CN104003397B - Trichlorosilane reduction process control method - Google Patents
Trichlorosilane reduction process control method Download PDFInfo
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- CN104003397B CN104003397B CN201410271960.1A CN201410271960A CN104003397B CN 104003397 B CN104003397 B CN 104003397B CN 201410271960 A CN201410271960 A CN 201410271960A CN 104003397 B CN104003397 B CN 104003397B
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Abstract
The present invention relates to a kind of trichlorosilane reduction process control method, this control method comprises initial reaction and controls the stage, stablizes reaction controlling stage and end of a period reaction controlling stage, SiHCl within the initial reaction control stage
3flow control at 260m
3/ below h, H
2flow control at 520m
3/ below h, current control between 30-1000A, at stable reaction controlling stage SiHCl
3flow control at 175-260m
3between/h, H
2flow control at 385-520m
3between/h, current control between 1000-2000A, at end of a period reaction controlling stage SiHCl
3flow control at 130-250m
3between/h, H
2flow control at 360-520m
3between/h, current control is between 100-800A.The present invention improves the productive rate of trichlorosilane and reduces energy consumption, greatly reduces the object of the production cost of enterprise.
Description
Technical field
The present invention relates to a kind of polysilicon production process control method, particularly relate to the control method of trichlorosilane reduction technique in polysilicon production process.
Background technology
At present, the production technique of polysilicon is mainly improved Siemens, and its principle is exactly reduce high-purity trichlorosilane by High Purity Hydrogen on the HIGH-PURITY SILICON core of about 1100 DEG C, generates polysilicon deposition on silicon core.Improvement Siemens process is on the basis of traditional Siemens process, possesses energy-conservation, consumption reduction simultaneously, recycles in production process a large amount of H supervened
2, HCI, SiCI
4deng the process matched therewith of by product and a large amount of by-product heat energy.Most producer all adopts improved Siemens to produce polysilicon in the world at present.Its production craft step is:
(1) quartz sand is smelted and is purified to 98% and generates its chemical reaction of industrial silicon SiO in electric arc furnace
2+ C → Si+CO
2, in order to meet highly purified needs, must purify further in ↑ (2).Industrial silicon pulverized and uses anhydrous hydrogen chloride (HCl) to react with it in a fluidized-bed reactor, generating the trichlorosilane (SiHCl intending dissolving
3).Its chemical reaction Si+HCl → SiHCl
3+ H2 ↑ temperature of reaction is 300 degree, and this reaction is heat release.Form gaseous mixture (H simultaneously
2, HCL, SiHCl
3, SiCl
4, Si).(3) gaseous mixture produced in second step also needs further purification, needs to decompose to filter silica flour, condensation SiHCl
3, SiCl
4, and gaseous state H
2, HCl turns back in reaction or is discharged in air.Then condensation product SiHCl is decomposed
3, SiCl
4, purification trichlorosilane (multistage rectification).(4) trichlorosilane after purification adopts high temperature reduction technique, with high-purity SiHCl
3at H
2in atmosphere, reduction deposits and generates polysilicon.Its chemical reaction SiHCl
3+ H
2→ Si+HCl.The reaction vessel of polysilicon is what seal, and with electrically heated silicon pond silicon rod (diameter 5-10 millimeter, length 1.5-2 rice, quantity 80), at 1050-1100 degree growing polycrystalline silicon on rod, diameter can reach 150-200 millimeter.The trichlorosilane of about like this 1/3rd reacts, and generates polysilicon.The same H of remainder
2, HCL, SiHCl
3, SiCl
4be separated from reaction vessel.These mixtures carry out low ternperature separation process, or recycling, or turn back in whole reaction.
In siemens's improved method production technique, some gordian technique China also do not grasp, and in extractive process, the polysilicon of more than 70% has all been discharged by chlorine, not only refine cost high, and environmental pollution are very serious.
Therefore how to improve the productive rate of polysilicon, reducing energy consumption is the most important thing that polysilicon production process improves.
Summary of the invention
In order to overcome existing polysilicon production process low yield, defect that energy consumption is high, the invention provides a kind of trichlorosilane reduction process control method, this control method, by reaching the productive rate and reduction energy consumption that improve trichlorosilane to the control of trichlorosilane reduction technique parameters, reduces the object of the production cost of enterprise greatly.
