CN104261413B - Plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride method and device thereof - Google Patents
Plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride method and device thereof Download PDFInfo
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Abstract
Plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride method of the present invention and device thereof.By the silicon tetrachloride as by-product of existing production of polysilicon, through being converted into the starting material trichlorosilane producing polysilicon with low-temperature plasma hydro-reduction, achieving and by product is converted into starting material, improve the productive rate about 30% producing polysilicon.The reaction of low-temperature plasma hydro-reduction is carried out in reaction unit, and agent structure comprises the reactor containing chuck, low-temperature plasma electrical source, positive and negative electrode, vaporizer and mixing section.Electric field accelerating electrons, makes electronic temp reach 5 ~ 10ev, and then collides with reactor reaction gases, forms a large amount of active ingredient, and reactive behavior will improve greatly, and the reaction making silicon tetrachloride hydrogenation generate trichlorosilane is very easily carried out, and per pass conversion is up to 60%.Technological process is simple, easy control of reaction, and by product becomes starting material, and the feature of environmental protection is strong; Equipment used structure is simple, and easy to operate, save energy, product yield is good.
Description
Technical field
The present invention relates to a kind of plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride method and device thereof, by the silicon tetrachloride as by-product produced in existing polysilicon production process, raw material trichlorosilane is converted into through plasma deoxidization in low termprature, the once through yield of trichlorosilane reaches 60%, thus make the production yield of polysilicon improve about 30%, save large energy.
Technical background
Polycrystalline silicon material is electronics and information industry and the most important base mateiral of solar energy power generating industry, and solar-grade polysilicon can be used for solar energy power generating, is a kind of efficient, environmental protection and clean WeiLai Technology, alternative existing power generation mode.And electronic-grade polycrystalline silicon can be used for manufacturing semiconductor material, for the manufacture of IC substrate, be widely used in space flight, artificial intelligence, the automatically field such as control and computer chip.Therefore polycrystalline silicon material has strategic importance for the development of national new forms of energy and new and high technology.
At present, the polysilicon production process of China's most enterprises is improved Siemens, its flow process is as follows: with chlorine and hydrogen synthesising hydrogen (or outsourcing hydrogenchloride), hydrogenchloride and industrial silica fume synthesizing trichlorosilane at a certain temperature, then rectifying separation purification is carried out to trichlorosilane, the liquid phase trichlorosilane of condensation after purifying is carrying out CVD reaction production high purity polycrystalline silicon through heat vaporized entering in hydrogen reduction furnace, a large amount of hypertoxic silicon tetrachloride as by-product is also produced while production polysilicon, by domestic mean level (ML), often produce the silicon tetrachloride of 1t polysilicon more than by-product 15t.Silicon tetrachloride wet wet air can react and generate silicic acid and hydrogenchloride, strong corrosion tissue; Directly topple over if silicon tetrachloride is not treated or buries, by making the soil of surrounding, not even a blade of grass grows.Therefore, the technology of processing silicon chloride is subject to global extensive concern.
How silicon tetrachloride is converted into the topic that trichlorosilane is common concern both at home and abroad, present domestic silicon tetrachloride is all at high temperature reduce with hydrogen, consume a large amount of energy, and yield is low especially, only about 10%.Some factories also with cold hydrogen treatment silicon tetrachloride, but cold hydrogenation process route to there is cost of equipment high, the shortcomings such as system pressure is high, and operational danger is large.We generate trichlorosilane technology with plasma deoxidization in low termprature silicon tetrachloride, need not at high temperature carry out, disposable transformation efficiency is up to 60% simultaneously, by contrast, high transformation efficiency is not only obtained with plasma deoxidization in low termprature silicon tetrachloride, the a large amount of save energy of energy, reduces the cost producing polysilicon simultaneously.
In recent years, along with polysilicon becomes the strategic industry that country first develops gradually, solve silicon tetrachloride as by-product of polysilicon be reduced into polysilicon raw materials trichlorosilane problem, impel polysilicon industry to reach energy-conservation further, consumption reduction, safety, environmental protection target seem increasingly important and urgent.
