CN106744685B - 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 PDFInfo
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- CN106744685B CN106744685B CN201611020410.8A CN201611020410A CN106744685B CN 106744685 B CN106744685 B CN 106744685B CN 201611020410 A CN201611020410 A CN 201611020410A CN 106744685 B CN106744685 B CN 106744685B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
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Abstract
The present invention provides the deep-purifying method of circulating hydrogen in a kind of production of electronic-grade polycrystalline silicon, 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 in plasma device and make Cl2Activation obtains chlorine radical, and chlorine radical obtains chlorine-containing compound with hydride reaction, chlorine-containing compound is detached with circulating hydrogen.In this deep-purifying method, micro Cl is contained in circulating hydrogen2, micro Cl2Since strong-electromagnetic field effect can be activated fully in plasma device, is formed to have and be taken by force for active chlorine radical, chlorine radical preferentially can occur substitution reaction with hydride, it is made to change higher boiling, highly polar substance, be easy to detach with circulating hydrogen；Do not introduce outer impurity, byproduct of reaction only has micro HCl, be easy detached with circulating hydrogen；It is plasma-activated to make Cl2Activation is more abundant, achievees the purpose that circulating hydrogen deep purifying.
Description
Technical field
The purification technique field of tail gas in being produced the present invention relates to electronic-grade polycrystalline silicon, 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 novel industry such as integrated circuit, aerospace, new energy.
Although polysilicon industry development in China's is swift and violent in recent years, the size of capacity leaps to the first in the world, but still cannot achieve 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 in China.
The advanced purification technology of circulating hydrogen is the key that production 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 be split under the high temperature conditions
Solution reaction forms B2H6、PH3Etc. small molecules form, B2H6、PH3The depth removal of equal small molecular weight impurities is that China realizes that electron level is more
The significant challenge of crystal silicon scale volume production.The hydrogen used in production of polysilicon at present is mainly circulating hydrogen, the prior art without
Method realizes the depth removal of impurity in circulating hydrogen, and therefore, circulating hydrogen quality cannot be satisfied the scale of electronic-grade polycrystalline silicon
Production.
Invention content
The deep-purifying method of circulating hydrogen in being produced the purpose of the present invention is to provide a kind of electronic-grade polycrystalline silicon, can
Cl in removal circulating hydrogen well2, the impurity such as hydride, to make circulating hydrogen stably reach electron level.
Realization that the present invention adopts the following technical solutions：
The deep-purifying method of circulating hydrogen, will contain Cl in a kind of production of electronic-grade polycrystalline silicon2, hydride impurity follows
Ring hydrogen, which is passed through in plasma device, makes Cl2Activation obtains chlorine radical, and chlorine radical obtains chloride containing with hydride reaction
Object is closed, chlorine-containing compound is detached 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 provides
Beneficial effect is：
The deep-purifying method of circulating hydrogen in electronic-grade polycrystalline silicon provided by the invention production, containing micro- in circulating hydrogen
Measure Cl2, plasma device offer electromagnetic field, Cl2It is passed through in plasma device, free electron adds under the action 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 is collided with hydride impurity, makes the increased activity of hydride, and chlorine radical is made to be easy to generate chloride containing with hydride reaction
Close object；Meanwhile circulating hydrogen becomes nonequilibrium plasma completely in plasma device, will produce the wide strong light spoke of frequency
It penetrates, which can make Cl2Chlorine radical is activated into, and light substitution reaction occurs with hydride, obtains chlorine-containing compound, with
Original hydride is compared, and the boiling point height of chlorine-containing compound, polarity are strong, is easy to be detached with circulating hydrogen, circulating hydrogen obtains
To deep purifying, to make circulating hydrogen stably reach electron level, it is conducive to large-scale production electronic-grade polycrystalline silicon.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The deep-purifying method of circulating hydrogen carries out specific in being produced below to the electronic-grade polycrystalline silicon of the embodiment of the present invention
Explanation.
The deep-purifying method of circulating hydrogen, will contain Cl in a kind of production of electronic-grade polycrystalline silicon2, hydride impurity follows
Ring hydrogen, which is passed through in plasma device, makes Cl2Activation obtains chlorine radical.
