CN103408016B - Prepare method and the fluidized-bed reactor thereof of silicon grain - Google Patents
Prepare method and the fluidized-bed reactor thereof of silicon grain Download PDFInfo
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- CN103408016B CN103408016B CN201310284689.0A CN201310284689A CN103408016B CN 103408016 B CN103408016 B CN 103408016B CN 201310284689 A CN201310284689 A CN 201310284689A CN 103408016 B CN103408016 B CN 103408016B
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Abstract
The present invention proposes the method and equipment thereof of preparing silicon grain, wherein, the method preparing silicon grain comprises: in a fluidized bed reactor, when there is the silicon minuteness particle of fluidized state, make silane generation decomposition reaction, to generate silicon, wherein, the silicon generated is attached to the surface of silicon minuteness particle thus forms silicon grain.Utilize the method can continous-stable prepare silicon grain, and then the efficiency preparing silicon grain can be significantly improved.
Description
Technical field
This law relates to chemical field, specifically, the present invention relates to the method and fluidized-bed reactor thereof of preparing silicon grain.
Background technology
Current, in photovoltaic industry, the production of most important intermediate-polysilicon remains based on improved Siemens, but the reduction low conversion rate of trichlorosilane in this technique, by-produced tetrachlorosilane amount are high, have a large amount of materials 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 declined is little.In addition, competition among enterprises is fierce, causes the polysilicon level of profitability of this explained hereafter not high.For this reason, the production development of polysilicon needs to design new operational path, reduces production cost, 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 at least provides a kind of useful business to select.For this reason, one object of the present invention is the fluidized-bed reactor proposing a kind of silicon grain preparation method and prepare silicon grain, utilizes the method and equipment effectively can improve the efficiency of producing silicon.
In one aspect of the invention, the present invention proposes a kind of method preparing silicon grain, according to embodiments of the invention, the method comprises: in a fluidized bed reactor, when there is the silicon minuteness particle of fluidized state, make silane generation decomposition reaction, to generate silicon, wherein, the silicon generated is attached to the surface of described silicon minuteness particle thus forms described silicon grain.
Utilize the method can significantly improve silane decomposes rate, following process can be convenient to for silicon grain by the low and product of continuous seepage, power consumption.Silane contacts with the silicon minuteness particle of high temperature and decomposition reaction occurs in fluidized-bed, and the siliceous deposits decomposed out is surperficial at silicon subparticle, makes its continuous increase become silicon grain and starts to deposit to the bottom of fluidized-bed reactor gradually, discharge silicon grain.Therefore the method does not need stopped reaction to take out silicon, can the continuous operation of long period, can improve the efficiency preparing silicon grain further thus.
In addition, the method preparing silicon grain according to the above embodiment of the present invention can also have following additional technical characteristic:
According to embodiments of the invention, in described fluidized-bed reactor, supply hydrogen, 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 one utilizes gas or liquid to make solid particulate be in suspended motion state by particulate solid layer, utilize hydrogen by silicon minuteness particle place suspended motion state in the present invention, according to embodiments of the invention, the median size of described silicon minuteness particle is 0.001 millimeter.Be convenient to it thus and be in fluidized state.
According to embodiments of the invention, before supply hydrogen, substitution gas is adopted to replace the gas in described fluidized-bed in advance.Because silane decomposes reaction produces silicon and hydrogen, for avoiding introducing other materials, the air in nitrogen fluid bedreactors first can be adopted to replace, and then adopt hydrogen to replace nitrogen, being convenient to the carrying out of subsequent reactions thus.
According to embodiments of the invention, described decomposition reaction carries out at the temperature of 600 ~ 900 degrees Celsius.The decomposition reaction of silane can be improved thus further.
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 prepare in fluidized-bed silicon grain reaction continue carry out.
According to embodiments of the invention, high pressure hydrogen is utilized to be supplied in described fluidized-bed reactor by described silicon minuteness particle.Be convenient to silicon minuteness particle thus and stablize lasting charging.
