CN200964354Y - Device for thermal decomposition of volatile compound and depositing particles formed due to the decomposition - Google Patents
Device for thermal decomposition of volatile compound and depositing particles formed due to the decomposition Download PDFInfo
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- CN200964354Y CN200964354Y CN 200520132158 CN200520132158U CN200964354Y CN 200964354 Y CN200964354 Y CN 200964354Y CN 200520132158 CN200520132158 CN 200520132158 CN 200520132158 U CN200520132158 U CN 200520132158U CN 200964354 Y CN200964354 Y CN 200964354Y
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- reaction tubes
- thermolysis
- deposition
- volatile compound
- pressurized vessel
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Abstract
A device for pyrolyzing fugitive component and depositing the granules generated by the pyrolysis, comprising at least: a pressure vessel (1); at least one reaction tube (2): the opening (2c) of the reaction tube extends into the pressure vessel, the other end is outside the pressure vessel and provided with an air input (3), the direction of the ordinate axis is vertically downward and parallel to the ordinate axis (1d) of the pressure vessel, the air inlet side (2a) of the reaction tube can be heated and the air outlet side (2b) can be refrigerated; a collection cone (1a) which is arranged on the lower part of the pressure vessel (1): the opening (2c) of one reaction tube or a plurality of reaction tubes extend into an air cavity (1b) of the collection cone; an outlet gate (6) of granules (P) which is connected with the collection cone 1a; air outlet component 7 which is provided with a air guide (7a) (the air inlet area (7b) is connected with the air cavity (1b) of the collection cone (1a)), a filtration device (8) and an air outlet (9) which is arranged outside the pressure vessel.
Description
Technical field
The present invention relates to a kind ofly, particularly be suitable for the equipment (back also abbreviates device, reactor or pyrolysis reactor as) of the Powdered silicon of photovoltaic applications and electronic application from the vapour deposition fines.
Background technology
Known for a long time, the vapour-phase pyrolysis by single silane can prepare HIGH-PURITY SILICON (referring to US4676967, DE 3311650, DE 752280, DE 1180346).The common issue with of all these methods is will produce superfine particle as far as possible effectively and separate from gas and collect this superfine particle.Finally researched and developed this method [Wigger in university of Duisburg (Duisburg), Starke, Roth: " Silicon Particle Formation by Pyrolysis ofSilane in a Hot wall Gasphase Reactor ", Chem.Eng.Technol.24 (2001) 3, the 261-264 page or leaf].
With single silane is that raw material has been realized preparing Powdered silicon by following reaction expression:
SiH
4→Si+2H
2
Usually the apparatus structure that is applicable to this is as follows: pyrolysis reactor is made of the vertically arranged pipe of being made by SiSiC or silica glass alternatively.Its upper semisection is heatable, and is assemblied in refrigerative stainless steel chuck.For avoiding the sintering on tube wall, this zone is with hydrogen purge from top to down.Single silane sprays into from above with form pure or that dilute with suitable gas, and decomposes in the hot-zone.The particle aggregation that forms in other pipeline section, and with produce by reaction and in order to the hydrogen of purge through cooling.Silicon and hydrogen leave this pipe at lower region.Then be blown into 100% nitrogen, with cooling hydrogen/solid mixture and pneumatic transport solid better.Silicon is sent into dust filter unit by conduit, there through collecting and metal filtering core separation of hydrogen by can pneumatic purification.Hydrogen leaves strainer and is imported into waste gas burner usually.Silicon is collected in the basin and is derived.
This device in the exit of reaction tubes by be basically level or upwards the conduit of orientation be imperfect to the conveying of silica soot.This regular meeting causes the obstruction of transfer lime.Another shortcoming is the cooling by quenching, because must add other gas here.Therefore the capacity of single tube is limited in addition, and adopting parallel single hose system is very big at equipment aspect expending.Moreover always also can cause during from the filter head housings discharging stopping up.Another shortcoming is that the silicon that produces can be polluted by stainless wearing and tearing.
Summary of the invention
The purpose of this invention is to provide a kind of possibility that reduces above-mentioned shortcoming.
