CN102557038A - Preparation method of polycrystalline silicon - Google Patents
Preparation method of polycrystalline silicon Download PDFInfo
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Abstract
The invention discloses a preparation method of polycrystalline silicon. The method comprises the following steps of: undergoing a chemical vapor deposition reaction on trichlorosilane and high-purity hydrogen serving as raw materials at the high temperature of 1,050-1,250 DEG C and under the pressure of 0-0.8 MPa in a reduction furnace reactor; and depositing polycrystalline silicon on the surface of a heat-emitting silicon core. The method is characterized in that: 0.1-20 percent of hydrogen halide gas is introduced into a reduction furnace in a chemical vapor deposition process. According to method, silicon powder produced in the bulk phase of the reduction furnace can be suppressed effectively, an atomization phenomenon is eliminated, heat produced by reacting can be applied to deposition of polycrystalline silicon, the energy utilization efficiency and silicon depositing rate are increased, and the reaction temperature and the halogenated silane concentration are not required to be lowered; and due to etching of hydrogen halide on the surface of a silicon stick, the surface appearance is improved, and a dense polycrystalline silicon stick is obtained.
Description
Technical field
The present invention relates to a kind of polysilicon preparation method, be specifically related to a kind of through adding the polysilicon preparation method that oxidizing gas reduces atomizing, improves the product surface pattern.
Background technology
Polysilicon is the most important raw materials for production of photovoltaic industry and electronic industry, on using, needs extreme high purity.In general, the purity of solar-grade polysilicon need reach 6 more than 9 (more than 99.9999%), and the purity of electronic-grade polycrystalline silicon need reach 9 more than 9 (more than 99.9999999%).Now; The polysilicon preparation method of main flow mainly contains: improvement Siemens Method, silane thermal decomposition process, metallurgy method, sodium reduction, zinc reduction etc.; The polysilicon of wherein improveing Siemens Method production accounts for more than 80% of Gross World Product; Its core processing procedure is that trichlorosilane is sent into reactor drum with High Purity Hydrogen after rectification and purification, and (the silicon core is heated to 1000～1150 to the silicon wicking surface in reactor drum
oC) chemical vapour deposition reaction taking place, make the silicon core grow up to rod-like polycrystal silicon gradually, comprise unreacted trichlorosilane, dichloro-dihydro silicon, silicon tetrachloride, hydrogen and hydrogenchloride in the tail gas, after CDI separates purification, recycles.The trichlorosilane reduction reaction is a complicated process, during numerous reactions have taken place, and following to the contributive principal reaction of chemical vapour deposition:
SiHCl3+H2＝Si+3HCl （1）
4SiHCl3=3SiCl4+2H2+Si （2）。
In numerous indexs in the Siemens process polycrystalline silicon production process; Polysilicon deposition speed is the index that paid close attention to by people with the reduction power consumption; And it is numerous with the factor of reduction power consumption to influence polysilicon deposition speed, comprises temperature of reaction, pressure, flow velocity, inlet amount, material proportion etc.Manyly in the production scene find out a cover through secular practice and be fit to on-the-spot more excellent operating procedure, adopt this technology can obtain preferable sedimentation rate and reduction power consumption.Yet, because the uncertainty of producing and the unstable of material supply obtain more excellent result even adopt identical operations technology also to be difficult to assurance, to control badly, atomizating phenomenon also appears in process of production easily.Atomizing is to be vaporific in the reduction furnace, atomizing can influence the interior sharpness of reduction furnace, at this moment, can't accurately observe the growing state of silicon rod in the reduction furnace through the reduction furnace visor, be unfavorable for producing accurate operation.General atomizating phenomenon appears at about deposition reaction 30h, may last till that reaction finishes.The conventional atomization style that suppresses strengthens the hydrogen air input exactly, and this will have a strong impact on the quality of polysilicon deposition speed, reduction power consumption and product, will cause too early blowing out under situation is serious.The major cause of atomizing is that at later stages, it is big that the silicon rod diameter becomes, and furnace inner space is reduced; And inlet amount increases, and makes unit volume material concentration increase in the reactor drum, has promoted the pyrolysis (formula 2) of trichlorosilane in gas phase; In addition, in the growth later stage, furnace inner space reduces; Radiation quantity increases between silicon rod, and reactor body phase temperature is raise, and has further aggravated the pyrolysis of trichlorosilane.The main means that solve atomizing have: reduce electric current, reduce the material inlet amount, improve the proportioning of hydrogen and trichlorosilane etc.; Its fundamental point is to start with from the angle that reduces trichlorosilane gas phase pyrolysis speed with solving the atomizing problem; But also cause silicon deposition rates to descend thus; And then influencing average sedimentation rate and reduction power consumption, this is that the production of polysilicon enterprise utmost point is reluctant the situation of seeing.