According to embodiments of the invention, the flue dust utilizing cleaning apparatus fluid bedreactors to discharge carries out dust removal process, to reclaim silicon minuteness particle.The flue gas of discharge is purified simultaneously, avoid contaminate environment.
According to embodiments of the invention, in described fluidized-bed reactor, the proportioning of hydrogen and silane is 10 ~ 50:1.The carrying out of reaction can be improved thus further.
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 fluidized-bed reaction space in described body; Silicon minuteness particle opening for feed, described silicon minuteness particle opening for feed is arranged on the body, for supplying silicon minuteness particle in described fluidized-bed reaction space; Silane opening for feed, described silane opening for feed is arranged on the body, for supplying silane in described fluidized-bed reaction space, so that when there is the silicon minuteness particle of fluidized state, silane generation decomposition reaction is made to generate silicon, wherein, the silicon generated is attached to the surface of described silicon minuteness particle thus forms described silicon grain; And silicon grain outlet, described silicon grain outlet is arranged on the body, for the silicon grain of formation is discharged described fluidized-bed reaction space.
In addition, the fluidized-bed reactor preparing silicon grain according to the above embodiment of the present invention can also have following additional technical characteristic:
According to embodiments of the invention, above-mentioned fluidized-bed reactor comprises hydrogen feed mouth further, and described hydrogen feed mouth is arranged on the body, for supplying hydrogen in described fluidized-bed reactor, to make described silicon minuteness particle be fluidized state.
According to embodiments of the invention, above-mentioned fluidized-bed reactor comprises substitution gas entrance further, for supplying substitution gas in described fluidized-bed reaction space, so that before supply hydrogen, substitution gas is adopted to replace the gas in described fluidized-bed in advance.
According to embodiments of the invention, described silicon minuteness particle opening for feed utilizes high pressure hydrogen to be supplied in described fluidized-bed reactor by described silicon minuteness particle.
According to embodiments of the invention, above-mentioned fluidized-bed reactor comprises further: flue dust exports, and described flue dust outlet is arranged on the body, for the flue dust produced in discharging current fluidized bed reactor; Cleaning apparatus, described cleaning apparatus exports with described flue dust and is connected, for carrying out dust removal process to described flue dust, to reclaim silicon minuteness particle; And silicon minuteness particle returns entrance, described silicon minuteness particle returns entrance and is arranged on described body, and is connected with described cleaning apparatus, for being back to being subject to hungry minuteness particle in fluidized-bed reaction space.
According to embodiments of the invention, along the longitudinal direction of described fluidized-bed reactor, from top to bottom, be disposed with the outlet of described flue dust, described silicon minuteness particle opening for feed, described silicon minuteness particle return 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 comprises heating unit further, and described heating unit is arranged on the body, for heating described fluidized-bed reaction space.According to embodiments of the invention, described heating unit is frequency heating device.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is the structural representation of the fluidized-bed reactor preparing silicon grain according to an embodiment of the invention.
Embodiment
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not limitation of the present invention be interpreted as.
In describing the invention, it will be appreciated that, term " " center ", " longitudinal direction ", " transverse direction ", " 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 the instruction 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, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore limitation of the present invention can not be interpreted as.
In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise one or more these features.In describing the invention, the implication of " multiple " is two or more, unless otherwise expressly limited specifically.
In the present invention, unless otherwise clearly defined and limited, the term such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or connect integratedly; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, above-mentioned term concrete meaning in the present invention can be understood as the case may be.
In the present invention, unless otherwise clearly defined and limited, fisrt feature second feature it " on " or D score can comprise the first and second features and directly contact, also can comprise the first and second features and not be directly contact but by the other characterisation contact between them.And, fisrt feature second feature " on ", " top " and " above " comprise fisrt feature directly over second feature and oblique upper, or only represent that fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " below " and " below " comprise fisrt feature immediately below second feature and tiltedly below, or only represent that fisrt feature level height is less than second feature.
In one aspect of the invention, the present invention proposes a kind of method preparing silicon grain.Be described in detail the method below, particularly, the method comprises: in a fluidized bed reactor, when there is the silicon minuteness particle of fluidized state, make silane generation decomposition reaction, to generate silicon, wherein, the silicon generated is attached to the surface of silicon minuteness particle thus forms silicon grain.