Preferably, the circulating hydrogen directly released in electronic-grade polycrystalline silicon being produced is passed directly into plasma device,
The temperature for the circulating hydrogen directly released in electronic-grade polycrystalline silicon production is higher, is conducive to subsequent priming reaction, meanwhile, electronics
Level polysilicon production later just directly purifies circulating hydrogen, and being conducive to purified circulating hydrogen, to carry out electron level again more
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 under the action of electromagnetic field by electronics2Collision, makes Cl2It is changed into reaction to live
The very strong chlorine radical of property；Meanwhile circulating hydrogen becomes nonequilibrium plasma completely in plasma device, will produce frequency
The wide high light radiation of rate, the light radiation can make Cl2Chlorine radical is activated into, the micro Cl in circulating hydrogen is made2It can be sufficient
It is converted to the very strong chlorine radical of reactivity.
The active activity of chlorine radical is very strong, and high energy electron is also collided with hydride impurity, makes the increased activity of hydride,
Highly active chlorine radical is easy to react with the hydride of increased activity generates chlorine-containing compound.
In the embodiment of the present invention, hydride is mainly B2H6And PH3Equal small molecular weight impurities, take with chlorine radical
Generation reaction can generate B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Equal chlorides.
It is provided with dielectric on the electrode of plasma device, is made using dielectric barrier discharge micro in circulating hydrogen
Cl2Activation, prevents metal electrode from ionizing, and avoids introducing metal impurities, avoids generating new impurity, keep circulating hydrogen dirty
Dye.It is preferably provided with：Dielectric is quartz or aluminium oxide.Quartz is high purity quartz, avoids introducing new impurity, avoid to electron level
Polysilicon pollutes.Similarly, aluminium oxide is high purity aluminium oxide.
Compared with original hydride, the boiling point height of chlorine-containing compound, polarity are strong, are easy to be detached with circulating hydrogen,
Chlorine-containing compound is detached with circulating hydrogen, deep purifying can be carried out to circulating hydrogen, to make circulating hydrogen stably reach electricity
Sub- grade is conducive to large-scale production electronic-grade polycrystalline silicon.
Complexing agent is added into plasma device, so that complex compound is obtained by the reaction with complexing agent in the chlorine-containing compound generated
Realize the separation of chlorine-containing compound and circulating hydrogen.Compared with original hydride, the polarity of chlorine-containing compound is strong, so,
It easily reacts to form stable complex compound with complexing agent, complex compound stays in plasma device, to realize B2H6And PH3Deng
The depth of small molecular weight impurity removes, and achievees the purpose that 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 all very quickly, reach microsecond
Grade.Complexing agent is filled into plasma device, the micro Cl in circulating hydrogen2It is free to activate into the very strong chlorine of reactivity
Base, and with after hydride generation substitution reaction generation chlorine-containing compound, continuation reacts to form stable complex compound with complexing agent,
Chlorine-containing compound and the formation of complex compound are almost synchronous formation, simple for process, purification efficiency is very high.
It is preferably provided with：Structure in plasma device is board-like mechanism, i.e. plasma device includes shell, multiple tools
It is cylinder to have the partition board of air hole, shell, there is cavity, multiple partition boards to be set to shell and in cavity, often in shell
Complexing agent is equipped on a partition board, there is shell air inlet and gas outlet, air inlet to be located at the lower section of shell, and gas outlet is located at
After entering plasma device micro Cl occurs at once for the top of shell, circulating hydrogen2Activate into the very strong chlorine of reactivity
Free radical, and substitution reaction occurs with hydride and generates chlorine-containing compound, the circulating hydrogen with chlorine-containing compound is in shell
Cavity moves upwards, and across partition board and chlorine-containing compound is made to react to form stable complex compound with the complexing agent on partition board, carries out
Circulating hydrogen after deep purifying is discharged from gas outlet, in the production for continuing on for electronic-grade polycrystalline silicon.Multiple partition boards are set
Complexing agent is placed, keeps contact of the chlorine-containing compound with complexing agent more abundant, chlorine-containing compound can adequately react to be formed surely
Fixed complex compound makes the purification efficiency higher of circulating hydrogen.
