CN106744685A - The deep-purifying method of circulating hydrogen in electronic-grade polycrystalline silicon production - Google Patents

The deep-purifying method of circulating hydrogen in electronic-grade polycrystalline silicon production Download PDF

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CN106744685A
CN106744685A CN201611020410.8A CN201611020410A CN106744685A CN 106744685 A CN106744685 A CN 106744685A CN 201611020410 A CN201611020410 A CN 201611020410A CN 106744685 A CN106744685 A CN 106744685A
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chlorine
circulating hydrogen
containing compound
deep
purifying method
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CN106744685B (en
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宗冰
张宝顺
王体虎
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Asia Silicon Qinghai Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465Composition of the impurity

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  • Organic Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The present invention provides a kind of deep-purifying method of circulating hydrogen in electronic-grade polycrystalline silicon production, belongs to the purification technique field of tail gas in electronic-grade polycrystalline silicon production.Cl will be contained2, hydride impurity circulating hydrogen be passed through plasma device in make Cl2Activation obtains chlorine radical, and chlorine radical obtains chlorine-containing compound, chlorine-containing compound is separated with circulating hydrogen with hydride reaction.In this deep-purifying method, micro Cl is contained in circulating hydrogen2, micro Cl2Because strong-electromagnetic field effect can be activated fully in plasma device, the chlorine radical for having and taking generation activity by force is formed, chlorine radical preferentially can occur substitution reaction with hydride, make its transformation higher boiling, highly polar material, easily be separated with circulating hydrogen;Outer impurity, byproduct of reaction are not introduced and there was only micro HCl, easily separated with circulating hydrogen;It is plasma-activated to make Cl2Activation more fully, reaches the purpose of circulating hydrogen deep purifying.

Description

The deep-purifying method of circulating hydrogen in electronic-grade polycrystalline silicon production
Technical field
The present invention relates to the purification technique field of tail gas in electronic-grade polycrystalline silicon production, in particular to a kind of electronics The deep-purifying method of circulating hydrogen in level polysilicon production.
Background technology
Electronic-grade polycrystalline silicon is the basic key function material of the new industry such as integrated circuit, Aero-Space, new energy. Although China's polysilicon industry development in recent years is swift and violent, the size of capacity leaps to the first in the world, but still cannot realize high-purity, ultra-pure The volume production of electronic-grade polycrystalline silicon, researching and developing high-purity, ultra-pure electronic-grade polycrystalline silicon material production technology and accomplishing scale production is The emphasis direction of the polysilicon industry development of China.
The advanced purification technology of circulating hydrogen is the key for producing electronic-grade polycrystalline silicon material in electronic-grade polycrystalline silicon production Technology.Temperature is very high when trichlorosilane reacts with hydrogen in reduction furnace, and various impurity can split under the high temperature conditions Solution reaction forms B2H6、PH3Etc. small molecule form, B2H6、PH3Depth removal Deng small molecular weight impurity is that China realizes that electron level is more The significant challenge of crystal silicon scale volume production.The hydrogen predominantly circulating hydrogen used in current production of polysilicon, prior art without Method realizes the depth removal of impurity in circulating hydrogen, therefore, circulating hydrogen quality cannot meet the scale of electronic-grade polycrystalline silicon Production.
The content of the invention
It is an object of the invention to provide the deep-purifying method of circulating hydrogen in a kind of production of electronic-grade polycrystalline silicon, can Cl in circulating hydrogen is removed well2, the impurity such as hydride so that circulating hydrogen stably reaches electron level.
The present invention is realized using following technical scheme:
The deep-purifying method of circulating hydrogen, will contain Cl in a kind of electronic-grade polycrystalline silicon production2, hydride impurity follows Ring hydrogen makes Cl in being passed through plasma device2Activation obtains chlorine radical, and chlorine radical obtains chloride containing with hydride reaction Compound, chlorine-containing compound is separated with circulating hydrogen.
