CN104003397A - Trichlorosilane reduction procedure controlling method - Google Patents

Abstract

The invention relates to a trichlorosilane reduction procedure controlling method. The controlling method comprises an initial reaction control stage, a stable reaction control stage and a finished reaction control stage. In the initial reaction control stage, the flow of SiHCl3 is controlled below 260m<3>/h, the flow of H2 is controlled below 520m<3>/h, and the current is controlled between 30A and 1000A. In the stable reaction control stage, the flow of SiHCl3 is controlled between 175 m<3>/h and 260 m<3>/h, the flow of H2 is controlled between 385 m<3>/h and 520 m<3>/h, and the current is controlled between 1000A and 2000A. In the finished reaction control stage, the flow of SiHCl3 is controlled between 130 m<3>/h and 250 m<3>/h, the flow of H2 is controlled between 360 m<3>/h and 520 m<3>/h, and the current is connected between 100A and 800A. The trichlorosilane reduction procedure controlling machine improves the productive rate of trichlorosilane, reduces energy consumption and achieves the purpose of greatly reducing production cost of enterprises.

Description

Trichlorosilane reducing process control method

Technical field

The present invention relates to a kind of production of polysilicon process control method, relate in particular to the control method of trichlorosilane reducing process in production of polysilicon technique.

Background technology

At present, the production technique of polysilicon is mainly improved Siemens, and its principle is exactly by High Purity Hydrogen, to reduce high-purity trichlorosilane on the HIGH-PURITY SILICON core of 1100 ℃ of left and right, generates polysilicon deposition on silicon core.Improvement Siemens process is on the basis of traditional Siemens process, possesses energy-conservation, consumption reduction simultaneously, recycles a large amount of H that supervene in production process ₂, HCI, SiCI ₄process matched therewith Deng by product and a large amount of by-product heat energy.Most producers all adopt 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 generate its chemical reaction of industrial silicon SiO in electric arc furnace ₂+ C → Si+CO ₂, in order to meet highly purified needs, must further purify in ↑ (2).Industrial silicon pulverized and used anhydrous hydrogen chloride (HCl) to react with it in a fluidized-bed reactor, generating the trichlorosilane (SiHCl that intends 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 producing in second step also needs further purification, needs to decompose filtration silica flour, condensation SiHCl ₃, SiCl ₄, and gaseous state H ₂, HCl turns back in reaction or is discharged in atmosphere.Then decompose condensation product SiHCl ₃, SiCl ₄, purify trichlorosilane (multistage rectification).(4) trichlorosilane after purification adopts high temperature reduction technique, with high-purity SiHCl ₃at H ₂reduce deposition in atmosphere and generate polysilicon.Its chemical reaction SiHCl ₃+ H ₂→ Si+HCl.The reaction vessel of polysilicon is sealing, and with electrically heated silicon pond silicon rod (diameter 5-10 millimeter, length 1.5-2 rice, 80 of quantity), at 1050-1100 degree growing polycrystalline silicon on rod, diameter can reach 150-200 millimeter.About like this 1/3rd trichlorosilane reacts, and generates polysilicon.The same H of remainder ₂, HCL, SiHCl ₃, SiCl ₄separated 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 the polysilicon in extractive process more than 70% has all discharged by chlorine, not only refines cost high, and environmental pollution is very serious.

Therefore how to improve the productive rate of polysilicon, reducing energy consumption is the most important thing of production of polysilicon process modification.

Summary of the invention

In order to overcome the defect that existing production of polysilicon process yield is low, energy consumption is high, the invention provides a kind of trichlorosilane reducing process control method, this control method improves the productive rate of trichlorosilane and reduces energy consumption by the control of trichlorosilane reducing process parameters is reached, and greatly reduces the object of the production cost of enterprise.

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 hot conditions, consume energy high, reduce energy consumption, also need this processing step reasonably to control.