In the one-tenth production art of polysilicon, use H
2the step that reduction trichlorosilane generates polysilicon on silicon rod is the most important step of this technique, the key point of the height of polysilicon productive rate is also the control to this processing step, the key point that therefore will improve polysilicon productive rate is the control to this processing step, and this processing step is the reaction process of carrying out under the high temperature conditions, consume energy high, reduce energy consumption, also need reasonably to control this processing step.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of trichlorosilane reduction process control method, it is characterized in that: this control method comprises initial reaction and controls the stage, stablizes reaction controlling stage and end of a period reaction controlling stage, the time that described initial reaction controls the stage is within first 24 hours of reaction beginning, the time in described stable reaction controlling stage is greater than 24 hours and within 64 hours, described end of a period reaction controlling phases-time is greater than 64 hours and within 100 hours, SiHCl within the initial reaction control stage
3flow control at 260m
3/ below h, H
2flow control at 520m
3/ below h, current control between 30-1000A, at stable reaction controlling stage SiHCl
3flow control at 175-260m
3between/h, H
2flow control at 385-520m
3between/h, current control between 1000-2000A, at end of a period reaction controlling stage SiHCl
3flow control at 130-250m
3between/h, H
2flow control at 360-520m
3between/h, current control is between 100-800A.
In the initial reaction control stage, in reaction beginning within 8 hours, SiHCl
3flow control at 0-180m
3/ h, H
2flow control at 0-370m
3/ h, current control, at 30-450A, is being greater than 8 hours and in 16 hours, SiHCl
3flow control at 180-240m
3/ h, H
2flow control at 390-500m
3/ h, current control, at 510-750A, is being greater than 16 hours and in 24 hours, SiHCl
3flow control at 180-260m
3/ h, H
2flow control at 390-520m
3/ h, current control is at 700-1000A.
In the stable reaction controlling stage, be greater than 24 hours and within 32 hours, SiHCl
3flow control at 175-260m
3/ h, H
2flow control at 385-520m
3/ h, current control, at 1000-1250A, is being greater than 32 hours and within 40 hours, SiHCl
3flow control at 170-260m
3/ h, H
2flow control at 380-520m
3/ h, current control, at 1200-1420A, is being greater than 40 hours and within 48 hours, SiHCl
3flow control at 165-260m
3/ h, H
2flow control at 375-520m
3/ h, current control, at 1200-1620A, is being greater than 48 hours and within 56 hours, SiHCl
3flow control at 160-250m
3/ h, H
2flow control at 370-520m
3/ h, current control, at 1200-1820A, is being greater than 56 hours and within 64 hours, SiHCl
3flow control at 155-250m
3/ h, H
2flow control at 365-520m
3/ h, current control is at 1200-2000A.
In the end of a period reaction controlling stage, be greater than 64 hours and within 72 hours, SiHCl
3flow control at 150-250m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 1000-2000A, is being greater than 72 hours and within 80 hours, SiHCl
3flow control at 145-240m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 800-2000A, is being greater than 80 hours and within 88 hours, SiHCl
3flow control at 140-240m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 600-2000A, is being greater than 88 hours and within 96 hours, SiHCl
3flow control at 135-230m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 400-2000A, is being greater than 96 hours and within 100 hours, SiHCl
3flow control at 130-220m
3/ h, H
2flow control at 360-520m
3/ h, current control is at 100-2000A.
In the initial reaction control stage, control as follows: in reaction at first, SiHCl
3flow control at 0-50m
3/ h, H
2flow control at 0-300m
3/ h, current control at 30-140A, in 8 hours, SiHCl
3flow control at 80-180m
3/ h, H
2flow control at 260-370m
3/ h, current control at 250-450A, in 16 hours, SiHCl
3flow control at 180-240m
3/ h, H
2flow control at 390-500m
3/ h, current control at 510-750A, in 24 hours, SiHCl
3flow control at 180-260m
3/ h, H
2flow control at 390-520m
3/ h, current control is at 700-1000A.
In the stable reaction controlling stage, in 32 hours, SiHCl
3flow control at 175-260m
3/ h, H
2flow control at 385-520m
3/ h, current control at 1000-1250A, in 40 hours, SiHCl
3flow control at 170-260m
3/ h, H
2flow control at 380-520m
3/ h, current control at 1200-1420A, in 48 hours, SiHCl
3flow control at 165-260m
3/ h, H
2flow control at 375-520m
3/ h, current control at 1200-1620A, in 56 hours, SiHCl
3flow control at 160-250m
3/ h, H
2flow control at 370-520m
3/ h, current control at 1200-1820A, in 64 hours, SiHCl
3flow control at 155-250m
3/ h, H
2flow control at 365-520m
3/ h, current control is at 1200-2000A.
