CN103408016A - Method for preparing silicon particles and fluidized bed reactor - Google Patents
Method for preparing silicon particles and fluidized bed reactor Download PDFInfo
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- CN103408016A CN103408016A CN2013102846890A CN201310284689A CN103408016A CN 103408016 A CN103408016 A CN 103408016A CN 2013102846890 A CN2013102846890 A CN 2013102846890A CN 201310284689 A CN201310284689 A CN 201310284689A CN 103408016 A CN103408016 A CN 103408016A
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Abstract
The invention discloses a method for preparing silicon particles and a device. The method for preparing silicon particles comprises the following step: conducting a decomposition reaction on the silane in a fluidized bed reactor in the presence of silicon fine particles in a fluidized state to generate silicon, wherein the generated silicon is attached to the surface of the silicon fine particles to generate silicon particles. The method can be used to prepare silicon particles continuously and stably and further dramatically improve the efficiency in preparing silicon particles.
Description
Technical field
This law relates to chemical field, particularly, the present invention relates to prepare method and the fluidized-bed reactor thereof of silicon grain.
Background technology
Current, in photovoltaic industry, the production of most important intermediate-polysilicon remains and take improved Siemens as main, but the reduction low conversion rate of trichlorosilane in this technique, by-produced tetrachlorosilane amount be high, a large amount of materials is arranged is to be in the state of constantly recycle, up to the present, although this technique is through constantly improvement, make production cost be reduced to a lower level, but the space descended is little.In addition, the competition among enterprises fierceness, cause the polysilicon level of profitability of this explained hereafter not high.For this reason, the production development of polysilicon need to design new operational path, reduces production costs, and improves the quality of products.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or provides at least a kind of useful business to select.For this reason, one object of the present invention is the fluidized-bed reactor that proposes a kind of silicon grain preparation method and prepare silicon grain, utilizes the method and equipment can effectively improve the efficiency of producing silicon.
In one aspect of the invention, the present invention proposes a kind of method for preparing silicon grain, according to embodiments of the invention, the method comprises: in fluidized-bed reactor, when having the silicon minuteness particle of fluidized state, make silane generation decomposition reaction, in order to generate silicon, wherein, thus the silicon generated is attached to the surface of described silicon minuteness particle forms described silicon grain.
Utilize the method can significantly improve the silane rate of decomposition, can produce continuously, power consumption is low and product is convenient to following process for silicon grain.Silane contacts with the silicon minuteness particle of high temperature decomposition reaction occurs in fluidized-bed, decompose out siliceous deposits on silicon subparticle surface, it is constantly increased and become silicon grain and start gradually, to the bottom deposition of fluidized-bed reactor, to discharge silicon grain.Therefore the method does not need stopped reaction to take out silicon, and continuous operation that can the long period, can further improve the efficiency for preparing silicon grain thus.
In addition, the method for preparing silicon grain according to the above embodiment of the present invention can also have following additional technical characterictic:
According to embodiments of the invention, in described fluidized-bed reactor, supply with hydrogen, in order to make described silicon minuteness particle be fluidized state.Above-mentioned silicon minuteness particle carries out fluidisation in the middle and upper part of fluidized-bed, " fluidized state " refers to that a kind of gas or liquid of utilizing makes solid particulate be in the suspended motion state by the particulate solid layer, in the present invention, utilize hydrogen by silicon minuteness particle place suspended motion state, according to embodiments of the invention, the median size of described silicon minuteness particle is 0.001 millimeter.Be convenient to thus it and be in fluidized state.
According to embodiments of the invention, before supplying with hydrogen, adopt in advance substitution gas to replace the gas in described fluidized-bed.Because the silane decomposition reaction produces silicon and hydrogen, for avoiding introducing other materials, can at first adopt the air in the nitrogen fluid bedreactors to replace, and then adopt hydrogen to replace nitrogen, be convenient to thus the carrying out of subsequent reactions.