In order to solve the problems of the technologies described above, the technical solution used in the present invention is:

A kind of trichlorosilane reducing process control method, it is characterized in that: this control method comprises initial reaction control stage, stable reaction control stage and ends the reaction control stage, described initial reaction is controlled the time in stage for reacting in first 24 hours that start, the time that the stage is controlled in described stable reaction is greater than 24 hours and in 64 hours, described end of a period reaction controls that phases-time is greater than 64 hours and in 100 hours, SiHCl within the initial reaction control stage ₃flow control at 260m ³below/h, H ₂flow control at 520m ³below/h, current control is between 30-1000A, at stable reaction control stage SiHCl ₃flow control at 175-260m ³between/h, H ₂flow control at 385-520m ³between/h, current control is between 1000-2000A, at the reaction control stage SiHCl of ending 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, start in 8 hours SiHCl ₃flow control at 0-180m ³/ h, H ₂flow control at 0-370m ³/ h, current control is 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 is 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 control stage, be greater than 24 hours and in 32 hours, SiHCl ₃flow control at 175-260m ³/ h, H ₂flow control at 385-520m ³/ h, current control is at 1000-1250A, is being greater than 32 hours and in 40 hours, SiHCl ₃flow control at 170-260m ³/ h, H ₂flow control at 380-520m ³/ h, current control is at 1200-1420A, is being greater than 40 hours and in 48 hours, SiHCl ₃flow control at 165-260m ³/ h, H ₂flow control at 375-520m ³/ h, current control is at 1200-1620A, is being greater than 48 hours and in 56 hours, SiHCl ₃flow control at 160-250m ³/ h, H ₂flow control at 370-520m ³/ h, current control is at 1200-1820A, is being greater than 56 hours and 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 reaction control stage of ending, be greater than 64 hours and in 72 hours, SiHCl ₃flow control at 150-250m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 1000-2000A, is being greater than 72 hours and in 80 hours, SiHCl ₃flow control at 145-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 800-2000A, is being greater than 80 hours and in 88 hours, SiHCl ₃flow control at 140-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 600-2000A, is being greater than 88 hours and in 96 hours, SiHCl ₃flow control at 135-230m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 400-2000A, is greater than hour and in 100 hours SiHCl 96 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 is at 30-140A, in 8 hours, SiHCl ₃flow control at 80-180m ³/ h, H ₂flow control at 260-370m ³/ h, current control is at 250-450A, in 16 hours, SiHCl ₃flow control at 180-240m ³/ h, H ₂flow control at 390-500m ³/ h, current control is 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 control stage, in 32 hours, SiHCl ₃flow control at 175-260m ³/ h, H ₂flow control at 385-520m ³/ h, current control is at 1000-1250A, in 40 hours, SiHCl ₃flow control at 170-260m ³/ h, H ₂flow control at 380-520m ³/ h, current control is at 1200-1420A, in 48 hours, SiHCl ₃flow control at 165-260m ³/ h, H ₂flow control at 375-520m ³/ h, current control is at 1200-1620A, in 56 hours, SiHCl ₃flow control at 160-250m ³/ h, H ₂flow control at 370-520m ³/ h, current control is 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 reaction control stage of ending, in 72 hours, SiHCl ₃flow control at 150-250m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 1000-2000A, in 80 hours, SiHCl ₃flow control at 145-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 800-2000A, in 88 hours, SiHCl ₃flow control at 140-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 600-2000A, in 96 hours, SiHCl ₃flow control at 135-230m ³/ h, H ₂flow control at 360-520m ³/ h, current control is 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 controls stage, stable reaction control stage and ends the reaction control stage, described initial reaction is controlled the time in stage for reacting in first 24 hours that start, the time that the stage is controlled in described stable reaction is greater than 24 hours and in 64 hours, described end of a period reaction controls that phases-time is greater than 64 hours and in 100 hours, SiHCl within the initial reaction control stage ₃flow control at 260m ³below/h, H ₂flow control at 520m ³below/h, current control is between 30-1000A, at stable reaction control stage SiHCl ₃flow control at 175-260m ³between/h, H ₂flow control at 385-520m ³between/h, current control is between 1000-2000A, at the reaction control stage SiHCl of ending ₃flow control at 130-250m ³between/h, H ₂flow control at 360-520m ³between/h, current control is between 100-800A.The present invention is subdivided into three control stages by trichlorosilane reducing process control method, in each control stage, trichlorosilane flow, hydrogen flowing quantity and electric current are controlled accurately, by the reasonable control that affects the parameter of polysilicon increment on silicon rod to these three, greatly improved the output of trichlorosilane.At initial reaction, control the stage, reaction is now slower, 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 is at silicon rod Surface Creation, and adhering to provide and putting forth effort bed of next step polysilicon is provided, be beneficial to the generation of adhering to of polysilicon, growing amount at this stage polysilicon is less, passes into a small amount of electric weight, trichlorosilane and hydrogen, can save the consumption of electric energy and the consumption of trichlorosilane and hydrogen; In the stable reaction control stage, be now a large amount of periods that polysilicon generates, the critical period of improving polysilicon output during this stage, in this stage current control between 1000-2000A, guarantee silicon rod surface temperature control at 1080 ℃ of left and right, SiHCl ₃flow control at 175-260m ³between/h, H ₂flow control at 385-520m ³between/h, allow SiHCl ₃rapid, high volume by hydrogen reducing, generated polysilicon, before adding, initial reaction is controlled the implantation in advance of a small amount of polysilicon in stage, now polysilicon will generate in a large number on silicon rod; Ending the reaction control 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 and be reduced into polysilicon, in this stage, reduce electric current, 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, start in 8 hours SiHCl ₃flow control at 0-180m ³/ h, H ₂flow control at 0-370m ³/ h, current control is 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 is 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 concrete is divided into 0-8 hour by the initial reaction control stage, 8-16 hour, 16-24 hour three phases, respectively the hydrogen flowing quantity of three phases, trichlorosilane flow and electric current are further limited to control, concrete cooperation by these parameters is controlled, when impelling the preliminary generation of polysilicon, the consumption of saves energy is, the consumption of the consumption of hydrogen and trichlorosilane, as far as possible with a small amount of raw material and a small amount of electric current, impel the preliminary generation of polysilicon and implantation in advance, be beneficial to and stablize the carrying out that reacts the control stage.

