon, and the mixing molar ratio thereof is 1: 5-1: 10, the air inlet temperature is 300K-350K, and the mixed gas pressure is 0.1 MPa-0.5 MPa.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (13)
1. A gas discharge system is characterized by comprising a gas distribution device, a rare gas circulation device, a tail gas treatment device and a gas discharge reactor, wherein the gas discharge reactor comprises an inner electrode, an outer electrode, a first dielectric medium and a second dielectric medium, the outer electrode is arranged outside the inner electrode, the second dielectric medium is arranged in the outer electrode, the first dielectric medium is arranged between the inner electrode and the outer electrode, a rare gas discharge cavity is formed between the inner electrode and the first dielectric medium, a material gas discharge cavity is formed between the first dielectric medium and the outer electrode, the gas discharge reactor is provided with a material gas inlet and a material gas outlet, and the material gas inlet and the material gas outlet are arranged on the outer electrode and are communicated with the material gas discharge cavity;
the gas distribution device comprises a hydrogen storage tank, a silicon tetrachloride storage tank, a gasifier and a buffer tank, wherein the hydrogen storage tank and the silicon tetrachloride storage tank are communicated with the buffer tank, the buffer tank is communicated with the gasifier and a material gas inlet, the rare gas circulation device is communicated with the two ends of the rare gas discharge cavity, and the tail gas treatment device is communicated with the material gas outlet.
2. The gas discharge system of claim 1 wherein said outer electrode and said first dielectric are both circular.
3. The gas discharge system of claim 2 wherein said inner electrode is annular in shape.
4. The gas discharge system of claim 3 wherein the distance between the inner electrode and the outer electrode is 1mm to 20 mm.
5. The gas discharge system of claim 4 wherein the distance between the inner electrode and the outer electrode is 3mm to 9 mm.
6. A gas discharge system according to claim 3 wherein the distance of the inner electrode from the first dielectric is 0.5 mm-5 mm.
7. The gas discharge system of claim 6 wherein the distance of the inner electrode from the first dielectric is 1 mm-1.5 mm.
8. The gas discharge system of claim 3 wherein said inner electrode and said outer electrode are both metallic materials.
9. The gas discharge system of claim 8 wherein said inner electrode and said outer electrode are both Cu.
10. The gas discharge system of claim 6 wherein the first dielectric is a transparent insulating material and the second dielectric is an opaque insulating material.
11. The gas discharge system of claim 10 wherein the first dielectric is quartz and the second dielectric is zirconia, alumina or silicon nitride.
12. The gas discharge system of claim 1, wherein a temperature measuring cavity is arranged at the material gas outlet, and a temperature detector is arranged on the wall of the temperature measuring cavity.
13. A method for preparing trichlorosilane by using the gas discharge system of any one of claims 1 to 12, wherein the method comprises the following steps:
mixing silicon tetrachloride in the silicon tetrachloride storage tank and hydrogen in the hydrogen storage tank in the buffer tank to obtain material gas, introducing the material gas into the material gas discharge chamber through the material gas inlet, introducing mixed gas consisting of two rare gases into the rare gas discharge chamber, reacting under the conditions that the excitation voltage is 5-12 kV and the excitation frequency is 0.5 kHz-30 KHz, introducing the mixed gas consisting of the rare gases into the rare gas circulating device, and introducing the material gas into the tail gas treatment device through the material gas outlet.
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| WO2006013129A1 (en) * | 2004-08-04 | 2006-02-09 | Degussa Ag | Process and apparatus for purifying silicon tetrachloride or germanium tetrachloride containing hydrogen compounds |
| CN101801518A (en) * | 2007-07-10 | 2010-08-11 | 创新发光体公司 | Methods and apparatus for the production of group IV nanoparticles in a flow-through plasma reactor |
| CN102335580A (en) * | 2011-06-21 | 2012-02-01 | 浙江大学 | Apparatus and method for preparing group IV nanoparticles with capacitive coupling plasma |
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