CN102557038B - Preparation method of polycrystalline silicon - Google Patents
Preparation method of polycrystalline silicon Download PDFInfo
- Publication number
- CN102557038B CN102557038B CN201110457997.XA CN201110457997A CN102557038B CN 102557038 B CN102557038 B CN 102557038B CN 201110457997 A CN201110457997 A CN 201110457997A CN 102557038 B CN102557038 B CN 102557038B
- Authority
- CN
- China
- Prior art keywords
- silicon
- reduction furnace
- hydrogen halide
- reaction
- hydrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Silicon Compounds (AREA)
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 by adding oxidizing gas minimizing atomization, improving the polysilicon preparation method of product surface pattern.
Background technology
Polysilicon is the most important raw materials for production of photovoltaic industry and electronic industry, and application 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: improved Siemens, silane thermal decomposition process, metallurgy method, sodium reduction, zinc reduction etc., the polysilicon that wherein improved Siemens is produced accounts for more than 80% of Gross World Product, its core processing procedure is that trichlorosilane sends into reactor after rectification and purification together with High Purity Hydrogen, and (silicon core is heated to 1000 ~ 1150 to the silicon wicking surface in reactor
oc) there is chemical vapour deposition reaction, make silicon core grow up to rod-like polycrystal silicon gradually, in tail gas, comprise unreacted trichlorosilane, dichlorosilane, silicon tetrachloride, hydrogen and hydrogenchloride, recycle after CDI separating-purifying.Trichlorosilane reduction reaction is a complicated process, and period there occurs numerous reaction, and as follows to the contributive principal reaction of chemical vapour deposition:
SiHCl3+H2＝Si+3HCl （1）
4SiHCl3=3SiCl4+2H2+Si （2）。
In numerous indexs in Siemens process polycrystalline silicon production process, polysilicon deposition rates and reduction power consumption are the indexs paid close attention to by people, and affect the many factors of polysilicon deposition rates and reduction power consumption, comprise temperature of reaction, pressure, flow velocity, inlet amount, material proportion etc.Much more excellent operating procedures being found out a set of applicable scene by long-term practice in production scene, adopt this technique can obtain preferably sedimentation rate and reduction power consumption.But, due to the uncertainty of production and the unstable of material supply, even if adopt identical operating procedure to be also difficult to guarantee obtain preferably result, control bad, also easily occur atomizating phenomenon in process of production.In vaporific in atomization and reduction furnace, atomization can affect the sharpness in reduction furnace, now, cannot the growing state of silicon rod in accurate observation reduction furnace by reduction furnace visor, be unfavorable for producing accurate operation.General atomizating phenomenon appears at deposition reaction about 30h, may last till that reaction terminates.The conventional mode of atomization that suppresses strengthens hydrogen gas amount exactly, and this will have a strong impact on the quality of polysilicon deposition rates, reduction power consumption and product, situation seriously under will cause too early blowing out.The major cause of atomization is, at later stages, silicon rod diameter becomes large, furnace inner space is reduced, and inlet amount increases, unit volume material concentration in reactor is increased, facilitates trichlorosilane pyrolysis in the gas phase (formula 2), in addition, Later growth, furnace inner space reduces, and between silicon rod, radiation quantity increases, reactor bulk temperature is raised, exacerbates the pyrolysis of trichlorosilane further.The Main Means solving atomization has: the proportioning etc. reducing electric current, reduce material feeding amount, improve hydrogen and trichlorosilane, its fundamental point to be started with solution fogging problem from the angle reducing trichlorosilane gas phase pyrolysis speed, but also cause silicon deposition rates to decline thus, and then affecting average sedimentation rate and reduction power consumption, this is the situation that production of polysilicon enterprise pole is reluctant to see.