The deep-purifying method of circulating hydrogen has in the electronic-grade polycrystalline silicon production that presently preferred embodiments of the present invention is provided Beneficial effect is:
The deep-purifying method of circulating hydrogen in the electronic-grade polycrystalline silicon production that the present invention is provided, containing micro- in circulating hydrogen Amount Cl2, plasma device offer electromagnetic field, Cl2It is passed through in plasma device, free electron adds in the presence of electromagnetic field Short-term training is high energy electron, high energy electron and activation Cl2Collision, makes Cl2It is changed into the very strong chlorine radical of reactivity.High energy electricity Son and the collision of hydride impurity, make the increased activity of hydride, make chlorine radical be easy to generate chloride containing with hydride reaction Compound;Meanwhile, circulating hydrogen is changed into nonequilibrium plasma completely in plasma device, can produce the high light spoke that frequency is wide Penetrate, the light radiation can make Cl2Chlorine radical is activated into, and light substitution reaction occurs with hydride, obtain chlorine-containing compound, with Original hydride is compared, and the boiling point of chlorine-containing compound is high, polarity is strong, is easily separated with circulating hydrogen, and circulating hydrogen is obtained To deep purifying, so that circulating hydrogen stably reaches electron level, beneficial to large-scale production electronic-grade polycrystalline silicon.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below will be in the embodiment of the present invention Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional product that can be obtained by commercially available purchase Product.
The deep-purifying method to circulating hydrogen in the electronic-grade polycrystalline silicon production of the embodiment of the present invention is carried out specifically below Explanation.
The deep-purifying method of circulating hydrogen, will contain Cl in a kind of electronic-grade polycrystalline silicon production2, hydride impurity follows Ring hydrogen makes Cl in being passed through plasma device2Activation obtains chlorine radical.
Preferably, the circulating hydrogen directly released during electronic-grade polycrystalline silicon is produced is passed directly into plasma device, The temperature of the circulating hydrogen directly released in electronic-grade polycrystalline silicon production is higher, is conducive to follow-up priming reaction, meanwhile, electronics Level polysilicon production is later just directly purified circulating hydrogen, is conducive to the circulating hydrogen after purification to carry out electron level again many The production of crystal silicon, is conducive to the recycling of circulating hydrogen, energy saving.
Contain micro Cl in circulating hydrogen2, plasma device offer electromagnetic field, Cl2It is passed through in plasma device, from High energy electron, high energy electron and activation Cl are accelerated as in the presence of electromagnetic field by electronics2Collision, makes Cl2It is changed into reaction to live The very strong chlorine radical of property;Meanwhile, circulating hydrogen is changed into nonequilibrium plasma completely in plasma device, can produce frequency The wide high light radiation of rate, the light radiation can make Cl2Chlorine radical is activated into, makes the micro Cl in circulating hydrogen2Can be sufficient Change into the very strong chlorine radical of reactivity.
The activity of chlorine radical activity is very strong, and high energy electron is also collided with hydride impurity, makes the increased activity of hydride, The very strong chlorine radical of activity is easy to reaction generation chlorine-containing compound with the hydride of increased activity.
In embodiments of the invention, hydride is mainly B2H6And PH3Deng small molecular weight impurity, it takes with chlorine radical Generation reaction can generate B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Deng chloride.
Dielectric is provided with the electrode of plasma device, is made using dielectric barrier discharge micro in circulating hydrogen Cl2Activation, prevents metal electrode from ionizing, it is to avoid introduce metal impurities, it is to avoid produces new impurity, makes circulating hydrogen dirty Dye.It is preferably provided with:Dielectric is quartz or aluminum oxide.Quartz is high purity quartz, it is to avoid introduce new impurity, it is to avoid to electron level Polysilicon is polluted.Similarly, aluminum oxide is high purity aluminium oxide.
Compared with original hydride, the boiling point of chlorine-containing compound is high, polarity is strong, is easily separated with circulating hydrogen, Chlorine-containing compound is separated with circulating hydrogen, deep purifying can be carried out to circulating hydrogen, so that circulating hydrogen stably reaches electricity Sub- level, beneficial to large-scale production electronic-grade polycrystalline silicon.
To complexing agent is added in plasma device, so that the chlorine-containing compound of generation obtains complex compound with complexing agent reaction Realize that chlorine-containing compound is separated with circulating hydrogen.Compared with original hydride, the polarity of chlorine-containing compound is strong, so, its The complex compound to form stabilization is easily reacted with complexing agent, complex compound is stayed in plasma device, so as to realize B2H6And PH3Deng The depth removal of small molecular weight impurity, reaches the purpose of decontamination cycle hydrogen, and the circulating hydrogen after deep purifying continues on for electricity In the production of sub- level polysilicon.