3,, in the stable reaction control stage, be greater than 24 hours and in 32 hours, SiHCl ₃flow control at 175-260m ³/ h, H ₂flow control at 385-520m ³/ h, current control is at 1000-1250A, is being greater than 32 hours and in 40 hours, SiHCl ₃flow control at 170-260m ³/ h, H ₂flow control at 380-520m ³/ h, current control is at 1200-1420A, is being greater than 40 hours and in 48 hours, SiHCl ₃flow control at 165-260m ³/ h, H ₂flow control at 375-520m ³/ h, current control is at 1200-1620A, is being greater than 48 hours and in 56 hours, SiHCl ₃flow control at 160-250m ³/ h, H ₂flow control at 370-520m ³/ h, current control is at 1200-1820A, is being greater than 56 hours and 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 this stage we control be divided into 24-32 hour, 32-40 hour, 40-48 hour, 48-56,56-64 hour double teacher control, accurate control to hydrogen, trichlorosilane and electric current in this double teacher, these three parameters are limited in the scope providing, can allow a large amount of generation of polysilicon.

4,, in the reaction control stage of ending, be greater than 64 hours and in 72 hours, SiHCl ₃flow control at 150-250m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 1000-2000A, is being greater than 72 hours and in 80 hours, SiHCl ₃flow control at 145-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 800-2000A, is being greater than 80 hours and in 88 hours, SiHCl ₃flow control at 140-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 600-2000A, is being greater than 88 hours and in 96 hours, SiHCl ₃flow control at 135-230m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 400-2000A, is greater than hour and in 100 hours SiHCl 96 ₃flow control at 130-220m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 100-2000A.In 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; by the control of these parameters, can make full use of the heat of furnace gas; the consumption of saving electric energy when allowing reaction go on; protect polysilicon simultaneously and reduce temperature in stove, being beneficial to the generation of polysilicon.

