CN102642834B - Method adopting trichlorosilane and dichlorosilane mixed raw materials to produce polycrystalline silicon - Google Patents
Method adopting trichlorosilane and dichlorosilane mixed raw materials to produce polycrystalline silicon Download PDFInfo
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Abstract
The invention discloses a method adopting trichlorosilane and dichlorosilane mixed raw materials to produce polycrystalline silicon. After trichlorosilane produced by hydrogenation of silicon tetrachloride or purchased outside is rectified and purified, the rectified and purified trichlorosilane is mixed with recycled trichlorosilane and dichlorosilane mixed materials, the volume percent of dichlorosilane in the mixed raw materials is controlled to be between 3% and 15%, preferably between 5% and 10%, then impurity removal by adsorption and vaporization operation are performed, vaporized chlorosilane mixed gas and high-purity hydrogen are mixed according to mole ratio of 1:2 to 1:10, preferably 1:4 to 1:6, and finally the vaporized chlorosilane mixed gas and the high-purity hydrogen enter into a reduction furnace to produce the polycrystalline silicon. After reactions, tail gas undergoes low-temperature condensation recycle, chlorosilane obtained by recycle is sent to a rectification process to perform separation of silicon tetrachloride and impurities, and the trichlorosilane and dichlorosilane mixed raw materials are obtained. The method makes full use of byproduct dichlorosilane in the polycrystalline silicon production process to improve sedimentation velocity of silicon and reduce power consumption and material consumption, simultaneously can reduce treatment cost and loss of silicon, and improves trichlorosilane utilization rate.
Description
Technical field
The present invention relates to polysilicon, be specifically related to a kind of method for preparing polysilicon.
Background technology
Along with the development of world economy, the demand of the energy is in continuous increase, and traditional fossil energy soon exhausts, and seeks the main themes that a kind of low-carbon (LC), cleaning, reproducible new forms of energy have become the world economy development.The plurality of advantages such as that the photovoltaic energy has is renewable, cleaning, low-carbon (LC), in the world energy sources evolution in future, photovoltaic solar will become the first-selection of countries in the world energy sources, therefore the photovoltaic industry is all being greatly developed at present in countries in the world, to reduce the dependency to traditional fossil energy.Solar-grade polysilicon is the most basic material of solar energy power generating.
At present domestic and international most production of polysilicon enterprise all adopts trichlorosilane and hydrogen hybrid reaction to produce solar-grade polysilicon, and recovery is condensed for unreacted trichlorosilane and other side reaction product (mainly being silicon tetrachloride and dichloro-dihydro silicon).The silicon tetrachloride that reclaims is as the raw material of producing gas-phase silica and production trichlorosilane.But it is individual relatively hard problem that the dichloro-dihydro silicon that reclaims is processed, usually the method that adopts is to be blended in silicon tetrachloride to carry out disproportionation reaction under the effect of catalyzer and make the trichlorosilane raw material, but adding catalyzer, the method can introduce impurity, the restriction that simultaneously facility investment height, the difficult control of technique, transformation efficiency be not high, be unfavorable for problems such as keeping the safety in production.Seek a kind of method that can effectively process dichloro-dihydro silicon and become the task of top priority that current production of polysilicon enterprise further expands the scale of production.
In actual production process, trichlorosilane mixes with hydrogen when producing polysilicon, owing to reasons such as temperature of reaction are high, side reaction is many, is unfavorable for the fast deposition of silicon, causes reduction power consumption and supplies consumption higher, and production cost is had certain impact.Fast development along with the polysilicon industry, the maximization of polycrystalline silicon producing device, the dichloro-dihydro silicon of by-product is more and more in the production process, can improve sedimentation velocity and guarantee quality product so the needs searching is a kind of, can effectively process again the novel method of dichloro-dihydro silicon, reduce enterprise's production cost with this, reduce the environmental pollution that causes when processing dichloro-dihydro silicon.