Raw material silane contacts with the silicon minuteness particle of high temperature and decomposition reaction occurs in fluidized-bed thus, and the siliceous deposits decomposed out is surperficial at silicon subparticle, makes its continuous increase become silicon grain and starts to deposit to the bottom of fluidized-bed reactor gradually, discharge silicon grain.Therefore the method does not need stopped reaction to take out silicon, can the continuous operation of long period, can improve the efficiency preparing silicon grain further thus.In addition the method produce polysilicon with Siemens Method compared with decomposition efficiency high, no coupling product, and silane decomposes reaction is for irreversible reaction, as long as therefore strictly control reaction conditions, silane thermolysis will obtain silicon.
According to one embodiment of present invention, in described fluidized-bed reactor, supply hydrogen, to make 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 one utilizes gas or liquid to make solid particulate be in suspended motion state by particulate solid layer, utilize hydrogen by silicon minuteness particle place suspended motion state in the present invention, according to embodiments of the invention, the median size of described silicon minuteness particle is 0.001 millimeter.Be convenient to it thus and be in fluidized state.
According to one embodiment of present invention, before supply hydrogen, the gas in substitution gas fluid bedreactors is adopted to replace in advance.Because silane decomposes reaction produces silicon and hydrogen, for avoiding introducing other materials, the air in nitrogen fluid bedreactors first can be adopted to replace, and then adopt hydrogen to replace nitrogen, being convenient to the carrying out of subsequent reactions thus.
According to one embodiment of present invention, the decomposition reaction of concrete silane carries out at the temperature of 600 ~ 900 degrees Celsius.According to a particular embodiment of the invention, fluidized-bed reactor can be carried out being heated to 600 ~ 900 degrees Celsius, the silicon minuteness particle being in fluidized state simultaneously in fluidized-bed is also heated to this temperature range.Therefore when silane gas passes into after in fluidized-bed reactor, contact with the silicon minuteness particle of a large amount of high temperature and at once decomposition reaction occurs, the most of silicon be obtained by reacting is attached to silicon minuteness particle surface, make it increase gradually, will constantly deposit to fluidized-bed bottom when increasing to 1 ~ 2 millimeter and becoming silicon grain.According to a particular embodiment of the invention, owing to there is silicon minuteness particle in fluidized-bed, it is conducive to maintaining the temperature-stable in fluidized-bed reactor after being heated, and 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 cannot keep fluidized state, and then deposit to the bottom of fluidized-bed gradually, thus can so that prepare in fluidized-bed silicon grain reaction continue carry out.The silicon grain uniform particle sizes of discharging bottom fluidized-bed reactor, facilitates following process.
According to one embodiment of present invention, when temperature in control flow check fluidized bed reactor is 600 ~ 900 degrees Celsius, pressure is 1 ~ 3atm, the rate of decomposition of silane can be significantly improved, according to a particular embodiment of the invention, the rate of decomposition of silane can reach more than 98%, can significantly improve the productive rate of silicon grain thus.According to a particular embodiment of the invention, by regulating the pressure in fluidized-bed reactor, maximum silicon grain diameter can be controlled, but pressure is not easily excessive, in order to avoid cause excessive pressure to equipment.According to a particular embodiment of the invention, when pressure is 1 ~ 3atm, can controls particle growth and will sedimentation go down to a certain extent, the mean particle size of this particle is 1 ~ 2 millimeter.
According to one embodiment of present invention, high pressure hydrogen is utilized to be supplied in described fluidized-bed reactor by described silicon minuteness particle.Make silicon minuteness particle uniform and stable constantly to charging in fluidized-bed reactor thus, adopt high pressure hydrogen to send into silicon minuteness particle simultaneously and can more be convenient to be converted into fluidized state after it enters fluidized-bed reactor.