Embodiment

Embodiment 1

In the initial reaction control stage, before reaction starts in 8 hours, SiHCl ₃flow control 50m ³/ h, H ₂flow control at 320m ³/ h, current control is at 200A, at 8-16 hour with interior (not comprising 8 hours), SiHCl ₃flow control at 186m ³/ h, H ₂flow control at 420m ³/ h, current control is at 600A, at 16-24 hour with interior (not comprising 16 hours), SiHCl ₃flow control at 210m ³/ h, H ₂flow control at 400m ³/ h, current control is at 785A.

In the stable reaction control stage, at 24-32 hour with interior (not comprising 24 hours), SiHCl ₃flow control at 185m ³/ h, H ₂flow control at 385m ³/ h, current control is at 1250A, at 32-40 hour with interior (not comprising 32 hours), SiHCl ₃flow control at 185m ³/ h, H ₂flow control at 380m ³/ h, current control is at 1200A, at 40-48 hour with interior (not comprising 40 hours), SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 520m ³/ h, current control is at 1200A, at 48-56 hour with interior (not comprising 48 hours), SiHCl ₃flow control at 250m ³/ h, H ₂flow control at 370m ³/ h, current control is at 1200A, at 56-64 hour with interior (not comprising 56 hours), SiHCl ₃flow control at 225m ³/ h, H ₂flow control at 384m ³/ h, current control is at 1248A.

In the reaction control stage of ending, at 64-72 hour with interior (not comprising 64 hours), SiHCl ₃flow control at 250m ³/ h, H ₂flow control at 360m ³/ h, current control is at 1000A, at 72-80 hour with interior (not comprising 72 hours), SiHCl ₃flow control at 240m ³/ h, H ₂flow control at 380m ³/ h, current control is at 800A, at 80-88 hour with interior (not comprising 80 hours), SiHCl ₃flow control at 140m ³/ h, H ₂flow control at 520m ³/ h, current control is at 600A, at 88-96 hour with interior (not comprising 88 hours), SiHCl ₃flow control at 150m ³/ h, H ₂flow control at 420m ³/ h, current control is 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, start in 8 hours SiHCl ₃flow control at 90m ³/ h, H ₂flow control at 150m ³/ h, current control is at 30A, at 8-16 hour with interior (not comprising 8 hours), SiHCl ₃flow control at 180m ³/ h, H ₂flow control at 400m ³/ h, current control is at 620A, at 16-24 hour with interior (not comprising 16 hours), SiHCl ₃flow control at 220m ³/ h, H ₂flow control at 390m ³/ h, current control is at 800A.

In the stable reaction control stage, at 24-32 hour with interior (not comprising 24 hours), SiHCl ₃flow control at 200m ³/ h, H ₂flow control at 420m ³/ h, current control is at 1100A, at 32-40 hour with interior (not comprising 32 hours), SiHCl ₃flow control at 170m ³/ h, H ₂flow control at 390m ³/ h, current control is at 1300A, at 40-48 hour with interior (not comprising 40 hours), SiHCl ₃flow control at 185m ³/ h, H ₂flow control at 425m ³/ h, current control is at 1450A, at 48-56 hour with interior (not comprising 48 hours), SiHCl ₃flow control at 168m ³/ h, H ₂flow control at 430m ³/ h, current control is at 1350A, at 56-64 hour with interior (not comprising 56 hours), SiHCl ₃flow control at 165m ³/ h, H ₂flow control at 410m ³/ h, current control is at 1400A.

In the reaction control stage of ending, at 64-72 hour with interior (not comprising 64 hours), SiHCl ₃flow control at 160m ³/ h, H ₂flow control at 360m ³/ h, current control is at 1200A, at 72-80 hour with interior (not comprising 72 hours), SiHCl ₃flow control at 165m ³/ h, H ₂flow control at 380m ³/ h, current control is at 900A, at 80-88 hour with interior (not comprising 80 hours), SiHCl ₃flow control at 160m ³/ h, H ₂flow control at 420m ³/ h, current control is at 800A, at 88-96 hour with interior (not comprising 88 hours), SiHCl ₃flow control at 145m ³/ h, H ₂flow control at 380m ³/ h, current control is at 600A, at 96-100 hour with interior (not comprising 96 hours), SiHCl 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, start in 8 hours SiHCl ₃flow control at 60m ³/ h, H ₂flow control at 120m ³/ h, current control is at 30A, at 8-16 hour with interior (not comprising 8 hours), SiHCl ₃flow control at 240m ³/ h, H ₂flow control at 420m ³/ h, current control is at 700A, at 16-24 hour with interior (not comprising 16 hours), SiHCl ₃flow control at 195m ³/ h, H ₂flow control at 440m ³/ h, current control is at 700A.