The present invention is directed to the problems referred to above and enter the improvement of production technique, not only can solve the fogging problem occurred in polysilicon production process, and do not need to reduce silicon rod surface temperature and material concentration, ensure that the sedimentation rate that production of polysilicon is high and low reduction power consumption, improve the surface topography of polycrystalline silicon rod.
Summary of the invention
The object of the invention is the polysilicon preparation method providing a kind of improvement, by adding a certain amount of hydrogen halide to reactor, the generation of silica flour in effectively suppressing reduction furnace endosome mutually, eliminate atomizating phenomenon, reacting the heat produced can for polysilicon deposition, improve energy utilization efficiency and silicon deposition rates, the etching energy of hydrogen chloride gas to silicon rod surface improves polysilicon surface pattern, obtains dense multicrystalline silicon rod.
Another object of the present invention is the polysilicon preparation method of provided improvement, when can there is atomization in reduction furnace, reducing temperature of reaction, material concentration or improving H2/ chlorosilane proportioning, just can eliminate atomizating phenomenon without the need to taking.
In polysilicon preparation process, when the surface contact of hydrogen chloride gas (as HCl) and solid state si material, generating gasification is reacted, form trichlorosilane or silicon tetrachloride.Reaction formula is as follows:
3HCl+Si＝SiHCl3+H2 （3）
4HCl+Si＝SiCl4+2H2 （4）。
Generally, when temperature is higher than 350 oC, reaction is mainly carried out with (4) formula.Because the depositing silicon in reactor is high-purity, do not have catalyzer, therefore, temperature of reaction is slightly high.And body in reactor mutually in, gas phase temperature is all higher than 500 oC, therefore, when body mutually in once there be silica flour to exist, reaction (3) and (4) can obviously occur, and eliminates silica flour, on the other hand, a large amount of SiCl4 that reaction (4) produces will suppress the thermolysis of SiHCl3, thus suppress the generation of silica flour.
The reaction occurred when only considering to introduce reactor due to hydrogen chloride gas (as HCl), consumes solid state si, which results in a kind of misunderstanding, after namely hydrogen chloride gas (as HCl) introduces reactor, causes the sedimentation rate of silicon to decline.In fact, when the amount of hydrogen chloride gas (as HCl) is no more than 60% molar content of chlorosilane, the obvious decline of silicon deposition rates can not be caused.
Reaction (3) and (4) is thermopositive reaction.When HCl and solid state si generating gasification are reacted ,/the reaction heat of TCS-mole when forming TCS or silicon tetrachloride, will be produced up to 52 kilocalories, react the heat absorbed far above siliceous deposits under equal conditions.
Object of the present invention is realized by following technical scheme:
A kind of preparation method of polysilicon, it is included in reduction furnace reactor, starting halo silane and high-purity hydrogen issue biochemical vapor deposition reaction in 1050-1250 DEG C of high temperature, 0 ~ 0.8MPa condition, and in the step that the silicon wicking surface deposit spathic silicon of heating makes silicon rod constantly grow up, it is characterized in that, in described chemical vapour deposition reaction process, in reduction furnace, passing into 0.1mol% ~ 20mol% hydrogen halide.
Wherein, described halogenated silanes comprises chlorosilane, bromosilane, iodosilane etc., and the general formula of halogenated silanes is SiHnX4-n, wherein n=0-3, X=Cl, Br, I.Preferably described halogenated silanes is selected from chlorosilane, wherein n=0-3, 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, and do not introduce the gas of other impurity, charge flow rate is 1-5Nm3/h simultaneously.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 intake of described hydrogen halide accounts for unstripped gas halogenated silanes is 1-8%.
In a concrete embodiment, question response 25-60h, silicon core grows into diameter about 35-60mm, and the molecular fraction that the intake of described hydrogen halide accounts for unstripped gas halogenated silanes is 8-20%.
In a concrete embodiment, question response 60-80h, silicon core grows into diameter about 50-90mm, turns the intake of described hydrogen halide down, make its molecular fraction accounting for unstripped gas halogenated silanes be 10-15%, and the phase maintain this constant rate until reactor blowing out after the reaction.
