CN102502647B - Polycrystalline silicon reduction system and feeding mode of reducing gas raw materials thereof - Google Patents
Polycrystalline silicon reduction system and feeding mode of reducing gas raw materials thereof Download PDFInfo
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- CN102502647B CN102502647B CN 201110335075 CN201110335075A CN102502647B CN 102502647 B CN102502647 B CN 102502647B CN 201110335075 CN201110335075 CN 201110335075 CN 201110335075 A CN201110335075 A CN 201110335075A CN 102502647 B CN102502647 B CN 102502647B
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Abstract
Provided are a polycrystalline silicon reduction system and a feeding mode of reducing gas raw materials thereof. The polycrystalline silicon reduction system comprises a bubbling vaporizer, a hydrogen heater, a plurality of static mixers connected with the bubbling vaporizer and the hydrogen heater and a plurality of polycrystalline silicon reduction furnaces respectively connected with corresponding static mixers. The polycrystalline silicon reduction system uses hydrogen to bubble in trichlorosilane liquid, simultaneously the trichlorosilane liquid is heated by an external heat source to enable trichlorosilane to be vaporized, and the mixed gas of trichlorosilane and hydrogen is finally obtained through hydrogen bubbling so that evaporation of trichlorosilane is speeded up. By controlling pressure and temperature of the bubbling vaporizer, the vented gas of the mixed gas of the bubbling vaporizer is controlled to be in a low proportion, after being heated through the hydrogen heater, bypass hydrogen is fully mixed with the vented gas of the mixed gas of the bubbling vaporizer in the static mixers to a high preset proportion, and then the mixture directly enters the corresponding reduction furnaces.
Description
Technical field
The present invention relates in general to polycrystalline silicon reduction system.Specifically, the feeding manner or the supplying method that relate to the reducing gas raw material in polycrystalline silicon reduction system.
Background technology
Polysilicon is important raw semiconductor, and the main flow technique of its production at present is improved Siemens.The polysilicon reduction is an important production link of improved Siemens, and its raw material is trichlorosilane and hydrogen.The output mode of polysilicon is for depositing on original silicon rod surface, and along with the carrying out of reaction, more at the silicon rod surface deposition, the diameter of silicon rod is larger, and the consumption of trichlorosilane and hydrogen also increases with the increase of diameter.Therefore, in whole polysilicon deposition process, the variation of trichlorosilane gas and hydrogen gas amount is very large.Because trichlorosilane and hydrogen gas amount directly affect the speed that polysilicon deposits on silicon rod, therefore need to control flexibly air input both.Simultaneously, in mixture of feed, the mol ratio of trichlorosilane and hydrogen also can affect sedimentation rate, therefore, how to control trichlorosilane gas and hydrogen gas amount, and the mol ratio of two kinds of gases becomes the important step that affects the polysilicon reduction.In addition, to exist with liquid state under important source material trichlorosilane normal temperature and pressure due to the polysilicon reduction, trichlorosilane through rectification and purification is also to enter polysilicon reduction operation with liquid state, so, select a kind of suitable trichlorosilane vaporizing liquid mode to become one of key of polysilicon reduction.
The polycrystalline silicon reduction system feeding manner mainly contains three kinds of modes at present, is respectively bubbling style vaporization, shell and tube vaporization and the vaporization of Liebig tubular type.
Bubbling style vaporization mode is to utilize hydrogen bubbling in the trichlorosilane liquid phase, and external heat source heat supply simultaneously makes the trichlorosilane vaporization, accelerates the evaporation of trichlorosilane by the bubbling of hydrogen, obtains the gas mixture of hydrogen and trichlorosilane.Fig. 1 is seen in the technical process of bubbling style vaporization mode.The advantage of this mode is: owing to adding hydrogen, make trichlorosilane become the required heat of gas phase and greatly reduce, if use steam heating, the pressure quality requirements to steam is not high, and general 0.2Mpa gets final product; In course of conveying, the trichlorosilicane in mixing can not liquefy simultaneously, has guaranteed the stable of subsequent production technique.Shortcoming: the bubbling style vaporizer contains two kinds of material compositions, for determining its proportioning, need to control respectively two parameters of temperature and pressure.Because of its follow-up production technique, mixed gases matching is had relatively high expectations again, need constantly to change in different growth period proportionings, vaporizing with this mode is unfavorable for the frequent adjusting of proportioning; Because a bubbling style vaporizer is many reduction furnace feed simultaneously, if wherein one or more reduction furnace need to change its proportioning, can have influence on other reduction furnace, be unfavorable for that the production of whole system is stable; And the air inlet of every reduction furnace can only be surveyed mixed gas flow, and temperature and pressure slightly has fluctuation, and component forms and will change.