Summary of the invention
The invention provides a kind of method that adopts dichloro-dihydro silicon and trichlorosilane mixing raw material to produce polysilicon, can effectively solve the difficult problem of by-product dichloro-dihydro silicon processing in the polysilicon production process.Because the existence of dichloro-dihydro silicon is arranged in raw materials for production, can suitably reduce reduction temperature, improve the sedimentation velocity of polysilicon in reduction furnace, thereby reduce reduction power consumption and the raw material consumption of polysilicon, solved the technical problem that exists in the prior art.
For realizing above-mentioned Technology target, the present invention by the following technical solutions:
A kind of method that adopts trichlorosilane and dichloro-dihydro silicon mixing raw material to produce polysilicon may further comprise the steps:
Step 1 is carried out rectification and purification with trichlorosilane in rectifying tower, obtain purity greater than 99.995% trichlorosilane raw material;
Step 2 reclaims the trichlorosilane that obtains with resulting trichlorosilane raw material in the step 1 and the rectifying of aftermentioned step 6 and the mixing raw material of dichloro-dihydro silicon mixes, and the volumn concentration of dichloro-dihydro silicon was within the scope of regulation after the control raw material mixed;
Step 3, the resulting trichlorosilane of step 2 and dichloro-dihydro silicon mixing raw material are delivered to vaporizer vaporizes, obtaining gas phase trichlorosilane and dichloro-dihydro silicon mixing raw material, is that 99.999% to 99.9999% high-purity hydrogen mol ratio according to the rules is mixed to get mixing raw material gas in mixing tank with purity again;
Step 4 enters reduction furnace with resulting mixing raw material pneumatic transmission in the step 3, and temperature is controlled at about 1020 ℃ to 1120 ℃ in the reduction furnace, and pressure is at 0.15MPa to 0.40MPa; Mixture material gas carries out the gas chemistry precipitin reaction and generates polysilicon in reduction furnace, generate simultaneously hydrogenchloride; Also can generate the side reaction of dichloro-dihydro silicon and silicon tetrachloride in the reduction furnace, reaction after finishing all gas-phase product and by product in company with unreacted completely material enter the vent gas treatment operation;
Step 5 is delivered to the tail gas recycle operation with the tail gas that produces in the step 4, the chlorosilane in the tail gas is carried out cryogenic condensation reclaim, and condensation is reclaimed and obtained the chlorosilane compound, wherein mainly comprises dichloro-dihydro silicon, trichlorosilane, silicon tetrachloride and other trace impurities;
Step 6, condensation recovery in the step 5 is obtained the chlorosilane compound carry out rectification and purification, through after the rectifying separation, silicon tetrachloride is wherein isolated and reclaimed for the production of trichlorosilane, trichlorosilane then need not separate with dichloro-dihydro silicon, forms the mixing raw material of trichlorosilane and dichloro-dihydro silicon;
Step 7, repeating step 2-step 6 to realize the recycle of polysilicon material, thoroughly solves the processing problem of dichloro-dihydro silicon.
Further be:
Described step 1 specifically may further comprise the steps:
Step 1-1 carries out preliminary rectification and purification with purity 〉=98% trichlorosilane in No. 1 rectifying tower of 0.20MPa to 0.40MPa operational condition, remove high boiling material;
Step 1-2 will deliver in No. 2 rectifying tower of 0.15MPa to 0.40MPa operational condition further rectification and purification through the trichlorosilane material that the preliminary rectification and purification of step 1-1 obtains, and remove low-boiling-point substance and trace impurity thereof;
Step 1-3 will deliver in No. 3 rectifying tower of 0.20MPa to 0.45MPa operational condition further rectification and purification through the trichlorosilane of step 1-2 rectification and purification, obtain qualified trichlorosilane raw material.