Wherein, described unstripped gas and hydrogen halide are introduced into respective inlet pipe, remix, enter reduction furnace reactor and participate in reaction.Another kind of embodiment, described unstripped gas and hydrogen halide, respectively through respective inlet pipe, independently enter reduction furnace reactor and participate in reaction.
Another technical scheme of the present invention: a kind of preparation method of polysilicon, it is included in reduction furnace reactor, starting halo silane and high-purity hydrogen are at 1050-1250 DEG C of high temperature, 0 ~ 0.8MPa condition issues biochemical vapor deposition reaction, and in the step of silicon wicking surface deposit spathic silicon of heating, it is characterized in that in described chemical vapour deposition reaction process, when there is atomizating phenomenon in reduction furnace reactor, the hydrogen halide of 8mol% ~ 20mol% is passed in reduction furnace, until atomizating phenomenon is eliminated, rear reduction hydrogen halide content is to 1%-8%, and be maintained until reaction end.
In a preferred embodiment, when occurring atomizating phenomenon in reduction furnace reactor, pass into the hydrogen halide of 10mol% ~ 15mol% in reduction furnace, until atomizating phenomenon is eliminated, rear reduction hydrogen halide content to 1%-8%, and is maintained until reaction end.
Beneficial effect:
(1) utilizing suitable hydrogen chloride gas effectively to inhibit the generation of atomizating phenomenon in polysilicon production process, after producing atomization, successfully weakening atomization by regulating hydrogen chloride gas ratio in the feed;
(2) in suppression or while eliminating atomization, the reaction heat being conducive to polysilicon deposition can be produced, reduce polysilicon deposition energy consumption;
(3), while eliminating atomization, without the need to reducing temperature of reaction, material quantity and halogenated silanes concentration, high sedimentation rate is guaranteed;
(4) hydrogen chloride gas is in the slow etching on silicon rod surface, contributes to improving surface topography, obtains dense multicrystalline silicon rod.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the reduction reactor that the polysilicon preparation method through improving uses.
Wherein, 1 is reduction furnace, and 2 is polycrystalline silicon rods, and 3 is reduction furnace cylinders, and 4 is mixed raw material gas inlet pipe, and 5 is oxidizing gas inlet pipe, and 6 is exhaust pipes, and 7 is chassis of reducing furnaces, and 8 is graphite components.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail; but; must it should be noted that; protection scope of the present invention is not by the restriction of these embodiments; concrete material involved in embodiment is for illustrating that the present invention enumerates in this embodiment, is not any limitation of the invention.The scope that the present invention protects, is determined by claims.
As shown in Figure 1, when carrying out production of polysilicon, unstripped gas through Hybrid Heating and hydrogen is passed into from inlet pipe 4, pass into oxidizing gas from inlet pipe 5, after mixing, enter reduction furnace 1, flow to the polycrystalline silicon rod 2 in stove uniformly, deposit on the surface of high temperature silicon rod, after reaction terminates, tail gas discharges reduction furnace 1 by vapor pipe 6.The intake method of unstripped gas and oxidizing gas can also be selected respectively through respective inlet pipe, independently enters reduction furnace reactor and participates in reaction (not shown).
One of ordinary skill in the art are clear that, polysilicon production process of the present invention and relevant operational flow completely conventionally can realize, uniquely pass into hydrogen chloride gas unlike in reduction furnace, the control of hydrogen chloride gas and pass into mode and also existing techniques in realizing can be taked.
