CN105329902B - The adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane - Google Patents
The adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane Download PDFInfo
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- CN105329902B CN105329902B CN201510823969.3A CN201510823969A CN105329902B CN 105329902 B CN105329902 B CN 105329902B CN 201510823969 A CN201510823969 A CN 201510823969A CN 105329902 B CN105329902 B CN 105329902B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
- C01B33/10784—Purification by adsorption
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Abstract
The present invention provides the adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane, is related to electronic-grade polycrystalline silicon production field.Liquid phase trichlorosilane by rectification and purification initially enters vaporizer, is vaporized after heating, and the trichlorosilane temperature after vaporization is 40~110 DEG C；Gas phase trichlorosilane adsorbs into fixed bed to boron and P elements impurity, obtains high-purity trichlorosilane.The present invention realizes the process that trichlorosilane removes boron, P elements impurity by adsorption process, significantly reduce the content of the boracic and P elements impurity in trichlorosilane, improve the quality of trichlorosilane, the technical monopoly of foreign countries is breached, can be to realize that stable yields electronic-grade polycrystalline silicon lays the foundation in future.The technological process is simple, easy to operate, and energy consumption is relatively low, and impurity-eliminating effect is obvious.
Description
Technical field
The present invention relates to the purification technique field of electronic-grade polycrystalline silicon production, more particularly in high-purity trichlorosilane
The removal technique of ppb levels boron and P elements impurity.
Background technology
China's polycrystalline silicon industry is started in the fifties in last century, and the mid-1960s realize industrialization.Electronic information and too
The development of positive energy photovoltaic industry has driven the growth of polysilicon demand, the overall background of particularly domestic solar energy industry high speed development
Under, the photovoltaic constantly beyond market expectations increases installation amount newly and drives device requirements vigorous so that the raw material polysilicon of upstream needs
Ask and increase substantially.Between 2005-2008 4 years, domestic various regions are introduced one after another or exploitation production of polysilicon technology, introduce thousand
Tonne polycrystalline silicon production line, thriving trend is integrally presented in the market of polysilicon.Meanwhile for a long time, external polycrystalline
Silicon manufacturer carries out technology blockage to China, and most domestic enterprise is domestic so far also without one using backward production technology
Enterprise can steady production electronic-grade polycrystalline silicon, technical merit still suffers from larger gap compared with external.Overall gap shows raw
Small scale is produced, production cost is high, and quality is unstable, and environmental pollution is serious, and even many manufacturers were difficult to maintain production, phase in recent years
After stopping production.
Improved Siemens are the prevailing technologies of current production polysilicon：Metallurgical grade silica flour and hydrogen chloride are given birth in the reactor
Into trichlorosilane, then Trichlorosilane purification is refined, finally trichlorosilane is obtained with hydrogen by reduction reaction in reduction furnace
To high purity polycrystalline silicon.Trichlorosilane is as the most important recycle stock in the technique, even if the impurity wherein containing ppb levels,
Finally it can also influence polysilicon product purity.The major source of impurity is the introducing of metallurgical grade silica flour in technique, including metal chlorine
Compound, the chloride of boracic phosphorus and hydride and carbonaceous organic material etc., thus also inevitably exist in chlorosilane boron,
The trace impurities such as phosphorus, and these impurity can produce tremendous influence to final products polysilicon quality.
The purification technology of trichlorosilane is mainly rectification method at present.It is domestic that repeatedly de- is typically carried out to trichlorosilane
Remove light impurity and slough heavy seeds, rectifying column series is more (being usually that 6 towers even more multitower is connected).Due to partial impurities and chlorine silicon
The boiling point of alkane approaches, and only by traditional rectification method high energy consumption, equipment investment expense height, unstable product quality etc. can be brought to ask
Topic.It is of the invention then adsorbent is used as by modified resin, by adsorbing the boracic and P elements impurity that remove in trichlorosilane, make
The level of final products polysilicon stable yields electron level is obtained, the problem for solving polysilicon enterprise well.
The content of the invention
It is an object of the invention to solve above-mentioned insufficient problem, there is provided high-purity three in a kind of electronic-grade polycrystalline silicon production process
The adsorption-edulcoration technique of ppb levels boron and P elements impurity in chlorine hydrogen silicon, realize the target of stable yields electronic-grade polycrystalline silicon.
Technical scheme is as follows：Liquid phase trichlorosilane by rectification and purification initially enters vaporizer, by adding
Vaporized after heat, the trichlorosilane temperature after vaporization is 40~110 DEG C；Gas phase trichlorosilane enters fixed bed to boron and phosphorus member
Plain impurity is adsorbed, and finally gives high-purity trichlorosilane.