In the described step 6, have two groups of towers to be used for that the chlorosilane compound that obtains is reclaimed in step 5 condensation and carry out rectification and purification, wherein No. 4 Tata stills are isolated silicon tetrachloride, and cat head distillates into No. 5 towers; No. 5 column overhead extraction trichlorosilanes and dichloro-dihydro silicon mixing raw material, as the production of polysilicon raw material, the tower reactor high boiling material returns No. 1 tower and reclaims.
Mix with the trichlorosilane raw material that replenishes through the mixture that obtains trichlorosilane and dichloro-dihydro silicon after the rectification and purification in the described step 2, the volume percent of control dichloro-dihydro silicon in mixing raw material is between 3% to 15%
Mix with the trichlorosilane raw material that replenishes through the mixture that obtains trichlorosilane and dichloro-dihydro silicon after the rectification and purification in the step 2, the volume percent of control dichloro-dihydro silicon in mixing raw material is between 5% to 10%;
Also comprise the resin absorption step between described step 2 and the step 3, utilize resin to the peculiar absorption property of impurity, remove the detrimental impurity such as B, P micro-in trichlorosilane and the dichloro-dihydro silicon mixing raw material and C, guarantee quality product.Wherein B, P, C represent respectively chemical element boron, phosphorus, carbon.
Vaporizer need to be controlled temperature, and actual temp is controlled at 38 ℃ to 75 ℃, adjusts according to the production phase that reduction furnace is different;
Gas phase trichlorosilane and dichloro-dihydro silicon mixing raw material and purity are that 99.999% to 99.9999% high-purity hydrogen mixes in mixing tank by the mol ratio of 1:2 to 1:10 in the described step 3.
Gas phase trichlorosilane and dichloro-dihydro silicon mixing raw material and purity are that 99.999% to 99.9999% high-purity hydrogen mixes in mixing tank by the mol ratio of 1:4 to 1:6 in the described step 3.
The described material mixed gas that enters reduction furnace, all be that a plurality of feed entrances from reduction furnace bottom enter in the reduction furnace, and described reduction furnace temperature control is to use infrared thermometer to monitor, and finish by the electric current on the silicon core carrier in the adjustment reduction furnace.
Compared with prior art, the invention has the beneficial effects as follows:
1, utilization of the present invention be trichlorosilane and dichloro-dihydro silicon mixing raw material as the production of polysilicon raw material, can effectively solve in the production of polysilicon technique by product dichloro-dihydro silicon and process difficult problem.New production process of the present invention is that dichloro-dihydro silicon, trichlorosilane, silicon tetrachloride in the reduction tail gas are condensed in the lump liquid and reclaim, then purify by the continuous rectification of two towers, isolate silicon tetrachloride, the material that obtains at last is the mixture of trichlorosilane and dichloro-dihydro silicon, do not need to increase rectifying tower trichlorosilane and dichloro-dihydro silicon are carried out separating-purifying, reduced the input of cost of equipment.
2, after trichlorosilane, dichloro-dihydro silicon enter reduction furnace with the gas mixture of hydrogen, at a certain temperature trichlorosilane reaction generates silicon, hydrogenchloride, hydrogen, silicon tetrachloride and dichloro-dihydro silicon, the dichloro-dihydro pasc reaction generates silicon and hydrogenchloride, and dichloro-dihydro silicon reaches a running balance in reduction furnace.Can reduce the trichlorosilane consumption that generates dichloro-dihydro silicon in the reaction process so in the reduction material mixed gas, add a certain amount of dichloro-dihydro silicon.
3, dichloro-dihydro silicon enters systemic circulation and uses the waste that can reduce element silicon, reduce simultaneously the investment cost of processing the dichloro the second light industry bureau, increase the economic benefit of enterprise, particularly in the large polycrystalline silicon production equipment, dichloro-dihydro silicon treatment capacity is larger, and its benefit is more obvious.
4, mixing raw material needs by the resin absorption device before vaporizing, and removes micro-B, P, C impurity, guarantees the quality of polysilicon product.The gas mixture raw material enters the mode of reduction furnace by original a bit concentrated charging, changes furnace bottom multiple feed mode into, has solved the even distribution problem of gas mixture, is conducive to improve the sedimentation velocity of silicon.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing implementation step of the present invention is further set forth.