Comparative example 1
Bell shape reactor is as shown in Figure 1 adopted to carry out the chemical vapour deposition of silicon.Silicon core diameter 8mm, high 2200mm, be closely connected silicon core one end with copper electrode with graphite mounting block, and upper end is connected with another root silicon core by silicon core crossbeam.After vacuum displacement, reactor is started by high frequency, and electric current flows through silicon core from the electrode be connected with reactor, makes silicon core be heated to 1080 ~ 1100 DEG C, and maintains silicon wicking surface temperature.Trichlorosilane and hydrogen, after being mixed and heated to 200 DEG C, pass in reactor, and trichlorosilane initial flow 2Nm3/h, remains constant after being at the uniform velocity increased to 42Nm3/h, speedup time 30h.Hydrogen initial flow 13Nm3/h, is increased 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 reaching 30h when reacted, obviously can see in reactor and occur atomizating phenomenon from the window of reactor, now by reducing silicon wicking surface temperature, raising hydrogen proportioning can alleviate the atomization in reactor gradually, time serious, need reduce the inlet amount of material.After atomizating phenomenon is eliminated, more slowly increase silicon wicking surface temperature and material feeding amount.After reaction times reaches 90h, stopped reaction, now silicon rod diameter can reach 110 ~ 120mm.
After blowing out, open reduction furnace bell jar, can find, chassis and inwall have piled up a lot of silica flour, and some silica flour also falls into the gap of graphite components, and cleaning inconvenience, also affects the production that goes into operation of next cycle.And, can see that gained polycrystalline silicon rod surface has rough gap and exoncoma.
Embodiment 1
Adopt the step identical with comparative example 1 to carry out polysilicon deposition reaction, HCl be preheated to 200 DEG C with given pace simultaneously and add in feed-pipe continuously, so that the ratio of HCl/TCS is about 5%(mole in reactant gases).After starting reaction, keep silicon wicking surface temperature 1080 ~ 1100 DEG C.Trichlorosilane and hydrogen, after being heated to 200 DEG C, pass in reactor, and trichlorosilane initial flow 2Nm3/h, remains constant after being at the uniform velocity increased to 42Nm3/h, speedup time 30h.Hydrogen initial flow 13Nm3/h, is increased 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 reaching 40 ~ 50h when reacted, in reactor, do not find atomizating phenomenon, continue to keep inlet amount, proportioning and silicon rod surface temperature to reacting end, now silicon rod diameter can reach 115 ~ 125mm, and unit reduction power consumption is decline 5% compared with comparative example 1.
Embodiment 2
The step identical with comparative example 1 is adopted to carry out polysilicon deposition reaction.After starting reaction, keep silicon wicking surface temperature 1080 ~ 1100 DEG C.Trichlorosilane and hydrogen, after being heated to 200 DEG C, pass in reactor, and trichlorosilane initial flow 2Nm3/h, remains constant after being at the uniform velocity increased to 42Nm3/h, speedup time 30h.Hydrogen initial flow 13Nm3/h, is increased 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 reaching 40 ~ 50h when reacted, atomizating phenomenon is there is in reactor, now continue to keep inlet amount, proportioning and silicon rod surface temperature constant, slow unlatching HCl valve, add continuously in feed-pipe after being preheated to 200 DEG C, the ratio of HCl/TCS in reactant gases is made to be about 10%(mole), reaction for some time, after phenomenon to be atomized is eliminated, reduction HCl intake is about 5%(mole to the ratio of HCl/TCS), until reaction terminates, now silicon rod diameter can reach 115 ~ 125mm, and unit reduction power consumption is decline 5% compared with comparative example 1.
Embodiment 3
The inventive method is adopted to carry out polysilicon deposition reaction.Raw material trichlorosilane and hydrogen are after being mixed and heated to 200 DEG C, pass in reactor, trichlorosilane initial flow 2Nm3/h, remain constant after being at the uniform velocity increased to 42Nm3/h, hydrogen initial flow 13Nm3/h, is increased to 189Nm3/h gradually, after 1100 DEG C of pyroreaction 20h, with the flow of 2Nm3/h, pass into reactor and account for the HCl gas (being preheated to 200 DEG C) that trichlorosilane percentage ratio is 6%.React 30h again, silicon core grows into diameter about 65mm, passes into and accounts for the HCl gas that trichlorosilane percentage ratio is 18%.React 30h again, silicon core grows into diameter about 100mm, passes into and accounts for the HCl gas that trichlorosilane percentage ratio is 15%.Sustained reaction 10h, the intake maintaining HCl gas is constant, to reactor blowing out.