The objective of the invention is to be used for by of the present invention that thermolysis volatile compound and the formed thus particulate equipment of deposition realizes, this equipment has following feature:
Pressurized vessel (1),
At least one reaction tubes (2), its opening end (2c) stretches in the described pressurized vessel, its the other end is positioned at outside the described pressurized vessel and is furnished with gas input (3), the longitudinal axis that is oriented to vertically downward and is parallel to pressurized vessel (1d) of the longitudinal axis of described reaction tubes, the gas feed side (2a) of described reaction tubes is heatable, pneumatic outlet side (2b) is coolable
The bottom of pressurized vessel (1) has collection cone (1a), and the opening end of described one or more reaction tubes (2c) extend in the air cavity (1b) of this collection cone,
Described collection cone (1a) and particle (P) go out that port strobe (6) is connected and
Pneumatic outlet parts (7), it is equipped with gas channeling (7a), the gas feed district (7b) of this gas channeling (7a) is connected with the air cavity (1b) of collecting cone (1a), and described pneumatic outlet parts (7) also are equipped with filtration unit (8) and are positioned at the pneumatic outlet (9) of pressurized vessel outside.
Find following favourable structure thus:
New pyrolysis reactor is made up of as 5 separate heatable pipes one or more reaction tubes, and these pipes are installed in one preferably in the refrigerative pressurized vessel.This is substantially and under the outlet side of vertical orientated reaction tubes product is installed and collects cone, be about to this design of pressure vessels and become its underpart can be used for accepting and being collected in the formed particle of decomposition reaction simultaneously, at this moment advantageously the foot position of this collection cone is that the port strobe that of product is connected with powder also.When the single silane of application prepared silicon, reaction tubes preferably was made of SiSiC or silica glass.Certainly other material such as metallic substance also are applicable to other products.The length of this pipe and diameter are relevant with diluent gas with required production capacity, used gas or target product usually.Preferred employing length is the reaction tubes that 0.6-7m and diameter are elected 30-400mm as.Tubulate upper section is equipped with one or more heating zone, preferred 2-6 heating zone.The advantageous applications resistive heating, making reaction tubes thus is the temperature that resolver in the reaction tubes can suitablely be heated to above the decomposition temperature of base material, preferred 800-1100 ℃.Accessible top temperature is 1000 ℃ to silica glass in pipe, is 1100 ℃ on tube wall.Particularly can improve the capacity of apparatus of the present invention greatly, improve the regulation technology of reactor jacket and peripherals such as gas device and the cost utilising efficiency of safety technique simultaneously by the device of 5 reaction tubess.Reaction tubes following half as accumulation area and condensation region, be suitable for solid being cooled to below 100 ℃, at the same time as water-cooled by double jacket.No longer need in quenching, to introduce external gas thus.Leave each reaction tubes through like this refrigerative gas/solid mixture, but and normally drip product (below be also referred to as particle, solid or powder) collect in the cone to falling into.Thus can various transfer mechanisms, the single and economic method of available like this tube reduces to be polluted and cost.But described solid is as can be advantageously entering in the container of bubble-tight and passivation downwards or enter in the smelting furnace or in other postprocessing working procedures through dual-active plate system.
Pneumatic discharging supplementary unit also can be installed as additional fluidisation assistor in the circular cone tagma, only otherwise weigh, this pneumatic discharging supplementary unit for example outputs to solid in the fixed container or in the smelting furnace through the hydrogen materials flow at a certain time interval.The on the suction side of this container or smelting furnace can be equipped with the charging trap, and this trap is opened with the discharging trap (6a) of reactor or as double pendulum type trap alternate run in the process of filling in.
Described hydrogen should make progress and leave pyrolysis reactor through incorporate filter element or the pneumatic outlet parts that are installed in the center.
Incorporate strainer in the reactor of the present invention preferably has one or more filter cores of being made by sintering metal, pottery, fiber or plastics, after reaching certain pressure reduction, can be used to pneumatic pressure pulses from pneumatic reservoir and one or more these filter cores are carried out blowback simultaneously wash, and can make filter core reach purification thus.This purification can be selected rare gas element such as argon gas for use or advantageously be used for the gas such as the hydrogen of self-decomposition reaction and be carried out.This gas or gaseous mixture leave strainer and can deliver to as off gas treatment.
All surfaces that contact with product are material preparation or the coating not make product contamination advantageously.Can advantageously use as pottery or plastics such as polyethylene (PE), ETFE (ETFE), polytetrafluoroethylene (PTFE) or silicon as product silicon.This can be avoided polluting silicon by metallic impurity with filter core.
The pipe in the present invention and the different heat expansion of chuck are preferred so to be considered, promptly going up can free expansion, this can be for example by manage and supporting member between suitable sealing member reach.In addition, described reaction tubes advantageously keeps by the steel flange through water-cooled in the steel chuck of pressurized vessel.