In the end of a period reaction controlling stage, in 72 hours, SiHCl
3flow control at 150-250m
3/ h, H
2flow control at 360-520m
3/ h, current control at 1000-2000A, in 80 hours, SiHCl
3flow control at 145-240m
3/ h, H
2flow control at 360-520m
3/ h, current control at 800-2000A, in 88 hours, SiHCl
3flow control at 140-240m
3/ h, H
2flow control at 360-520m
3/ h, current control at 600-2000A, in 96 hours, SiHCl
3flow control at 135-230m
3/ h, H
2flow control at 360-520m
3/ h, current control at 400-2000A, in 100 hours, SiHCl
3flow control at 130-220m
3/ h, H
2flow control at 360-520m
3/ h, current control is at 100-2000A.
The present invention has the following advantages:
The present invention includes initial reaction to control the stage, stablize reaction controlling stage and end of a period reaction controlling stage, the time that described initial reaction controls the stage is within first 24 hours of reaction beginning, the time in described stable reaction controlling stage is greater than 24 hours and within 64 hours, described end of a period reaction controlling phases-time is greater than 64 hours and within 100 hours, SiHCl within the initial reaction control stage
3flow control at 260m
3/ below h, H
2flow control at 520m
3/ below h, current control between 30-1000A, at stable reaction controlling stage SiHCl
3flow control at 175-260m
3between/h, H
2flow control at 385-520m
3between/h, current control between 1000-2000A, at end of a period reaction controlling stage SiHCl
3flow control at 130-250m
3between/h, H
2flow control at 360-520m
3between/h, current control is between 100-800A.Trichlorosilane reduction process control method is subdivided into three control stages by the present invention, in each control stage, trichlorosilane flow, hydrogen flowing quantity and electric current are controlled accurately, by affecting the conservative control of polysilicon parameter of increment on silicon rod to these three, substantially increase the output of trichlorosilane.The stage is controlled at initial reaction, reaction is now comparatively slow, slowly passes into small electric stream, allows silicon rod preheating, pass into a small amount of trichlorosilane and hydrogen, allow sluggish start, a small amount of polysilicon, at silicon rod Surface Creation, provides to the attachment of next step polysilicon and puts forth effort bed, the attachment being beneficial to polysilicon generates, less at the growing amount of this stage polysilicon, pass into a small amount of electricity, trichlorosilane and hydrogen, the consumption of electric energy and the consumption of trichlorosilane and hydrogen can be saved; In the stable reaction controlling stage, be now a large amount of periods that polysilicon generates, during this stage, improve the critical period of polysilicon output, in this stage current control between 1000-2000A, ensure silicon rod surface temperature control at about 1080 DEG C, SiHCl
3flow control at 175-260m
3between/h, H
2flow control at 385-520m
3between/h, allow SiHCl
3rapid, high volume generated polysilicon by hydrogen reducing, before adding, initial reaction controls the implantation in advance of a small amount of polysilicon in stage, and now polysilicon will generate in a large number on silicon rod; In the end of a period reaction controlling stage; gradually reduce passing into of hydrogen and trichlorosilane flow; now; the Main Function of hydrogen is protection dilution and cooling; be beneficial to trichlorosilane reduction and become polysilicon, reduce electric current in this stage, utilize the temperature of stove inner exhaust gas to impel the generation of polysilicon; reduce the consumption of electric energy, the reduction of temperature can also well impel the polysilicon deposition of generation to get off.
2, in the initial reaction control stage, in reaction beginning within 8 hours, SiHCl
3flow control at 0-180m
3/ h, H
2flow control at 0-370m
3/ h, current control, at 30-450A, is being greater than 8 hours and in 16 hours, SiHCl
3flow control at 180-240m
3/ h, H
2flow control at 390-500m
3/ h, current control, at 510-750A, is being greater than 16 hours and in 24 hours, SiHCl
3flow control at 180-260m
3/ h, H
2flow control at 390-520m
3/ h, current control is at 700-1000A.The present invention is divided into 0-8 hour at concrete stage that controlled by initial reaction, 8-16 hour, 16-24 hour three phases, carry out restriction further to the hydrogen flowing quantity of three phases, trichlorosilane flow and electric current respectively to control, controlled by the concrete cooperation of these parameters, the consumption of the consumption of saves energy while impelling polysilicon tentatively to generate, the consumption of hydrogen and trichlorosilane, impel preliminary generation and the implantation in advance of polysilicon with a small amount of raw material and a small amount of electric current as far as possible, be beneficial to the carrying out in stable reaction controlling stage.
