CN104118879B - A kind of preparation method of silicon core masterbatch - Google Patents
A kind of preparation method of silicon core masterbatch Download PDFInfo
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Abstract
The preparation method that the present invention provides a kind of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, then select from polycrystalline silicon rod product material diameter be 110-130mm meet the polycrystalline silicon rod that silicon core masterbatch requires, cut into the length required for drawing silicon core, after clean process, obtain silicon core masterbatch。Adopting the present invention to produce silicon core masterbatch and can reduce the consumption of reduction hydrogen, can effectively reducing the energy consumption producing silicon core masterbatch, thus reducing production cost。
Description
Technical field
The present invention relates to technical field of polysilicon production, particularly to the preparation method of a kind of silicon core masterbatch。
Background technology
What be widely adopted at present in the production method of polysilicon has Siemens in the method for manufacturing polycrystalline silicon (also referred to as Siemens Method) of invention in 1954: adopt high-purity trichlorosilane gas and high-purity hydrogen to mix composition mixed raw material gas according to certain proportioning, pass in reduction reactor, constantly depositing on the HIGH-PURITY SILICON core of heating, the diameter making silicon core is thicker gradually and forms polycrystalline silicon rod。The production technology of silicon core used herein above mainly has two kinds, one is silicon core furnace drawing silicon core, and one is cutting side's silicon core, through improving, silicon core furnace drawing silicon core is drawn by the single of early stage and is transformed to existing five cores and draws, and has namely reformed into once drawing five silicon cores by once drawing one。
In prior art, in order to ensure the normal of silicon core pulling process, safety carries out, also for the quality ensureing the silicon core drawn, so the quality requirements of silicon core masterbatch requires high than polycrystalline silicon rod, silicon core masterbatch need to meet following requirements: without deep layer crack, non-oxidation interlayer, without needle-like interlayer, be layered without silicon core circle, concave-convex surface degree is less than 1mm, flexibility≤0.3%。In order to obtain the silicon core masterbatch of above-mentioned requirements, it is this up till now, it is all in the industry produced by special reducing process, namely produce on the basis of polycrystalline silicon rod, strengthen the proportioning of hydrogen and trichlorosilane gas, control its growth temperature at 1060-1070 degree, to reduce silicon rod growth rate to make silicon rod surface deposition uniform, slow thus obtaining satisfactory silicon core masterbatch。This operational drawbacks is, because increasing the proportioning of hydrogen and trichlorosilane gas so that hydrogen consumption is high；Reducing throughput rate can make growth cycle extend, so that power consumption increases, in the production of polysilicon, polycrystalline silicon rod product material power consumption is about 55-65KWh/kg-Si, and be 100-110KWh/kg-Si to produce the power consumption of the technique that the polycrystalline silicon rod meeting silicon core masterbatch requirement adopts, it can be seen that every kilogram of silicon core masterbatch power consumption power consumption more than 40 degree more than every kilogram of polysilicon。Therefore it is badly in need of one and can produce satisfactory silicon core masterbatch, the production method of the silicon core masterbatch of energy consumption can be reduced again。
At periodical " Yunnan metallurgy " the 36th interim document disclosing a section " application of polysilicon and production technology " of volume the 5th that in October, 2007 publishes, pointing out in document, in order to reach the purpose saved energy and reduce the cost, polycrystalline silicon reducing furnace must maximize。The feature of large-scale energy-saving reduction furnace is: can heating the heat loss that rod at the beginning of many causes to reduce furnace wall to radiate in stove, the inwall of reduction furnace carries out mirror process, makes radiant heat energy reflect, to reduce heat loss simultaneously；Furnace pressure and air demand are improved, and increase the speed of siliceous deposits reaction。Adopting the method for this improvement reduction furnace to reduce energy consumption, process is complicated, and reduction furnace improving cost is high。
Summary of the invention
The preparation method that the present invention provides a kind of silicon core masterbatch, adopting this kind of method to produce silicon core masterbatch, can reduce the consumption of reduction hydrogen, can effectively reducing the energy consumption producing silicon core masterbatch, thus reducing production cost。
For solving above-mentioned technical problem, the present invention is achieved through the following technical solutions:
A kind of preparation method of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, then select from polycrystalline silicon rod product material diameter be 110-130mm meet the polycrystalline silicon rod that silicon core masterbatch requires, cut into the length required for drawing silicon core, after clean process, obtain silicon core masterbatch。
When production process occurs split rod, equipment faults etc. need blowing out in advance, make silicon rod but without when growing into the diameter of pre-manufactured, as long as the diameter meeting silicon core masterbatch requirement also can be elected as silicon core masterbatch at 110-130mm polycrystalline silicon rod, as when the diameter of the polycrystalline silicon rod product material of pre-manufactured being the polycrystalline silicon rod of 130mm, but it is because occurring in that and splits the problem such as rod or equipment fault, now the diameter of polycrystalline silicon rod is but without growing into 130mm with regard to blowing out, in this case, tear furnace rear open, diameter can also be selected from these polycrystalline silicon rods and meet polycrystalline silicon rod that silicon core masterbatch requires as silicon core masterbatch more than 110mm。
The preparation technology of described polycrystalline silicon rod product material is as follows: in reduction furnace, silicon core is suppressed and immediately silicon core electric current is added to 140-150A after successfully, hydrogen sky burns 30-60min, trichlorosilane gas after passing into from purification to reduction furnace and hydrogen, power up stream to silicon core to react simultaneously, response time is 80h, wherein:
In the 0-10h stage of reaction: trichlorosilane gas and hydrogen being increased to 140-160kg/h and 340-360kg/h uniformly respectively from the flow of 0kg/h, silicon core electric current uniformly increases to 440-460A from 140-150A；
The 10-20h stage of reaction: increased uniformly from 140-160kg/h by trichlorosilane gas to 240-260kg/h, hydrogen increases from 340-360kg/h uniformly to 490-510kg/h, and silicon core electric current increases to 740-760A uniformly from 440-460A；
The 20-80h stage of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 240-260kg/h and 490-510kg/h respectively, silicon core electric current: uniformly increase to 990-1010A at 20-30h, 30-40h uniformly increases to 1290-1310A, 40-50h increases to 1390-1410A, and it is constant that 50-80h maintains 1390-1410A；After having reacted, blowing out, tear stove open。
The described polycrystalline silicon rod meeting silicon core masterbatch requirement refer to without deep layer crack, non-oxidation interlayer, without needle-like interlayer, be layered without silicon core circle, concave-convex surface degree is less than 1mm, the polycrystalline silicon rod of flexibility≤0.3%。
Described polycrystalline silicon rod product material resistivity is 40 ~ 100 Ω .cm。
Described silicon core diameter is 10mm, long for 2900mm。
Described polycrystalline silicon rod product material is gradually increased at 0-80h interior diameter, wherein the polycrystalline silicon rod product material diameter when 10h is 28-32mm, 20h diameter is 48-52mm, 30h diameter is 68-72mm, 40h diameter is 88-92mm, 50h diameter be 103-107mm, 60h diameter is 113-117mm, 70h diameter is 123-127mm, 80h diameter is 128-132mm。
Silicon core is suppressed, observe silicon core, it is that silicon core is suppressed successfully when silicon core is aglow, silicon core electric current being added to 140-150A, makes silicon core temperature reach reaction temperature required, hydrogen sky burns 30-60min, trichlorosilane gas and hydrogen is passed into again in reduction furnace, so can remove other impurity such as the hydrone made in stove, make in stove cleaner, it is ensured that polycrystalline silicon rod product material is free from foreign meter。
Beneficial effect:
1, the present invention directly select from polycrystalline silicon rod product material diameter be 110-130mm meet polycrystalline silicon rod that silicon core masterbatch requires as silicon core masterbatch, the power consumption of this silicon core masterbatch is compared with the silicon core masterbatch adopting special reduction furnace and proprietary production technology to produce, the electricity of degree more than 40 can be saved for every kilogram, can be seen that, one polysilicon enterprise producing 10000 tons per year, about need silicon core masterbatch 500 tons every year, the power consumption difference of silicon core masterbatch and product material is with 40 degree of words calculated, the electricity that so 500 tons of silicon core masterbatch can be saved is 2,000 ten thousand degree, energy consumption is greatly reduced, reduce production cost。
2, the present invention changes in prior art by strengthening the proportioning of trichlorosilane gas and hydrogen, control its growth temperature method producing silicon core masterbatch at 1060-1070 degree, but do not increasing hydrogen consumption, keep growth temperature constant, on the basis that throughput rate is constant, optimize the production technology of polycrystalline silicon rod product material: by controlling the proportioning of trichlorosilane gas and hydrogen, flow accurately and stable, silicon core electric current in production process, and adjust the magnitude of current accordingly according to trichlorosilane gas and hydrogen flowing quantity, make the polycrystalline silicon rod temperature of any time, throughput rate and polycrystalline silicon rod presentation quality reach optimum state, not only save the consumption of hydrogen, shorten the production cycle, the effective quality improving polycrystalline silicon rod product material, reduce the production cost of silicon core masterbatch, improve per unit area yield。Make the polycrystalline silicon rod meeting silicon core masterbatch requirement account for the 10-15% of polycrystalline silicon rod product material gross mass, be fully able to and meet production needs。