According to embodiments of the invention, described decomposition reaction is to carry out at the temperature of 600～900 degrees centigrade.Can further improve the decomposition reaction of silane thus.
According to embodiments of the invention, the pressure in described fluidized-bed reactor is 1～3atm.According to embodiments of the invention, the median size of described silicon grain is 1～2 millimeter.Thus can so that in fluidized-bed, prepare silicon grain reaction continue carry out.
According to embodiments of the invention, utilize high pressure hydrogen that described silicon minuteness particle is supplied in described fluidized-bed reactor.Be convenient to thus the stable charging continued of silicon minuteness particle.
According to embodiments of the invention, the flue dust that utilizes the cleaning apparatus fluid bedreactors to discharge carries out dust removal process, in order to reclaim the silicon minuteness particle.Simultaneously the flue gas of discharge purified, avoid contaminate environment.
According to embodiments of the invention, in described fluidized-bed reactor, the proportioning of hydrogen and silane is 10～50:1.Can further improve the carrying out of reaction thus.
In another aspect of this invention, the present invention proposes a kind of fluidized-bed reactor for the preparation of silicon grain, according to embodiments of the invention, this fluidized-bed reactor comprises: body limits the fluidized-bed reaction space in described body; Silicon minuteness particle opening for feed, described silicon minuteness particle opening for feed is arranged on described body, in described fluidized-bed reaction space, supplying with the silicon minuteness particle; The silane opening for feed, described silane opening for feed is arranged on described body, for in described fluidized-bed reaction space, supplying with silane, so that when having the silicon minuteness particle of fluidized state, make silane generation decomposition reaction generate silicon, wherein, thus the silicon generated is attached to the surface of described silicon minuteness particle forms described silicon grain; And the silicon grain outlet, described silicon grain outlet is arranged on described body, discharges described fluidized-bed reaction space for the silicon grain that will form.
In addition, the fluidized-bed reactor for preparing silicon grain according to the above embodiment of the present invention can also have following additional technical characterictic:
According to embodiments of the invention, above-mentioned fluidized-bed reactor further comprises the hydrogen feed mouth, and described hydrogen feed mouth is arranged on described body, for to described fluidized-bed reactor, supplying with hydrogen, in order to make described silicon minuteness particle be fluidized state.
According to embodiments of the invention, above-mentioned fluidized-bed reactor further comprises the substitution gas entrance, for in described fluidized-bed reaction space, supplying with substitution gas, in order to, before supplying with hydrogen, adopt in advance substitution gas to replace the gas in described fluidized-bed.
According to embodiments of the invention, described silicon minuteness particle opening for feed utilizes high pressure hydrogen that described silicon minuteness particle is supplied in described fluidized-bed reactor.
According to embodiments of the invention, above-mentioned fluidized-bed reactor further comprises: flue dust outlet, and described flue dust outlet is arranged on described body, the flue dust produced for the discharging current fluidized bed reactor; Cleaning apparatus, described cleaning apparatus is connected with described flue dust outlet, for described flue dust is carried out to dust removal process, in order to reclaim the silicon minuteness particle; And the silicon minuteness particle returns to entrance, described silicon minuteness particle returns to entrance and is arranged on described body, and is connected with described cleaning apparatus, for by being subject to starving minuteness particle, being back to the fluidized-bed reaction space.
According to embodiments of the invention, longitudinal direction along described fluidized-bed reactor, be disposed with described flue dust outlet, described silicon minuteness particle opening for feed, described silicon minuteness particle from top to bottom, and return to entrance, described silane opening for feed, described hydrogen feed mouth, described substitution gas entrance and silicon grain outlet.
According to embodiments of the invention, above-mentioned fluidized-bed reactor further comprises heating unit, and described heating unit is arranged on described body, for described fluidized-bed reaction space is heated.According to embodiments of the invention, described heating unit is frequency heating device.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
The accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding the description of embodiment, becoming in conjunction with following accompanying drawing, wherein:
Fig. 1 is the structural representation for preparing according to an embodiment of the invention the fluidized-bed reactor of silicon grain.