3, in the stable reaction controlling stage, 24 hours are being greater than and within 32 hours, SiHCl
3flow control at 175-260m
3/ h, H
2flow control at 385-520m
3/ h, current control, at 1000-1250A, is being greater than 32 hours and within 40 hours, SiHCl
3flow control at 170-260m
3/ h, H
2flow control at 380-520m
3/ h, current control, at 1200-1420A, is being greater than 40 hours and within 48 hours, SiHCl
3flow control at 165-260m
3/ h, H
2flow control at 375-520m
3/ h, current control, at 1200-1620A, is being greater than 48 hours and within 56 hours, SiHCl
3flow control at 160-250m
3/ h, H
2flow control at 370-520m
3/ h, current control, at 1200-1820A, is being greater than 56 hours and within 64 hours, SiHCl
3flow control at 155-250m
3/ h, H
2flow control at 365-520m
3/ h, current control is at 1200-2000A.In this stage, we control to be divided into 24-32 hour, 32-40 hour, 40-48 hour, 48-56,56-64 hour double teacher control, to the accurate control of hydrogen, trichlorosilane and electric current in this double teacher, these three parameters are limited in the scope provided, can allow the generation that polysilicon is a large amount of.
4, in the end of a period reaction controlling stage, 64 hours are being greater than and within 72 hours, SiHCl
3flow control at 150-250m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 1000-2000A, is being greater than 72 hours and within 80 hours, SiHCl
3flow control at 145-240m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 800-2000A, is being greater than 80 hours and within 88 hours, SiHCl
3flow control at 140-240m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 600-2000A, is being greater than 88 hours and within 96 hours, SiHCl
3flow control at 135-230m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 400-2000A, is being greater than 96 hours and within 100 hours, SiHCl
3flow control at 130-220m
3/ h, H
2flow control at 360-520m
3/ h, current control is at 100-2000A.This stage be divided into 64-72 hour, 72-80 hour, 80-88 hour, 88-96 hour, 96-100 hour double teacher; the hydrogen of this double teacher, electric current and trichlorosilane design parameter are controlled; the heat of furnace gas can be made full use of by the control of these parameters; the consumption of electric energy is saved while allowing reaction go on; protect polysilicon simultaneously and reduce in-furnace temperature, being beneficial to the generation of polysilicon.
Embodiment
Embodiment 1
In the initial reaction control stage, before starting the reaction in 8 hours, SiHCl
3flow control 50m
3/ h, H
2flow control at 320m
3/ h, current control, at 200A, (did not comprise 8 hours), SiHCl within 8-16 hour
3flow control at 186m
3/ h, H
2flow control at 420m
3/ h, current control, at 600A, (did not comprise 16 hours), SiHCl within 16-24 hour
3flow control at 210m
3/ h, H
2flow control at 400m
3/ h, current control is at 785A.
In the stable reaction controlling stage, within 24-32 hour, (do not comprise 24 hours), SiHCl
3flow control at 185m
3/ h, H
2flow control at 385m
3/ h, current control, at 1250A, (did not comprise 32 hours), SiHCl within 32-40 hour
3flow control at 185m
3/ h, H
2flow control at 380m
3/ h, current control, at 1200A, (did not comprise 40 hours), SiHCl within 40-48 hour
3flow control at 260m
3/ h, H
2flow control at 520m
3/ h, current control, at 1200A, (did not comprise 48 hours), SiHCl within 48-56 hour
3flow control at 250m
3/ h, H
2flow control at 370m
3/ h, current control, at 1200A, (did not comprise 56 hours), SiHCl within 56-64 hour
3flow control at 225m
3/ h, H
2flow control at 384m
3/ h, current control is at 1248A.
In the end of a period reaction controlling stage, within 64-72 hour, (do not comprise 64 hours), SiHCl
3flow control at 250m
3/ h, H
2flow control at 360m
3/ h, current control, at 1000A, (did not comprise 72 hours), SiHCl within 72-80 hour
3flow control at 240m
3/ h, H
2flow control at 380m
3/ h, current control, at 800A, (did not comprise 80 hours), SiHCl within 80-88 hour
3flow control at 140m
3/ h, H
2flow control at 520m
3/ h, current control, at 600A, (did not comprise 88 hours), SiHCl within 88-96 hour
3flow control at 150m
3/ h, H
2flow control at 420m
3/ h, current control at 400A, within 96-100 hour (not comprising 96 hours), SiHCl
3flow control at 190m
3/ h, H
2flow control at 400m
3/ h, current control is at 100A.
Embodiment 2
In the initial reaction control stage, in reaction beginning 8 hours, SiHCl
3flow control at 90m
3/ h, H
2flow control at 150m
3/ h, current control, at 30A, (did not comprise 8 hours), SiHCl within 8-16 hour
3flow control at 180m
3/ h, H
2flow control at 400m
3/ h, current control, at 620A, (did not comprise 16 hours), SiHCl within 16-24 hour
3flow control at 220m
3/ h, H
2flow control at 390m
3/ h, current control is at 800A.
