CN101654249A - Production method of polysilicon rod - Google Patents
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- CN101654249A CN101654249A CN200910183451A CN200910183451A CN101654249A CN 101654249 A CN101654249 A CN 101654249A CN 200910183451 A CN200910183451 A CN 200910183451A CN 200910183451 A CN200910183451 A CN 200910183451A CN 101654249 A CN101654249 A CN 101654249A
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Abstract
The invention discloses a production method of a polysilicon rod, comprising the following steps: when the surface temperature of a silicon core is 1100-1250 DEG C, leading in hydrogen to react with trichlorosilane for 30-45 hours; when the silicon core grows to have the diameter of 50mm, stopping current, and adding hydrogen flow rate to continuously react for 3-10 hours; when the surface temperature of the polysilicon rod is reduced to1000-1050 DEG C, applying the current, reducing the hydrogen flow rate, raising the surface temperature of the polysilicon rod to about 1080-1100 DEG C and keeping the surface temperature of the polysilicon rod for 30 hours; stopping the current, and increasing the hydrogen flow rate again to react for 2-6 hours; when the surface temperature of the polysilicon rod is reduced to 970-1020 DEG C, reducing the hydrogen flow rate again, applying the current, raising the surface temperature of the polysilicon rod to 1050-1080 DEG C, and then keeping the surface temperature of the polysilicon rod till a reduction reactor is stopped. The production method of the polysilicon rod can obviously improve the surface appearance of solar polysilicon in the production process, and the surface bump area of the polysilicon can be controlled within 8 percent.
Description
Technical field
The present invention relates to the production method of silicon, be specifically related to a kind of method of trichlorosilane reduction for producing polysilicon silicon rod.
Background technology
It is in the reactor of a bell-jar that the improvement Siemens Method is produced polysilicon, and trichlorosilane and hydrogen reaction generate the high-purity polycrystalline material.Because many-sided factor affecting such as air-flow distribution, temperature distribution and side reaction influences, the surface of polysilicon can produce rough slit and exoncoma.The gentle body of the residual silica flour of meeting in these slits, and influence silicon materials corrosion and pickling effectiveness, the difficulty that causes monocrystalline to be produced increases and quality reduces.The enterprise that adopts the improvement Siemens Method to carry out production of polysilicon is all studied as an important topic improving surface topography.
Generally speaking, in the improvement Siemens Method production process, temperature is high more, and the speed of growth of polysilicon is fast more, and surface topography is poor more simultaneously.Improve surface topography, traditional way is to reduce the silicon rod surface temperature, and surface topography improves and do not make fully that growth velocity is influenced to be considered to impossible, directly adopts the way that reduces surface temperature will cause polycrystalline silicon growth speed to descend greatly, influences the performance of enterprises.
We analyze the formation of polysilicon surface exoncoma, it is generally acknowledged three reasons.The one, temperature is too high, and the 2nd, the air-flow skewness, the 3rd, small molecules products such as HCl form bright fluid layer on the surface.Temperature Influence maximum wherein.Temperature to the influence of surface topography mainly from two aspects.On the one hand, polycrystalline silicon growth has an optimum temps, and below the temperature, temperature high growth rates more is fast more at this, and more than the temperature, the high more speed of growth of temperature is slow more on the contrary at this.This be because temperature too high after, side reaction aggravation, cause main reaction---the ratio that reduction reaction takes place in system reduces.Because the restriction of improvement Siemens Method production technique is influenced by its airflow design and cooling system, the silicon rod surface temperature distribution is inhomogeneous, and the lower end temperature is low, upper end temperature height, and temperature outside is low, inboard temperature height.During near optimum growth temp, the temperature on part surface has in fact surpassed optimum growth temp at average surface temperature.We know, in the process that polycrystalline forms, grain size and crystal shape have certain difference, form tiny " brilliant trace ", brilliant trace is projection a bit, and some is recessed, general visual inspection less than, but particularly adopt the tunnel flying-spot microscope at powerful microscope, we can see the existence of these brilliant traces very clearly.After brilliant trace produced, the brilliant trace of projection was because more thorough with the heat exchange of outer gas stream, and general temperature can be lower than silicon rod surface and little recessed brilliant trace slightly.When brilliant trace is created in surface temperature and is higher than polysilicon optimum growth temp regional, the bossing speed of growth that temperature is lower can be higher faster than temperature recessed portion, at this time, lug boss branch is long more big more, lower concave part branch is more and more darker, finally forms tangible surperficial exoncoma.On the other hand, recessed portion is because to carry out the speed of exchange of substance slow with outer gas stream, and the concentration of HCl can be than higher, and under the temperature of reaction of polysilicon (1100 ℃), the reverse corrosion reaction of HCl takes place simultaneously:
Si+2HCl→SiH
2Cl
2
The slit on the reverse corrosion reaction meeting aggravation silicon rod surface of HCl is the important factor that causes silicon rod surface topography difference.