Summary of the invention
The domestic trichlorosilane that is reduced into by hydrogenation of silicon tetrachloride mainly adopts hot hydrogenation now, hot hydrogenation could will occur more than 1000 degree, low conversion rate simultaneously, power consumption is large, technical process is complicated, the object of the invention is to the shortcoming overcoming prior art existence, seek a kind of method and the using appts that are applicable to the hypertoxic silicon tetrachloride as by-product of polysilicon production process to be converted into production of polysilicon raw material trichlorosilane, the hydrogen atom utilizing low-temperature plasma volume ionization hydrogen to produce and silicon tetrachloride react and generate trichlorosilane.
For achieving the above object, the method for plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride of the present invention, its technique comprises following step:
A working method for low-temperature plasma volume ionization hydrogen reducing producing trichlorosilane by using silicon tetrachloride, its step is as follows:
1). first the silicon tetrachloride as by-product producing purity >=99% in polysilicon production process is collected in storage tank;
2). with air in nitrogen rejection unit, to make in device air all by nitrogen replacement;
3). allow silicon tetrachloride enter vaporizer gasification;
4). mix at mixing section with hydrogen after silicon tetrachloride gasification, enter in reactor afterwards, open low-temperature plasma generator power supply, react, obtain product.
Described step 3) in, the flow flow control of silicon tetrachloride is at 0.1ml/min-10000L/min.
Described step 4) in, the ratio of silicon tetrachloride and hydrogen amount is 1:1.0 ~ 8.0.
Described step 4) in, low-temperature plasma electrical source power controls at 1-300KW, and reactor is normal pressure.
Plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride device of the present invention, is provided with chuck in reactor; Arrange in its jackets inner wall one with the steel pipe of reaction tubes equal length or copper rod (mainly playing electric action); Jackets outer wall arranges one deck foil paper layer (mainly playing electric action), the outer uniform winding copper wire of foil paper layer, (mainly playing electric action), links up copper wire coil with electric wire, forming reactions device negative pole; Reactor outer wall is arranged upper and lower two outlets; In addition, aluminium-foil paper wraps up insulating cotton; Positive and negative two-stage is connected with the positive and negative two-stage of low-temperature plasma generator; Reactor outer wall is arranged upper feeding mouth and lower discharge port; Hydrogen-holder is in parallel with nitrogen storage tank, connect with gas mixing chamber again, be connected by pipeline between storage tank with mixing section and on pipeline, under meter be installed, silicon tetrachloride storage tank is connected with vaporizer, middle is connected by pipeline, and on pipeline installation pump, vaporizer is connected with gas mixing chamber, gas mixing chamber with containing the reactors in series of chuck, between connected by pipeline, product is by reactor outlet extraction.
Method and the device thereof of plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride of the present invention have the following advantages:
[1] the present invention compared with prior art, and its preparation method technological process is simple, easy control of reaction, becoming starting material trichlorosilane, improving producing the hypertoxic silicon tetrachloride as by-product produced in polysilicon process the yield of polysilicon, reducing production cost.
[2] utilize the mode of electric discharge to make hydrogen form plasma body, the temperature of system is promoted to more than hydrogen dissociation temperature instantaneously, produces a large amount of hydrogen atoms.After hydrogen molecule is dissociated into hydrogen atom, reactive behavior will improve greatly, and the reaction making silicon tetrachloride hydrogenation generate trichlorosilane is very easily carried out, and per pass conversion is up to 60%.
[3] this technology silicon tetrachloride is reduced per pass conversion up to 60%, and traditional high temperature makes hydrogen gas ionizes, and the transformation efficiency of reduction silicon tetrachloride only has about 10%.
[4] this technology had both processed highly toxic substance silicon tetrachloride, protection of the environment, also allowed by product be converted into the starting material producing polysilicon simultaneously, reduced cost, saved the energy, and in addition, equipment is simple, and processing ease, also saves cost of investment.
Accompanying drawing explanation
Fig. 1 plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride of the present invention technical scheme schema.