In the stable reaction controlling stage, within 24-32 hour, (do not comprise 24 hours), SiHCl
3flow control at 200m
3/ h, H
2flow control at 420m
3/ h, current control, at 1100A, (did not comprise 32 hours), SiHCl within 32-40 hour
3flow control at 170m
3/ h, H
2flow control at 390m
3/ h, current control, at 1300A, (did not comprise 40 hours), SiHCl within 40-48 hour
3flow control at 185m
3/ h, H
2flow control at 425m
3/ h, current control, at 1450A, (did not comprise 48 hours), SiHCl within 48-56 hour
3flow control at 168m
3/ h, H
2flow control at 430m
3/ h, current control, at 1350A, (did not comprise 56 hours), SiHCl within 56-64 hour
3flow control at 165m
3/ h, H
2flow control at 410m
3/ h, current control is at 1400A.
In the end of a period reaction controlling stage, within 64-72 hour, (do not comprise 64 hours), SiHCl
3flow control at 160m
3/ h, H
2flow control at 360m
3/ h, current control, at 1200A, (did not comprise 72 hours), SiHCl within 72-80 hour
3flow control at 165m
3/ h, H
2flow control at 380m
3/ h, current control, at 900A, (did not comprise 80 hours), SiHCl within 80-88 hour
3flow control at 160m
3/ h, H
2flow control at 420m
3/ h, current control, at 800A, (did not comprise 88 hours), SiHCl within 88-96 hour
3flow control at 145m
3/ h, H
2flow control at 380m
3/ h, current control, at 600A, (did not comprise 96 hours), SiHCl within 96-100 hour
3flow control at 130m
3/ h, H
2flow control at 360m
3/ h, current control is at 400A.
Embodiment 3
In the initial reaction control stage, in reaction beginning 8 hours, SiHCl
3flow control at 60m
3/ h, H
2flow control at 120m
3/ h, current control, at 30A, (did not comprise 8 hours), SiHCl within 8-16 hour
3flow control at 240m
3/ h, H
2flow control at 420m
3/ h, current control, at 700A, (did not comprise 16 hours), SiHCl within 16-24 hour
3flow control at 195m
3/ h, H
2flow control at 440m
3/ h, current control is at 700A.
In the stable reaction controlling stage, within 24-32 hour, (do not comprise 24 hours), SiHCl
3flow control at 210m
3/ h, H
2flow control at 440m
3/ h, current control, at 1200A, (did not comprise 32 hours), SiHCl within 32-40 hour
3flow control at 260m
3/ h, H
2flow control at 500m
3/ h, current control, at 1300A, (did not comprise 40 hours), SiHCl within 40-48 hour
3flow control at 185m
3/ h, H
2flow control at 500m
3/ h, current control, at 1400A, (did not comprise 48 hours), SiHCl within 48-56 hour
3flow control at 178m
3/ h, H
2flow control at 510m
3/ h, current control, at 1600A, (did not comprise 56 hours), SiHCl within 56-64 hour
3flow control at 158m
3/ h, H
2flow control at 520m
3/ h, current control is at 1200A.
In the end of a period reaction controlling stage, within 64-72 hour, (do not comprise 64 hours), SiHCl
3flow control at 230m
3/ h, H
2flow control at 480m
3/ h, current control, at 1400A, (did not comprise 72 hours), SiHCl within 72-80 hour
3flow control at 145m
3/ h, H
2flow control at 360m
3/ h, current control, at 1500A, (did not comprise 80 hours), SiHCl within 80-88 hour
3flow control at 160m
3/ h, H
2flow control at 400m
3/ h, current control, at 1800A, (did not comprise 88 hours), SiHCl within 88-96 hour
3flow control at 230m
3/ h, H
2flow control at 480m
3/ h, current control, at 800A, (did not comprise 96 hours), SiHCl within 96-100 hour
3flow control at 182m
3/ h, H
2flow control at 360m
3/ h, current control is at 500A.
Embodiment 4
In the initial reaction control stage, in reaction beginning 8 hours, SiHCl
3flow control at 20m
3/ h, H
2flow control at 40m
3/ h, current control, at 300A, (did not comprise 8 hours), SiHCl within 8-16 hour
3flow control at 240m
3/ h, H
2flow control at 420m
3/ h, current control, at 555A, (did not comprise 16 hours), SiHCl within 16-24 hour
3flow control at 200m
3/ h, H
2flow control at 520m
3/ h, current control is at 900A.
