CN104118879A - Preparation method of silicon core master batch - Google Patents
Preparation method of silicon core master batch Download PDFInfo
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- CN104118879A CN104118879A CN201410382967.0A CN201410382967A CN104118879A CN 104118879 A CN104118879 A CN 104118879A CN 201410382967 A CN201410382967 A CN 201410382967A CN 104118879 A CN104118879 A CN 104118879A
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Abstract
The invention provides a preparation method of silicon core master batch. The preparation method comprises the following steps: introducing trichlorosilane gas and hydrogen into a reduction furnace to react to prepare polysilicon bar product materials, selecting polysilicon bars meeting requirements of the silicon core master batch with the diameter of 110-130mm from the polysilicon bar product materials, cutting the polysilicon bars to have the length required for drawing the silicon core, thereby obtaining the silicon core master batch after cleaning treatment. By producing the silicon core master batch with the preparation method, use level of hydrogen for reduction can be reduced, and energy consumption for producing the silicon core master batch can be effectively reduced so that the production cost is reduced.
Description
Technical field
The present invention relates to technical field of polysilicon production, particularly a kind of preparation method of silicon core masterbatch.
Background technology
The method for manufacturing polycrystalline silicon (also referred to as Siemens Method) that has Siemens to invent in 1954 being widely adopted at present in the production method of polysilicon: adopt high-purity trichlorosilane gas and high-purity hydrogen to mix formation mixed raw material gas according to certain proportioning, pass in reduction reactor, continuous deposition on the HIGH-PURITY SILICON core of heating, the diameter that makes silicon core chap and form polycrystalline silicon rod gradually.The production technique of the silicon core that used here mainly contains two kinds, a kind of is silicon core stove drawing silicon core, a kind of is cutting side's silicon core, through improving, silicon core stove drawing silicon core is drawn and has been transformed into existing five cores and draws by the single core in early stage, by once drawing one, has reformed into once drawing five silicon cores.
In prior art, in order to guarantee the normal of silicon core pulling process, safety is carried out, also in order to guarantee the quality of the silicon core of drawing, so the quality requirements of silicon core masterbatch requires high than polycrystalline silicon rod, silicon core masterbatch need meet following requirement: without deep layer crack, non-oxidation interlayer, without needle-like interlayer, be less than 1mm, sinuousness≤0.3% without the layering of silicon core circle, concave-convex surface degree.In order to obtain the silicon core masterbatch of above-mentioned requirements, up till now for this reason, all in the industry to produce by special-purpose reducing process, produce on the basis of polycrystalline silicon rod, strengthen the proportioning of hydrogen and trichlorosilane gas, control its growth temperature at 1060-1070 degree, thereby silicon rod growth velocity makes silicon rod surface uniform, slowly deposition obtains satisfactory silicon core masterbatch to reduce.This operational drawbacks is, because increase the proportioning of hydrogen and trichlorosilane gas, to make hydrogen consumption high; Reducing throughput rate can make growth cycle extend, thereby power consumption is increased, in the production of polysilicon, polycrystalline silicon rod product material power consumption is about 55-65KWh/kg-Si, and the power consumption of the technique that the polycrystalline silicon rod that meets the requirement of silicon core masterbatch in order to produce adopts is 100-110KWh/kg-Si, can find out that every kilogram of silicon core masterbatch power consumption is than every kilogram of many power consumptions of polysilicon degree more than 40.Therefore be badly in need of a kind ofly can producing satisfactory silicon core masterbatch, can reduce again the production method of the silicon core masterbatch of energy consumption.
The interim document that discloses a piece " application of polysilicon and production technology " of periodical < < Yunnan metallurgy > > the 36th volume the 5th of publishing in October, 2007, in document, point out, in order to reach energy-saving and cost-reducing object, polycrystalline silicon reducing furnace must maximize.The feature of large-scale energy-saving reduction furnace is: in stove, can heat the thermosteresis that at the beginning of many, rod is caused to reduce furnace wall radiation, the inwall of reduction furnace carries out mirror process simultaneously, makes radiant heat energy reflection, to reduce thermosteresis; Furnace pressure and air demand are improved, and have strengthened the speed of siliceous deposits reaction.Adopt 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 invention provides a kind of preparation method of silicon core masterbatch, adopt this kind of method to produce silicon core masterbatch, can reduce the consumption of hydrogen for reduction, can effectively reduce the energy consumption of producing silicon core masterbatch, thereby reduce production costs.