Hydrogen-holder (1), nitrogen storage tank (14), silicon tetrachloride storage tank (2), pump (3), under meter (13), vaporizer (4), gas mixing chamber (5), reactor (6) containing chuck, reactor steel pipe positive pole (7), reactor negative potential connection jaws (8), reactor aluminium foil surface electrode (9), insulating cotton (10), copper wire circle (11), low-temperature plasma electrical source (12) reactor jacket (15), jackets outer wall (16), jackets inner wall (17), reactor upper feeding mouth (18), reactor lower discharge port (19).
Embodiment
Also by reference to the accompanying drawings invention is described further below by embodiment.
Plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride device of the present invention, comprise hydrogen-holder (1), nitrogen storage tank (14), silicon tetrachloride storage tank (2), pump (3), under meter (13), vaporizer (4), gas mixing chamber (5), reactor (6) containing chuck, reactor steel pipe positive pole (7), reactor negative potential connection jaws (8), reactor aluminium foil surface electrode (9), insulating cotton (10), copper wire circle (11), low-temperature plasma electrical source (12), reactor jacket (15), jackets outer wall (16), jackets inner wall (17), reactor upper feeding mouth (18), reactor lower discharge port (19), chuck (15) is provided with in reactor, its jackets inner wall (17) adopts vitreosil glass, insert the fine steel tube (7) grown the same as reaction tubes in inner sleeve simultaneously, with electric wire, steel pipe two ends are linked up as reactor positive pole, jackets outer wall also adopts vitreosil glass in (16), outer wall wraps up one deck aluminium-foil paper (9), aluminium-foil paper bundlees with copper wire, with electric wire, copper wire is linked up, forming reactions device negative pole, reactor outer wall is arranged upper feeding mouth (18) and lower discharge port (19).The gordian technique of this technical process is reactor (6), adopts low-temperature plasma electrical source discharge technology, by silicon tetrachloride and hydrogen plasma, form highly active plasma body, reduce the activation energy of reaction, thus reduce temperature of reaction, reduce energy consumption of reaction, realize energy-conservation.Hydrogen-holder (1) is in parallel with nitrogen storage tank (14), connect with gas mixing chamber (5) again, be connected by pipeline between storage tank with mixing section and under meter (13) is installed on pipeline, silicon tetrachloride storage tank (2) is connected with vaporizer (4), centre is connected by pipeline, and on pipeline installation pump (3), vaporizer (4) is connected with gas mixing chamber (5), gas mixing chamber (5) and the reactors in series containing chuck, between connected by pipeline, product is by reactor outlet extraction.Tetracol phenixin enters gasification in vaporizer (4), enters mixing section (5) afterwards mix with hydrogen, finally enters reaction in reactor (6).Hydrogen-holder (1) is in parallel with nitrogen storage tank (14), connect with gas mixing chamber (5) again, be connected by pipeline between storage tank with mixing section and under meter (13) is installed on pipeline, silicon tetrachloride storage tank (2) is connected with vaporizer (4), centre is connected by pipeline, and on pipeline installation pump (3), vaporizer (4) is connected with gas mixing chamber (5), gas mixing chamber (5) and the reactors in series containing chuck, between connected by pipeline, product is by reactor outlet extraction.Tetracol phenixin enters gasification in vaporizer (4), enters mixing section (5) afterwards mix with hydrogen, finally enters reaction in reactor (6).A positive electrode fine steel tube, and the negative potential face electrode of an aluminium-foil paper, make it more easily produce low-temperature plasma, improves product yield, reach the object of save energy simultaneously.
Operation steps is as follows:
1). first the silicon tetrachloride as by-product of purity >=99% produced in polysilicon production process is collected in storage tank
2). first use the air in nitrogen rejection unit, to make in device air all by nitrogen replacement
3). open pump, regulate the flow of silicon tetrachloride, flow control is at (0.1ml/min-10000L/min)
4). silicon tetrachloride enters vaporizer gasification
5). mix at mixing section with hydrogen after silicon tetrachloride gasification, the ratio of amount and silicon tetrachloride: hydrogen=1-8
6). low-temperature plasma electrical source power controls at 1-300KW, at ambient pressure and under low pressure, reacts
7). the positive and negative two-stage in reaction tubes is connected with the positive and negative two-stage of low-temperature plasma generator, open low-temperature plasma generator power supply, under normal pressure, carry out the reaction of low-temperature plasma volume ionization hydrogen reducing producing trichlorosilane by using silicon tetrachloride, obtain reacting rear gaseous product
8). by the reacted gas gas chromatographic detection wherein each substances content collected, calculate each substances content, obtain product yield, and according to product yield, suitably regulate the power of low-temperature plasma generator.