In the stable reaction control stage, at 24-32 hour with interior (not comprising 24 hours), SiHCl ₃flow control at 210m ³/ h, H ₂flow control at 440m ³/ h, current control is at 1200A, at 32-40 hour with interior (not comprising 32 hours), SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 500m ³/ h, current control is at 1300A, at 40-48 hour with interior (not comprising 40 hours), SiHCl ₃flow control at 185m ³/ h, H ₂flow control at 500m ³/ h, current control is at 1400A, at 48-56 hour with interior (not comprising 48 hours), SiHCl ₃flow control at 178m ³/ h, H ₂flow control at 510m ³/ h, current control is at 1600A, at 56-64 hour with interior (not comprising 56 hours), SiHCl ₃flow control at 158m ³/ h, H ₂flow control at 520m ³/ h, current control is at 1200A.

In the reaction control stage of ending, at 64-72 hour with interior (not comprising 64 hours), SiHCl ₃flow control at 230m ³/ h, H ₂flow control at 480m ³/ h, current control is at 1400A, at 72-80 hour with interior (not comprising 72 hours), SiHCl ₃flow control at 145m ³/ h, H ₂flow control at 360m ³/ h, current control is at 1500A, at 80-88 hour with interior (not comprising 80 hours), SiHCl ₃flow control at 160m ³/ h, H ₂flow control at 400m ³/ h, current control is at 1800A, at 88-96 hour with interior (not comprising 88 hours), SiHCl ₃flow control at 230m ³/ h, H ₂flow control at 480m ³/ h, current control is at 800A, at 96-100 hour with interior (not comprising 96 hours), SiHCl 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, start in 8 hours SiHCl ₃flow control at 20m ³/ h, H ₂flow control at 40m ³/ h, current control is at 300A, at 8-16 hour with interior (not comprising 8 hours), SiHCl ₃flow control at 240m ³/ h, H ₂flow control at 420m ³/ h, current control is at 555A, at 16-24 hour with interior (not comprising 16 hours), SiHCl ₃flow control at 200m ³/ h, H ₂flow control at 520m ³/ h, current control is at 900A.

In the stable reaction control stage, at 24-32 hour with interior (not comprising 24 hours), SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 400m ³/ h, current control is at 1250A, at 32-40 hour with interior (not comprising 32 hours), SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 440m ³/ h, current control is at 1350A, at 40-48 hour with interior (not comprising 40 hours), SiHCl ₃flow control at 199m ³/ h, H ₂flow control at 420m ³/ h, current control is at 1600A, at 48-56 hour with interior (not comprising 48 hours), SiHCl ₃flow control at 225m ³/ h, H ₂flow control at 450m ³/ h, current control is at 1750A, at 56-64 hour with interior (not comprising 56 hours), SiHCl ₃flow control 195m ³/ h, H ₂flow control at 445m ³/ h, current control is at 1800A.