Used polymeric adsorbent is modified macroporous weakly-basic anion polymeric adsorbent, and full volumetric exchange capacity is more than
1.5eq/l, size distribution are 500~1400 μm, and bulk density is 550~850kg/m3。
Vaporizer is fixed tube sheet form, and fixed bed is tubulation structure.
Vaporizer is vertical fixed tube-sheet exchanger, and tube side walks trichlorosilane, material bottom in and top out, and the heating of shell side is situated between
Matter is 200kPa (G) saturated vapor, and temperature is 133 DEG C.
Fixed bed is tubulation structure, and tubulation fills polymeric adsorbent, material bottom in and top out, and shell side is passed through conduction oil to regulate and control to inhale
Enclosure temperature, adsorption temp is in the range of 40~110 DEG C.
The beneficial effects of the invention are as follows be reduced to B, P impurity in trichlorosilane to meet wanting for production electronic-grade polycrystalline silicon
Ask, it is as follows with specific reference to technical indicator：
| Industrial trichlorosilane | By the trichlorosilane of rectifying | Trichlorosilane Jing Guo adsorption treatment again | |
| B impurity (ppba) | 100 | 0.15~10 | <0.05 |
| P impurity (ppba) | ~100 | 0.5~10 | <0.05 |
| C impurity (ppba) | ~2000 | <500 | <25 |
Industrial trichlorosilane first passes through rectifying, then the high-purity trichlorosilane (index such as upper table) obtained after absorption, can
To cause final products polysilicon to stably reach the level of electron level.
Brief description of the drawings
Fig. 1 is ppb levels boron and P elements in high-purity trichlorosilane in electronic-grade polycrystalline silicon production process of the present invention
The adsorption-edulcoration process flow diagram of impurity.
Figure number and explanation：1- vaporizers, 2- adsorption columns, 3- heat conduction oil circulating pumps, 4-200KPa (G) steam, 5- steam
Vapour lime set, 6- liquid phase trichlorosilanes, 7- conduction oil oil returns, the high-purity gas phase trichlorosilanes of 8-.
Embodiment
Below in conjunction with the accompanying drawings 1, the technical scheme in inventive embodiments is clearly and completely described, it is clear that described
Embodiment be only part of the embodiment of the present invention, rather than whole embodiment.Based on the embodiment in the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained under the premise of creative work is not made, belongs to guarantor of the present invention
The scope of shield.
Embodiment 1
The adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane, the liquid phase three by rectification and purification
Chlorine hydrogen silicon initially enters vaporizer 1, and described vaporizer is vertical fixed tube-sheet exchanger, and tube side walks trichlorosilane, material
Bottom in and top out, the heating medium of shell side is 200kPa saturated vapors, and temperature is 133 DEG C.Vaporized after heating, after vaporization
Trichlorosilane temperature be 80 DEG C；Gas phase trichlorosilane adsorbs into fixed bed 2 to boron and P elements impurity, and fixed bed is
Tubulation structure, tubulation filling polymeric adsorbent, material bottom in and top out, shell side are passed through conduction oil to regulate and control adsorption temp, adsorption temp
In the range of 100 DEG C, it is down to by boracic in high-purity trichlorosilane of adsorption treatment and P elements impurity by 10ppba
Below 0.05ppba, meets the needs of polysilicon enterprise stable yields electronic-grade polycrystalline silicon.
All resins of described absorption be macroreticular weakly base the moon that polyhydroxy acid amide is modified, that polystyrene is skeleton from
Sub- polymeric adsorbent.
It is as follows with specific reference to technical indicator：
| Industrial trichlorosilane | By the trichlorosilane of rectifying | Trichlorosilane Jing Guo adsorption treatment again | |
| B impurity (ppba) | 100 | 1.5 | 0.01 |
| P impurity (ppba) | ~100 | 3 | 0.02 |
| C impurity (ppba) | ~2000 | 200 | 18 |
Embodiment 2
The adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane, by the liquid phase Jing Guo rectification and purification
Trichlorosilane initially enters vaporizer, is vaporized after heating, and described vaporizer is vertical fixed tube-sheet exchanger,
Tube side walks trichlorosilane, and material bottom in and top out, the heating medium of shell side is 200kPa saturated vapors, and temperature is 133 DEG C, after vaporization
Trichlorosilane temperature be 110 DEG C；Gas phase trichlorosilane adsorbs into fixed bed to boron and P elements impurity, and fixed bed is
Tubulation structure, tubulation filling polymeric adsorbent, material bottom in and top out, shell side are passed through conduction oil to regulate and control adsorption temp, adsorption temp
In the range of 80 DEG C.0.05ppba is down to by 10ppba by boracic in high-purity trichlorosilane of adsorption treatment and P elements impurity
Hereinafter, meets the needs of polysilicon enterprise stable yields electronic-grade polycrystalline silicon.