Embodiment 4
The inventive method is adopted to carry out polysilicon deposition reaction.Raw material trichlorosilane and hydrogen are after being mixed and heated to 200 DEG C, pass in reactor, trichlorosilane initial flow 3Nm3/h, remain constant after being at the uniform velocity increased to 40Nm3/h, hydrogen initial flow 15Nm3/h, is increased to 200Nm3/h gradually, after 1150 DEG C of pyroreaction 15h, with the flow of 1.5Nm3/h, pass into reactor and account for the HCl gas (being preheated to 200 DEG C) that trichlorosilane percentage ratio is 3%.React 40h again, silicon core grows into diameter about 70mm, passes into and accounts for the HCl gas that trichlorosilane percentage ratio is 15%.React 35h again, silicon core grows into diameter about 110mm, passes into and accounts for the HCl gas that trichlorosilane percentage ratio is 10%.Sustained reaction 10h, the intake maintaining HCl gas is constant, to reactor blowing out.
Compared with comparative example 1, obviously, the silica flour produced in the reactor of embodiment 3 and 4 obviously reduces, and atomizating phenomenon obtains effective suppression, and the exoncoma on polycrystalline silicon rod surface is less, and pattern is complete, more smooth, fine and close.And compared with comparative example 1, unit reduction power consumption have dropped 5% and 9% respectively.
Although give detailed description and explanation to the specific embodiment of the present invention above; but what should indicate is; those skilled in the art can carry out various equivalence according to conception of the present invention to above-mentioned embodiment and change and amendment; its function produced do not exceed that specification sheets contains yet spiritual time, all should within protection scope of the present invention.
Claims (10)
1. the preparation method of a polysilicon, it is included in reduction furnace reactor, starting halo silane and high-purity hydrogen issue biochemical vapor deposition reaction in 1050-1250 DEG C of high temperature, 0 ~ 0.8MPa condition, and in the step that the silicon wicking surface deposit spathic silicon of heating makes silicon rod constantly grow up, it is characterized in that in described chemical vapour deposition reaction process, 0.1mol% ~ 20mol% hydrogen halide is passed in reduction furnace, wherein:
Reaction 10-25h growing period, the molecular fraction that the intake of described hydrogen halide accounts for unstripped gas halogenated silanes is 1-8%;
Question response 25-60h, silicon core grows into diameter 35-60mm, and the molecular fraction that the intake of described hydrogen halide accounts for unstripped gas halogenated silanes is 8-20%;
Question response 60-80h, silicon core grows into diameter 50-90mm, turns the intake of described hydrogen halide down, makes its molecular fraction accounting for unstripped gas halogenated silanes be 10-15%, and the phase maintains this constant rate until reactor blowing out after the reaction.
2. polysilicon preparation method according to claim 1, is characterized in that, described halogenated silanes comprises chlorosilane, bromosilane, iodosilane, and the general formula of halogenated silanes is SiH
nx
4-n, wherein n=0-3, X=Cl, Br, I.
3. polysilicon preparation method according to claim 2, is characterized in that, described halogenated silanes is selected from chlorosilane, wherein n=0-3, 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, and do not introduce the gas of other impurity, charge flow rate is 1-5Nm simultaneously
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, described unstripped gas and hydrogen halide are introduced into respective inlet pipe, remix, enters reduction furnace reactor and participates in reaction.
8. polysilicon preparation method according to claim 1, is characterized in that, described unstripped gas and hydrogen halide, respectively through respective inlet pipe, independently enter reduction furnace reactor and participate in reaction.