Summary of the invention
Technical problem to be solved by this invention provides a kind of production method of improving the polysilicon rod of polysilicon surface pattern.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of production method of polysilicon rod comprises the steps:
(1) in the reduction furnace reactor, when 1100～1250 ℃ of silicon wicking surface temperature, feeds hydrogen and trichlorosilane reaction 30～45h; Trichlorosilane initial flow 80～90Nm
3/ h is with 1～2Nm
3The speed of/h at the uniform velocity increases to 220Nm
3/ h, keep afterwards constant, until the reduction reactor blowing out; Hydrogen flowing quantity maintains 80～120Nm
3/ h;
(2) when the silicon core grows into diameter 50mm, stop to apply electric current, regulate hydrogen flowing quantity to 170～250Nm
3/ h continues reaction 3～10h;
(3) treat that the silicon rod surface temperature reduces to 1000～1050 ℃, recover to apply electric current, simultaneously hydrogen flowing quantity is transferred to 100～150Nm
3/ h rises to about 1080～1100 ℃ with 40～45h with the silicon rod surface temperature, keeps 30h again;
(4) stop to apply electric current, regulate hydrogen flowing quantity to 300～400Nm
3/ h, reaction 2～6h;
(5) treat that the silicon rod surface temperature reduces to 970～1020 ℃, regulate hydrogen flowing quantity to 180～250Nm
3/ h applies electric current simultaneously, with 40～50h the silicon rod surface temperature is risen to 1050～1080 ℃, keeps hydrogen flowing quantity and temperature then to the reduction reactor blowing out.
In the step (1), the silicon core diameter is 5～8mm.
In the step (1), preferred, during 1100 ℃ of silicon wicking surface temperature, feed hydrogen reaction 35h, hydrogen flowing quantity 100Nm
3/ h.
In the step (2), preferred, when the silicon core grows into diameter 50mm, stop to apply electric current, regulate hydrogen flowing quantity to 200Nm
3/ h continues reaction 6h.
In the step (3), preferred, treat that the silicon rod surface temperature reduces to 1020 ℃, recover to apply electric current, simultaneously hydrogen flowing quantity is transferred to 120Nm
3/ h rises to about 1080 ℃ with 45h with the silicon rod surface temperature, keeps 30h again.
In the step (4), preferred, stop to apply electric current, regulate hydrogen flowing quantity to 350Nm
3/ h, reaction 3h.
In the step (5), preferred, treat that the silicon rod surface temperature reduces to 1000 ℃, regulate hydrogen flowing quantity to 180Nm
3/ h applies electric current simultaneously, with 45h the silicon rod surface temperature is risen to 1060 ℃, keeps hydrogen flowing quantity and temperature then to reduction reactor blowing out (about 30～40h).
That describes in above-mentioned steps (3) and the step (5) rises to another temperature with the silicon rod surface temperature by a certain temperature in for some time, during this, the speed that heats up without any restriction, is risen to a certain temperature as long as guarantee in the time range that requires.Preferably at the uniform velocity heat up.
Above-mentioned steps (1) in (5), trichlorosilane initial flow 80～90Nm
3/ h is then with 1～2Nm
3The speed of/h at the uniform velocity increases to 220Nm always
3/ h, keep afterwards constant, until the reduction reactor blowing out; And hydrogen flowing quantity carries out change operation according to the description of step (1) to (5).