For solving the problems of the technologies described above, the present invention is achieved through the following technical solutions:
A kind of preparation method of silicon core masterbatch, comprise that trichlorosilane gas and hydrogen are passed into reaction in reduction furnace prepares polycrystalline silicon rod product material, then from polycrystalline silicon rod product material, selecting diameter is the polycrystalline silicon rod that silicon core masterbatch requires that meets of 110-130mm, cut into the needed length of drawing silicon core, after clean processing, obtain silicon core masterbatch.
In production process, there is splitting rod, equipment failures etc. need to shift to an earlier date blowing out, silicon rod is not also grown in the situation of diameter of pre-production, as long as meeting the diameter of silicon core masterbatch requirement also can elect as silicon core masterbatch at 110-130mm polycrystalline silicon rod, if the diameter when the pre-polycrystalline silicon rod product material of producing is the polycrystalline silicon rod of 130mm, but because there is splitting the problems such as rod or equipment failure, now the diameter of polycrystalline silicon rod does not also grow into 130mm with regard to blowing out, in this case, tear open after stove, that also can from these polycrystalline silicon rods, select that diameter is greater than 110mm meets polycrystalline silicon rod that silicon core masterbatch requires as silicon core masterbatch.
The preparation technology of described polycrystalline silicon rod product material is as follows: in reduction furnace, silicon core is added to 140-150A by silicon core electric current after suppressing successfully immediately, the empty 30-60min that burns of hydrogen, to reduction furnace, pass into trichlorosilane gas and the hydrogen after purification, power up stream to silicon core reacts simultaneously, reaction times is 80h, wherein:
In 0-10h step of reaction: trichlorosilane gas and hydrogen are increased to respectively to 140-160kg/h and 340-360kg/h uniformly from the flow of 0kg/h, and silicon core electric current is evenly increased to 440-460A from 140-150A;
10-20h step of reaction: trichlorosilane gas is increased to 240-260kg/h uniformly from 140-160kg/h, and hydrogen is increased to 490-510kg/h uniformly from 340-360kg/h, silicon core electric current is increased to 740-760A uniformly from 440-460A;
20-80h step of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 240-260kg/h and 490-510kg/h respectively, silicon core electric current: be evenly increased to 990-1010A at 20-30h, 30-40h is evenly increased to 1290-1310A, 40-50h is increased to 1390-1410A, and it is constant that 50-80h maintains 1390-1410A; After having reacted, blowing out, tears stove open.
The described polycrystalline silicon rod that meets the requirement of silicon core masterbatch refers to without deep layer crack, non-oxidation interlayer, without needle-like interlayer, without the layering of silicon core circle, concave-convex surface degree, is less than 1mm, the polycrystalline silicon rod of sinuousness≤0.3%.
Described polycrystalline silicon rod product material resistivity is 40 ~ 100 Ω .cm.
Described silicon core diameter is 10mm, and long is 2900mm.
Described polycrystalline silicon rod product material increases gradually 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, and 50h diameter is 103-107mm, and 60h diameter is 113-117mm, 70h diameter is 123-127mm, and 80h diameter is 128-132mm.
Silicon core is suppressed, observe silicon core, when silicon core is aglow, be that silicon core is suppressed successfully, silicon core electric current is added to 140-150A, makes silicon core temperature reach reaction temperature required, the empty 30-60min that burns of hydrogen, in reduction furnace, pass into trichlorosilane gas and hydrogen again, can remove other impurity such as water molecules that make in stove like this, make in stove cleanlyer, guarantee that polycrystalline silicon rod product material is free from foreign meter.