Adsorbent used in described absorption is the titanium dioxide that purity is 99.8%.
It is as follows with specific reference to technical indicator：
| Industrial trichlorosilane | By the trichlorosilane of rectifying | Trichlorosilane Jing Guo adsorption treatment again | |
| B impurity (ppba) | 100 | 5 | 0.04 |
| P impurity (ppba) | ~100 | 3.8 | 0.035 |
| C impurity (ppba) | ~2000 | 160 | 5 |
Embodiment 3
The adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane, by the liquid phase Jing Guo rectification and purification
Trichlorosilane initially enters vaporizer, and described vaporizer is vertical fixed tube-sheet exchanger, and tube side walks trichlorosilane, material
Bottom in and top out, the heating medium of shell side is 200kPa saturated vapors, and temperature is 133 DEG C.Vaporized after heating, after vaporization
Trichlorosilane temperature be 70 DEG C；Gas phase trichlorosilane adsorbs into fixed bed to boron and P elements impurity, and fixed bed is
Tubulation structure, tubulation filling polymeric adsorbent, material bottom in and top out, shell side are passed through conduction oil to regulate and control adsorption temp, adsorption temp
In the range of 50 DEG C.0.05ppba is down to by 10ppba by boracic in high-purity trichlorosilane of adsorption treatment and P elements impurity
Hereinafter, meets the needs of polysilicon enterprise stable yields electronic-grade polycrystalline silicon.Adsorbent used in described absorption is modified titanium dioxide for N
Titanium.
It is as follows with specific reference to technical indicator：
| Industrial trichlorosilane | By the trichlorosilane of rectifying | Trichlorosilane Jing Guo adsorption treatment again | |
| B impurity (ppba) | 100 | 2 | 0.01 |
| P impurity (ppba) | ~100 | 6 | 0.02 |
| C impurity (ppba) | ~2000 | 250 | 12 |
Embodiment 4
The adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane, by the liquid phase Jing Guo rectification and purification
Trichlorosilane initially enters vaporizer, and described vaporizer is vertical fixed tube-sheet exchanger, and tube side walks trichlorosilane, material
Bottom in and top out, the heating medium of shell side is 200kPa saturated vapors, and temperature is 133 DEG C.Vaporized after heating, after vaporization
Trichlorosilane temperature be 80 DEG C；Gas phase trichlorosilane adsorbs into fixed bed to boron and P elements impurity, and fixed bed is
Tubulation structure, tubulation filling polymeric adsorbent, material bottom in and top out, shell side are passed through conduction oil to regulate and control adsorption temp, adsorption temp
In the range of 60 DEG C.
Below 0.05ppba is down to by 10ppba by boracic in high-purity trichlorosilane of adsorption treatment and P elements impurity,
Meets the needs of polysilicon enterprise stable yields electronic-grade polycrystalline silicon.Adsorbent used in described absorption is modified dioxy for stearic acid sodium
Change titanium.
It is as follows with specific reference to technical indicator：
| Industrial trichlorosilane | By the trichlorosilane of rectifying | Trichlorosilane Jing Guo adsorption treatment again | |
| B impurity (ppba) | 100 | 0.3 | 0.01 |
| P impurity (ppba) | ~100 | 0.8 | 0.02 |
| C impurity (ppba) | ~2000 | 380 | 10 |
Embodiment 5
The adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane, by the liquid phase Jing Guo rectification and purification
Trichlorosilane initially enters vaporizer, and described vaporizer is vertical fixed tube-sheet exchanger, and tube side walks trichlorosilane, material
Bottom in and top out, the heating medium of shell side is 200kPa saturated vapors, and temperature is 133 DEG C.Vaporized after heating, after vaporization
Trichlorosilane temperature be 50 DEG C；Gas phase trichlorosilane adsorbs into fixed bed to boron and P elements impurity, and fixed bed is
Tubulation structure, tubulation filling polymeric adsorbent, material bottom in and top out, shell side are passed through conduction oil to regulate and control adsorption temp, adsorption temp
In the range of 100 DEG C.It is down to by boracic in high-purity trichlorosilane of adsorption treatment and P elements impurity by 10ppba
Below 0.05ppba, meets the needs of polysilicon enterprise stable yields electronic-grade polycrystalline silicon.
Adsorbent used in described absorption is stearic acid sodium modifying titanium dioxide.