The present invention is directed to the problems referred to above and advanced the improvement of production technique; Not only can solve the atomizing problem that occurs in the polysilicon production process; And need not reduce silicon rod surface temperature and material concentration; Guarantee sedimentation rate that production of polysilicon is high and low reduction power consumption, improved the surface topography of polycrystalline silicon rod.
Summary of the invention
The object of the invention is to provide a kind of improved polysilicon preparation method; Through add a certain amount of hydrogen halide to reactor drum, come effectively to suppress the generation of middle silica flour mutually of reduction furnace endosome, eliminate atomizating phenomenon; The heat that reaction is produced can supply polysilicon deposition to use; Improve energy utilization efficiency and silicon deposition rates, hydrogen chloride gas improves the polysilicon surface pattern to the etching energy on silicon rod surface, obtains the dense multicrystalline silicon rod.
Another purpose of the present invention is the improved polysilicon preparation method that provides, and can in reduction furnace, take place under the situation of atomizing, need not to take to reduce temperature of reaction, material concentration or improve H2/ chlorosilane proportioning, just can eliminate atomizating phenomenon.
Prepare in the process at polysilicon, when hydrogen chloride gas (like HCl) contacts with the surface of solid state si material,, form trichlorosilane or silicon tetrachloride the generating gasification reaction.Reaction formula is following:
3HCl+Si＝SiHCl3+H2 （3）
4HCl+Si＝SiCl4+2H2 （4）。
Generally speaking, when temperature was higher than 350 oC, reaction was mainly carried out with (4) formula.Because the depositing silicon in the reactor drum is high-purity, does not have catalyzer, therefore, temperature of reaction is high slightly.And the body in reactor drum mutually in, gas phase temperature all is higher than 500 oC, therefore; When body mutually in case there is silica flour to exist; Reaction (3) and (4) can obviously take place, and eliminates silica flour, on the other hand; Reaction (4) a large amount of SiCl4 that produced will suppress the thermolysis of SiHCl3, thereby suppress the generation of silica flour.
When only considering to have consumed solid state si owing to hydrogen chloride gas (like HCl) is introduced the reaction that reactor drum takes place, this has caused a kind of misunderstanding, after promptly hydrogen chloride gas (like HCl) is introduced reactor drum, causes the sedimentation rate of silicon to descend.In fact, when the amount of hydrogen chloride gas (like HCl) is no more than 60% molar content of chlorosilane, can not cause the obvious decline of silicon deposition rates.
Reaction (3) and (4) is thermopositive reaction.When HCl and the reaction of solid state si generating gasification, when forming TCS or silicon tetrachloride, will produce reaction heat up to 52 kilocalories/TCS-mole, react the heat that is absorbed far above siliceous deposits under the equal conditions.
The object of the invention is realized by following technical scheme:
A kind of preparation method of polycrystalline silicon; It is included in the reduction furnace reactor drum; Raw material halogenated silanes and high-purity hydrogen issue biochemical vapor deposition reaction in 1050-1250 ℃ of high temperature, 0 ~ 0.8MPa condition; And make and it is characterized in that the step that silicon rod is constantly grown up in reduction furnace, feeding 0.1mol% ~ 20mol% hydrogen halide in the said chemical vapour deposition reaction process at the silicon wicking surface deposit spathic silicon of heating.