9. the preparation method of a polysilicon, it is included in reduction furnace reactor, starting halo silane and high-purity hydrogen issue biochemical vapor deposition reaction in 1050-1250 DEG C 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 described chemical vapour deposition reaction process, when there is atomizating phenomenon in reduction furnace reactor, the hydrogen halide of 8mol% ~ 20mol% is passed in reduction furnace, until atomizating phenomenon is eliminated, rear reduction hydrogen halide content to 1 mol %-8 mol %, and be maintained until reaction end.
10. polysilicon preparation method according to claim 9, it is characterized in that, when there is atomizating phenomenon in reduction furnace reactor, the hydrogen halide of 10mol% ~ 15mol% is passed in reduction furnace, until atomizating phenomenon is eliminated, rear reduction hydrogen halide content to 1 mol %-8 mol %, and be maintained until reaction end.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110457997.XA CN102557038B (en) | 2011-12-31 | 2011-12-31 | Preparation method of polycrystalline silicon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110457997.XA CN102557038B (en) | 2011-12-31 | 2011-12-31 | Preparation method of polycrystalline silicon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102557038A CN102557038A (en) | 2012-07-11 |
| CN102557038B true CN102557038B (en) | 2015-05-13 |
Family
ID=46403865
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110457997.XA Active CN102557038B (en) | 2011-12-31 | 2011-12-31 | Preparation method of polycrystalline silicon |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102557038B (en) |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102012218747A1 (en) * | 2012-10-15 | 2014-04-17 | Wacker Chemie Ag | Method of depositing 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 |
| CN107515274A (en) * | 2016-06-15 | 2017-12-26 | 上海韵申新能源科技有限公司 | A kind of polycrystalline silicon production system quality evaluating method and device |
| CN109467090A (en) * | 2017-09-07 | 2019-03-15 | 江苏中能硅业科技发展有限公司 | The method of continuous production granular polycrystalline silicon |
| CN109467089B (en) * | 2017-09-07 | 2024-02-09 | 江苏中能硅业科技发展有限公司 | Polycrystalline silicon production method |
| JP6951936B2 (en) * | 2017-10-20 | 2021-10-20 | 信越化学工業株式会社 | Manufacturing method for polycrystalline silicon rods and single crystal silicon |
| CN107720756A (en) * | 2017-11-03 | 2018-02-23 | 亚洲硅业（青海）有限公司 | A kind of polycrystalline silicon reducing furnace |
| CN112110449B (en) * | 2019-06-21 | 2022-06-28 | 新特能源股份有限公司 | Polycrystalline silicon production method and system |
| CN113544090B (en) * | 2019-07-16 | 2024-06-04 | 瓦克化学股份公司 | Method for preparing polycrystalline silicon |
| CN110257909A (en) * | 2019-07-16 | 2019-09-20 | 河北工业大学 | A kind of chemical vapour deposition technique prepares the method and device thereof of polycrystalline silicon target |
| CN110436467B (en) * | 2019-08-16 | 2024-03-19 | 洛阳中硅高科技有限公司 | Feeding system of polysilicon reduction furnace |
| CN111410197B (en) * | 2020-04-17 | 2021-05-28 | 华东交通大学 | Method for producing polyhedral silicon crystal |
| CN113371717B (en) * | 2021-06-10 | 2022-12-27 | 青海亚洲硅业半导体有限公司 | Method for preparing polysilicon by sectional control |
| CN113708665B (en) * | 2021-06-16 | 2024-01-02 | 大力电工襄阳股份有限公司 | TCS (train control system) falling and supplementing solid state soft start device control method and system |
| CN114014322A (en) * | 2021-11-30 | 2022-02-08 | 江苏鑫华半导体材料科技有限公司 | Method for improving purity of polycrystalline silicon |
| CN114212794B (en) * | 2021-12-30 | 2023-03-28 | 新疆大全新能源股份有限公司 | Production method of primary polycrystalline silicon rod for preparing electronic grade square silicon core |