The shell and tube vaporization is with the externally lower direct boiling of thermal source heating of liquid phase trichlorosilane.Control the pressure of the rear saturated gas of vaporization, fully mix with hydrogen with certain flow, form gas mixture, referring to Fig. 2.The advantage of this mode is that in production process, its component proportion adjusting is very easy.Shortcoming: need amount of heat to make the liquid trichlorosilane become gaseous state, if use steam heating, the pressure quality requirements to steam is higher, generally needs the 0.6Mpa can; And be easy to again liquefaction in course of conveying.
Liebig tubular type vaporization is after trichlorosilane liquid and hydrogen are controlled by Flow-rate adjustment, to enter a kind of mixing tank, then enters Liebig and manages, and utilizes thermal source to provide heat to make the trichlorosilane vaporizing liquid, referring to Fig. 3.The advantage of this mode is that its component proportion adjusting is very easy in process of production.But can not guarantee that liquid trichlorosilane is vaporized fully.
Summary of the invention
The purpose of this invention is to provide a kind of production of polysilicon reduction feeding manner that can control flexibly the charging proportioning and the trichlorosilane in charging can be vaporized fully.
According to an aspect of the present invention, provide a kind of and directly provide respectively the method for polysilicon reducing gas raw material at least two polycrystalline silicon reducing furnaces.The method comprises:
Utilize hydrogen bubbling and carry out simultaneously indirect heating to make the trichlorosilane vaporizing liquid and obtain the mol ratio of hydrogen and trichlorosilane and be the mixed gas of fixed value in trichlorosilane liquid;
Described mixed gas is divided into first via mixed gas and the second road mixed gas;
Hydrogen is provided in addition and be heated after be divided into the first via and add hot hydrogen and the second tunnel and add hot hydrogen;
After being added the polysilicon reducing gas raw material that mol ratio that hot hydrogen and first via mixed gas be mixed to get hydrogen and trichlorosilane is the first preset value, the first via directly passes into the first polycrystalline silicon reducing furnace; And
Directly pass into the second polycrystalline silicon reducing furnace after adding with the second the tunnel polysilicon reducing gas raw material that mol ratio that hot hydrogen and the second road mixed gas be mixed to get hydrogen and trichlorosilane is the second preset value;
Wherein said fixed value is less than described the first preset value and described the second preset value.
In the method for the invention, the first preset value and the second preset value are usually all between 3.5: 1 to 4.5: 1.Preferred fixed value is 3: 1.
In the method for the invention, the first preset value and the second preset value can equate also can not wait.
The mol ratio that in the method for the invention, can obtain by the temperature and pressure of controlling mixed gas hydrogen and trichlorosilane is the mixed gas of fixed value.
The mol ratio that the flow that in the method for the invention, can add by controlling respectively the first via flow of hot hydrogen and first via mixed gas obtains hydrogen and trichlorosilane is the polysilicon reducing gas raw material of the first preset value; And the mol ratio that can obtain by controlling respectively the second tunnel flow that adds the flow of hot hydrogen and the second road mixed gas hydrogen and trichlorosilane is the polysilicon reducing gas raw material of the second preset value.
According to another aspect of the present invention, provide a kind of polycrystalline silicon reduction system.This system comprises:
The bubbling style vaporizer;
The hydrogen well heater;
A plurality of static mixers that are connected with the hydrogen well heater with the bubbling style vaporizer respectively; And
A plurality of polycrystalline silicon reducing furnaces that are connected with corresponding static mixer respectively.
Polycrystalline silicon reduction system of the present invention can also comprise the exhaust gas recovery system that all is connected with described a plurality of polycrystalline silicon reducing furnaces.
In polycrystalline silicon reduction system of the present invention, static mixer can be connected with the hydrogen well heater with the bubbling style vaporizer by corresponding flow control valve respectively.
The present invention utilizes hydrogen bubbling in trichlorosilane liquid, and external heat source heating simultaneously makes the trichlorosilane vaporization, accelerates the evaporation of trichlorosilane by the hydrogen bubbling, finally obtains the gas mixture of trichlorosilane and hydrogen.By controlling the pressure and temperature of bubbling style vaporizer, bubbling style vaporizer gas mixture is given vent to anger be controlled at a lower proportioning (mol ratio of hydrogen and trichlorosilane); Given vent to anger with bubbling style vaporizer gas mixture after by the hydrogen heater heats by dypass hydrogen again and directly enter corresponding reduction furnace be fully mixed to higher preset blending ratio in static mixer after.
Description of drawings
Fig. 1 is the schema of the production of polysilicon reduction charging of existing employing bubbling style vaporization mode.
Fig. 2 is the schema of the production of polysilicon reduction charging of existing employing shell and tube vaporization mode.