In the stable reaction controlling stage, within 24-32 hour, (do not comprise 24 hours), SiHCl
3flow control at 260m
3/ h, H
2flow control at 400m
3/ h, current control, at 1250A, (did not comprise 32 hours), SiHCl within 32-40 hour
3flow control at 260m
3/ h, H
2flow control at 440m
3/ h, current control, at 1350A, (did not comprise 40 hours), SiHCl within 40-48 hour
3flow control at 199m
3/ h, H
2flow control at 420m
3/ h, current control, at 1600A, (did not comprise 48 hours), SiHCl within 48-56 hour
3flow control at 225m
3/ h, H
2flow control at 450m
3/ h, current control, at 1750A, (did not comprise 56 hours), SiHCl within 56-64 hour
3flow control 195m
3/ h, H
2flow control at 445m
3/ h, current control is at 1800A.
In the end of a period reaction controlling stage, within 64-72 hour, (do not comprise 64 hours), SiHCl
3flow control at 185m
3/ h, H
2flow control at 445m
3/ h, current control, at 1000A, (did not comprise 72 hours), SiHCl within 72-80 hour
3flow control at 900m
3/ h, H
2flow control at 440m
3/ h, current control, at 800A, (did not comprise 80 hours), SiHCl within 80-88 hour
3flow control at 160m
3/ h, H
2flow control at 420m
3/ h, current control, at 700A, (did not comprise 88 hours), SiHCl within 88-96 hour
3flow control at 165m
3/ h, H
2flow control at 420m
3/ h, current control, at 400A, (did not comprise 96 hours), SiHCl within 96-100 hour
3flow control at 205m
3/ h, H
2flow control at 452m
3/ h, current control is at 600A.
Embodiment 5
In the initial reaction control stage, control as follows: in reaction at first, SiHCl
3flow control at 50m
3/ h, H
2flow control at 220m
3/ h, current control at 120A, in 8 hours, SiHCl
3flow control at 80m
3/ h, H
2flow control at 300m
3/ h, current control at 350A, in 16 hours, SiHCl
3flow control at 240m
3/ h, H
2flow control at 390m
3/ h, current control at 750A, in 24 hours, SiHCl
3flow control at 260m
3/ h, H
2flow control at 390m
3/ h, current control is at 700A.
In the stable reaction controlling stage, in 32 hours, SiHCl
3flow control at 260m
3/ h, H
2flow control at 385m
3/ h, current control at 1000A, in 40 hours, SiHCl
3flow control at 260m
3/ h, H
2flow control at 380m
3/ h, current control at 1200A, in 48 hours, SiHCl
3flow control at 260m
3/ h, H
2flow control at 375m
3/ h, current control at 1200A, in 56 hours, SiHCl
3flow control at 160m
3/ h, H
2flow control at 520m
3/ h, current control at 1200A, in 64 hours, SiHCl
3flow control at 250m
3/ h, H
2flow control at 520m
3/ h, current control is at 1200A.
In the end of a period reaction controlling stage, in 72 hours, SiHCl
3flow control at 150m
3/ h, H
2flow control at 520m
3/ h, current control at 2000A, in 80 hours, SiHCl
3flow control at 240m
3/ h, H
2flow control at 360m
3/ h, current control at 800A, in 88 hours, SiHCl
3flow control at 140m
3/ h, H
2flow control at 520m
3/ h, current control at 600A, in 96 hours, SiHCl
3flow control at 135m
3/ h, H
2flow control at 520m
3/ h, current control at 400A, in 100 hours, SiHCl
3flow control at 130m
3/ h, H
2flow control at 520m
3/ h, current control is at 2000A.
Embodiment 6
In the initial reaction control stage, control as follows: in reaction at first, SiHCl
3flow control at 25m
3/ h, H
2flow control at 200m
3/ h, current control at 30A, in 8 hours, SiHCl
3flow control at 180m
3/ h, H
2flow control at 370m
3/ h, current control at 450A, in 16 hours, SiHCl
3flow control at 240m
3/ h, H
2flow control at 390m
3/ h, current control at 510A, in 24 hours, SiHCl
3flow control at 260m
3/ h, H
2flow control at 520m
3/ h, current control is at 700A.
In the stable reaction controlling stage, in 32 hours, SiHCl
3flow control at 260m
3/ h, H
2flow control at 520m
3/ h, current control at 1250A, in 40 hours, SiHCl
3flow control at 260m
3/ h, H
2flow control at 520m
3/ h, current control at 1200A, in 48 hours, SiHCl
3flow control at 260m
3/ h, H
2flow control at 520m
3/ h, current control at 1620A, in 56 hours, SiHCl
3flow control at 160m
3/ h, H
2flow control at 370m
3/ h, current control at 1820A, in 64 hours, SiHCl
3flow control at 250m
3/ h, H
2flow control at 365m
3/ h, current control is at 1200A.