Embodiment
Below describe embodiments of the invention in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label means same or similar element or the element with identical or similar functions from start to finish.Below by the embodiment be described with reference to the drawings, be exemplary, be intended to be used to explaining the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention, it will be appreciated that, term " " center ", " vertically ", " laterally ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", orientation or the position relationship of indications such as " counterclockwise " are based on orientation shown in the drawings or position relationship, only the present invention for convenience of description and simplified characterization, rather than device or the element of indication or hint indication must have specific orientation, with specific orientation structure and operation, therefore can not be interpreted as limitation of the present invention.
In addition, term " first ", " second " be only be used to describing purpose, and can not be interpreted as indication or hint relative importance or the implicit quantity that indicates indicated technical characterictic.Thus, one or more these features can be expressed or impliedly be comprised to the feature that is limited with " first ", " second ".In description of the invention, the implication of " a plurality of " is two or more, unless otherwise expressly limited specifically.
In the present invention, unless otherwise clearly defined and limited, broad understanding should be done in the terms such as term " installation ", " being connected ", " connection ", " fixing ", for example, can be to be fixedly connected with, and can be also to removably connect, or connect integratedly; Can be mechanical connection, can be also to be electrically connected to; Can be directly to be connected, also can indirectly be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, can understand as the case may be above-mentioned term concrete meaning in the present invention.
In the present invention, unless otherwise clearly defined and limited, First Characteristic Second Characteristic it " on " or D score can comprise that the first and second features directly contact, also can comprise that the first and second features are not directly contacts but by the other feature contact between them.And, First Characteristic Second Characteristic " on ", " top " and " above " comprise First Characteristic directly over Second Characteristic and oblique upper, or only mean that the First Characteristic level height is higher than Second Characteristic.First Characteristic Second Characteristic " under ", " below " and " below " comprise that First Characteristic is under Second Characteristic and tiltedly, or only mean that the First Characteristic level height is less than Second Characteristic.
In one aspect of the invention, the present invention proposes a kind of method for preparing silicon grain.Below the method is described in detail, particularly, the method comprises: in fluidized-bed reactor, when having the silicon minuteness particle of fluidized state, make silane generation decomposition reaction, in order to generate silicon, wherein, thus the silicon generated is attached to the surface of silicon minuteness particle forms silicon grain.
Raw material silane contacts with the silicon minuteness particle of high temperature decomposition reaction occurs in fluidized-bed thus, decomposes out siliceous deposits on silicon subparticle surface, it is constantly increased and become silicon grain and start gradually, to the bottom deposition of fluidized-bed reactor, to discharge silicon grain.Therefore the method does not need stopped reaction to take out silicon, and continuous operation that can the long period, can further improve the efficiency for preparing silicon grain thus.The method and Siemens Method are produced polysilicon to compare decomposition efficiency high in addition, no coupling product, and the silane decomposition reaction is irreversible reaction, and as long as therefore the strict reaction conditions of controlling, silane will thermolysis obtain silicon.
According to one embodiment of present invention, supply with hydrogen in described fluidized-bed reactor, in order to make the silicon minuteness particle be fluidized state.Above-mentioned silicon minuteness particle carries out fluidisation in the middle and upper part of fluidized-bed, " fluidized state " refers to that a kind of gas or liquid of utilizing makes solid particulate be in the suspended motion state by the particulate solid layer, in the present invention, utilize hydrogen by silicon minuteness particle place suspended motion state, according to embodiments of the invention, the median size of described silicon minuteness particle is 0.001 millimeter.Be convenient to thus it and be in fluidized state.
According to one embodiment of present invention, before supplying with hydrogen, adopt in advance the gas in the substitution gas fluid bedreactors to replace.Because the silane decomposition reaction produces silicon and hydrogen, for avoiding introducing other materials, can at first adopt the air in the nitrogen fluid bedreactors to replace, and then adopt hydrogen to replace nitrogen, be convenient to thus the carrying out of subsequent reactions.