Flow process of the present invention is roughly such as Fig. 1.May further comprise the steps:
Step 1 is carried out rectification and purification with the trichlorosilane raw material that replenishes in rectifying tower, obtain purity greater than 99.995% trichlorosilane raw material; In this step, the trichlorosilane raw material adopts the silicon tetrachloride of outsourcing or recovery to make by cold hydrogenation, and additional trichlorosilane material purity does not reach the index request into reduction furnace, carries out continuous rectification and purification so three groups of rectifying tower need to be set.Specifically need through following steps: the additional trichlorosilane with initial purity 〉=98% carries out preliminary rectification and purification in the rectifying tower of 0.20MPa to 0.40MPa operational condition first, removes high boiling material; To deliver in the rectifying tower of 0.15MPa to 0.40MPa operational condition further rectification and purification through the trichlorosilane of preliminary rectification and purification again, remove low-boiling-point substance and trace impurity thereof; To deliver in the rectifying tower of 0.20MPa to 0.45MPa operational condition further rectification and purification through the trichlorosilane of above-mentioned steps rectification and purification at last, obtain qualified trichlorosilane raw material.Qualified trichlorosilane raw material is returned former operation raw material storage tank.
Step 2, the trichlorosilane that obtains is reclaimed in resulting trichlorosilane raw material in the step 1 and the rectifying of aftermentioned step 6 to be mixed with dichloro-dihydro silicon mixing raw material, the volume percent (preferred 5% to 10%) between 3% to 15% of dichloro-dihydro silicon after the control raw material mixes, if the per-cent of dichloro-dihydro silicon is too high, be unfavorable for the safety control of production process.Mixed raw material is passed into the resin absorption device, the detrimental impurity such as B, the P in the removal mixing raw material and C, the quality of assurance polysilicon product.
Step 3 is delivered to vaporizer with the mixing raw material in the step 2 and is vaporized, and is that 99.999% to 99.9999% high-purity hydrogen mixes (preferred 1:4 to 1:6) according to the mol ratio of 1:2 to 1:10 in mixing tank with purity then;
Step 4 is sent resulting material mixed gas in the step 3 into reduction furnace, controls by the electric current of regulating silicon core carrier in the reduction furnace that temperature is between 1020 ℃ to 1120 ℃ in the reduction furnace, and furnace pressure is controlled at 0.15MPa to 0.40MPa; Material mixed gas carries out the polysilicon deposition of gas chemistry precipitin reaction generation on silicon core carrier in reduction furnace, generate simultaneously hydrogenchloride; Also can generate the side reaction of dichloro-dihydro silicon and silicon tetrachloride in the reduction furnace, reaction after finishing all gas-phase product and by product in company with unreacted completely material enter the vent gas treatment operation;
Step 5, the tail gas that produces in the step 4 is carried out cryogenic condensation to be reclaimed, condensation is reclaimed the chlorosilane mixture that obtains and is carried out the rectification and purification separation, mainly comprise dichloro-dihydro silicon, trichlorosilane, silicon tetrachloride and other trace impurities in the chlorosilane mixture, after rectification and purification is removed silicon tetrachloride and trace impurity, obtain the mixture of trichlorosilane and dichloro-dihydro silicon as the production of polysilicon raw material;
In the step 6, chlorosilane rectifying is reclaimed needs two groups of rectifying tower to carry out the continuous rectification separation specifically, and wherein first group of Tata still isolated silicon tetrachloride and trace metal impurities; Second group of column overhead distillates qualified trichlorosilane and dichloro-dihydro silicon mixed solution as the raw material of production of polysilicon, and tower reactor discharging high boiling material enters tower circulation rectification and purification No. 1.
Repeating step 2-step 6 is to realize producing the cyclic production utilization of polycrystalline silicon raw material.