In plasma device, the formation of chlorine radical and the generation of chlorine-containing compound are all very quick, reach microsecond Level.To filling complexing agent in plasma device, the micro Cl in circulating hydrogen2Activate into the very strong chlorine freedom of reactivity Base, and with hydride occur substitution reaction generation chlorine-containing compound after, continue with complexing agent react to be formed stabilization complex compound, The formation of chlorine-containing compound and complex compound is almost synchronous formation, and process is simple, purification efficiency are very high.
It is preferably provided with:Structure in plasma device is that board-like mechanism, i.e. plasma device include shell, multiple tools There is the dividing plate of air-vent, shell is have cavity in cylinder, shell, and multiple dividing plates are arranged at shell and are located in cavity, often Complexing agent is equipped with individual dividing plate, shell has air inlet and gas outlet, and air inlet is located at the lower section of shell, and gas outlet is located at There is micro Cl at once after entering plasma device in the top of shell, circulating hydrogen2Activate into the very strong chlorine of reactivity Free radical, and there is substitution reaction generation chlorine-containing compound with hydride, the circulating hydrogen with chlorine-containing compound is in shell Cavity is moved upwards, through dividing plate and the complexing agent on chlorine-containing compound and dividing plate is reacted the complex compound to form stabilization, is carried out Circulating hydrogen after deep purifying is discharged from gas outlet, in continuing on for the production of electronic-grade polycrystalline silicon.Multiple dividing plates are set to come Complexing agent is placed, makes contact of the chlorine-containing compound with complexing agent more abundant, chlorine-containing compound can sufficiently react to form steady Fixed complex compound, makes the purification efficiency of circulating hydrogen higher.
Circulating hydrogen with chlorine-containing compound is passed through in liquefying plant, chlorine-containing compound is liquefied chloride so as to realize Compound is separated with circulating hydrogen.Compared with original hydride, the boiling point of chlorine-containing compound is high, so, it easily liquefies, So that it is separated with gaseous circulating hydrogen, the circulating hydrogen after purification is then used in the production of electronic-grade polycrystalline silicon.
The boiling point of hydride is relatively low, such as:PH3Boiling point be -87.7 DEG C, B2H6Boiling point be -92.5 DEG C, chlorine-containing compound Boiling point it is higher, such as PCl3Boiling point be 76.1 DEG C, B2H6Chlorine substituent and B2H6The Nomenclature Composition and Structure of Complexes it is similar, PH3Chlorine substituent With PH3The Nomenclature Composition and Structure of Complexes it is similar, so, B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2 Boiling point Deng the chlorine-containing compound of material is all significantly improved.
So, separate is carried out under conditions of temperature is for -20 DEG C~10 DEG C, that is, it is -20 to control the temperature in liquefying plant DEG C~10 DEG C, when the circulating hydrogen with chlorine-containing compound is passed through in liquefying plant, what chlorine-containing compound can be quickly Liquefaction, makes chlorine-containing compound be separated from circulating hydrogen, and the circulating hydrogen after deep purifying to continue on for electron level more In the production of crystal silicon.Control is relatively easy to realize in this temperature range, and chlorine-containing compound fast liquefying is can guarantee that again.
Similar implementation method can also be:It is 1 × 10 to separate in pressure6Pa~5 × 106Carried out under conditions of Pa, will After circulating hydrogen with chlorine-containing compound is passed through in liquefying plant, it is 1 that pressure is applied to the circulating hydrogen in liquefying plant ×106Pa~5 × 106The pressure of Pa, makes the chlorine-containing compound fast liquefying in circulating hydrogen, and the recycle hydrogen after deep purifying Gas continues on in the production of electronic-grade polycrystalline silicon.