The decomposition reaction of according to one embodiment of present invention, concrete silane is to carry out at the temperature of 600～900 degrees centigrade.According to a particular embodiment of the invention, fluidized-bed reactor can be heated to 600～900 degrees centigrade, the silicon minuteness particle that is in fluidized state in fluidized-bed also is heated to this temperature range simultaneously.Therefore after in silane gas passes into fluidized-bed reactor, with the silicon minuteness particle of a large amount of high temperature, contact decomposition reaction occurs at once, most of silicon that reaction obtains is attached to silicon minuteness particle surface, it is increased gradually, will be constantly to fluidized-bed bottom deposition while becoming silicon grain when increasing to 1～2 millimeter.According to a particular embodiment of the invention, owing in fluidized-bed, there being the silicon minuteness particle, it is conducive to after being heated maintain the temperature-stable in fluidized-bed reactor, can save a part of heat energy thus.
Thus, according to a particular embodiment of the invention, the median size of the above-mentioned silicon grain prepared is 1～2 millimeter.The silicon grain of this particle size range can't keep fluidized state, and then gradually to the bottom of fluidized-bed deposition, thus can so that in fluidized-bed, prepare the silicon grain reaction continue carry out.Even from the silicon grain particle diameter that discharge the fluidized-bed reactor bottom, facilitate following process.
According to one embodiment of present invention, temperature is 600～900 degrees centigrade in controlling fluidized-bed reactor, pressure is 1～3atm, can significantly improve the rate of decomposition of silane, according to a particular embodiment of the invention, the rate of decomposition of silane can reach more than 98%, can significantly improve thus the productive rate of silicon grain.According to a particular embodiment of the invention, by regulating the pressure in fluidized-bed reactor, can control maximum silicon grain diameter, excessive but pressure is difficult for, in order to avoid equipment is caused to excessive pressure.According to a particular embodiment of the invention, when pressure is 1～3atm, can controls particle and grow up will sedimentation to go down to a certain extent, the mean particle size of this particle is 1～2 millimeter.
According to one embodiment of present invention, utilize high pressure hydrogen that described silicon minuteness particle is supplied in described fluidized-bed reactor.Make thus the silicon minuteness particle uniform and stable constantly to charging in fluidized-bed reactor, adopt simultaneously high pressure hydrogen to send into the silicon minuteness particle and can more be convenient to after it enters fluidized-bed reactor be converted into fluidized state.
According to one embodiment of present invention, can produce some flue gases in above-mentioned fluidized-bed reactor, this flue gas can be carried some silicon minuteness particles secretly and discharge from the top of fluidized-bed reactor.For this reason, according to a particular embodiment of the invention, the flue dust that can utilize the cleaning apparatus fluid bedreactors to discharge carries out dust removal process, in order to reclaim the silicon minuteness particle.Simultaneously the flue gas of discharge purified, avoid contaminate environment.According to a particular embodiment of the invention, the silicon minuteness particle of above-mentioned recovery can adopt high pressure hydrogen that it is sent in fluidized-bed reactor.
According to one embodiment of present invention, can by the flow velocity that control passes into hydrogen, control the fluidized state of silicon minuteness particle, can make granularity be less than the silicon grain of 1 millimeter and silicon microparticle and be in the suspended motion state and get final product.When the granularity of silicon grain reaches 1～2 millimeter, just can't be fluidized, the bottom to fluidized-bed deposits gradually.According to a particular embodiment of the invention, the proportioning of hydrogen and silane being not particularly limited in fluidized-bed reactor, according to concrete example of the present invention, the proportioning of hydrogen and silane can be 10～50:1.Can promote thus the continuous and effective of reacting to carry out, improve the preparation efficiency of silicon grain.According to a particular embodiment of the invention, said ratio obtains by many experiments, when the proportioning of hydrogen and silane is controlled at the generation that can reduce silicon powder in above-mentioned scope, be that silane decomposes the surface that the silicon obtained is attached to silicon powder substantially, make thus the fluidisation in fluidized-bed reactor more stable.