Beneficial effect:
1, the present invention directly from polycrystalline silicon rod product material, select diameter be 110-130mm meet polycrystalline silicon rod that silicon core masterbatch requires as silicon core masterbatch, the silicon core masterbatch that the reduction furnace that the current consumption of this silicon core masterbatch is special-purpose with employing and proprietary production technique are produced is compared, the every kilogram of electricity that can save degree more than 40, can find out, a polysilicon enterprise that produces 10000 tons per year, approximately need every year 500 tons of silicon core masterbatch, the poor words for calculating with 40 degree of power consumption of silicon core masterbatch and product material, the electricity that 500 tons of silicon core masterbatch can be saved is so 2,000 ten thousand degree, reduced greatly energy consumption, reduced production cost.
2, the present invention changes in prior art by strengthening the proportioning of trichlorosilane gas and hydrogen, control its growth temperature in the method for the production silicon core masterbatch of 1060-1070 degree, but do not increasing hydrogen consumption, keep growth temperature constant, on the constant basis of throughput rate, optimize the production technique 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 accordingly the magnitude of current according to trichlorosilane gas and hydrogen flowing quantity, make the polycrystalline silicon rod temperature of any time, throughput rate and polycrystalline silicon rod visual appearance reach optimum state, not only saved the consumption of hydrogen, shortened the production cycle, effectively improve the quality of polycrystalline silicon rod product material, reduced the production cost of silicon core masterbatch, improve per unit area yield.The polycrystalline silicon rod that makes to meet the requirement of silicon core masterbatch accounts for the 10-15% of polycrystalline silicon rod product material total mass, can meet need of production completely.
Embodiment
Below in conjunction with embodiment, describe the present invention in detail.
Embodiment 1
A kind of preparation method of silicon core masterbatch, comprise that trichlorosilane gas and hydrogen are passed into reaction in reduction furnace prepares polycrystalline silicon rod product material, then by drawing personnel to tear open stove scene from polycrystalline silicon rod product material, select diameter be 110-130mm to meet the polycrystalline silicon rod that silicon core masterbatch requires (can be whole, can be pipe nipple), cut into the needed length of drawing silicon core, after clean processing, obtain silicon core masterbatch.
Embodiment 2
A kind of preparation method of silicon core masterbatch, comprise that trichlorosilane gas and hydrogen are passed into reaction in reduction furnace prepares polycrystalline silicon rod product material, concrete technology is as follows, in reduction furnace, silicon core is added to 140A by silicon core electric current after suppressing successfully immediately, hydrogen is empty to be burnt after 30min, to reduction furnace, pass into trichlorosilane gas and the hydrogen after purification, power up stream to silicon core reacts simultaneously, reaction times is 80h, wherein: in 0-10h step of reaction: trichlorosilane gas and hydrogen are increased to respectively to 140kg/h and 340-kg/h uniformly from the flow of 0kg/h, silicon core electric current is evenly increased to 440A from 140A, 10-20h step of reaction: trichlorosilane gas is increased to 240kg/h uniformly from 140kg/h, and hydrogen is increased to 490kg/h uniformly from 340kg/h, silicon core electric current is increased to 740A uniformly from 440A, 20-80h step of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 240kg/h and 490kg/h respectively, silicon core electric current: be evenly increased to 990A at 20-30h, 30-40h is evenly increased to 1290A, and 40-50h is increased to 1390A, and it is constant that 50-80h maintains 1390A, after having reacted, the polycrystalline silicon rod diameter obtaining is 128-132mm, and blowing out, tears stove open.
After tearing stove open, by drawing personnel to tear open stove scene from these diameters are the polycrystalline silicon rod product material of 128-132 mm, select diameter be 128-130 mm to meet the polycrystalline silicon rod that silicon core masterbatch requires (can be whole, can be pipe nipple), cut into the masterbatch length that drawing needs, after clean processing, obtain silicon core masterbatch. by the preparation of the present embodiment, the silicon core masterbatch obtaining accounts for 10% of polycrystalline silicon rod product material total mass.