In order that the liquefaction effect of the chlorine-containing compound in the circulating hydrogen with chlorine-containing compound is more preferable, separate in temperature For -20 DEG C~10 DEG C, pressure are 1 × 106Pa~5 × 106Carried out under conditions of Pa, that is, the temperature for controlling liquefying plant is -20 DEG C ~10 DEG C, after the circulating hydrogen with chlorine-containing compound is passed through in liquefying plant, the circulating hydrogen in liquefying plant is applied It is 1 × 10 that pressurization is strong6Pa~5 × 106The pressure of Pa, makes the chlorine-containing compound fast liquefying in circulating hydrogen, and its purification efficiency is more Height, and during the circulating hydrogen after deep purifying continues on for the production of electronic-grade polycrystalline silicon.
More preferably, liquefying plant is rectifying column, when the circulating hydrogen with chlorine-containing compound is passed through in rectifying column, Outside condensed water can make in chlorine-containing compound liquefaction inflow rectifying column, and the circulating hydrogen after deep purifying continues on for electronics In the production of level polysilicon.
Complex compound of the chlorine-containing compound with complexing agent reaction generation stabilization in plasma device is carried out and circulating hydrogen When separation, the reaction of chlorine-containing compound may be not thorough enough, so, two step separating treatments can also be implemented:To plasma Complexing agent is added in body device, so that the chlorine-containing compound of generation obtains complex compound with complexing agent reaction;By remaining chloride containing Compound is passed through in liquefying plant with circulating hydrogen, chlorine-containing compound is liquefied so as to realize chlorine-containing compound and recycle hydrogen qi leel From reaching the purpose of deep purifying circulating hydrogen.
Embodiment 1
Micro Cl will be contained2、B2H6And PH3Circulating hydrogen Deng impurity is passed through in the plasma device with complexing agent, High purity quartz, micro Cl are provided with the electrode of plasma device2It is changed into the very strong chlorine radical of reactivity, with B2H6 And PH3Deng small molecular weight impurity reaction generation B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、 PCl3Deng chloride, chloride reacts to form stable complex compound with the complexing agent in plasma device, and depth is net Circulating hydrogen after change continues on in the production of electronic-grade polycrystalline silicon.
Embodiment 2
Micro Cl will be contained2、B2H6And PH3Circulating hydrogen Deng impurity is passed through in plasma device, plasma device Electrode on be provided with high purity aluminium oxide, micro Cl2It is changed into the very strong chlorine radical of reactivity, with B2H6And PH3Etc. small point Sub- impurity reaction generation B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Deng chloride containing Thing.
Circulating hydrogen with chlorine-containing compound is passed through in the liquefying plant that temperature is -20 DEG C, makes chlorine-containing compound liquid Change, so that chlorine-containing compound is separated with circulating hydrogen, the circulating hydrogen after deep purifying continues on for electronic-grade polycrystalline silicon In production.
Embodiment 3
Micro Cl will be contained2、B2H6And PH3Circulating hydrogen Deng impurity is passed through in plasma device, plasma device Electrode on be provided with high purity quartz, micro Cl2It is changed into the very strong chlorine radical of reactivity, with B2H6And PH3Etc. small molecule Impurity reaction generation B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Deng chloride.
Circulating hydrogen with chlorine-containing compound is passed through in liquefying plant, and the circulating hydrogen in liquefying plant is applied Pressure is 1 × 106The pressure of Pa, makes chlorine-containing compound liquefy, so that chlorine-containing compound is separated with circulating hydrogen, deep purifying Circulating hydrogen afterwards continues on in the production of electronic-grade polycrystalline silicon.
Embodiment 4
Micro Cl will be contained2、B2H6And PH3Circulating hydrogen Deng impurity is passed through in plasma device, plasma device Electrode on be provided with high purity aluminium oxide, micro Cl2It is changed into the very strong chlorine radical of reactivity, with B2H6And PH3Etc. small point Sub- impurity reaction generation B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Deng chloride containing Thing.
Circulating hydrogen with chlorine-containing compound is passed through in the liquefying plant that temperature is 10 DEG C, and in liquefying plant It is 5 × 10 that circulating hydrogen applies pressure6The pressure of Pa, makes chlorine-containing compound liquefy, so that chlorine-containing compound and circulating hydrogen Separate, the circulating hydrogen after deep purifying continues on in the production of electronic-grade polycrystalline silicon.
Embodiment 5
Micro Cl will be contained2、B2H6And PH3Circulating hydrogen Deng impurity is passed through in plasma device, plasma device Electrode on be provided with high purity aluminium oxide, micro Cl2It is changed into the very strong chlorine radical of reactivity, with B2H6And PH3Etc. small point Sub- impurity reaction generation B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Deng chloride containing Thing.