In the end of a period reaction controlling stage, in 72 hours, SiHCl
3flow control at 250m
3/ h, H
2flow control at 360m
3/ h, current control at 1400A, in 80 hours, SiHCl
3flow control at 145m
3/ h, H
2flow control at 360m
3/ h, current control at 800A, in 88 hours, SiHCl
3flow control at 140m
3/ h, H
2flow control at 360m
3/ h, current control at 600A, in 96 hours, SiHCl
3flow control at 135m
3/ h, H
2flow control at 360m
3/ h, current control at 1800A, in 100 hours, SiHCl
3flow control at 130m
3/ h, H
2flow control at 360m
3/ h, current control is at 1600A.
Claims (9)
1. a trichlorosilane reduction process control method, it is characterized in that: this control method comprises initial reaction and controls the stage, stablizes reaction controlling stage and end of a period reaction controlling stage, the time that described initial reaction controls the stage is within first 24 hours of reaction beginning, the time in described stable reaction controlling stage is greater than 24 hours and within 64 hours, described end of a period reaction controlling phases-time is greater than 64 hours and within 100 hours, SiHCl within the initial reaction control stage
3flow control at 260m
3/ below h, H
2flow control at 520m
3/ below h, current control between 30-1000A, at stable reaction controlling stage SiHCl
3flow control at 175-260m
3between/h, H
2flow control at 385-520m
3between/h, current control between 1000-2000A, at end of a period reaction controlling stage SiHCl
3flow control at 130-250m
3between/h, H
2flow control at 360-520m
3between/h, current control is between 100-800A.
2. a kind of trichlorosilane reduction process control method according to claim 1, is characterized in that: in the initial reaction control stage, in reaction beginning within 8 hours, and SiHCl
3flow control at 0-180m
3/ h, H
2flow control at 0-370m
3/ h, current control, at 30-450A, is being greater than 8 hours and in 16 hours, SiHCl
3flow control at 180-240m
3/ h, H
2flow control at 390-500m
3/ h, current control, at 510-750A, is being greater than 16 hours and in 24 hours, SiHCl
3flow control at 180-260m
3/ h, H
2flow control at 390-520m
3/ h, current control is at 700-1000A.
3. a kind of trichlorosilane reduction process control method according to claim 1 and 2, is characterized in that: in the stable reaction controlling stage, had been greater than 24 hours and within 32 hours, SiHCl
3flow control at 175-260m
3/ h, H
2flow control at 385-520m
3/ h, current control, at 1000-1250A, is being greater than 32 hours and within 40 hours, SiHCl
3flow control at 170-260m
3/ h, H
2flow control at 380-520m
3/ h, current control, at 1200-1420A, is being greater than 40 hours and within 48 hours, SiHCl
3flow control at 165-260m
3/ h, H
2flow control at 375-520m
3/ h, current control, at 1200-1620A, is being greater than 48 hours and within 56 hours, SiHCl
3flow control at 160-250m
3/ h, H
2flow control at 370-520m
3/ h, current control, at 1200-1820A, is being greater than 56 hours and within 64 hours, SiHCl
3flow control at 155-250m
3/ h, H
2flow control at 365-520m
3/ h, current control is at 1200-2000A.
4. a kind of trichlorosilane reduction process control method according to claim 3, is characterized in that: in the end of a period reaction controlling stage, had been greater than 64 hours and within 72 hours, SiHCl
3flow control at 150-250m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 1000-2000A, is being greater than 72 hours and within 80 hours, SiHCl
3flow control at 145-240m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 800-2000A, is being greater than 80 hours and within 88 hours, SiHCl
3flow control at 140-240m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 600-2000A, is being greater than 88 hours and within 96 hours, SiHCl
3flow control at 135-230m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 400-2000A, is being greater than 96 hours and within 100 hours, SiHCl
3flow control at 130-220m
3/ h, H
2flow control at 360-520m
3/ h, current control is at 100-2000A.