In said process, material mixed gas enters in the reduction furnace from the reduction furnace bottom, uses infrared thermometer to measure reduction furnace silicon core temperature, and the electric current of adjusting on the silicon core carrier is controlled the interior temperature of reduction furnace between 1020 ℃ to 1120 ℃.According to the difference in growth time stage in the reduction furnace, adjust hydrogen and the mole proportioning of mixed chlorosilane and the inlet amount of material mixed gas, guarantee the high sedimentation velocity of silicon in the stove.Reduction furnace bottom feed mouth adopts the mode of multiple feed, avoids causing the material mixed gas skewness in the stove because a large amount of material mixed gas is concentrated to be entered in the stove, affects the sedimentation velocity of silicon and increases the side reaction odds.
Trichlorosilane above-mentioned hydrogenation of silicon tetrachloride production or outsourcing adopts three tower continuous rectifications; And the chlorosilane mixture of reduction tail gas recycle adopts two tower continuous rectification techniques.Hydrogenation of silicon tetrachloride trichlorosilane that produce or outsourcing is through the purity after the rectification and purification 〉=99.995%, the trichlorosilane that reclaims and the purity of dichloro-dihydro silicon mixture 〉=99.99%, B after the rectifying in the raw material, P and metallic impurity total amount are lower than 50ppm, behind the resin absorption device, its total impurities content is lower than 5ppm.The high-purity hydrogen dew point of production and application≤-55 ℃, purity 〉=99.9995%.Overall inlet amount increases over time, guarantees that the silicon rod surface in the stove has enough material mixed gas to react, and increases polysilicon deposition speed with this, improves the reduction furnace production intensity, reduces simultaneously the reduction power consumption.
Claims (7)
1. method that adopts trichlorosilane and dichloro-dihydro silicon mixing raw material to produce polysilicon is characterized in that: may further comprise the steps:
Step 1 is carried out rectification and purification with trichlorosilane in rectifying tower, obtain purity greater than 99.995% trichlorosilane raw material; Specifically may further comprise the steps:
Step 1-1 carries out preliminary rectification and purification more than or equal to 98% trichlorosilane with purity in No. 1 rectifying tower of 0.20MPa to 0.40MPa operational condition, remove high boiling material;
Step 1-2 will deliver in No. 2 rectifying tower of 0.15MPa to 0.40MPa operational condition further rectification and purification through the trichlorosilane material that the preliminary rectification and purification of step 1-1 obtains, and remove low-boiling-point substance and trace impurity thereof;
Step 1-3 will deliver in No. 3 rectifying tower of 0.20MPa to 0.45MPa operational condition further rectification and purification through the trichlorosilane of step 1-2 rectification and purification, obtain qualified trichlorosilane raw material;
Step 2 reclaims the trichlorosilane that obtains with resulting trichlorosilane raw material in the step 1 and the rectifying of aftermentioned step 6 and the mixing raw material of dichloro-dihydro silicon mixes, and the volumn concentration of dichloro-dihydro silicon was between 3% to 15% after the control raw material mixed;
Step 3, the resulting trichlorosilane of step 2 and dichloro-dihydro silicon mixing raw material are delivered to vaporizer vaporizes, obtaining gas phase trichlorosilane and dichloro-dihydro silicon mixing raw material, is that 99.999% to 99.9999% high-purity hydrogen is mixed to get mixing raw material gas by the mol ratio by 1:2 to 1:10 in mixing tank with purity again; Vaporizer need to be controlled temperature, and actual temp is controlled at 38 ℃ to 75 ℃, adjusts according to the production phase that reduction furnace is different;
Step 4 enters reduction furnace with resulting mixing raw material pneumatic transmission in the step 3, and temperature is controlled at about 1020 ℃ to 1120 ℃ in the reduction furnace, and pressure is at 0.15MPa to 0.40MPa; Mixture material gas carries out the gas chemistry precipitin reaction and generates polysilicon in reduction furnace, generate simultaneously hydrogenchloride; Also can generate the side reaction of dichloro-dihydro silicon and silicon tetrachloride in the reduction furnace, reaction after finishing all gas-phase product and by product in company with unreacted completely material enter the vent gas treatment operation;
Step 5 is delivered to the tail gas recycle operation with the tail gas that produces in the step 4, the chlorosilane in the tail gas is carried out cryogenic condensation reclaim, and condensation is reclaimed and obtained the chlorosilane compound, wherein mainly comprises dichloro-dihydro silicon, trichlorosilane, silicon tetrachloride and other trace impurities;
Step 6 obtains the chlorosilane compound with condensation recovery in the step 5 and carries out rectification and purification, through after the rectifying separation, silicon tetrachloride is wherein isolated, and trichlorosilane then need not separate with dichloro-dihydro silicon, forms the mixing raw material of trichlorosilane and dichloro-dihydro silicon;
Step 7, repeating step 2-step 6 to realize the recycle of polysilicon material, thoroughly solves the processing problem of dichloro-dihydro silicon.