Circulating hydrogen with chlorine-containing compound is passed through in rectifying column, chlorine-containing compound is liquefied, so that chloride containing Compound is separated with circulating hydrogen, and the circulating hydrogen after deep purifying continues on in the production of electronic-grade polycrystalline silicon.
Embodiment 6
Micro Cl will be contained2、B2H6And PH3Circulating hydrogen Deng impurity is passed through in the plasma device with complexing agent, High purity quartz, micro Cl are provided with the electrode of plasma device2It is changed into the very strong chlorine radical of reactivity, with B2H6 And PH3Deng small molecular weight impurity reaction generation B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、 PCl3Deng chloride, chloride reacts to form stable complex compound with the complexing agent in plasma device.
Circulating hydrogen of the residue with a small amount of chlorine-containing compound is passed through in rectifying column, chlorine-containing compound is liquefied, so that Chlorine-containing compound is separated with circulating hydrogen, and the circulating hydrogen after deep purifying continues on in the production of electronic-grade polycrystalline silicon.
Embodiment 7
Micro Cl will be contained2、B2H6And PH3Circulating hydrogen Deng impurity is passed through in the plasma device with complexing agent, High purity aluminium oxide, micro Cl are provided with the electrode of plasma device2It is changed into the very strong chlorine radical of reactivity, with B2H6And PH3Deng small molecular weight impurity reaction generation B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、 PHCl2、PCl3Deng chloride, chloride reacts to form stable complex compound with the complexing agent in plasma device.
Circulating hydrogen of the residue with a small amount of chlorine-containing compound is passed through in the liquefying plant that temperature is 0 DEG C, makes chloride chemical combination Thing liquid, so that chlorine-containing compound is separated with circulating hydrogen, the circulating hydrogen after deep purifying continues on for electron level polycrystalline In the production of silicon.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.Reality of the invention The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of selected implementation of the invention Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made Every other embodiment, belongs to the scope of protection of the invention.

Claims (10)

1. the deep-purifying method of circulating hydrogen during a kind of electronic-grade polycrystalline silicon is produced, it is characterised in that Cl will be contained2, hydride The circulating hydrogen of impurity makes the Cl in being passed through plasma device2Activation obtains chlorine radical, the chlorine radical with it is described Hydride reaction obtains chlorine-containing compound, and the chlorine-containing compound is separated with the circulating hydrogen.
2. deep-purifying method according to claim 1, it is characterised in that set on the electrode of the plasma device There is dielectric.
3. deep-purifying method according to claim 2, it is characterised in that the dielectric is quartz or aluminum oxide.
4. deep-purifying method according to claim 1, it is characterised in that to adding complexing in the plasma device Agent so that the chlorine-containing compound and the complexing agent reaction of generation obtain complex compound realize the chlorine-containing compound with it is described The separation of circulating hydrogen.
5. deep-purifying method according to claim 1, it is characterised in that by with being followed described in the chlorine-containing compound Ring hydrogen is passed through in liquefying plant, makes the chlorine-containing compound liquefaction so as to realize the chlorine-containing compound with the circulating hydrogen Separate.
6. deep-purifying method according to claim 5, it is characterised in that the separation is -20 DEG C~10 DEG C in temperature Under conditions of carry out.
7. deep-purifying method according to claim 5, it is characterised in that the separation is 1 × 10 in pressure6Pa~5 × 106Carried out under conditions of Pa.
8. deep-purifying method according to claim 5, it is characterised in that the separation temperature be -20 DEG C~10 DEG C, Pressure is 1 × 106Pa~5 × 106Carried out under conditions of Pa.
9. deep-purifying method according to claim 5, it is characterised in that the liquefying plant is rectifying column.
10. deep-purifying method according to claim 1, it is characterised in that to adding network in the plasma device Mixture, so that the chlorine-containing compound of generation obtains complex compound with complexing agent reaction, by the remaining chloride chemical combination Thing is passed through in liquefying plant with the circulating hydrogen, makes the chlorine-containing compound liquefaction so as to realize the chlorine-containing compound and institute State circulating hydrogen separation.
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