Embodiment 3
A kind of preparation method of silicon core masterbatch, comprise that trichlorosilane gas and hydrogen are passed into reaction in reduction furnace prepares polycrystalline silicon rod product material, the preparation technology of described polysilicon product material is as follows: in reduction furnace, silicon core is added to 145A by silicon core electric current after suppressing successfully immediately, the empty 45min that burns of hydrogen, to reduction furnace, pass into trichlorosilane gas and the hydrogen after purification, power up stream to silicon core reacts simultaneously, reaction times is 80h, wherein: in 0-10h step of reaction: trichlorosilane gas and hydrogen are increased to respectively to 150kg/h and 350kg/h uniformly from the flow of 0kg/h, silicon core electric current is evenly increased to 450A from 145A, 10-20h step of reaction: trichlorosilane gas is increased to 250kg/h uniformly from 150kg/h, and hydrogen is increased to 500kg/h uniformly from 350kg/h, silicon core electric current is increased to 750A uniformly from 450A, 20-80h step of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 250kg/h and 500kg/h respectively, silicon core electric current: be evenly increased to 1000A at 20-30h, 30-40h is evenly increased to 1300A, and 40-50h is increased to 1400A, and it is constant that 50-80h maintains 1400A, after having reacted, the diameter of the polycrystalline silicon rod product material making is 128-132mm, and blowing out, tears stove open.
After tearing stove open, by drawing personnel, to tearing stove scene open, from polycrystalline silicon rod product material, to select diameter be that the polycrystalline silicon rod that 128-130mm meets the requirement of silicon core masterbatch (can be whole, can be pipe nipple), cut into the masterbatch length that drawing needs, after clean processing, obtain silicon core masterbatch, the silicon core masterbatch that the present embodiment obtains accounts for 15% of polycrystalline silicon rod product material total mass.
Embodiment 4
A kind of preparation method of silicon core masterbatch, comprise that trichlorosilane gas and hydrogen are passed into reaction in reduction furnace prepares polycrystalline silicon rod product material, the preparation technology of described polysilicon product material is as follows: in reduction furnace, silicon core is added to 150A by silicon core electric current after suppressing successfully immediately, wait for 60min, to reduction furnace, pass into trichlorosilane gas and the hydrogen after purification, power up stream to silicon core reacts simultaneously, reaction times is 80h, wherein: in 0-10h step of reaction: trichlorosilane gas and hydrogen are increased to respectively to 160kg/h and 360kg/h uniformly from the flow of 0kg/h, silicon core electric current is evenly increased to 460A from 150A, 10-20h step of reaction: trichlorosilane gas is increased to 260kg/h uniformly from 160kg/h, and hydrogen is increased to 510kg/h uniformly from 360kg/h, silicon core electric current is increased to 760A uniformly from 460A, 20-80h step of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 260kg/h and 510kg/h respectively, silicon core electric current: be evenly increased to 1010A at 30h, 30-40h is evenly increased to 1310A, and 40-50h is increased to 1410A, and it is constant that 50-80h maintains 1410A, after having reacted, the diameter of the polycrystalline silicon rod product material making is 128-132mm, and blowing out, tears stove open.
After tearing stove open, by drawing personnel, to tearing stove scene open, from polycrystalline silicon rod product material, select the polycrystalline silicon rod (can be whole, can be pipe nipple) that meets the requirement of silicon core masterbatch, cut into the masterbatch length that drawing needs, after clean processing, obtain silicon core masterbatch.The silicon core masterbatch that the present embodiment obtains accounts for 13% of polycrystalline silicon rod product material total mass.
Embodiment 5
A kind of preparation method of silicon core masterbatch, comprise that trichlorosilane gas and hydrogen are passed into reaction in reduction furnace prepares polycrystalline silicon rod product material, the preparation technology of described polysilicon product material is as follows: in reduction furnace, silicon core is added to 150A by silicon core electric current after suppressing successfully immediately, the empty 55min that burns of hydrogen, to reduction furnace, pass into trichlorosilane gas and the hydrogen after purification, power up stream to silicon core reacts simultaneously, reaction times is 80h, wherein: in 0-10h step of reaction: trichlorosilane gas and hydrogen are increased to respectively to 155kg/h and 355kg/h uniformly from the flow of 0kg/h, silicon core electric current is evenly increased to 455A from 150A, 10-20h step of reaction: trichlorosilane gas is increased to 255kg/h uniformly from 155kg/h, and hydrogen is increased to 505kg/h uniformly from 355kg/h, silicon core electric current is increased to 755A uniformly from 455A, 20-80h step of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 255kg/h and 505kg/h respectively, silicon core electric current: be evenly increased to 1005A at 30h, 30-40h is evenly increased to 1305A, and 40-50h is increased to 1405A, and it is constant that 50-80h maintains 1405A, after having reacted, the diameter of the polycrystalline silicon rod product material making is 128-132mm, and blowing out, tears stove open.