Wherein, described halogenated silanes comprises chlorosilane, bromosilane, iodo silane etc., and the general formula of halogenated silanes is SiHnX4-n, n=0-3 wherein, X=Cl, Br, I.Preferred described halogenated silanes is selected from chlorosilane, n=0-3 wherein, X=Cl.More preferably, described halogenated silanes is selected from trichlorosilane.
Wherein, described hydrogen halide is selected from hydrogen fluoride, hydrogenchloride, hydrogen bromide, hydrogen iodide gas, does not introduce the gas of other impurity simultaneously, and charge flow rate is 1-5Nm3/h.Preferably, described hydrogen halide is selected from hydrogenchloride, and charge flow rate is 2Nm3/h.
In a concrete embodiment, at reaction 10-25h growing period, the molecular fraction that the feeding amount of described hydrogen halide accounts for the virgin gas halogenated silanes is 1-8%.
In a concrete embodiment, question response 25-60h, silicon core grow into about diameter 35-60mm, and the molecular fraction that the feeding amount of described hydrogen halide accounts for the virgin gas halogenated silanes is 8-20%.
In a concrete embodiment; Question response 60-80h, the silicon core grows into about diameter 50-90mm, turns the feeding amount of described hydrogen halide down; Making its molecular fraction that accounts for the virgin gas halogenated silanes is 10-15%, and keeps this constant rate until the reactor drum blowing out in the reaction later stage.
Wherein, described virgin gas and hydrogen halide are introduced into inlet pipe separately, and remix gets into the reduction furnace reactor drum and participates in reaction.Another kind of embodiment, described virgin gas and hydrogen halide be warp inlet pipe separately respectively, and the independent reduction furnace reactor drum that gets into is participated in reaction.
Another technical scheme of the present invention: a kind of preparation method of polycrystalline silicon; It is included in the reduction furnace reactor drum, and raw material halogenated silanes and high-purity hydrogen issue biochemical vapor deposition reaction in 1050-1250 ℃ of high temperature, 0 ~ 0.8MPa condition, and in the step of silicon wicking surface deposit spathic silicon of heating; It is characterized in that in the said chemical vapour deposition reaction process; When atomizating phenomenon occurring in the reduction furnace reactor drum, in reduction furnace, feed the hydrogen halide of 8mol% ~ 20mol%, eliminate until atomizating phenomenon; The back reduces hydrogen halide content to 1%-8%, and is maintained until the reaction end.
In a preferred embodiment, when atomizating phenomenon occurring in the reduction furnace reactor drum, in reduction furnace, feed the hydrogen halide of 10mol% ~ 15mol%, eliminate until atomizating phenomenon, the back reduces hydrogen halide content to 1%-8%, and is maintained until the reaction end.
Beneficial effect:
(1) utilizes suitable hydrogen chloride gas effectively to suppress the generation of atomizating phenomenon in the polysilicon production process, after the generation atomizing, successfully weaken atomizing through regulating the ratio of hydrogen chloride gas in raw material;
(2) when suppressing or eliminating atomizing, can produce the reaction heat that helps polysilicon deposition, reduce the polysilicon deposition energy consumption;
When (3) eliminating atomizing, need not to reduce temperature of reaction, material quantity and halogenated silanes concentration, guarantee high sedimentation rate;
(4) hydrogen chloride gas helps to improve surface topography in the slow etching on silicon rod surface, obtains the dense multicrystalline silicon rod.
Description of drawings
Fig. 1 is the synoptic diagram through the employed reduction reactor of improved polysilicon preparation method.
Wherein, the 1st, reduction furnace, the 2nd, polycrystalline silicon rod, the 3rd, reduction furnace stove tube, the 4th, mixed raw material gas inlet pipe, the 5th, oxidizing gas inlet pipe, the 6th, exhaust pipe, the 7th, reduction furnace chassis, the 8th, graphite components.
Embodiment
Be elaborated below in conjunction with the accompanying drawing specific embodiments of the invention; But; What must explain is; Protection scope of the present invention does not receive the restriction of these embodiments, and related concrete material is for explanation the present invention is set forth in this embodiment in the embodiment, is not to any restriction of the present invention.The scope that the present invention protected is confirmed by claims.