In another aspect of this invention, the present invention proposes a kind of fluidized-bed reactor for the preparation of silicon grain.Below with reference to Fig. 1, this fluidized-bed reactor is described in detail.
According to one embodiment of present invention, as shown in Figure 1, this fluidized-bed reactor comprises: body 100, silicon minuteness particle, silane opening for feed 300, and silicon grain outlet 400.
According to a particular embodiment of the invention, in body 100, limit fluidized-bed reaction space 101; Silicon minuteness particle opening for feed 200 is arranged on body 100, for to fluidized-bed reaction space 101 interior supply silicon minuteness particle; Silane opening for feed 300 is arranged on body 100, for the interior supply silane to fluidized-bed reaction space 101, so that when having the silicon minuteness particle of fluidized state, make silane generation decomposition reaction generate silicon, wherein, thus the silicon generated is attached to the surface of silicon minuteness particle forms described silicon grain; Silicon grain outlet 400 is arranged on body 100, discharges fluidized-bed reaction compartment 101 for the silicon grain that will form.
Raw material silane contacts with the silicon minuteness particle of high temperature decomposition reaction occurs in fluidized-bed reaction space 101 thus, decomposition siliceous deposits out is on silicon subparticle surface, making its continuous increase become silicon grain starts gradually to 101De bottom, fluidized-bed reaction space deposition, from silicon grain outlet 400 discharge silicon grains.Therefore utilize this fluidized-bed reactor not need stopped reaction to take out silicon, continuous operation that can the long period, can further improve the efficiency for preparing silicon grain thus.The method and Siemens Method are produced polysilicon to compare decomposition efficiency high in addition, no coupling product, and the silane decomposition reaction is irreversible reaction, and as long as therefore the strict reaction conditions of controlling, silane will thermolysis obtain silicon.
According to one embodiment of present invention, above-mentioned fluidized-bed reactor further comprises hydrogen feed mouth 500, and hydrogen feed mouth 500 is arranged on body 100, for to fluidized-bed reactor, supplying with hydrogen, in order to make the silicon minuteness particle be fluidized state.According to a particular embodiment of the invention, the median size of silicon minuteness particle is 0.001 millimeter.Be convenient to thus make it to keep fluidized state.
According to one embodiment of present invention, above-mentioned fluidized-bed reactor further comprises heating unit 102, and heating unit 102 is arranged on body 100, for the fluidized-bed reaction compartment is heated.According to a particular embodiment of the invention, this heating unit 102 can be frequency heating device, utilizes thus vertical middle part that this device can fluid bedreactors to heat.The decomposition reaction of concrete silane is to carry out at the temperature of 600～900 degrees centigrade.According to a particular embodiment of the invention, can utilize frequency heating device that fluidized-bed reactor is heated to 600～900 degrees centigrade, the silicon minuteness particle that is in fluidized state in fluidized-bed also is heated to this temperature range simultaneously.Therefore after in silane gas passes into fluidized-bed reactor, with the silicon minuteness particle of a large amount of high temperature, contact decomposition reaction occurs at once, most of silicon that reaction obtains is attached to silicon minuteness particle surface, it is increased gradually, when increasing to 1～2 millimeter, will, constantly to fluidized-bed bottom deposition, discharge from the silicon grain outlet while becoming silicon grain.According to a particular embodiment of the invention, owing in fluidized-bed, there being the silicon minuteness particle, it is conducive to after being heated maintain the temperature-stable in fluidized-bed reactor, can save a part of heat energy thus.
According to one embodiment of present invention, above-mentioned fluidized-bed reactor further comprises substitution gas entrance 600, for the interior supply substitution gas to fluidized-bed reaction space 101, in order to, before supplying with hydrogen, adopt in advance substitution gas to replace the gas in fluidized-bed.Because the silane decomposition reaction produces silicon and hydrogen, for avoiding introducing other materials, can at first adopt the air in the nitrogen fluid bedreactors to replace, and then adopt hydrogen to replace nitrogen, be convenient to thus the carrying out of subsequent reactions.