It is as follows with specific reference to technical indicator：
| Industrial trichlorosilane | By the trichlorosilane of rectifying | Trichlorosilane Jing Guo adsorption treatment again | |
| B impurity (ppba) | 100 | 3 | 0.04 |
| P impurity (ppba) | ~100 | 4 | 0.01 |
| C impurity (ppba) | ~2000 | 400 | 20 |
Embodiment 6
The adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane, by the liquid phase Jing Guo rectification and purification
Trichlorosilane initially enters vaporizer, and described vaporizer is vertical fixed tube-sheet exchanger, and tube side walks trichlorosilane, material
Bottom in and top out, the heating medium of shell side is 200kPa saturated vapors, and temperature is 133 DEG C.Vaporized after heating, after vaporization
Trichlorosilane temperature be 100 DEG C；Gas phase trichlorosilane adsorbs into fixed bed to boron and P elements impurity, and fixed bed is
Tubulation structure, tubulation filling polymeric adsorbent, material bottom in and top out, shell side are passed through conduction oil to regulate and control adsorption temp, adsorption temp
In the range of 40 DEG C.0.05ppba is down to by 10ppba by boracic in high-purity trichlorosilane of adsorption treatment and P elements impurity
Hereinafter, meets the needs of polysilicon enterprise stable yields electronic-grade polycrystalline silicon.Adsorbent used in described absorption is bismuth oxybromide.
It is as follows with specific reference to technical indicator：
| Industrial trichlorosilane | By the trichlorosilane of rectifying | Trichlorosilane Jing Guo adsorption treatment again | |
| B impurity (ppba) | 100 | 0.15 | 0.008 |
| P impurity (ppba) | ~100 | 2 | 0.01 |
| C impurity (ppba) | ~2000 | 180 | 20 |
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (3)
1. the adsorption-edulcoration technique of ppb levels boron and P elements impurity in a kind of trichlorosilane, it is characterised in that rectifying will be passed through
The liquid phase trichlorosilane of purification initially enters vaporizer, is vaporized after heating, and the trichlorosilane temperature after vaporization is 40
~110 DEG C；Gas phase trichlorosilane adsorbs into fixed bed to boron and P elements impurity, finally gives high-purity trichlorosilane,
Polymeric adsorbent includes modifying titanium dioxide used by described absorption boron and P elements impurity, and BiOX is described
Modifying titanium dioxide includes N modifying titanium dioxides, stearic acid sodium modifying titanium dioxide, and poly ethyldiol modified titanium dioxide is described
BiOX be bismuth oxybromide.
2. the technique as described in claim 1, it is characterised in that described vaporizer is vertical fixed tube-sheet exchanger,
Tube side walks trichlorosilane, and material bottom in and top out, the heating medium of shell side is 200 kPa saturated vapors, and temperature is 133 DEG C.
3. the technique as described in claim 1, it is characterised in that fixed bed is tubulation structure, and tubulation fills polymeric adsorbent, thing
Expect bottom in and top out, shell side is passed through conduction oil to regulate and control adsorption temp, and adsorption temp is in the range of 40~110 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731465A (en) * | 2016-02-29 | 2016-07-06 | 天津大学 | Method and equipment for removing boron and phosphorous by utilizing chlorosilane fixed bed chemical adsorption reaction method |
| CN107235494A (en) * | 2017-07-05 | 2017-10-10 | 四川瑞能硅材料有限公司 | A kind of apparatus and method for removing high-purity chlorosilane trace impurity |
| TWI640473B (en) | 2017-12-07 | 2018-11-11 | 財團法人工業技術研究院 | Method and apparatus for removing boron |
| CN109205627A (en) * | 2018-11-08 | 2019-01-15 | 天津科技大学 | A kind of device and method that adsorbing and removing methylchlorosilane impurity prepares high-purity trichlorosilane |
| CN109575065B (en) * | 2018-12-25 | 2023-05-16 | 金宏气体股份有限公司 | Production method and production system of high-purity ethyl silicate |
| CN115023407B (en) * | 2020-11-05 | 2024-05-24 | 瓦克化学股份公司 | Method for removing impurities from chlorosilane mixtures |
| CN113402640A (en) * | 2021-06-10 | 2021-09-17 | 青海亚洲硅业半导体有限公司 | Adsorption resin for impurity removal of chlorosilane and preparation method thereof |
| CN113292664A (en) * | 2021-06-10 | 2021-08-24 | 青海亚洲硅业半导体有限公司 | Adsorption resin and preparation method thereof |
| CN113716570B (en) * | 2021-09-30 | 2023-08-01 | 四川永祥多晶硅有限公司 | Method for improving quality of trichlorosilane |
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