Circulating hydrogen with chlorine-containing compound is passed through in liquefying plant, chlorine-containing compound liquefaction is made to contain chlorine to realize
The separation of compound and circulating hydrogen.Compared with original hydride, the boiling point of chlorine-containing compound is high, so, easily liquefy,
To make it be detached with gaseous circulating hydrogen, purified circulating hydrogen 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
The boiling point of the chlorine-containing compound of equal substances is all significantly improved.
So separation carries out under conditions of temperature is -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 to continue on for electron level more for the circulating hydrogen after deep purifying
In the production of crystal silicon.Control is relatively easy to realize in this temperature range, and can guarantee chlorine-containing compound fast liquefying.
Similar embodiment can also be：Separation is 1 × 10 in pressure6Pa~5 × 106It carries out, i.e., will under conditions of Pa
After circulating hydrogen with chlorine-containing compound is passed through in liquefying plant, it is 1 to apply pressure 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 in the production of electronic-grade polycrystalline silicon.
In order to keep the liquefaction effect for the chlorine-containing compound for having in the circulating hydrogen of chlorine-containing compound more preferable, detach in temperature
For -20 DEG C~10 DEG C, pressure be 1 × 106Pa~5 × 106It is carried 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
Pressurization is 1 × 10 by force6Pa~5 × 106The pressure of Pa makes the chlorine-containing compound fast liquefying in circulating hydrogen, and purification efficiency is more
Height, and the circulating hydrogen after deep purifying continues in 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,
External condensed water can be such that chlorine-containing compound liquefaction flows into rectifying column, and the circulating hydrogen after deep purifying continues on for electronics
In the production of level polysilicon.
Chlorine-containing compound, which reacts in plasma device with complexing agent, generates stable complex compound progress 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 complex compound is obtained by the reaction with complexing agent in the chlorine-containing compound generated；By remaining chloride containing
It closes object to be passed through in liquefying plant with circulating hydrogen, makes chlorine-containing compound liquefaction to realize chlorine-containing compound and recycle hydrogen qi leel
From achieving the purpose that deep purifying circulating hydrogen.
Embodiment 1
Micro Cl will be contained2、B2H6And PH3The circulating hydrogen of equal impurity is passed through in the plasma device with complexing agent,
High purity quartz, micro Cl are provided on the electrode of plasma device2It is changed into the very strong chlorine radical of reactivity, with B2H6
And PH3Equal small molecular weight impurities reaction generates B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、
PCl3Equal chlorides, chloride is reacted with the complexing agent in plasma device to form stable complex compound, and depth is net
Circulating hydrogen after change continues in the production of electronic-grade polycrystalline silicon.
Embodiment 2
Micro Cl will be contained2、B2H6And PH3The circulating hydrogen of equal 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 generates B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Equal chloride containings
Object.
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, to make chlorine-containing compound be detached 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 PH3The circulating hydrogen of equal 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 molecules
Impurity reaction generates B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Equal chlorides.
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, to make chlorine-containing compound be detached with circulating hydrogen, deep purifying
Circulating hydrogen afterwards continues in the production of electronic-grade polycrystalline silicon.
Embodiment 4
Micro Cl will be contained2、B2H6And PH3The circulating hydrogen of equal 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 generates B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Equal chloride containings
Object.
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, which applies pressure,6The pressure of Pa, makes chlorine-containing compound liquefy, to make chlorine-containing compound and circulating hydrogen
It detaches, the circulating hydrogen after deep purifying continues in the production of electronic-grade polycrystalline silicon.
Embodiment 5
Micro Cl will be contained2、B2H6And PH3The circulating hydrogen of equal 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 generates B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、PCl3Equal chloride containings
Object.
Circulating hydrogen with chlorine-containing compound is passed through in rectifying column, chlorine-containing compound is made to liquefy, to make chloride containing
It closes object to detach with circulating hydrogen, the circulating hydrogen after deep purifying continues in the production of electronic-grade polycrystalline silicon.