According to one embodiment of present invention, silicon minuteness particle opening for feed 200 utilizes high pressure hydrogen that the silicon minuteness particle is supplied in fluidized-bed reactor.Make thus the silicon minuteness particle uniform and stable constantly to charging in fluidized-bed reactor, adopt simultaneously high pressure hydrogen to send into the silicon minuteness particle and can more be convenient to after it enters fluidized-bed reactor be converted into fluidized state.
According to one embodiment of present invention, above-mentioned fluidized-bed reactor further comprises: flue dust outlet 700, cleaning apparatus and silicon minuteness particle return to entrance 900, the outlet of described flue dust is arranged on body 100, the flue dust produced for the discharging current fluidized bed reactor; Cleaning apparatus 800 is connected with flue dust outlet 700, for flue dust is carried out to dust removal process, in order to reclaim the silicon minuteness particle; The silicon minuteness particle returns to entrance 900 and is arranged on body 100, and is connected with cleaning apparatus 800, is back to fluidized-bed reaction space 101 for the silicon minuteness particle by reclaiming.Simultaneously the flue gas of discharge purified, avoid contaminate environment.According to a particular embodiment of the invention, the silicon minuteness particle of above-mentioned recovery can adopt high pressure hydrogen that it is sent in fluidized-bed reactor.
According to one embodiment of present invention, as shown in Figure 1, longitudinal direction along described fluidized-bed reactor, be disposed with flue dust outlet 700, silicon minuteness particle opening for feed 200, silicon minuteness particle from top to bottom, and return to entrance 900, silane opening for feed 300, hydrogen feed mouth 500, substitution gas entrance 600 and silicon grain outlet 400.Make thus flue dust discharge from the top of fluidized-bed reactor, enter cleaning apparatus 800 and reclaim the silicon minuteness particle.Silicon minuteness particle opening for feed 200, silicon minuteness particle return to the middle part that entrance 900 is positioned at the body 100 of fluidized-bed reactor, make the silicon minuteness particle be delivered to 101Nei De middle and upper part, fluidized-bed reaction space by high pressure hydrogen, and made it be in fluidized state from being arranged on the hydrogen that body 100 bottom hydrogen feed mouths 500 pass into.Silane opening for feed 300 is arranged on the bottom of intermediate frequency heater, the top of hydrogen feed mouth 500, making thus silane be passed into 101Nei Xiang top, fluidized-bed reaction space moves, with the silicon minuteness particle of high temperature, contact decomposition reaction occurs, degradation production silicon is attached to silicon minuteness particle surface, make the particle diameter of silicon minuteness particle become gradually large and constantly deposit downwards, finally from the silicon grain outlet 400 that is arranged on fluidized-bed reactor body 100 bottoms, discharge.Above-mentioned fluidized-bed reactor also comprises substitution gas entrance 600, and this entrance is arranged on body 100 bottoms, can utilize thus substitution gas that the gas displacement in fluidized-bed reaction space 101 is complete, avoids disturbing and producing at reaction impurities gas.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiment are only descriptive, and do not limit the present invention in any way.