Fig. 3 is the schema of the production of polysilicon reduction charging of existing employing Liebig tubular type vaporization mode.
Fig. 4 is the schema according to production of polysilicon reduction charging of the present invention.
Embodiment
Describe the present invention in detail below in conjunction with accompanying drawing.It will be appreciated by those skilled in the art that the embodiment that describes in detail below only is used for explaining and explanation the present invention, is not for it is carried out any restriction.
Referring to Fig. 4, polycrystalline silicon reduction system of the present invention comprises: the bubbling style vaporizer; The hydrogen well heater; A plurality of static mixers (static mixer A, static mixer ...) that are connected with the hydrogen well heater with the bubbling style vaporizer respectively; And a plurality of polycrystalline silicon reducing furnaces that are connected with corresponding static mixer respectively (reduction furnace A, reduction furnace ...).Static mixer can be connected with the hydrogen well heater with the bubbling style vaporizer by corresponding flow control valve respectively.In addition, polycrystalline silicon reduction system of the present invention can also comprise the exhaust gas recovery system that all is connected with a plurality of polycrystalline silicon reducing furnaces.
Feeding manner in polycrystalline silicon reduction system of the present invention is described below.
The present invention can directly provide respectively polysilicon reducing gas raw material at least two polycrystalline silicon reducing furnaces, thereby can satisfy the different process requirement of each reduction furnace.
Refer again to Fig. 4, at first, trichlorosilane liquid enters the bubbling style vaporizer, and then pass into hydrogen in the bubbling style vaporizer, utilize hydrogen bubbling and carry out simultaneously indirect heating to make the trichlorosilane vaporizing liquid and the mol ratio that obtains hydrogen and trichlorosilane is the fixed value mixed gas of 3: 1 for example in trichlorosilane liquid.The mixed gas that can obtain having above-mentioned mol ratio by the temperature and pressure of controlling mixed gas.According to the quantity of reduction furnace, mixed gas can correspondingly be divided into the multichannel for example first via and the second road mixed gas.
Then, with (dypass) hydrogen of providing in addition by the hydrogen well heater heat rear same corresponding be divided into multichannel add hot hydrogen for example the first via and the second tunnel add hot hydrogen.
The first via is added hot hydrogen to enter (first) static mixer A after by variable valve A adjust flux and first via mixed gas is also entered static mixer A after by variable valve A adjust flux, making hydrogen in static mixer A and the mol ratio of trichlorosilane is the first preset value for example 4: 1, then will directly pass into (first) polycrystalline silicon reducing furnace A from static mixer A mixed gas feed out.
equally, adding hot hydrogen with the second the tunnel enters the second static mixer (being illustrated as static mixer ...) after by corresponding variable valve (being illustrated as variable valve ...) adjust flux and the second road mixed gas is also entered the second static mixer after by corresponding variable valve (being illustrated as variable valve ...) adjust flux, making hydrogen in the second static mixer and the mol ratio of trichlorosilane is the second preset value for example 4.5: 1, then will directly pass into the second polycrystalline silicon reducing furnace (being illustrated as reduction furnace ...) from the second static mixer mixed gas feed out.
Certainly, can directly pass into exhaust gas recovery system from each reduction furnace tail gas out.
As from the foregoing, the present invention has the following advantages:
1) because proportioning that bubbling style vaporizer gas mixture is given vent to anger has been transferred to lower value, as: 3: 1 (hydrogen is than trichlorosilane), trichlorosilane only account for wherein 25%, with the heat decrease of its vaporization, if use steam to reduce again the pressure quality of steam.
2) the bubbling style vaporizer gas mixture proportioning of giving vent to anger is modulated to low value, in follow-up workshop section, if need the higher dypass hydrogen that passes into of proportioning, evenly mixes in static mixing gas with gas mixture, readjusts to enter reduction furnace after joining.As: if the required proportioning of follow-up workshop section is 4: 1, only need to pass into 1 part of hydrogen in the dypass hydrogen pipeline, proportioning can be adjusted to 4: 1.
3) because the bubbling style vaporizer is the dual control of the temperature and pressure proportioning of giving vent to anger, guaranteed the vaporization fully of giving vent to anger.
4) because hydrogen specific heat is very large, the transfer line loses heat is minimum on the mixture temperature impact, and therefore trichlorosilane gas is not prone to liquefaction phenomenon in course of conveying, has guaranteed the stable of subsequent production technique.
5) in the present invention, bubbling style vaporizer, dypass hydrogen are all many reduction furnace feed simultaneously, can according to the condition of production of every stove, regulate at any time the required proportioning of this stove by mixture control valve, dypass hydrogen variable valve, and not affect other reduction furnaces.