Embodiment 6
Micro Cl will be contained2、B2H6And PH3The circulating hydrogen of equal impurity is passed through in the plasma device with complexing agent,
High purity quartz, micro Cl are provided on the electrode of plasma device2It is changed into the very strong chlorine radical of reactivity, with B2H6
And PH3Equal small molecular weight impurities reaction generates B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、PHCl2、
PCl3Equal chlorides, chloride react to form stable complex compound with the complexing agent in plasma device.
There is residue the circulating hydrogen of a small amount of chlorine-containing compound to be passed through in rectifying column, so that chlorine-containing compound is liquefied, to make
Chlorine-containing compound is detached with circulating hydrogen, and the circulating hydrogen after deep purifying continues in the production of electronic-grade polycrystalline silicon.
Embodiment 7
Micro Cl will be contained2、B2H6And PH3The circulating hydrogen of equal impurity is passed through in the plasma device with complexing agent,
High purity aluminium oxide, micro Cl are provided on the electrode of plasma device2It is changed into the very strong chlorine radical of reactivity, with
B2H6And PH3Equal small molecular weight impurities reaction generates B2H5Cl、B2H4Cl2、B2H3Cl3、B2H2Cl4、B2HCl5、B2Cl6、PH2Cl、
PHCl2、PCl3Equal chlorides, chloride react to form stable complex compound with the complexing agent in plasma device.
There is residue the circulating hydrogen of a small amount of chlorine-containing compound to be passed through in the liquefying plant that temperature is 0 DEG C, and chloride containing is made to close
Thing liquid, to make chlorine-containing compound be detached 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 the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (8)
1. the deep-purifying method of circulating hydrogen in a kind of electronic-grade polycrystalline silicon production, which is characterized in that Cl will be contained2, hydride
The circulating hydrogen of impurity, which is passed through in plasma device, makes the Cl2Activation obtains chlorine radical, the chlorine radical with it is described
Hydride reaction obtains chlorine-containing compound, and complexing agent is added into the plasma device, so that the chloride containing generated
It closes object and the separation that complex compound realizes the chlorine-containing compound and the circulating hydrogen is obtained by the reaction with the complexing agent.
2. deep-purifying method according to claim 1, which is characterized in that be arranged on the electrode of the plasma device
There is dielectric.
3. deep-purifying method according to claim 2, which is characterized in that the dielectric is quartz or aluminium oxide.
4. deep-purifying method according to claim 1, which is characterized in that will be with being followed described in the chlorine-containing compound
Ring hydrogen is passed through in liquefying plant, makes the chlorine-containing compound liquefaction to realize the chlorine-containing compound and the circulating hydrogen
Separation.
5. deep-purifying method according to claim 4, which is characterized in that the separation is -20 DEG C~10 DEG C in temperature
Under conditions of carry out.
6. deep-purifying method according to claim 4, which is characterized in that the separation is 1 × 10 in pressure6Pa~5 ×
106It is carried out under conditions of Pa.
7. deep-purifying method according to claim 4, which is characterized in that it is described separation temperature be -20 DEG C~10 DEG C,
Pressure is 1 × 106Pa~5 × 106It is carried out under conditions of Pa.
8. deep-purifying method according to claim 4, which is characterized in that the liquefying plant is rectifying column.
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| FR1518553A (en) * | 1960-03-11 | 1968-03-29 | Pechiney Prod Chimiques Sa | Process for the purification of volatile compounds of germanium and silicon |
| DE1792651A1 (en) * | 1968-09-28 | 1971-11-25 | Dynamit Nobel Ag | Process for cleaning chlorosilanes |
| US4372834A (en) * | 1981-06-19 | 1983-02-08 | Bell Telephone Laboratories, Incorporated | Purification process for compounds useful in optical fiber manufacture |
| DE102004037675A1 (en) * | 2004-08-04 | 2006-03-16 | Degussa Ag | Process and apparatus for purifying hydrogen-containing silicon tetrachloride or germanium tetrachloride |
| ITRM20040570A1 (en) * | 2004-11-19 | 2005-02-19 | Memc Electronic Materials | PROCEDURE AND PLANT FOR THE PURIFICATION OF TRICHLOROSILANE AND SILICON TETRACLORIDE. |
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