| CN115092931B (en) * | 2022-06-29 | 2023-10-27 | 新特能源股份有限公司 | Control method and control system for producing polycrystalline silicon |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1250491A (en) * | 1997-03-13 | 2000-04-12 | 韩国化学研究所 | Process for preparing polysilicon using exothermic reaction |
| CN102020277A (en) * | 2010-12-24 | 2011-04-20 | 中科协鑫（苏州）工业研究院有限公司 | Method for depositing polycrystalline silicon by adopting surface microstructure silicon core |
-
2011
- 2011-12-31 CN CN201110457997.XA patent/CN102557038B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1250491A (en) * | 1997-03-13 | 2000-04-12 | 韩国化学研究所 | Process for preparing polysilicon using exothermic reaction |
| CN102020277A (en) * | 2010-12-24 | 2011-04-20 | 中科协鑫（苏州）工业研究院有限公司 | Method for depositing polycrystalline silicon by adopting surface microstructure silicon core |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102557038A (en) | 2012-07-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102557038B (en) | Preparation method of polycrystalline silicon | |
| CN103058195B (en) | Method for increasing efficiency of reductive deposition reaction for polycrystalline silicon production | |
| CN102874814B (en) | Polycrystalline-silicon reducing and producing process and device | |
| CN101724895B (en) | Production process of polycrystalline silicon | |
| CN102502646B (en) | Equipment and method for preparing polysilicon by fast circulating fluidized bed-based chemical vapor deposition | |
| CN102107873B (en) | New multicrystal silicon reduction production technology | |
| CN102001661B (en) | Method for slagging, boron removal and purification of metalluragical silicon | |
| CN101531367B (en) | Process for producing silicane | |
| CN201473329U (en) | Polysilicon reducing furnace | |
| CN102275929A (en) | Method for improving purity of metallurgical silicon and apparatus for realizing method | |
| KR101395249B1 (en) | Method for producing polycrystalline silicon | |
| CN103449442B (en) | System for preparing polysilicon granules in fluidized bed and process for preparing polysilicon by using same | |
| CN107074561B (en) | Use the poly plant and method of high-efficiency hybrid horizontal reactor | |
| CN101723370B (en) | Polysilicon production method without silicon tetrachloride emission | |
| JP5823058B2 (en) | Method for manufacturing polysilicon | |
| CN114180580A (en) | Method and reaction system for continuously producing disilane | |
| CN208454506U (en) | A kind of monosilane thermal decomposition furnace of truncated cone-shaped cooling jacket | |
| JPH0694365B2 (en) | Silicon manufacturing method and manufacturing apparatus | |
| CN102020277B (en) | Method for depositing polycrystalline silicon by adopting surface microstructure silicon core | |
| CN103626184B (en) | A kind of preparation method of high-purity liquid polysilicon | |
| JPH02279513A (en) | Production of high-purity polycrystal silicon | |
| CN108394904A (en) | A kind of monosilane thermal decomposition furnace of truncated cone-shaped cooling jacket | |
| CN103998657B (en) | The method manufacturing polysilicon | |
| CN102321916B (en) | Polysilicon production method and apparatus thereof | |
| CN101787565A (en) | Polycrystalline germanium-alloyed silicon and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170802 Address after: 831800 the Xinjiang Uygur Autonomous Region Hui Autonomous Prefecture of Changji economic and Technological Development Zone East Red Sand Springs North Industrial Zone, four Cross Road East Patentee after: Xinjiang GCL new energy Mstar Technology Ltd Address before: 66 No. 221004 Jiangsu city in Xuzhou province Xin Road Economic Development Zone Patentee before: Jiangsu Zhongneng Polysilicon Technology Development Co., Ltd. |
|
| TR01 | Transfer of patent right |