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 cleaning apparatus fluid bedreactors can be utilized to discharge carries out dust removal process, to reclaim silicon minuteness particle.The flue gas of discharge is purified simultaneously, avoid contaminate environment.According to a particular embodiment of the invention, the silicon minuteness particle of above-mentioned recovery can adopt high pressure hydrogen to be sent in fluidized-bed reactor.
According to one embodiment of present invention, the fluidized state of silicon minuteness particle can be controlled by the flow velocity controlling to pass into hydrogen, granularity can be made to be less than the silicon grain of 1 millimeter and silicon microparticle is in suspended motion state.Just cannot be fluidized when the granularity of silicon grain reaches 1 ~ 2 millimeter, gradually to the bottom deposit of fluidized-bed.According to a particular embodiment of the invention, in fluidized-bed reactor hydrogen and silane proportioning and be not particularly limited, according to concrete example of the present invention, the proportioning of hydrogen and silane can be 10 ~ 50:1.Can promote that the continuous and effective of reacting is carried out thus, improve the preparation efficiency of silicon grain.According to a particular embodiment of the invention, said ratio is obtained by many experiments, when the burden control of hydrogen and silane can reduce the generation of silicon powder in above-mentioned scope, be the surface that silicon that silane decomposes obtains is attached to silicon powder substantially, make the fluidisation in fluidized-bed reactor more stable thus.
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, fluidized-bed reaction space 101 is limited in body 100; Silicon minuteness particle opening for feed 200 is arranged on body 100, for supplying silicon minuteness particle in fluidized-bed reaction space 101; Silane opening for feed 300 is arranged on body 100, for supplying silane in fluidized-bed reaction space 101, so that when there is the silicon minuteness particle of fluidized state, silane generation decomposition reaction is made to generate silicon, wherein, the silicon generated is attached to the surface of silicon minuteness particle thus 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 be formed.
Raw material silane contacts with the silicon minuteness particle of high temperature and decomposition reaction occurs in fluidized-bed reaction space 101 thus, the siliceous deposits decomposed out is surperficial at silicon subparticle, make its continuous increase become silicon grain to start to deposit to the bottom in fluidized-bed reaction space 101 gradually, discharge silicon grains from silicon grain outlet 400.Therefore this fluidized-bed reactor is utilized not need stopped reaction to take out silicon, can the continuous operation of long period, the efficiency preparing silicon grain can be improved further thus.In addition the method produce polysilicon with Siemens Method compared with decomposition efficiency high, no coupling product, and silane decomposes reaction is for irreversible reaction, as long as therefore strictly control reaction conditions, silane thermolysis will obtain silicon.
According to one embodiment of present invention, above-mentioned fluidized-bed reactor comprises hydrogen feed mouth 500 further, and hydrogen feed mouth 500 is arranged on body 100, for supplying hydrogen in fluidized-bed reactor, to make 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 keep fluidized state.
According to one embodiment of present invention, above-mentioned fluidized-bed reactor comprises heating unit 102 further, and heating unit 102 is arranged on body 100, for heating fluidized-bed reaction compartment.According to a particular embodiment of the invention, this heating unit 102 can be frequency heating device, utilizes this device longitudinal middle part of fluid bedreactors to heat thus.The decomposition reaction of concrete silane carries out at the temperature of 600 ~ 900 degrees Celsius.According to a particular embodiment of the invention, frequency heating device can be utilized to be carried out being heated to 600 ~ 900 degrees Celsius by fluidized-bed reactor, the silicon minuteness particle being in fluidized state simultaneously in fluidized-bed is also heated to this temperature range.Therefore when silane gas passes into after in fluidized-bed reactor, contact with the silicon minuteness particle of a large amount of high temperature and at once decomposition reaction occurs, the most of silicon be obtained by reacting is attached to silicon minuteness particle surface, it is made to increase gradually, constantly to fluidized-bed bottom deposition, will discharge from silicon grain outlet when increasing to 1 ~ 2 millimeter and becoming silicon grain.According to a particular embodiment of the invention, owing to there is silicon minuteness particle in fluidized-bed, it is conducive to maintaining the temperature-stable in fluidized-bed reactor after being heated, and can save a part of heat energy thus.