Detailed description of the invention
The present invention is described in detail below in conjunction with detailed description of the invention。
Embodiment 1
A kind of preparation method of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, then by drawing personnel, to tearing stove scene open, to select the polycrystalline silicon rod that silicon core masterbatch requires that meets that diameter is 110-130mm from polycrystalline silicon rod product material (can be whole, can be pipe nipple), cut into the length required for drawing silicon core, after clean process, obtain silicon core masterbatch。
Embodiment 2
A kind of preparation method of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, concrete technology is as follows, in reduction furnace, silicon core is suppressed and immediately silicon core electric current is added to 140A after successfully, after hydrogen sky burns 30min, trichlorosilane gas after passing into from purification to reduction furnace and hydrogen, power up stream to silicon core to react simultaneously, response time is 80h, wherein: in the 0-10h stage of reaction: trichlorosilane gas and hydrogen are increased to 140kg/h and 340-kg/h from the flow of 0kg/h is uniform respectively, silicon core electric current uniformly increases to 440A from 140A；The 10-20h stage of reaction: increased uniformly from 140kg/h by trichlorosilane gas to 240kg/h, hydrogen increases from 340kg/h uniformly to 490kg/h, and silicon core electric current increases to 740A uniformly from 440A；The 20-80h stage of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 240kg/h and 490kg/h respectively, silicon core electric current: uniformly increase to 990A at 20-30h, 30-40h uniformly increases to be increased to 1390A to 1290A, 40-50h, and it is constant that 50-80h maintains 1390A；After having reacted, the polycrystalline silicon rod diameter obtained is 128-132mm, and stove is torn in blowing out open。
Furnace rear to be torn open, by drawing personnel, to tearing stove scene open, to select the polycrystalline silicon rod that silicon core masterbatch requires that meets that diameter is 128-130mm from the polycrystalline silicon rod product material that these diameters are 128-132mm (can be whole, can be pipe nipple), cut into and draw the masterbatch length needed, silicon core masterbatch is obtained after clean process. by the preparation of the present embodiment, the silicon core masterbatch obtained accounts for the 10% of polycrystalline silicon rod product material gross mass。
Embodiment 3
A kind of preparation method of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, the preparation technology of described polysilicon product material is as follows: in reduction furnace, silicon core is suppressed and immediately silicon core electric current is added to 145A after successfully, hydrogen sky burns 45min, trichlorosilane gas after passing into from purification to reduction furnace and hydrogen, power up stream to silicon core to react simultaneously, response time is 80h, wherein: in the 0-10h stage of reaction: trichlorosilane gas and hydrogen are increased to 150kg/h and 350kg/h from the flow of 0kg/h is uniform respectively, silicon core electric current uniformly increases to 450A from 145A；The 10-20h stage of reaction: increased uniformly from 150kg/h by trichlorosilane gas to 250kg/h, hydrogen increases from 350kg/h uniformly to 500kg/h, and silicon core electric current increases to 750A uniformly from 450A；The 20-80h stage of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 250kg/h and 500kg/h respectively, silicon core electric current: uniformly increase to 1000A at 20-30h, 30-40h uniformly increases to be increased to 1400A to 1300A, 40-50h, and it is constant that 50-80h maintains 1400A；After having reacted, the diameter of the polycrystalline silicon rod product material prepared is 128-132mm, and stove is torn in blowing out open。
Furnace rear to be torn open, by drawing personnel, to tearing stove scene open, to select diameter from polycrystalline silicon rod product material be that to meet the polycrystalline silicon rod of silicon core masterbatch requirement (can be whole to 128-130mm, can be pipe nipple), cut into and draw the masterbatch length needed, obtaining silicon core masterbatch after clean process, the silicon core masterbatch that the present embodiment obtains accounts for the 15% of polycrystalline silicon rod product material gross mass。
Embodiment 4