Embodiment 1:
The present embodiment carries out in reaction unit, silicon tetrachloride purity being greater than 99% enters vaporizer gasification with liquid 1.0ml/min, entering mixing section, dried high-purity hydrogen enters mixing section with 0.29L/min and mixes the ratio=1:1.5 of silicon tetrachloride and hydrogen amount (after mixing) with the silicon tetrachloride of gasification, gas mixture enters reaction tubes, steel pipe is inserted in jackets inner wall, jackets outer wall wraps up one deck aluminium-foil paper, be normal pressure in reaction tubes, low-temperature plasma generator power is 2KW; Collect reacted gas, detect by gas-chromatography, wherein the content of trichlorosilane is up to 57%, and reaction conversion ratio reaches 57%.
Embodiment 2
The present embodiment carries out in reaction unit, silicon tetrachloride purity being greater than 99% enters vaporizer gasification with liquid 200.0ml/min, entering mixing section, dried high-purity hydrogen enters mixing section with 154L/min and mixes the ratio=1:4 of silicon tetrachloride and hydrogen amount (after mixing) with the silicon tetrachloride of gasification, gas mixture enters reaction tubes, steel pipe is inserted in jackets inner wall, jackets outer wall wraps up one deck aluminium-foil paper, be normal pressure in reaction tubes, low-temperature plasma generator power is 2KW; Collect reacted gas, detect by gas-chromatography, wherein the content of trichlorosilane is up to 55%, and reaction conversion ratio reaches 51%.
Embodiment 3
The present embodiment carries out in reaction unit, and silicon tetrachloride purity being greater than 99% enters vaporizer gasification with liquid 10000.0L/min, and entering mixing section, dried high-purity hydrogen is with 1.54 × 10
7l/min enters mixing section and mixes the ratio=1:8 of silicon tetrachloride and hydrogen amount (after mixing) with the silicon tetrachloride of gasification, gas mixture enters reaction tubes, steel pipe is inserted in jackets inner wall, jackets outer wall wraps up one deck aluminium-foil paper, be normal pressure in reaction tubes, low-temperature plasma generator power is 300KW; Collect reacted gas, detect by gas-chromatography, wherein the content of trichlorosilane is up to 55%, and reaction conversion ratio reaches 52%.
Embodiment 4
The present embodiment carries out in reaction unit, and silicon tetrachloride purity being greater than 99% enters vaporizer gasification with liquid 200.0L/min, and entering mixing section, dried high-purity hydrogen is with 1.54 × 10
5l/min enters mixing section and mixes the ratio=1:4 of silicon tetrachloride and hydrogen amount (after mixing) with the silicon tetrachloride of gasification, gas mixture enters reaction tubes, steel pipe is inserted in jackets inner wall, jackets outer wall wraps up one deck aluminium-foil paper, be normal pressure in reaction tubes, low-temperature plasma generator power is 20KW; Collect reacted gas, detect by gas-chromatography, wherein the content of trichlorosilane is up to 52%, and reaction conversion ratio reaches 51%.
Embodiment 5
The present embodiment carries out in reaction unit, silicon tetrachloride purity being greater than 99% enters vaporizer gasification with liquid 0.1mL/min, entering mixing section, dried high-purity hydrogen enters mixing section with 15.4mL/min and mixes the ratio=1:8 of silicon tetrachloride and hydrogen amount (after mixing) with the silicon tetrachloride of gasification, gas mixture enters reaction tubes, steel pipe is inserted in jackets inner wall, jackets outer wall wraps up one deck aluminium-foil paper, be normal pressure in reaction tubes, low-temperature plasma generator power is 1KW; Collect reacted gas, detect by gas-chromatography, wherein the content of trichlorosilane is up to 58%, and reaction conversion ratio reaches 53%.