Description of drawings
The sketch of the preferred embodiment of the invention shown in Fig. 1.
Embodiment
Theme of the present invention is to provide a kind of equipment (following device, reactor or the pyrolysis reactor of also claiming), and to be used for thermolysis volatile compound (the following base material that also is called for short) and the formed thus particle of deposition, this equipment has following feature at least:
Pressurized vessel (1),
At least one reaction tubes (2), its opening end (2c) stretches in the described pressurized vessel, its the other end is outside described pressurized vessel and be furnished with gas input (3), so that charging into product, collects in the cone (1b) its opening end (2c), the longitudinal axis that is oriented to vertically downward and is parallel to pressurized vessel (1d) of the longitudinal axis of described reaction tubes, the gas feed side of described reaction tubes is heatable (2a), and the pneumatic outlet side is coolable (2b)
The bottom of pressurized vessel (1) has collection cone (1a), and the opening end of described one or more reaction tubess (2c) extend in the air cavity (1b) of this collection cone,
This collection cone (1a) and particle (P) go out that port strobe (6) is connected and
Pneumatic outlet parts (7), the pneumatic outlet (9) that it is equipped with gas channeling (7a) (its gas feed district (7b) is connected with the air cavity (1b) of collecting cone (1a)), filtering system (8) and is positioned at the pressurized vessel outside.
The outer wall (1c) of preferred this pressurized vessel (1) is coolable in equipment of the present invention, as can be by the double jacket of water as refrigerant.
In addition, equipment of the present invention also can be equipped at least one tube bottom plate (1e), and this base plate comprises and stablizes reaction tubes (2) and the filter tube (7) that suits at outlet side.This is advantageously made strainer tube (7) and reaction tubes (2) and the relative tube bottom plate of reactor (1) (1e) sealing by O-ring (1f), referring to Fig. 1.
The length of the reaction tubes of present device (2) is preferably 60-700cm, preferred especially 100-600cm, and diameter is preferably 30-400mm, preferred especially 50-200mm.
In the present device, described reaction tubes (2) is suitable to be that silicon dialysis silicon carbide or silica glass constitute by metal, silicon nitride, silicon carbide, SiSiC.
In the present device, the gas feed side of reaction tubes (2) preferably is heated by resistive element (4) and adds cover, should make the 30-70% of reaction tubes (2) length, and the 40-60% of preferred especially its length is heatable.
In addition, reaction tubes (2) is centered on by cooling-part (5) up to its open side (2b).
In addition, equipment of the present invention should be furnished with the 2-36 root, preferred 3-18 root, preferred especially 4-6 root, particularly 5 reaction tubess (2).
Collect the pour into angle of cone (1a) in design with respect to the appropriate to the occasion consideration product in inclination angle of the axle of pressurized vessel (1).Thus, the wall and the angle between the pressurized vessel axle (1d) of collection cone (1a) are preferably 70 °-20 °, preferred especially 45 °-15 °.
In addition, equipment of the present invention have band dual-active plate system (6a, 6b) go out port strobe (6), thus, product can be simply and economy and do not damage the mode discharging of product, and get ready for aftertreatment.
Formed gaseous mixture G ' (referring to Fig. 1) can preferably discharge through the filtering system (8) with one or more filter core in the decomposition reaction of being undertaken by G → P+G ' in equipment of the present invention, and this filter core should be made of sintering metal, pottery, fiber or plastics.
Reaction tubes in present device (2) preferably is connected with pressurized vessel (1) through water-cooled steel flange with gas spout member (7).
Present device is applied to for example be used for the thermolysis and the formed thus particulate method of deposition of at least a volatile compound, wherein:
Each reaction tubes (2) on the suction side (2a) is heated to the decomposition temperature of volatile compound, and cools off the inferior segment (2b) of this reaction tubes,
Optionally using is the compound that inert gasses is diluted this heat decomposable volatile compound such as elements Si, Ge, C, N, Fe, Ti, Zr, Al, Ga or its mixture basically, this rare gas element is preferably argon gas or hydrogen, these gases or gaseous mixture (G) are sent into reaction tubes (2) through each gas input (3)
That in decomposition, form and in collecting cone (1a) sedimentary particle (P) through gate part (6) discharge and
Gas that forms in decomposition reaction or gaseous mixture (G ') (below abbreviation branch vent one's spleen) are discharged through pneumatic outlet (9), and at this moment the pressure in pressurized vessel (1) is kept substantially constant.