A kind of preparation method of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, the preparation technology of described polysilicon product material is as follows: in reduction furnace, silicon core is suppressed and immediately silicon core electric current is added to 150A after successfully, wait 60min, trichlorosilane gas after passing into from purification to reduction furnace and hydrogen, power up stream to silicon core to react simultaneously, response time is 80h, wherein: in the 0-10h stage of reaction: trichlorosilane gas and hydrogen are increased to 160kg/h and 360kg/h from the flow of 0kg/h is uniform respectively, silicon core electric current uniformly increases to 460A from 150A；The 10-20h stage of reaction: increased uniformly from 160kg/h by trichlorosilane gas to 260kg/h, hydrogen increases from 360kg/h uniformly to 510kg/h, and silicon core electric current increases to 760A uniformly from 460A；The 20-80h stage of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 260kg/h and 510kg/h respectively, silicon core electric current: uniformly increase to 1010A at 30h, 30-40h uniformly increases to be increased to 1410A to 1310A, 40-50h, and it is constant that 50-80h maintains 1410A；After having reacted, the diameter of the polycrystalline silicon rod product material prepared is 128-132mm, and stove is torn in blowing out open。
Furnace rear to be torn open, by drawing personnel, to tearing open, stove is on-the-spot selects the polycrystalline silicon rod (can be whole, it is possible to be pipe nipple) meeting silicon core masterbatch requirement from polycrystalline silicon rod product material, cuts into and draws the masterbatch length needed, obtains silicon core masterbatch after clean process。The silicon core masterbatch that the present embodiment obtains accounts for the 13% of polycrystalline silicon rod product material gross mass。
Embodiment 5
A kind of preparation method of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, the preparation technology of described polysilicon product material is as follows: in reduction furnace, silicon core is suppressed and immediately silicon core electric current is added to 150A after successfully, hydrogen sky burns 55min, trichlorosilane gas after passing into from purification to reduction furnace and hydrogen, power up stream to silicon core to react simultaneously, response time is 80h, wherein: in the 0-10h stage of reaction: trichlorosilane gas and hydrogen are increased to 155kg/h and 355kg/h from the flow of 0kg/h is uniform respectively, silicon core electric current uniformly increases to 455A from 150A；The 10-20h stage of reaction: increased uniformly from 155kg/h by trichlorosilane gas to 255kg/h, hydrogen increases from 355kg/h uniformly to 505kg/h, and silicon core electric current increases to 755A uniformly from 455A；The 20-80h stage of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 255kg/h and 505kg/h respectively, silicon core electric current: uniformly increase to 1005A at 30h, 30-40h uniformly increases to be increased to 1405A to 1305A, 40-50h, and it is constant that 50-80h maintains 1405A；After having reacted, the diameter of the polycrystalline silicon rod product material prepared is 128-132mm, and stove is torn in blowing out open。
Furnace rear to be torn open, by drawing personnel, to tearing stove scene open, to select the polycrystalline silicon rod that diameter is 128-130mm meeting silicon core masterbatch requirement from polycrystalline silicon rod product material (can be whole, can be pipe nipple), cut into and draw the masterbatch length needed, after clean process, obtain silicon core masterbatch。The silicon core masterbatch that the present embodiment obtains accounts for the 14% of polycrystalline silicon rod product material gross mass。
Embodiment 6
A kind of preparation method of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, then select from polycrystalline silicon rod product material diameter be 110-130mm meet the polycrystalline silicon rod that silicon core masterbatch requires, cut into the length required for drawing silicon core, after clean process, obtain silicon core masterbatch。The described polycrystalline silicon rod meeting silicon core masterbatch requirement refer to without deep layer crack, non-oxidation interlayer, without needle-like interlayer, be layered without silicon core circle, concave-convex surface degree is less than 1mm, the polycrystalline silicon rod of flexibility≤0.3%。
Embodiment 7
A kind of preparation method of silicon core masterbatch, polycrystalline silicon rod product material is prepared including trichlorosilane gas and hydrogen being passed into reaction in reduction furnace, the preparation technology of described polysilicon product material is as follows: in reduction furnace, silicon core is suppressed and immediately silicon core electric current is added to 145A after successfully, hydrogen sky burns 50min, trichlorosilane gas after passing into from purification to reduction furnace and hydrogen, power up stream to silicon core to react simultaneously, response time is 80h, wherein: in the 0-10h stage of reaction: trichlorosilane gas and hydrogen are increased to 145kg/h and 345kg/h from the flow of 0kg/h is uniform respectively, silicon core electric current uniformly increases to 445A from 145A；The 10-20h stage of reaction: increased uniformly from 145kg/h by trichlorosilane gas to 245kg/h, hydrogen increases from 345kg/h uniformly to 495kg/h, and silicon core electric current increases to 745A uniformly from 445A；The 20-80h stage of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 245kg/h and 495kg/h respectively, silicon core electric current: uniformly increase to 995A at 20-30h, 30-40h uniformly increases to be increased to 1395A to 1295A, 40-50h, and it is constant that 50-80h maintains 1395A；After having reacted, the diameter of polycrystalline silicon rod product material is 128-132mm, and stove is torn in blowing out open。