2. employing trichlorosilane as claimed in claim 1 and dichloro-dihydro silicon mixing raw material are produced the method for polysilicon, it is characterized in that: in the described step 6, there are two groups of towers to be used for that the chlorosilane compound that obtains is reclaimed in step 5 condensation and carry out rectification and purification, wherein No. 4 Tata stills are isolated silicon tetrachloride, and cat head distillates into No. 5 towers; No. 5 column overhead extraction trichlorosilanes and dichloro-dihydro silicon mixing raw material, as the production of polysilicon raw material, the tower reactor high boiling material returns No. 1 tower and reclaims.
3. employing trichlorosilane as claimed in claim 1 and dichloro-dihydro silicon mixing raw material are produced the method for polysilicon, it is characterized in that: mix with the trichlorosilane raw material that replenishes through the mixture that obtains trichlorosilane and dichloro-dihydro silicon after the rectification and purification in the described step 2, the volume percent of control dichloro-dihydro silicon in mixing raw material is between 5% to 10%.
4. employing trichlorosilane as claimed in claim 1 and dichloro-dihydro silicon mixing raw material are produced the method for polysilicon, it is characterized in that: also comprise the resin absorption step between described step 2 and the step 3, utilize resin to the peculiar absorption property of impurity, remove B, P and the C detrimental impurity of trace in trichlorosilane and the dichloro-dihydro silicon mixing raw material.
5. employing trichlorosilane as claimed in claim 1 and dichloro-dihydro silicon mixing raw material are produced the method for polysilicon, and it is characterized in that: the carburettor temperature in the described step 3 is controlled between 38 ℃ to 75 ℃.
6. employing trichlorosilane as claimed in claim 1 and dichloro-dihydro silicon mixing raw material are produced the method for polysilicon, it is characterized in that: gas phase trichlorosilane and dichloro-dihydro silicon mixing raw material and purity are that 99.999% to 99.9999% high-purity hydrogen mixes in mixing tank by the mol ratio of 1:4 to 1:6 in the described step 3.
7. such as the described method that any adopts trichlorosilane and dichloro-dihydro silicon mixing raw material to produce polysilicon of claim 1-6, it is characterized in that: the described material mixed gas that enters reduction furnace, all be that a plurality of feed entrances from reduction furnace bottom enter in the reduction furnace, and described reduction furnace temperature control is to use infrared thermometer to monitor, and finish by the electric current on the silicon core carrier in the adjustment reduction furnace.