As shown in Figure 1, when carrying out production of polysilicon, from virgin gas and the hydrogen of inlet pipe 4 feedings through Hybrid Heating; Feed oxidizing gas from inlet pipe 5, after mixing, get into reduction furnace 1; Flow to the polycrystalline silicon rod 2 in the stove uniformly; Surface at the high temperature silicon rod deposits, and after reaction finished, tail gas was discharged reduction furnace 1 through vapor pipe 6.The intake method of virgin gas and oxidizing gas can also be selected warp inlet pipe separately respectively, and the independent reduction furnace reactor drum that gets into is participated in the reaction (not shown).
One of ordinary skill in the art are clear that; Production of polysilicon technology of the present invention and relating operation flow process can realize according to prior art fully; Unique different be in reduction furnace, to feed hydrogen chloride gas, the control of hydrogen chloride gas and feeding mode also can be taked existing techniques in realizing.
Comparative Examples 1
Adopt bell shape reactor drum as shown in Figure 1 to carry out the chemical vapour deposition of silicon.Silicon core diameter 8mm, high 2200mm closely links to each other silicon core one end with copper electrode with the graphite mounting block, and the upper end joins through silicon core crossbeam and another root silicon core.Behind the vacuum displacement, reactor drum starts through high frequency, and electric current is crossed the silicon core from the electrode stream that links to each other with reactor drum, makes the silicon core be heated to 1080～1100 ℃, and keeps silicon wicking surface temperature.Trichlorosilane and hydrogen feed in the reactor drum after being mixed and heated to 200 ℃, trichlorosilane initial flow 2Nm3/h, at the uniform velocity increase to keep after the 42Nm3/h constant, speedup time 30h.Hydrogen initial flow 13Nm3/h increases to 189Nm3/h gradually, and in whole deposition process, the mol ratio of hydrogen and trichlorosilane is reduced to 4.5 gradually from 6.5.When the reaction times reaches 30h, can see obviously from the window of reactor drum occurring atomizating phenomenon in the reactor drum that improve hydrogen proportioning and can gradually alleviate atomizing reactor drum in through reducing silicon wicking surface temperature this moment, when serious, needs to reduce the inlet amount of material.After atomizating phenomenon is eliminated, slowly increase silicon wicking surface temperature and material inlet amount again.After reaction times reaches 90h, stopped reaction, this moment, the silicon rod diameter can reach 110～120mm.
After the blowing out, open the reduction furnace bell jar, can find, chassis and inwall have been piled up a lot of silica flours, and some silica flour also falls into the slit of graphite components, and cleaning inconvenience also influences the production that goes into operation of next cycle.And, can see that gained polycrystalline silicon rod surface has rough slit and exoncoma.
Embodiment 1
Adopt with Comparative Examples 1 identical step and carry out the polysilicon deposition reaction, simultaneously HCl is preheated to 200 ℃ with given pace and also adds in the feed-pipe continuously, so that the ratio of HCl/TCS is about 5% (mole) in reactant gases.After beginning reaction, keep 1080～1100 ℃ of silicon wicking surface temperature.Trichlorosilane and hydrogen feed in the reactor drum after being heated to 200 ℃, trichlorosilane initial flow 2Nm3/h, at the uniform velocity increase to keep after the 42Nm3/h constant, speedup time 30h.Hydrogen initial flow 13Nm3/h increases to 189Nm3/h gradually, and in whole deposition process, the mol ratio of hydrogen and trichlorosilane is reduced to 4.5 gradually from 6.5.When the reaction times reaches 40～50h, in reactor drum, do not find atomizating phenomenon, continue to keep inlet amount, proportioning and silicon rod surface temperature to reaction to finish, this moment, the silicon rod diameter can reach 115～125mm, and unit reduction power consumption is compared with Comparative Examples 1 and is descended 5%.