Tear open furnace rear select from polycrystalline silicon rod product material diameter be 128-130mm meet the polycrystalline silicon rod that silicon core masterbatch requires, cut into the length required for drawing silicon core, clean process after silicon core masterbatch。The present embodiment silicon core masterbatch accounts for the 12% of polycrystalline silicon rod product material gross mass, and silicon core diameter used in the present embodiment is 10mm, long for 2900mm。
In the growth course of polycrystalline silicon rod, 0-80h interior diameter is gradually increased, wherein the diameter of the polycrystalline silicon rod product material when 10h is 28-32mm, when when during 20h, diameter is 48-52mm, 30h, diameter is 68-72mm, 40h, diameter is 88-92mm, during 50h, diameter is 103-107mm, when when during 60h, diameter is 113-117mm, 70h, diameter is 123-127mm, 80h, diameter is 128-132mm。The resistivity of described polycrystalline silicon rod product material is 40 ~ 100 Ω .cm。
Claims (6)
1. the preparation method of a silicon core masterbatch, it is characterized in that: after trichlorosilane gas and hydrogen are passed into the prepared polycrystalline silicon rod product material of reaction in reduction furnace, select from polycrystalline silicon rod product material again diameter be 110-130mm meet the polycrystalline silicon rod that silicon core masterbatch requires, cut into the length required for drawing silicon core, after clean process, obtain silicon core masterbatch；The preparation technology of described polycrystalline silicon rod product material is as follows: in reduction furnace, silicon core is suppressed and immediately silicon core electric current is added to 140-150A after successfully, wait 30-60min, trichlorosilane gas after passing into from purification to reduction furnace and hydrogen, power up stream to silicon core to react simultaneously, response time is 80h, wherein:
In the 0-10h stage of reaction: trichlorosilane gas and hydrogen being increased to 140-160kg/h and 340-360kg/h uniformly respectively from the flow of 0kg/h, silicon core electric current uniformly increases to 440-460A from 140-150A；
The 10-20h stage of reaction: increased uniformly from 140-160kg/h by trichlorosilane gas to 240-260kg/h, hydrogen increases from 340-360kg/h uniformly to 490-510kg/h, and silicon core electric current increases to 740-760A uniformly from 440-460A；
The 20-80h stage of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 240-260kg/h and 490-510kg/h respectively, silicon core electric current: uniformly increase to 990-1010A at 20-30h, 30-40h uniformly increases to 1290-1310A, 40-50h increases to 1390-1410A, and it is constant that 50-80h maintains 1390-1410A；After having reacted, blowing out, tear stove open。
2. the preparation method of a kind of silicon core masterbatch according to claim 1, it is characterized in that: described in meet the polycrystalline silicon rod of silicon core masterbatch requirement refer to without deep layer crack, non-oxidation interlayer, without needle-like interlayer, be layered without silicon core circle, concave-convex surface degree is less than 1mm, the polycrystalline silicon rod of flexibility≤0.3%。
3. the preparation method of a kind of silicon core masterbatch according to claim 1, it is characterised in that: described polycrystalline silicon rod product material resistivity is 40 ~ 100 Ω cm。
4. the preparation method of a kind of silicon core masterbatch according to claim 1, it is characterised in that: described silicon core diameter is 10mm, long for 280mm。
5. the preparation method of a kind of silicon core masterbatch according to claim 1, it is characterized in that: described polycrystalline silicon rod product material is gradually increased at 0-80h interior diameter, wherein the polycrystalline silicon rod product material diameter when 10h is 28-32mm, 20h diameter is 48-52mm, 30h diameter be 68-72mm, 40h diameter is 88-92mm, 50h diameter is 103-107mm, 60h diameter is 113-117mm, 70h diameter be 123-127mm, 80h diameter is 128-132mm。
6. the preparation method of a kind of silicon core masterbatch according to claim 1 and 2, it is characterized in that: when production process occurs split rod, equipment fault needs blowing out in advance, make silicon rod but without when growing into the diameter of pre-manufactured, the diameter meeting silicon core masterbatch requirement is elected as silicon core masterbatch at 110-130mm polycrystalline silicon rod。
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| CN112251807B (en) * | 2020-10-21 | 2022-08-30 | 亚洲硅业(青海)股份有限公司 | Silicon core preparation system and preparation method |
| CN114408927B (en) * | 2021-12-23 | 2023-08-01 | 亚洲硅业(青海)股份有限公司 | Preparation method of high-purity silicon core |
| 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 |
| CN114875486B (en) * | 2022-04-24 | 2024-03-22 | 新疆大全新能源股份有限公司 | Post-treatment process of polycrystalline silicon |
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