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| CN102786056B (en) * | 2012-09-03 | 2014-02-12 | 内蒙古盾安光伏科技有限公司 | Device and method for polycrystalline reduction production |
| CN103058195B (en) * | 2013-01-22 | 2014-10-22 | 华陆工程科技有限责任公司 | Method for increasing efficiency of reductive deposition reaction for polycrystalline silicon production |
| CN103058140B (en) * | 2013-01-23 | 2015-03-18 | 内蒙古盾安光伏科技有限公司 | Recovery system and recovery method of by-product in polycrystalline silicon production |
| CN103408018A (en) * | 2013-07-10 | 2013-11-27 | 中国恩菲工程技术有限公司 | Method for preparing mixed gas feed for reduction production of polycrystalline silicon |
| CN103408019A (en) * | 2013-07-10 | 2013-11-27 | 中国恩菲工程技术有限公司 | Device for preparing mixed gas feed used for reduction production of polycrystalline silicon |
| CN103950933B (en) * | 2014-03-31 | 2016-08-17 | 中国恩菲工程技术有限公司 | The method preparing polysilicon |
| CN105293501B (en) * | 2014-06-10 | 2017-09-15 | 新特能源股份有限公司 | A kind of polycrystalline silicon production system and method |
| CN104556054B (en) * | 2015-01-19 | 2017-03-29 | 新疆大全新能源有限公司 | The recoverying and utilizing method and device of light component in trichlorosilane synthesis material |
| TW201718922A (en) * | 2015-08-24 | 2017-06-01 | 漢洛克半導體公司 | Dichlorosilane compensating control strategy for improved polycrystalline silicon growth |
| CN107720755A (en) * | 2017-11-02 | 2018-02-23 | 成都蜀菱科技发展有限公司 | A kind of production of polysilicon raw material and method for preparing polysilicon |
| CN108862281A (en) * | 2018-07-17 | 2018-11-23 | 亚洲硅业（青海）有限公司 | A kind of combine production method of rod-like polycrystal silicon and granular polycrystalline silicon |
| CN108840340A (en) * | 2018-09-14 | 2018-11-20 | 四川永祥多晶硅有限公司 | A kind of preparation method of polysilicon |
| CN109319787B (en) * | 2018-11-02 | 2021-12-21 | 中国南玻集团股份有限公司 | Reduction device and process for efficiently producing polycrystalline silicon |
| CN109607547B (en) * | 2018-11-21 | 2019-12-10 | 亚洲硅业（青海）有限公司 | Method for preparing high-purity chlorosilane |
| CN109448800B (en) * | 2018-12-24 | 2022-12-06 | 内蒙古神舟硅业有限责任公司 | Method for judging mass gliding time of refined trichlorosilane |
| CN114180578B (en) * | 2022-02-16 | 2022-05-17 | 中国恩菲工程技术有限公司 | Production process and production system for ultra-pure polycrystalline silicon and silicon derivatives |
| CN115092934A (en) * | 2022-06-21 | 2022-09-23 | 云南通威高纯晶硅有限公司 | Method and system for controlling content of dichlorosilane in refined trichlorosilane |
| CN115445231B (en) * | 2022-10-09 | 2023-06-16 | 新特能源股份有限公司 | On-line monitoring and adjusting system, method and device for rectifying tower product |
| CN116495741B (en) * | 2023-05-31 | 2024-06-18 | 宁夏润阳硅材料科技有限公司 | Method and system for recycling polysilicon production associated disilicide raw materials |
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| JP5040717B2 (en) * | 2007-03-19 | 2012-10-03 | Ｊｎｃ株式会社 | Manufacturing method of high purity silicon |
| CN101486465B (en) * | 2009-01-09 | 2011-06-01 | 北京先锋创新科技发展有限公司 | Production method of refined trichlorosilane |
| CN102058992B (en) * | 2010-11-13 | 2013-02-13 | 天津大学 | Clapboard adsorption device and method for removing boron impurities in chlorosilane system |
| CN102009978B (en) * | 2011-01-06 | 2012-09-12 | 四川永祥多晶硅有限公司 | Polysilicon production method |
| CN202072477U (en) * | 2011-03-08 | 2011-12-14 | 内蒙古盾安光伏科技有限公司 | Polycrystalline silicon production system |
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