According to one embodiment of present invention, above-mentioned fluidized-bed reactor comprises substitution gas entrance 600 further, for supplying substitution gas in fluidized-bed reaction space 101, so that before supply hydrogen, substitution gas is adopted to replace the gas in fluidized-bed in advance.Because silane decomposes reaction produces silicon and hydrogen, for avoiding introducing other materials, the air in nitrogen fluid bedreactors first can be adopted to replace, and then adopt hydrogen to replace nitrogen, being convenient to the carrying out of subsequent reactions thus.
According to one embodiment of present invention, silicon minuteness particle opening for feed 200 utilizes high pressure hydrogen to be supplied in fluidized-bed reactor by silicon minuteness particle.Make silicon minuteness particle uniform and stable constantly to charging in fluidized-bed reactor thus, adopt high pressure hydrogen to send into silicon minuteness particle simultaneously and can more be convenient to be converted into fluidized state after it enters fluidized-bed reactor.
According to one embodiment of present invention, above-mentioned fluidized-bed reactor comprises further: flue dust outlet 700, cleaning apparatus and silicon minuteness particle return entrance 900, described flue dust outlet is arranged on body 100, for the flue dust produced in discharging current fluidized bed reactor; Cleaning apparatus 800 and flue dust export 700 and are connected, for carrying out dust removal process to flue dust, to reclaim silicon minuteness particle; Silicon minuteness particle returns entrance 900 and is arranged on body 100, and is connected with cleaning apparatus 800, for being back in fluidized-bed reaction space 101 by reclaimed silicon minuteness particle.The flue gas of discharge is purified simultaneously, avoid contaminate environment.According to a particular embodiment of the invention, the silicon minuteness particle of above-mentioned recovery can adopt high pressure hydrogen to be sent in fluidized-bed reactor.
According to one embodiment of present invention, as shown in Figure 1, along the longitudinal direction of described fluidized-bed reactor, from top to bottom, be disposed with flue dust outlet 700, silicon minuteness particle opening for feed 200, silicon minuteness particle return entrance 900, silane opening for feed 300, hydrogen feed mouth 500, substitution gas entrance 600 and silicon grain outlet 400.Make flue dust discharge from the top of fluidized-bed reactor thus, enter cleaning apparatus 800 and carry out recovery 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 silicon minuteness particle be delivered to the middle and upper part in fluidized-bed reaction space 101 by high pressure hydrogen, and made it be in fluidized state by from being arranged on the hydrogen that body 100 lower hydrogen opening for feed 500 passes into.Silane opening for feed 300 is arranged on the bottom of intermediate frequency heater, the top of hydrogen feed mouth 500, make silane be passed in fluidized-bed reaction space 101 thus to move to top, contact with the silicon minuteness particle of high temperature and decomposition reaction occurs, degradation production silicon is attached to silicon minuteness particle surface, make the particle diameter of silicon minuteness particle become large gradually and constantly deposit downwards, finally discharging from the silicon grain outlet 400 being arranged on fluidized-bed reactor body 100 bottom.Above-mentioned fluidized-bed reactor also comprises substitution gas entrance 600, and this entrance is arranged on body 100 bottom, can utilize substitution gas that the gas displacement in fluidized-bed reaction space 101 is complete thus, avoids producing in the interference of reaction impurities gas.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiments are only descriptive, and do not limit the present invention in any way.