Embodiment 2
Adopt with Comparative Examples 1 identical step and carry out the polysilicon deposition reaction.After beginning reaction, keep 1080～1100 ℃ of silicon wicking surface temperature.Trichlorosilane and hydrogen feed in the reactor drum after being heated to 200 ℃, trichlorosilane initial flow 2Nm3/h, at the uniform velocity increase to keep after the 42Nm3/h constant, speedup time 30h.Hydrogen initial flow 13Nm3/h increases to 189Nm3/h gradually, and in whole deposition process, the mol ratio of hydrogen and trichlorosilane is reduced to 4.5 gradually from 6.5.When the reaction times reaches 40～50h, atomizating phenomenon appears in reactor drum, continues this moment to keep inlet amount, proportioning and silicon rod surface temperature constant; Slowly open the HCl valve, after being preheated to 200 ℃, add continuously in the feed-pipe, make that the ratio of HCl/TCS is about 10% (mole) in the reactant gases; Reaction for some time; After phenomenon to be atomized is eliminated, reduce the HCl feeding and measure to the ratio of HCl/TCS and be about 5% (mole), until the reaction end; This moment, the silicon rod diameter can reach 115～125mm, and unit reduction power consumption is compared with Comparative Examples 1 and descended 5%.
Embodiment 3
Adopt the inventive method to carry out the polysilicon deposition reaction.Raw material trichlorosilane and hydrogen feed in the reactor drum trichlorosilane initial flow 2Nm3/h after being mixed and heated to 200 ℃; At the uniform velocity increasing to 42Nm3/h keeps constant afterwards; Hydrogen initial flow 13Nm3/h increases to 189Nm3/h gradually, behind 1100 ℃ of pyroreaction 20h; With the flow of 2Nm3/h, feed to reactor drum that to account for trichlorosilane percentage ratio be 6% HCl gas (being preheated to 200 ℃).React 30h again, the silicon core grows into about diameter 65mm, and feeding and accounting for trichlorosilane percentage ratio is 18% HCl gas.React 30h again, the silicon core grows into about diameter 100mm, and feeding and accounting for trichlorosilane percentage ratio is 15% HCl gas.Sustained reaction 10h, the feeding amount of keeping HCl gas is constant, to the reactor drum blowing out.
Embodiment 4
Adopt the inventive method to carry out the polysilicon deposition reaction.Raw material trichlorosilane and hydrogen feed in the reactor drum trichlorosilane initial flow 3Nm3/h after being mixed and heated to 200 ℃; At the uniform velocity increasing to 40Nm3/h keeps constant afterwards; Hydrogen initial flow 15Nm3/h increases to 200Nm3/h gradually, behind 1150 ℃ of pyroreaction 15h; With the flow of 1.5Nm3/h, feed to reactor drum that to account for trichlorosilane percentage ratio be 3% HCl gas (being preheated to 200 ℃).React 40h again, the silicon core grows into about diameter 70mm, and feeding and accounting for trichlorosilane percentage ratio is 15% HCl gas.React 35h again, the silicon core grows into about diameter 110mm, and feeding and accounting for trichlorosilane percentage ratio is 10% HCl gas.Sustained reaction 10h, the feeding amount of keeping HCl gas is constant, to the reactor drum blowing out.
Compare with Comparative Examples 1, obviously, the silica flour that produces in embodiment 3 and 4 the reactor drum obviously reduces, and atomizating phenomenon has obtained effective inhibition, and the surperficial exoncoma of polycrystalline silicon rod is less, and complete shape and appearance is more smooth, fine and close.And, to compare with Comparative Examples 1, unit reduction power consumption has descended 5% and 9% respectively.
Although the preceding text specific embodiments of the invention has given to describe in detail and explanation; But should indicatedly be; Those skilled in the art can carry out various equivalences to above-mentioned embodiment according to conception of the present invention and change and modification; When the function that it produced does not exceed spiritual that specification sheets contains yet, all should be within protection scope of the present invention.