5. a kind of trichlorosilane reduction process control method according to claim 1, is characterized in that: in the end of a period reaction controlling stage, had been greater than 64 hours and within 72 hours, SiHCl
3flow control at 150-250m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 1000-2000A, is being greater than 72 hours and within 80 hours, SiHCl
3flow control at 145-240m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 800-2000A, is being greater than 80 hours and within 88 hours, SiHCl
3flow control at 140-240m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 600-2000A, is being greater than 88 hours and within 96 hours, SiHCl
3flow control at 135-230m
3/ h, H
2flow control at 360-520m
3/ h, current control, at 400-2000A, is being greater than 96 hours and within 100 hours, SiHCl
3flow control at 130-220m
3/ h, H
2flow control at 360-520m
3/ h, current control is at 100-2000A.
6. a kind of trichlorosilane reduction process control method according to claim 1, is characterized in that: in the initial reaction control stage, controlled as follows: in reaction at first, SiHCl
3flow control at 0-50m
3/ h, H
2flow control at 0-300m
3/ h, current control at 30-140A, in 8 hours, SiHCl
3flow control at 80-180m
3/ h, H
2flow control at 260-370m
3/ h, current control at 250-450A, in 16 hours, SiHCl
3flow control at 180-240m
3/ h, H
2flow control at 390-500m
3/ h, current control at 510-750A, in 24 hours, SiHCl
3flow control at 180-260m
3/ h, H
2flow control at 390-520m
3/ h, current control is at 700-1000A.
7. a kind of trichlorosilane reduction process control method according to claim 1 or 6, is characterized in that: in the stable reaction controlling stage, in 32 hours, SiHCl
3flow control at 175-260m
3/ h, H
2flow control at 385-520m
3/ h, current control at 1000-1250A, in 40 hours, SiHCl
3flow control at 170-260m
3/ h, H
2flow control at 380-520m
3/ h, current control at 1200-1420A, in 48 hours, SiHCl
3flow control at 165-260m
3/ h, H
2flow control at 375-520m
3/ h, current control at 1200-1620A, in 56 hours, SiHCl
3flow control at 160-250m
3/ h, H
2flow control at 370-520m
3/ h, current control at 1200-1820A, in 64 hours, SiHCl
3flow control at 155-250m
3/ h, H
2flow control at 365-520m
3/ h, current control is at 1200-2000A.
8. a kind of trichlorosilane reduction process control method according to claim 7, is characterized in that: in the end of a period reaction controlling stage, in 72 hours, and SiHCl
3flow control at 150-250m
3/ h, H
2flow control at 360-520m
3/ h, current control at 1000-2000A, in 80 hours, SiHCl
3flow control at 145-240m
3/ h, H
2flow control at 360-520m
3/ h, current control at 800-2000A, in 88 hours, SiHCl
3flow control at 140-240m
3/ h, H
2flow control at 360-520m
3/ h, current control at 600-2000A, in 96 hours, SiHCl
3flow control at 135-230m
3/ h, H
2flow control at 360-520m
3/ h, current control at 400-2000A, in 100 hours, SiHCl
3flow control at 130-220m
3/ h, H
2flow control at 360-520m
3/ h, current control is at 100-2000A.
9. a kind of trichlorosilane reduction process control method according to claim 6, is characterized in that: in the end of a period reaction controlling stage, in 72 hours, and SiHCl
3flow control at 150-250m
3/ h, H
2flow control at 360-520m
3/ h, current control at 1000-2000A, in 80 hours, SiHCl
3flow control at 145-240m
3/ h, H
2flow control at 360-520m
3/ h, current control at 800-2000A, in 88 hours, SiHCl
3flow control at 140-240m
3/ h, H
2flow control at 360-520m
3/ h, current control at 600-2000A, in 96 hours, SiHCl
3flow control at 135-230m
3/ h, H
2flow control at 360-520m
3/ h, current control at 400-2000A, in 100 hours, SiHCl
3flow control at 130-220m
3/ h, H
2flow control at 360-520m
3/ h, current control is at 100-2000A.
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| US4676967A (en) * | 1978-08-23 | 1987-06-30 | Union Carbide Corporation | High purity silane and silicon production |
| CN101654249A (en) * | 2009-09-22 | 2010-02-24 | 江苏中能硅业科技发展有限公司 | Production method of polysilicon rod |
| CN101717088A (en) * | 2009-11-25 | 2010-06-02 | 江苏中能硅业科技发展有限公司 | Method and device for efficiently producing polycrystalline silicon |
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| US4676967A (en) * | 1978-08-23 | 1987-06-30 | Union Carbide Corporation | High purity silane and silicon production |
| CN101654249A (en) * | 2009-09-22 | 2010-02-24 | 江苏中能硅业科技发展有限公司 | Production method of polysilicon rod |
| CN101717088A (en) * | 2009-11-25 | 2010-06-02 | 江苏中能硅业科技发展有限公司 | Method and device for efficiently producing polycrystalline silicon |
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