Claims (10)
1. one kind at least two polycrystalline silicon reducing furnaces directly provide respectively the method for polysilicon reducing gas raw material, comprising:
Utilize hydrogen bubbling and carry out simultaneously indirect heating to make the trichlorosilane vaporizing liquid and obtain the mol ratio of hydrogen and trichlorosilane and be the mixed gas of fixed value in trichlorosilane liquid;
Described mixed gas is divided into first via mixed gas and the second road mixed gas;
Hydrogen is provided in addition and be heated after be divided into the first via and add hot hydrogen and the second tunnel and add hot hydrogen;
After being added the polysilicon reducing gas raw material that mol ratio that hot hydrogen and first via mixed gas be mixed to get hydrogen and trichlorosilane is the first preset value, the first via directly passes into the first polycrystalline silicon reducing furnace; And
Directly pass into the second polycrystalline silicon reducing furnace after adding with the second the tunnel polysilicon reducing gas raw material that mol ratio that hot hydrogen and the second road mixed gas be mixed to get hydrogen and trichlorosilane is the second preset value;
Wherein said fixed value is less than described the first preset value and described the second preset value.
2. the process of claim 1 wherein that described the first preset value and described the second preset value are all between 3.5: 1 to 4.5: 1.
3. the method for claim 2, wherein said fixed value is 3: 1.
4. the method for claim 1, described the first preset value and described the second preset value equate.
5. the method for claim 1, described the first preset value and described the second preset value do not wait.
6. the process of claim 1 wherein that the mol ratio that obtains hydrogen and trichlorosilane by the temperature and pressure of controlling mixed gas is the mixed gas of fixed value.
7. the process of claim 1 wherein that the mol ratio that the flow that adds the flow of hot hydrogen and first via mixed gas by controlling respectively the first via obtains hydrogen and trichlorosilane is the polysilicon reducing gas raw material of the first preset value; And the mol ratio that obtains hydrogen and trichlorosilane by controlling respectively the second tunnel flow that adds the flow of hot hydrogen and the second road mixed gas is the polysilicon reducing gas raw material of the second preset value.
8. polycrystalline silicon reduction system comprises:
The bubbling style vaporizer;
The hydrogen well heater;
A plurality of static mixers that are connected with the hydrogen well heater with the bubbling style vaporizer respectively; And
A plurality of polycrystalline silicon reducing furnaces that are connected with corresponding static mixer respectively.
9. the polycrystalline silicon reduction system of claim 8, also comprise the exhaust gas recovery system that all is connected with described a plurality of polycrystalline silicon reducing furnaces.
10. the polycrystalline silicon reduction system of claim 8, wherein static mixer is connected with the hydrogen well heater with the bubbling style vaporizer by corresponding flow control valve respectively.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101333678A (en) * | 2007-06-25 | 2008-12-31 | 北京有色金属研究总院 | Control pipeline for distributing and evaluating supply system of trichlorosilane or silicon tetrachloride |
| CN101417802A (en) * | 2008-11-24 | 2009-04-29 | 四川永祥多晶硅有限公司 | Method for mixing chlorosilane and hydrogen in polycrystalline silicon production |
| CN101723374A (en) * | 2009-11-30 | 2010-06-09 | 乐山乐电天威硅业科技有限责任公司 | Chlorosilane vapourizing mixed process and device |
| CN102009978A (en) * | 2011-01-06 | 2011-04-13 | 四川永祥多晶硅有限公司 | Polysilicon production method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333678A (en) * | 2007-06-25 | 2008-12-31 | 北京有色金属研究总院 | Control pipeline for distributing and evaluating supply system of trichlorosilane or silicon tetrachloride |
| CN101417802A (en) * | 2008-11-24 | 2009-04-29 | 四川永祥多晶硅有限公司 | Method for mixing chlorosilane and hydrogen in polycrystalline silicon production |
| CN101723374A (en) * | 2009-11-30 | 2010-06-09 | 乐山乐电天威硅业科技有限责任公司 | Chlorosilane vapourizing mixed process and device |
| CN102009978A (en) * | 2011-01-06 | 2011-04-13 | 四川永祥多晶硅有限公司 | Polysilicon production method |
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Effective date of registration: 20201113 Address after: 015500 southeast of the intersection of jingsan road and Weisi Road, Qingshan Industrial Park, wulatehouqi, Bayannur City, Inner Mongolia Autonomous Region Patentee after: Bayannur concentrated Silicon Industry Co., Ltd Address before: 015543 the Inner Mongolia Autonomous Region Bayannaoer wulatehouqi Qingshan Industrial Park Patentee before: INNER MONGOLIA DUN'AN PHOTOVOLTAIC TECHNOLOGY Co.,Ltd. |
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