In reaction in earlier stage, because the silicon rod surface temperature distribution is more even, reaction can be carried out under a comparatively high temps.When the silicon rod diameter reached 50mm, the surface was about to occur or has occurred because temperature distributing disproportionation is spared the exoncoma that produces, and reduce temperature of reaction this moment, prevented the further generation of exoncoma.Exoncoma is in case generation only depends on the reduction temperature it can't be alleviated, and therefore, must increase hydrogen flowing quantity this moment.
Reducing temperature and increasing under the hydrogen usage dual function, the slit on silicon rod surface obtains repairing, and exoncoma disappears.At this moment, slowly elevated temperature at this moment because the silicon rod diameter is less, and temperature is lower, does not have exoncoma and produces in the process of growth.When temperature rises to 1080～1100 ℃, though this moment, the surface can occur unsmoothly, the silicon rod diameter is bigger, and reaction is near the later stage, and the generation of exoncoma and worsen limited time is not so the surface topography of silicon rod can be too poor.And this moment because the silicon rod surface-area increases, speed of response is far longer than the speed of response hour under this temperature of silicon rod diameter, so adopt this method, the influence that the speed of response of silicon rod integral body is reduced by temperature is less.
Beneficial effect: the present invention compared with prior art has following advantage:
(1) method of improving the polysilicon surface exoncoma disclosed by the invention can effectively be improved the surface topography of polysilicon, production efficiency is not produced considerable influence simultaneously;
(2) present method is simple, is easy to control, and has greatly improved the performance of enterprises;
(3) this method is through repeatedly commerical test checking, and respond well, in a plurality of batches of industrial practices, polysilicon surface exoncoma area can be controlled in 8%.
Embodiment
According to following embodiment, the present invention may be better understood.Yet, those skilled in the art will readily understand that the described concrete material proportion of embodiment, processing condition and result thereof only are used to illustrate the present invention, and should also can not limit the present invention described in detail in claims.
Embodiment 1:
Adopt the silicon core growing polycrystalline silicon of diameter 5mm.After the reduction furnace reactor comes into operation, set the surface reaction temperature at 1100 ℃, feed hydrogen and trichlorosilane reaction 35 hours.Trichlorosilane initial flow 80Nm
3/ h is with 1Nm
3The speed of/h at the uniform velocity increases to 220Nm
3/ h (about 140h), keep afterwards constant, until the reduction reactor blowing out.The hydrogen initial flow maintains 100Nm
3/ h.When the silicon rod diameter reaches 50mm, stop to apply electric current, simultaneously, increase hydrogen flowing quantity to 200Nm
3/ h.Through 6 hours, treat that the silicon rod surface temperature reduces to 1020 ℃, recover to apply electric current, simultaneously hydrogen flowing quantity is transferred to 120Nm
3/ h.Slowly increase electric current, rising silicon rod surface temperature rose to about 1080 ℃ with 45 hours with the silicon rod surface temperature.Kept 30 hours.Stop to apply electric current afterwards, hydrogen flowing quantity is increased to 350Nm
3/ h.After about 3 hours, after the silicon rod surface temperature is reduced to 1000 ℃, reduce hydrogen flowing quantity to 180Nm
3/ h increases electric current simultaneously, and the silicon rod surface temperature slowly raises.The silicon rod surface temperature is risen to 1060 ℃ with 45 hour time, keep 30h then to the reduction reactor blowing out.
Embodiment 2:
Adopt the silicon core growing polycrystalline silicon of diameter 8mm.After the reduction furnace reactor comes into operation, set the surface reaction temperature at 1180 ℃, feed hydrogen and trichlorosilane reaction 40 hours.Trichlorosilane initial flow 90Nm
3/ h is with 1Nm
3The speed of/h at the uniform velocity increases to 220Nm
3/ h (about 130h), keep afterwards constant, until the reduction reactor blowing out.The hydrogen initial flow maintains 120Nm
3/ h.When the silicon rod diameter reaches 50mm, stop to apply electric current, simultaneously, increase hydrogen flowing quantity to 220Nm
3/ h.Through 5 hours, treat that the silicon rod surface temperature reduces to 1020 ℃, recover normally to apply electric current, simultaneously hydrogen flowing quantity is transferred to 120Nm
3/ h.Slowly increase electric current, rising silicon rod surface temperature rose to about 1080 ℃ with 45 hours with the silicon rod surface temperature.Kept 30 hours.Stop to apply electric current afterwards, regulate hydrogen flowing quantity to 350Nm
3/ h.After about 3 hours, after the silicon rod surface temperature is reduced to 995 ℃, reduce the hydrogen flow to 200m
3/ h increases electric current simultaneously, and the silicon rod surface temperature slowly raises.The silicon rod surface temperature is risen to 1060 ℃ with 45 hour time, keep 32h then to the reduction reactor blowing out.