Embodiment 6
The present embodiment carries out in reaction unit, silicon tetrachloride purity being greater than 99% enters vaporizer gasification with liquid 0.1mL/min, entering mixing section, dried high-purity hydrogen enters mixing section with 15.4mL/min and mixes the ratio=1:8 of silicon tetrachloride and hydrogen amount (after mixing) with the silicon tetrachloride of gasification, gas mixture enters reaction tubes, steel pipe is inserted in jackets inner wall, jackets outer wall wraps up one deck Copper Foil paper, be normal pressure in reaction tubes, low-temperature plasma generator power is 1KW; Collect reacted gas, detect by gas-chromatography, wherein the content of trichlorosilane is up to 57%, and reaction conversion ratio reaches 52%.
Embodiment 7
The present embodiment carries out in reaction unit, silicon tetrachloride purity being greater than 99% enters vaporizer gasification with liquid 0.1mL/min, entering mixing section, dried high-purity hydrogen enters mixing section with 15.4mL/min and mixes the ratio=1:8 of silicon tetrachloride and hydrogen amount (after mixing) with the silicon tetrachloride of gasification, gas mixture enters reaction tubes, steel pipe is inserted in jackets inner wall, jackets outer wall wraps up one deck stainless steel foil paper, be normal pressure in reaction tubes, low-temperature plasma generator power is 1KW; Collect reacted gas, detect by gas-chromatography, wherein the content of trichlorosilane is up to 56%, and reaction conversion ratio reaches 51%.
Embodiment 8
The present embodiment carries out in reaction unit, silicon tetrachloride purity being greater than 99% enters vaporizer gasification with liquid 0.1mL/min, entering mixing section, dried high-purity hydrogen enters mixing section with 15.4mL/min and mixes the ratio=1:8 of silicon tetrachloride and hydrogen amount (after mixing) with the silicon tetrachloride of gasification, gas mixture enters reaction tubes, copper pipe is inserted in jackets inner wall, jackets outer wall wraps up one deck stainless steel foil paper, be normal pressure in reaction tubes, low-temperature plasma generator power is 1KW; Collect reacted gas, detect by gas-chromatography, wherein the content of trichlorosilane is up to 59%, and reaction conversion ratio reaches 52%.
Claims (3)
1. plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride device, is characterized in that being provided with chuck in reactor; Arrange in its jackets inner wall one with the steel pipe of reactor equal length or copper rod, as reactor positive pole; Jackets outer wall is arranged one deck foil paper layer, the outer uniform winding copper wire of foil paper layer, links up copper wire coil with electric wire, forming reactions device negative pole; In addition, foil paper layer wraps up insulating cotton; Reactor positive and negative polarities are connected with the positive and negative polarities of low-temperature plasma generator; Reactor outer wall is arranged upper feeding mouth and lower discharge port; Hydrogen-holder is in parallel with nitrogen storage tank, connect with gas mixing chamber again, be connected by pipeline between storage tank with mixing section and on pipeline, under meter be installed, silicon tetrachloride storage tank is connected with vaporizer, middle is connected by pipeline, and on pipeline installation pump, vaporizer is connected with gas mixing chamber, gas mixing chamber with containing the reactors in series of chuck, between connected by pipeline, product is by reactor outlet extraction.
2. device as claimed in claim 1, is characterized in that the inner and outer wall of described chuck adopts vitreosil glass material.
3. device as claimed in claim 1, is characterized in that described foil paper layer is aluminium-foil paper, Copper Foil paper or stainless steel foil paper.
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CN106495165B (en) * | 2016-11-23 | 2018-02-16 | 亚洲硅业(青海)有限公司 | A kind of device and method that trichlorosilane is prepared with silicon tetrachloride |
CN108383124A (en) * | 2018-04-12 | 2018-08-10 | 南通山剑防腐科技有限公司 | A kind of environment protection energy-saving equipment being used to prepare trichlorosilane |
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US4309259A (en) * | 1980-05-09 | 1982-01-05 | Motorola, Inc. | High pressure plasma hydrogenation of silicon tetrachloride |
CN101475175A (en) * | 2009-01-21 | 2009-07-08 | 东方电气集团东方汽轮机有限公司 | Method for preparing trichlorosilane by plasma hydrogenization of silicon tetrachloride |
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