After tearing stove open, by drawing personnel, to tearing stove scene open, from polycrystalline silicon rod product material, select that to meet the polycrystalline silicon rod that the diameter of silicon core masterbatch requirement is 128-130mm (can be whole, can be pipe nipple), cut into the masterbatch length that drawing needs, after clean processing, obtain silicon core masterbatch.The silicon core masterbatch that the present embodiment obtains accounts for 14% of polycrystalline silicon rod product material total mass.
Embodiment 6
A kind of preparation method of silicon core masterbatch, comprise that trichlorosilane gas and hydrogen are passed into reaction in reduction furnace prepares polycrystalline silicon rod product material, then from polycrystalline silicon rod product material, selecting diameter is the polycrystalline silicon rod that silicon core masterbatch requires that meets of 110-130mm, cut into the needed length of drawing silicon core, after clean processing, obtain silicon core masterbatch.The described polycrystalline silicon rod that meets the requirement of silicon core masterbatch refers to without deep layer crack, non-oxidation interlayer, without needle-like interlayer, without the layering of silicon core circle, concave-convex surface degree, is less than 1mm, the polycrystalline silicon rod of sinuousness≤0.3%.
Embodiment 7
A kind of preparation method of silicon core masterbatch, comprise that trichlorosilane gas and hydrogen are passed into reaction in reduction furnace prepares polycrystalline silicon rod product material, the preparation technology of described polysilicon product material is as follows: in reduction furnace, silicon core is added to 145A by silicon core electric current after suppressing successfully immediately, the empty 50min that burns of hydrogen, to reduction furnace, pass into trichlorosilane gas and the hydrogen after purification, power up stream to silicon core reacts simultaneously, reaction times is 80h, wherein: in 0-10h step of reaction: trichlorosilane gas and hydrogen are increased to respectively to 145kg/h and 345kg/h uniformly from the flow of 0kg/h, silicon core electric current is evenly increased to 445A from 145A, 10-20h step of reaction: trichlorosilane gas is increased to 245kg/h uniformly from 145kg/h, and hydrogen is increased to 495kg/h uniformly from 345kg/h, silicon core electric current is increased to 745A uniformly from 445A, 20-80h step of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 245kg/h and 495kg/h respectively, silicon core electric current: be evenly increased to 995A at 20-30h, 30-40h is evenly increased to 1295A, and 40-50h is increased to 1395A, and it is constant that 50-80h maintains 1395A, after having reacted, the diameter of polycrystalline silicon rod product material is 128-132mm, and blowing out, tears stove open.After tearing stove open, from polycrystalline silicon rod product material, select the polycrystalline silicon rod that silicon core masterbatch requires that meets that diameter is 128-130mm, cut into the needed length of drawing silicon core, after clean processing, obtain silicon core masterbatch.The present embodiment silicon core masterbatch accounts for 12% of polycrystalline silicon rod product material total mass, and in the present embodiment, silicon core diameter used is 10mm, and long is 2900mm.
In the process of growth of polycrystalline silicon rod, 0-80h interior diameter increases gradually, wherein the diameter of the polycrystalline silicon rod product material when 10h is 28-32mm, during 20h, diameter is 48-52mm, and during 30h, diameter is 68-72mm, and during 40h, diameter is 88-92mm, during 50h, diameter is 103-107mm, during 60h, diameter is 113-117mm, and during 70h, diameter is 123-127mm, and during 80h, diameter is 128-132mm.The resistivity of described polycrystalline silicon rod product material is 40 ~ 100 Ω .cm.