In the reaction control stage of ending, at 64-72 hour with interior (not comprising 64 hours), SiHCl ₃flow control at 185m ³/ h, H ₂flow control at 445m ³/ h, current control is at 1000A, at 72-80 hour with interior (not comprising 72 hours), SiHCl ₃flow control at 900m ³/ h, H ₂flow control at 440m ³/ h, current control is at 800A, at 80-88 hour with interior (not comprising 80 hours), SiHCl ₃flow control at 160m ³/ h, H ₂flow control at 420m ³/ h, current control is at 700A, at 88-96 hour with interior (not comprising 88 hours), SiHCl ₃flow control at 165m ³/ h, H ₂flow control at 420m ³/ h, current control is at 400A, at 96-100 hour with interior (not comprising 96 hours), SiHCl 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 is at 120A, in 8 hours, SiHCl ₃flow control at 80m ³/ h, H ₂flow control at 300m ³/ h, current control is at 350A, in 16 hours, SiHCl ₃flow control at 240m ³/ h, H ₂flow control at 390m ³/ h, current control is 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 control stage, in 32 hours, SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 385m ³/ h, current control is at 1000A, in 40 hours, SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 380m ³/ h, current control is at 1200A, in 48 hours, SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 375m ³/ h, current control is at 1200A, in 56 hours, SiHCl ₃flow control at 160m ³/ h, H ₂flow control at 520m ³/ h, current control is 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 reaction control stage of ending, in 72 hours, SiHCl ₃flow control at 150m ³/ h, H ₂flow control at 520m ³/ h, current control is at 2000A, in 80 hours, SiHCl ₃flow control at 240m ³/ h, H ₂flow control at 360m ³/ h, current control is at 800A, in 88 hours, SiHCl ₃flow control at 140m ³/ h, H ₂flow control at 520m ³/ h, current control is at 600A, in 96 hours, SiHCl ₃flow control at 135m ³/ h, H ₂flow control at 520m ³/ h, current control is 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 is at 30A, in 8 hours, SiHCl ₃flow control at 180m ³/ h, H ₂flow control at 370m ³/ h, current control is at 450A, in 16 hours, SiHCl ₃flow control at 240m ³/ h, H ₂flow control at 390m ³/ h, current control is 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 control stage, in 32 hours, SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 520m ³/ h, current control is at 1250A, in 40 hours, SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 520m ³/ h, current control is at 1200A, in 48 hours, SiHCl ₃flow control at 260m ³/ h, H ₂flow control at 520m ³/ h, current control is at 1620A, in 56 hours, SiHCl ₃flow control at 160m ³/ h, H ₂flow control at 370m ³/ h, current control is 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 reaction control stage of ending, in 72 hours, SiHCl ₃flow control at 250m ³/ h, H ₂flow control at 360m ³/ h, current control is at 1400A, in 80 hours, SiHCl ₃flow control at 145m ³/ h, H ₂flow control at 360m ³/ h, current control is at 800A, in 88 hours, SiHCl ₃flow control at 140m ³/ h, H ₂flow control at 360m ³/ h, current control is at 600A, in 96 hours, SiHCl ₃flow control at 135m ³/ h, H ₂flow control at 360m ³/ h, current control is 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. trichlorosilane reducing process control method, it is characterized in that: this control method comprises initial reaction control stage, stable reaction control stage and ends the reaction control stage, described initial reaction is controlled the time in stage for reacting in first 24 hours that start, the time that the stage is controlled in described stable reaction is greater than 24 hours and in 64 hours, described end of a period reaction controls that phases-time is greater than 64 hours and in 100 hours, SiHCl within the initial reaction control stage ₃flow control at 260m ³below/h, H ₂flow control at 520m ³below/h, current control is between 30-1000A, at stable reaction control stage SiHCl ₃flow control at 175-260m ³between/h, H ₂flow control at 385-520m ³between/h, current control is between 1000-2000A, at the reaction control stage SiHCl of ending ₃flow control at 130-250m ³between/h, H ₂flow control at 360-520m ³between/h, current control is between 100-800A.

2. trichlorosilane reducing process control method according to claim 1, is characterized in that: in the initial reaction control stage, start in 8 hours SiHCl in reaction ₃flow control at 0-180m ³/ h, H ₂flow control at 0-370m ³/ h, current control is 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 is 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. trichlorosilane reducing process control method according to claim 1 and 2, is characterized in that: in the stable reaction control stage, be greater than 24 hours and in 32 hours, SiHCl ₃flow control at 175-260m ³/ h, H ₂flow control at 385-520m ³/ h, current control is at 1000-1250A, is being greater than 32 hours and in 40 hours, SiHCl ₃flow control at 170-260m ³/ h, H ₂flow control at 380-520m ³/ h, current control is at 1200-1420A, is being greater than 40 hours and in 48 hours, SiHCl ₃flow control at 165-260m ³/ h, H ₂flow control at 375-520m ³/ h, current control is at 1200-1620A, is being greater than 48 hours and in 56 hours, SiHCl ₃flow control at 160-250m ³/ h, H ₂flow control at 370-520m ³/ h, current control is at 1200-1820A, is being greater than 56 hours and 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.