Claims (13)
1. preparation method of polycrystalline silicon; It is included in the reduction furnace reactor drum; Raw material halogenated silanes and high-purity hydrogen issue biochemical vapor deposition reaction in 1050-1250 ℃ of high temperature, 0 ~ 0.8MPa condition; And make and it is characterized in that the step that silicon rod is constantly grown up in reduction furnace, feeding 0.1mol% ~ 20mol% hydrogen halide in the said chemical vapour deposition reaction process at the silicon wicking surface deposit spathic silicon of heating.
2. polysilicon preparation method according to claim 1 is characterized in that, described halogenated silanes comprises chlorosilane, bromosilane, iodo silane etc., and the general formula of halogenated silanes is SiHnX4-n, n=0-3 wherein, X=Cl, Br, I.
3. polysilicon preparation method according to claim 2 is characterized in that described halogenated silanes is selected from chlorosilane, n=0-3 wherein, X=Cl.
4. polysilicon preparation method according to claim 3 is characterized in that described halogenated silanes is selected from trichlorosilane.
5. polysilicon preparation method according to claim 1 is characterized in that, described hydrogen halide is selected from hydrogen fluoride, hydrogenchloride, hydrogen bromide, hydrogen iodide gas, does not introduce the gas of other impurity simultaneously, and charge flow rate is 1-5Nm
3/ h.
6. polysilicon preparation method according to claim 5 is characterized in that described hydrogen halide is selected from hydrogenchloride, and charge flow rate is 2Nm
3/ h.
7. polysilicon preparation method according to claim 1 is characterized in that, reaction 10-25h growing period, and the molecular fraction that the feeding amount of described hydrogen halide accounts for the virgin gas halogenated silanes is 1-8%.
8. polysilicon preparation method according to claim 1 is characterized in that, question response 25-60h, silicon core grow into about diameter 35-60mm, and the molecular fraction that the feeding amount of described hydrogen halide accounts for the virgin gas halogenated silanes is 8-20%.
9. polysilicon preparation method according to claim 1; It is characterized in that; Question response 60-80h, the silicon core grows into about diameter 50-90mm, turns the feeding amount of described hydrogen halide down; Making its molecular fraction that accounts for the virgin gas halogenated silanes is 10-15%, and keeps this constant rate until the reactor drum blowing out in the reaction later stage.
10. polysilicon preparation method according to claim 1 is characterized in that described virgin gas and hydrogen halide are introduced into inlet pipe separately, and remix gets into the reduction furnace reactor drum and participates in reaction.
11. polysilicon preparation method according to claim 1 is characterized in that, described virgin gas and hydrogen halide be warp inlet pipe separately respectively, and the independent reduction furnace reactor drum that gets into is participated in reaction.
12. preparation method of polycrystalline silicon; It is included in the reduction furnace reactor drum, and raw material halogenated silanes and high-purity hydrogen issue biochemical vapor deposition reaction in 1050-1250 ℃ of high temperature, 0 ~ 0.8MPa condition, and in the step of silicon wicking surface deposit spathic silicon of heating; It is characterized in that in the said chemical vapour deposition reaction process; When atomizating phenomenon occurring in the reduction furnace reactor drum, in reduction furnace, feed the hydrogen halide of 8mol% ~ 20mol%, eliminate until atomizating phenomenon; The back reduces hydrogen halide content to 1%-8%, and is maintained until the reaction end.
13. polysilicon preparation method according to claim 12; It is characterized in that; When atomizating phenomenon occurring in the reduction furnace reactor drum, in reduction furnace, feed the hydrogen halide of 10mol% ~ 15mol%, eliminate until atomizating phenomenon; The back reduces hydrogen halide content to 1%-8%, and is maintained until the reaction end.
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| EP2719663A1 (en) * | 2012-10-15 | 2014-04-16 | Wacker Chemie AG | Process for deposition of polycrystalline silicon |
| CN107352545A (en) * | 2016-05-09 | 2017-11-17 | 新特能源股份有限公司 | Using the method and polycrystalline silicon reduction system of polycrystalline silicon reduction system production polysilicon |
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| TWI494273B (en) * | 2012-10-15 | 2015-08-01 | Wacker Chemie Ag | Process for deposition of polycrystalline silicon |
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