Embodiment 3:
Adopt the silicon core growing polycrystalline silicon of diameter 6mm.After the reduction furnace reactor comes into operation, set the surface reaction temperature at 1130 ℃, feed hydrogen and trichlorosilane reaction 37 hours.Trichlorosilane initial flow 80Nm
3/ h is with 2Nm
3The speed of/h at the uniform velocity increases to 220Nm
3/ h (about 70h), keep afterwards constant, until the reduction reactor blowing out.The initial flow of hydrogen maintains 110Nm
3/ h.When the silicon rod diameter reaches 50mm, stop to apply electric current, simultaneously, increase hydrogen flowing quantity to 200Nm
3/ h.Through 5 hours, treat that the silicon rod surface temperature reduces to 1020 ℃, recover normally to apply electric current, simultaneously hydrogen flowing quantity is transferred to 120Nm
3/ h.Slowly increase electric current, rising silicon rod surface temperature rose to about 1080 ℃ with 45 hours with the silicon rod surface temperature.Kept 30 hours.Stop to apply electric current afterwards, hydrogen flowing quantity is increased to 350Nm
3/ h.After about 3 hours, after the silicon rod surface temperature is reduced to 1000 ℃, reduce hydrogen flowing quantity to 200m
3/ h increases electric current simultaneously, and the silicon rod surface temperature slowly raises.The silicon rod surface temperature is risen to 1060 ℃ with 45 hour time, keep 30h then to the reduction reactor blowing out.
The contriver just uses present method respectively, use United States Patent 5904981 methods, keep 1100 ℃ temperature of reaction all the time and keep 1050 ℃ temperature of reaction all the time and carried out repeatedly commerical test contrast, and test-results is as shown in table 1.
We can see by table 1, use the inventive method can well improve the polysilicon surface pattern, and are less to the growth velocity influence of polysilicon simultaneously.Do not adopt the effect of this method (keeping 1100 ℃ of productions all the time) to compare, the surface exoncoma has reduced by 17%, and the speed of growth only reduces 1Kg/h, compares with United States Patent 5904981, the surface exoncoma has reduced by 7%, and the speed of growth has increased 1Kg/h.
Table 1 differential responses method comparative result
Claims (7)
1, a kind of production method of polysilicon rod is characterized in that this method comprises the steps:
(1) in the reduction furnace reactor, when 1100～1250 ℃ of silicon wicking surface temperature, feeds hydrogen and trichlorosilane reaction 30～45h; Trichlorosilane initial flow 80～90Nm
3/ h is with 1～2Nm
3The speed of/h at the uniform velocity increases to 220Nm
3/ h, keep afterwards constant, until the reduction reactor blowing out; Hydrogen flowing quantity maintains 80～120Nm
3/ h;
(2) when the silicon core grows into diameter 50mm, stop to apply electric current, regulate hydrogen flowing quantity to 170～250Nm
3/ h continues reaction 3～10h;
(3) treat that the silicon rod surface temperature reduces to 1000～1050 ℃, recover to apply electric current, simultaneously hydrogen flowing quantity is transferred to 100～150Nm
3/ h rises to about 1080～1100 ℃ with 40～45h with the silicon rod surface temperature, keeps 30h again;
(4) stop to apply electric current, regulate hydrogen flowing quantity to 300～400Nm
3/ h, reaction 2～6h;
(5) treat that the silicon rod surface temperature reduces to 970～1020 ℃, regulate hydrogen flowing quantity to 180～250Nm
3/ h applies electric current simultaneously, with 40～50h the silicon rod surface temperature is risen to 1050～1080 ℃, keeps hydrogen flowing quantity and temperature then to the reduction reactor blowing out.