Embodiment
With reference to topic 1, fluidized-bed reactor mainly consists of fluidized-bed 100, silica flour storehouse 103, cyclonic separator 800 3 parts.At first, use the air in the nitrogen replacement fluidized-bed reactor, use afterwards hydrogen exchange nitrogen, the gas displacement in fluidized-bed reaction space 101 is reached to requirement.Then, silicon minuteness particle after treatment is stored in silica flour storehouse 103, the median size of silicon minuteness particle is about 0.001 millimeter, the silicon minuteness particle joins the middle part of fluidized-bed by conduit, the silicon minuteness particle that enters fluidized-bed is fluidized the hydrogen fluidisation in bed, silicon minuteness particle in the fluidized-bed reaction section is heated to about 900 ℃ by frequency heating device 102, the pressure of controlling in the fluidized-bed reaction space is 1～3atm, after silicon minuteness particle fluidisation is stable, pass into silane, the ratio that passes into hydrogen and silane is 23:1.Pyrolysis occurs after the process risen, running into the high temperature silicon minuteness particle in the silane entered from the fluidized-bed bottom, decomposition siliceous deposits out is on the silicon grain surface, continuous weightening finish along with silicon grain, silicon grain drops to the bottom of fluidized-bed reactor gradually, then from silicon grain outlet 400, flow out, the median size of silicon grain is 1～2 millimeter.Top at fluidized-bed, from flue dust outlet 700, entered in cyclonic separator 800 by the silicon minuteness particle that gas entrainment goes out the fluidized-bed reaction section, after most silicon minuteness particle is separated, be returned to the middle lower end of fluidized-bed reaction section, the gas of process rough dusting is sent to subsequent handling.In addition, in order to deliver to the fluidized-bed reaction section to the silicon minuteness particle swimmingly, return to entrance 900 use high pressure hydrogens at silicon minuteness particle opening for feed 200 and silicon minuteness particle.
Utilize aforesaid method, the about 35kwh/kg-Si of the power consumption of fluidized-bed, the rate of decomposition of silane can reach 98%.Siemens's reduction furnace power consumption approximately with respect to 36 pairs of bar types is 55kwh/kg-Si, and fluidized-bed reactor of the present invention can significantly reduce power consumption, has simultaneously higher silane rate of decomposition, has improved silicon productivity.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the characteristics of this embodiment or example description.In this manual, the schematic statement of above-mentioned term not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or characteristics can be with suitable mode combinations in any one or more embodiment or example.
Although the above has illustrated and has described embodiments of the invention, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art is not in the situation that break away from principle of the present invention and aim can change above-described embodiment within the scope of the invention, modification, replacement and modification.
Claims (18)
1. a method for preparing silicon grain, is characterized in that, comprising:
In fluidized-bed reactor, when having the silicon minuteness particle of fluidized state, make silane generation decomposition reaction, in order to generate silicon,
Wherein, thus the silicon generated is attached to the surface of described silicon minuteness particle forms described silicon grain.
2. method according to claim 1, is characterized in that, supplies with hydrogen in described fluidized-bed reactor, in order to make described silicon minuteness particle be fluidized state.
3. method according to claim 2, is characterized in that, before supplying with hydrogen, adopts in advance substitution gas to replace the gas in described fluidized-bed.
4. method according to claim 1, is characterized in that, described decomposition reaction is to carry out at the temperature of 600～900 degrees centigrade.
5. method according to claim 1, is characterized in that, the pressure in described fluidized-bed reactor is 1～3atm.
6. method according to claim 1, is characterized in that, the median size of described silicon minuteness particle is 0.001 millimeter.
7. method according to claim 1, is characterized in that, the median size of described silicon grain is 1～2 millimeter.
8. method according to claim 1, is characterized in that, utilizes high pressure hydrogen that described silicon minuteness particle is supplied in described fluidized-bed reactor.
9. method according to claim 1, is characterized in that, the flue dust that utilizes the cleaning apparatus fluid bedreactors to discharge carries out dust removal process, in order to reclaim the silicon minuteness particle.
10. method according to claim 2, is characterized in that, in described fluidized-bed reactor, the proportioning of hydrogen and silane is 10～50:1.
11. the fluidized-bed reactor for the preparation of silicon grain, is characterized in that, comprising:
Body, limit the fluidized-bed reaction space in described body;
Silicon minuteness particle opening for feed, described silicon minuteness particle is arranged on described body, in described fluidized-bed reaction space, supplying with the silicon minuteness particle;
The silane opening for feed, described silane opening for feed is arranged on described body, for in described fluidized-bed reaction space, supplying with silane, so that when having the silicon minuteness particle of fluidized state, make silane generation decomposition reaction generate silicon, wherein, thus the silicon generated is attached to the surface of described silicon minuteness particle forms described silicon grain; And
The silicon grain outlet, described silicon grain outlet is arranged on described body, discharges described fluidized-bed reaction space for the silicon grain that will form.