The preferred feeding side part (2a) of reaction tubes should be heated to 800-1100 ℃, and preferred 900-1000 ℃ especially, (2b 2c) should be cooled to≤100 ℃ the lower part of this reaction tubes, preferred 10-60 ℃.
Particularly in above-mentioned implementation method, send into single silane (G) of not diluted or with single silane (G) of diluted in hydrogen to pyrolysis reactor.Advantageously obtain HIGH-PURITY SILICON powder (P) thus in the methods of the invention, preferably (6a 6b) discharges this product (P) by collecting the dual-active plate system of cone (5) through discharge valve (6) off and on.
In addition, also can advantageously use present device advantageously the pyrolysis by volatile compound decompose other the thinnest particle of preparation, as by SiH
4And NH
3Preparation silicon nitride or by SiCl
4, H
2Prepare SiO with air
2
Claims (12)
1. one kind is used for thermolysis volatile compound and the formed thus particulate equipment of deposition, it is characterized in that:
1) pressurized vessel (1),
2) at least one reaction tubes (2), its opening end (2c) stretches in the described pressurized vessel, its the other end is positioned at outside the described pressurized vessel and is furnished with gas input (3), the longitudinal axis that is oriented to vertically downward and is parallel to pressurized vessel (1d) of the longitudinal axis of described reaction tubes, the gas feed side (2a) of described reaction tubes is heatable, pneumatic outlet side (2b) is coolable
3) bottom of pressurized vessel (1) has collection cone (1a), and the opening end of described one or more reaction tubes (2c) extend in the air cavity (1b) of this collection cone,
4) described collection cone (1a) and particle (P) go out that port strobe (6) is connected and
5) pneumatic outlet parts (7), it is equipped with gas channeling (7a), the gas feed district (7b) of this gas channeling (7a) is connected with the air cavity (1b) of collecting cone (1a), and described pneumatic outlet parts (7) also are equipped with filtration unit (8) and are positioned at the pneumatic outlet (9) of pressurized vessel outside.
2. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 is characterized in that the outer wall (1c) of pressurized vessel (1) is coolable.
3. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that the length of reaction tubes (2) is 60-700cm.
4. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that the diameter of reaction tubes (2) is 30-400mm.
5. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that reaction tubes (2) is made of metal, silicon nitride, silicon carbide, the silicon carbide that is impregnated with Si or silica glass.
6. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that the gas feed side of reaction tubes (2) is heated by resistive element (4) and adds cover.
7. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that reaction tubes (2) is centered on by cooling-part (5) up to the part (2b) of its open side (2c).
8. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that the length of the 30-70% of reaction tubes (2) is heatable.
9. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that having 2-36 root reaction tubes (2).
10. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that, have band dual-active plate system (6a, 6b) go out port strobe (6).
11. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that having the filtering system (8) with one or more filter core.
12. thermolysis volatile compound and the formed thus particulate equipment of deposition of being used for according to claim 1 and 2 is characterized in that reaction tubes (2) is connected with pressurized vessel (1) through water-cooled steel flange with gas spout member (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520132158 CN200964354Y (en) | 2005-12-09 | 2005-12-09 | Device for thermal decomposition of volatile compound and depositing particles formed due to the decomposition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520132158 CN200964354Y (en) | 2005-12-09 | 2005-12-09 | Device for thermal decomposition of volatile compound and depositing particles formed due to the decomposition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN200964354Y true CN200964354Y (en) | 2007-10-24 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200520132158 Expired - Lifetime CN200964354Y (en) | 2005-12-09 | 2005-12-09 | Device for thermal decomposition of volatile compound and depositing particles formed due to the decomposition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN200964354Y (en) |
-
2005
- 2005-12-09 CN CN 200520132158 patent/CN200964354Y/en not_active Expired - Lifetime
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: EVONIK DEGUSSA CO., LTD. Free format text: FORMER NAME: DEGUSSA CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: Dusseldorf Patentee after: DEGUSSA GmbH Address before: Dusseldorf Patentee before: Degussa AG |
|
| CP03 | Change of name, title or address |
Address after: essen Patentee after: EVONIK DEGUSSA GmbH Address before: Dusseldorf Patentee before: Degussa GmbH |
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| CX01 | Expiry of patent term |
Granted publication date: 20071024 |
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| EXPY | Termination of patent right or utility model |