2, the production method of polysilicon rod according to claim 1 is characterized in that in the step (1), the silicon core diameter is 5～8mm.
3, the production method of polysilicon rod according to claim 1 is characterized in that in the step (1), when 1100 ℃ of silicon wicking surface temperature, feeds hydrogen reaction 35h, hydrogen flowing quantity 100Nm
3/ h.
4, the production method of polysilicon rod according to claim 1 is characterized in that when the silicon core grows into diameter 50mm, stopping to apply electric current in the step (2), regulates hydrogen flowing quantity to 200Nm
3/ h continues reaction 6h.
5, the production method of polysilicon rod according to claim 1 is characterized in that in the step (3), treats that the silicon rod surface temperature reduces to 1020 ℃, recovers to apply electric current, simultaneously hydrogen flowing quantity is transferred to 120Nm
3/ h rises to about 1080 ℃ with 45h with the silicon rod surface temperature, keeps 30h again.
6, the production method of polysilicon rod according to claim 1 is characterized in that stopping to apply electric current in the step (4), regulates hydrogen flowing quantity to 350Nm
3/ h, reaction 3h.
7, the production method of polysilicon rod according to claim 1 is characterized in that in the step (5), treats that the silicon rod surface temperature reduces to 1000 ℃, regulates hydrogen flowing quantity to 180Nm
3/ h applies electric current simultaneously, with 45h the silicon rod surface temperature is risen to 1060 ℃, keeps hydrogen flowing quantity and temperature then to the reduction reactor blowing out.
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| CN102107873A (en) * | 2011-04-06 | 2011-06-29 | 连云港中彩科技有限公司 | New multicrystal silicon reduction production technology |
| CN102557035A (en) * | 2010-10-25 | 2012-07-11 | 瓦克化学股份公司 | Method for producing polycrystalline silicon rods |
| CN102608913A (en) * | 2011-01-19 | 2012-07-25 | 内蒙古盾安光伏科技有限公司 | System and method for controlling blowing out of reduction furnace in production of polycrystalline silicon |
| CN102923709A (en) * | 2011-08-11 | 2013-02-13 | 内蒙古盾安光伏科技有限公司 | Feeding system for polycrystalline silicon production, and method thereof |
| CN104003397A (en) * | 2014-06-18 | 2014-08-27 | 四川永祥多晶硅有限公司 | Trichlorosilane reduction procedure controlling method |
| CN104118879A (en) * | 2014-08-06 | 2014-10-29 | 四川永祥多晶硅有限公司 | Preparation method of silicon core master batch |
| CN111596636A (en) * | 2020-06-19 | 2020-08-28 | 亚洲硅业(青海)股份有限公司 | Polycrystalline silicon reduction furnace control method and device and electronic equipment |
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| US5976481A (en) * | 1996-05-21 | 1999-11-02 | Tokuyama Corporation | Polycrystal silicon rod and production process therefor |
| KR100210261B1 (en) * | 1997-03-13 | 1999-07-15 | 이서봉 | Method of production for poly crystal silicon |
| DE102007023041A1 (en) * | 2007-05-16 | 2008-11-20 | Wacker Chemie Ag | Polycrystalline silicon rod for zone pulling and a method for its production |
| CN101323449A (en) * | 2008-07-04 | 2008-12-17 | 上海通用硅晶体材料有限公司 | Method and apparatus for enhancing polysilicon production |
| CN101508151B (en) * | 2009-04-07 | 2012-03-21 | 宝鸡宝色特种金属有限责任公司 | Polysilicon rod thermodynamics breaking technique and device |
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| CN104003397A (en) * | 2014-06-18 | 2014-08-27 | 四川永祥多晶硅有限公司 | Trichlorosilane reduction procedure controlling method |
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Assignee: Suzhou GCL Photovoltaic Technology Co., Ltd. Assignor: Jiangsu Zhongneng Polysilicon Technology Development Co., Ltd. Contract record no.: 2011320010020 Denomination of invention: Production method of polysilicon rod License type: Exclusive License Open date: 20100224 Record date: 20110317 |