Claims (7)
1. the preparation method of a silicon core masterbatch, it is characterized in that: trichlorosilane gas and hydrogen are passed into reaction in reduction furnace and make after polycrystalline silicon rod product material, from polycrystalline silicon rod product material, selecting diameter is the polycrystalline silicon rod that silicon core masterbatch requires that meets of 110-130mm again, cut into the needed length of drawing silicon core, after clean processing, obtain silicon core masterbatch.
2. the preparation method of a kind of silicon core masterbatch according to claim 1, it is characterized in that: the preparation technology of described polycrystalline silicon rod product material is as follows: in reduction furnace, silicon core is added to 140-150A by silicon core electric current after suppressing successfully immediately, wait for 30-60min, to reduction furnace, pass into trichlorosilane gas and the hydrogen after purification, power up stream to silicon core simultaneously and react, the reaction times is 80h, wherein:
In 0-10h step of reaction: trichlorosilane gas and hydrogen are increased to respectively to 140-160kg/h and 340-360kg/h uniformly from the flow of 0kg/h, and silicon core electric current is evenly increased to 440-460A from 140-150A;
10-20h step of reaction: trichlorosilane gas is increased to 240-260kg/h uniformly from 140-160kg/h, and hydrogen is increased to 490-510kg/h uniformly from 340-360kg/h, silicon core electric current is increased to 740-760A uniformly from 440-460A;
20-80h step of reaction: trichlorosilane gas and hydrogen maintain 60h with the flow of 240-260kg/h and 490-510kg/h respectively, silicon core electric current: be evenly increased to 990-1010A at 20-30h, 30-40h is evenly increased to 1290-1310A, 40-50h is increased to 1390-1410A, and it is constant that 50-80h maintains 1390-1410A; After having reacted, blowing out, tears stove open.
3. the preparation method of a kind of silicon core masterbatch according to claim 1, it is characterized in that: the described polycrystalline silicon rod that meets the requirement of silicon core masterbatch refers to without deep layer crack, non-oxidation interlayer, without needle-like interlayer, without the layering of silicon core circle, concave-convex surface degree, is less than 1mm, the polycrystalline silicon rod of sinuousness≤0.3%.
4. the preparation method of a kind of silicon core masterbatch according to claim 2, is characterized in that: described polycrystalline silicon rod product material resistivity is 40 ~ 100 Ω .cm.
5. the preparation method of a kind of silicon core masterbatch according to claim 2, is characterized in that: described silicon core diameter is 10mm, and long is 280mm.
6. the preparation method of a kind of silicon core masterbatch according to claim 2, it is characterized in that: described polycrystalline silicon rod product material increases gradually at 0-80h interior diameter, wherein the polycrystalline silicon rod product material diameter when 10h is 28-32mm, 20h diameter is 48-52mm, and 30h diameter is 68-72mm, and 40h diameter is 88-92mm, 50h diameter is 103-107mm, 60h diameter is 113-117mm, and 70h diameter is 123-127mm, and 80h diameter is 128-132mm.
7. the preparation method of a kind of silicon core masterbatch according to claim 1 and 2, it is characterized in that: in production process, occur splitting rod, equipment failure need to shift to an earlier date blowing out, silicon rod is not also grown in the situation of diameter of pre-production, is also can elect as silicon core masterbatch as long as meet the diameter of silicon core masterbatch requirement at 110-130mm polycrystalline silicon rod.
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| CN112251807A (en) * | 2020-10-21 | 2021-01-22 | 亚洲硅业(青海)股份有限公司 | Silicon core preparation system and preparation method |
| CN114212794A (en) * | 2021-12-30 | 2022-03-22 | 新疆大全新能源股份有限公司 | Production method for preparing primary polycrystalline silicon rod of electronic grade square silicon core and reduction furnace |
| CN114408927A (en) * | 2021-12-23 | 2022-04-29 | 亚洲硅业(青海)股份有限公司 | Preparation method and preparation device of high-purity silicon core |
| CN114875486A (en) * | 2022-04-24 | 2022-08-09 | 新疆大全新能源股份有限公司 | Post-treatment process of polycrystalline silicon |
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