4. trichlorosilane reducing process control method according to claim 3, is characterized in that: in the reaction control stage of ending, be greater than 64 hours and in 72 hours, SiHCl ₃flow control at 150-250m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 1000-2000A, is being greater than 72 hours and in 80 hours, SiHCl ₃flow control at 145-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 800-2000A, is being greater than 80 hours and in 88 hours, SiHCl ₃flow control at 140-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 600-2000A, is being greater than 88 hours and in 96 hours, SiHCl ₃flow control at 135-230m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 400-2000A, is greater than hour and in 100 hours SiHCl 96 ₃flow control at 130-220m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 100-2000A.

5. trichlorosilane reducing process control method according to claim 1, is characterized in that: in the reaction control stage of ending, be greater than 64 hours and in 72 hours, SiHCl ₃flow control at 150-250m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 1000-2000A, is being greater than 72 hours and in 80 hours, SiHCl ₃flow control at 145-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 800-2000A, is being greater than 80 hours and in 88 hours, SiHCl ₃flow control at 140-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 600-2000A, is being greater than 88 hours and in 96 hours, SiHCl ₃flow control at 135-230m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 400-2000A, is greater than hour and in 100 hours SiHCl 96 ₃flow control at 130-220m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 100-2000A.

6. trichlorosilane reducing process control method according to claim 1, is characterized in that: in the initial reaction control stage, control as follows: reacting at first SiHCl ₃flow control at 0-50m ³/ h, H ₂flow control at 0-300m ³/ h, current control is at 30-140A, in 8 hours, SiHCl ₃flow control at 80-180m ³/ h, H ₂flow control at 260-370m ³/ h, current control is at 250-450A, in 16 hours, SiHCl ₃flow control at 180-240m ³/ h, H ₂flow control at 390-500m ³/ h, current control is 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. according to the trichlorosilane reducing process control method described in claim 1 or 6, it is characterized in that: in the stable reaction control stage, in 32 hours, SiHCl ₃flow control at 175-260m ³/ h, H ₂flow control at 385-520m ³/ h, current control is at 1000-1250A, in 40 hours, SiHCl ₃flow control at 170-260m ³/ h, H ₂flow control at 380-520m ³/ h, current control is at 1200-1420A, in 48 hours, SiHCl ₃flow control at 165-260m ³/ h, H ₂flow control at 375-520m ³/ h, current control is at 1200-1620A, in 56 hours, SiHCl ₃flow control at 160-250m ³/ h, H ₂flow control at 370-520m ³/ h, current control is 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. trichlorosilane reducing process control method according to claim 7, is characterized in that: in the reaction control stage of ending, and in 72 hours, SiHCl ₃flow control at 150-250m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 1000-2000A, in 80 hours, SiHCl ₃flow control at 145-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 800-2000A, in 88 hours, SiHCl ₃flow control at 140-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 600-2000A, in 96 hours, SiHCl ₃flow control at 135-230m ³/ h, H ₂flow control at 360-520m ³/ h, current control is 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. trichlorosilane reducing process control method according to claim 6, is characterized in that: in the reaction control stage of ending, and in 72 hours, SiHCl ₃flow control at 150-250m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 1000-2000A, in 80 hours, SiHCl ₃flow control at 145-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 800-2000A, in 88 hours, SiHCl ₃flow control at 140-240m ³/ h, H ₂flow control at 360-520m ³/ h, current control is at 600-2000A, in 96 hours, SiHCl ₃flow control at 135-230m ³/ h, H ₂flow control at 360-520m ³/ h, current control is 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.