12. fluidized-bed reactor according to claim 11, it is characterized in that, further comprise the hydrogen feed mouth, described hydrogen feed mouth is arranged on described body, for in described fluidized-bed reaction space, supplying with hydrogen, in order to make described silicon minuteness particle be fluidized state.
13. fluidized-bed reactor according to claim 12, it is characterized in that, further comprise the substitution gas entrance, in described fluidized-bed reaction space, supplying with substitution gas, in order to, before supplying with hydrogen, adopt in advance substitution gas to replace the gas in described fluidized-bed.
14. fluidized-bed reactor according to claim 13, is characterized in that, described silicon minuteness particle opening for feed utilizes high pressure hydrogen that described silicon minuteness particle is supplied in described fluidized-bed reaction space.
15. fluidized-bed reactor according to claim 13, is characterized in that, further comprises:
The flue dust outlet, described flue dust outlet is arranged on described body, be used to discharging the flue dust produced in the fluidized-bed reaction compartment;
Cleaning apparatus, described cleaning apparatus is connected with described flue dust outlet, for described flue dust is carried out to dust removal process, in order to reclaim the silicon minuteness particle; And
The silicon minuteness particle returns to entrance, and described silicon minuteness particle returns to entrance and is arranged on described body, and is connected with described cleaning apparatus, is back to the fluidized-bed reaction space for the silicon fine particle by reclaiming.
16. fluidized-bed reactor according to claim 15, it is characterized in that, longitudinal direction along described fluidized-bed reactor, be disposed with described flue dust outlet, described silicon minuteness particle opening for feed, described silicon minuteness particle from top to bottom, and return to entrance, described silane opening for feed, described hydrogen feed mouth, described substitution gas entrance and silicon grain outlet.
17. fluidized-bed reactor according to claim 11, is characterized in that, further comprises heating unit, described heating unit is arranged on described body, for described fluidized-bed reaction space is heated.
18. fluidized-bed reactor according to claim 17, is characterized in that, described heating unit is frequency heating device.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318654A (en) * | 2008-07-04 | 2008-12-10 | 清华大学 | Method for preparing high purity polysilicon particle with fluidized bed and bed fluidizing reactor |
| CN102502646A (en) * | 2011-10-10 | 2012-06-20 | 中国科学院过程工程研究所 | Equipment and method for preparing polysilicon by fast circulating fluidized bed-based chemical vapor deposition |
| CN102718219A (en) * | 2012-07-20 | 2012-10-10 | 上海森松压力容器有限公司 | Fluidized bed reactor used for producing polysilicon and preparation method of polysilicon |
| CN102815702A (en) * | 2012-08-09 | 2012-12-12 | 浙江中宁硅业有限公司 | Device and process of producing high-purity granular polycrystalline silicon by silanizing fluidized bed |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318654A (en) * | 2008-07-04 | 2008-12-10 | 清华大学 | Method for preparing high purity polysilicon particle with fluidized bed and bed fluidizing reactor |
| CN102502646A (en) * | 2011-10-10 | 2012-06-20 | 中国科学院过程工程研究所 | Equipment and method for preparing polysilicon by fast circulating fluidized bed-based chemical vapor deposition |
| CN102718219A (en) * | 2012-07-20 | 2012-10-10 | 上海森松压力容器有限公司 | Fluidized bed reactor used for producing polysilicon and preparation method of polysilicon |
| CN102815702A (en) * | 2012-08-09 | 2012-12-12 | 浙江中宁硅业有限公司 | Device and process of producing high-purity granular polycrystalline silicon by silanizing fluidized bed |
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