Embodiment
With reference to topic 1, fluidized-bed reactor is formed primarily of fluidized-bed 100, silica flour storehouse 103, cyclonic separator 800 3 part.First, use the air in nitrogen replacement fluidized-bed reactor, use hydrogen exchange nitrogen afterwards, the gas displacement in fluidized-bed reaction space 101 is reached requirement.Then, silicon minuteness particle is after treatment stored in silica flour storehouse 103, the median size of silicon minuteness particle is about 0.001 millimeter, silicon minuteness particle joins the middle part of fluidized-bed by conduit, the silicon minuteness particle entering fluidized-bed is fluidized the hydrogen fluidisation in bed, silicon minuteness particle in fluidized-bed reaction section is heated to about 900 DEG C by frequency heating device 102, the pressure controlled in fluidized-bed reaction compartment is 1 ~ 3atm, after silicon minuteness particle fluidisation is stable, pass into silane, the ratio passing into hydrogen and silane is 23:1.Pyrolysis is there is in the silane entered from fluidized-bed bottom run into high temperature silicon minuteness particle the process risen after, the siliceous deposits decomposed out is surperficial at silicon grain, along with the continuous weightening finish of silicon grain, silicon grain drops to the bottom of fluidized-bed reactor gradually, then flow out from silicon grain outlet 400, the median size of silicon grain is 1 ~ 2 millimeter.On the top of fluidized-bed, exporting 700 from flue dust is entered in cyclonic separator 800 by the silicon minuteness particle that gas entrainment goes out fluidized-bed reaction section, be returned to the middle lower end of fluidized-bed reaction section after most silicon minuteness particle is separated, the gas through rough dusting is sent to subsequent handling.In addition, in order to swimmingly silicon minuteness particle be delivered to fluidized-bed reaction section, return entrance 900 at silicon minuteness particle opening for feed 200 and silicon minuteness particle and use high pressure hydrogen.
Utilize aforesaid method, the power consumption of fluidized-bed is about 35kwh/kg-Si, and the rate of decomposition of silane can reach 98%.Be 55kwh/kg-Si relative to siemens's reduction furnace power consumption about of 36 pairs of bar types, fluidized-bed reactor of the present invention significantly can reduce power consumption, has higher silane decomposes rate simultaneously, improves silicon productivity.
In the description of this specification sheets, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and describe embodiments of the invention above, 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 can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (3)
1. for the preparation of a fluidized-bed reactor for silicon grain, it is characterized in that, comprising:
Body, limits fluidized-bed reaction space in described body;
Silicon minuteness particle opening for feed, described silicon minuteness particle is arranged on the body, for supplying silicon minuteness particle in described fluidized-bed reaction space;
Silane opening for feed, described silane opening for feed is arranged on the body, for supplying silane in described fluidized-bed reaction space, so that when there is the silicon minuteness particle of fluidized state, silane generation decomposition reaction is made to generate silicon, wherein, the silicon generated is attached to the surface of described silicon minuteness particle thus forms described silicon grain; And
Silicon grain exports, and described silicon grain outlet is arranged on the body, for the silicon grain of formation is discharged described fluidized-bed reaction space,
Wherein,
Comprise hydrogen feed mouth further, described hydrogen feed mouth is arranged on the body, for supplying hydrogen in described fluidized-bed reaction space, to make described silicon minuteness particle be fluidized state,
Comprising substitution gas entrance further, for supplying substitution gas in described fluidized-bed reaction space, so that before supply hydrogen, adopting substitution gas to replace the gas in described fluidized-bed in advance,
Described silicon minuteness particle opening for feed utilizes high pressure hydrogen to be supplied in described fluidized-bed reaction space by described silicon minuteness particle,
Comprise further:
Flue dust exports, and described flue dust outlet is arranged on the body, for discharging the flue dust produced in fluidized-bed reaction compartment;
Cleaning apparatus, described cleaning apparatus exports with described flue dust and is connected, for carrying out dust removal process to described flue dust, to reclaim silicon minuteness particle; And
Silicon minuteness particle returns entrance, and described silicon minuteness particle returns entrance and is arranged on described body, and is connected with described cleaning apparatus, for reclaimed silicon fine particle is back in fluidized-bed reaction space,
Along the longitudinal direction of described fluidized-bed reactor, from top to bottom, be disposed with the outlet of described flue dust, described silicon minuteness particle opening for feed, described silicon minuteness particle return entrance, described silane opening for feed, described hydrogen feed mouth, described substitution gas entrance and silicon grain outlet.
2. fluidized-bed reactor according to claim 1, is characterized in that, comprises heating unit further, and described heating unit is arranged on the body, for heating described fluidized-bed reaction space.
3. fluidized-bed reactor according to claim 2, is characterized in that, described heating unit is frequency heating device.
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| 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 |
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