CN112390257B - Electronic grade polycrystalline silicon production system and method - Google Patents
Electronic grade polycrystalline silicon production system and method Download PDFInfo
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- CN112390257B CN112390257B CN202011301481.1A CN202011301481A CN112390257B CN 112390257 B CN112390257 B CN 112390257B CN 202011301481 A CN202011301481 A CN 202011301481A CN 112390257 B CN112390257 B CN 112390257B
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000001179 sorption measurement Methods 0.000 claims abstract description 86
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000000926 separation method Methods 0.000 claims abstract description 74
- 238000000151 deposition Methods 0.000 claims abstract description 37
- 230000008021 deposition Effects 0.000 claims abstract description 37
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 27
- 238000003860 storage Methods 0.000 claims abstract description 17
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims abstract description 11
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims abstract description 11
- 229940045803 cuprous chloride Drugs 0.000 claims abstract description 11
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 claims abstract description 11
- 239000000969 carrier Substances 0.000 claims abstract description 5
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 114
- 239000005052 trichlorosilane Substances 0.000 claims description 114
- 239000007789 gas Substances 0.000 claims description 109
- 229920005591 polysilicon Polymers 0.000 claims description 46
- 238000005984 hydrogenation reaction Methods 0.000 claims description 41
- 229910052739 hydrogen Inorganic materials 0.000 claims description 37
- 239000001257 hydrogen Substances 0.000 claims description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 31
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 30
- 239000005049 silicon tetrachloride Substances 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 26
- 230000008569 process Effects 0.000 claims description 20
- 239000011148 porous material Substances 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003456 ion exchange resin Substances 0.000 claims description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 47
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 17
- 229910052796 boron Inorganic materials 0.000 abstract description 17
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 17
- 239000011574 phosphorus Substances 0.000 abstract description 17
- 238000005265 energy consumption Methods 0.000 abstract description 12
- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 239000002184 metal Substances 0.000 abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000011863 silicon-based powder Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 4
- 229940050176 methyl chloride Drugs 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000005234 chemical deposition Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007323 disproportionation reaction Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- 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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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses an electronic grade polycrystalline silicon production system and method. Wherein, electronic grade polycrystalline silicon production system includes: the pretreatment device comprises a plurality of adsorption columns connected in series, wherein adsorption carriers and adsorption load components are arranged in the adsorption columns, and the adsorption load components comprise at least one of platinum tetrachloride and cuprous chloride; a rectification device; a deposition device; a first tail gas separation device; and the dichlorosilane storage tank is connected with the first tail gas separation device, is suitable for storing dichlorosilane separated by the first tail gas separation device, and supplies dichlorosilane separated by the first tail gas separation device to the deposition device for chemical vapor deposition treatment. The system can obviously reduce the content of impurities such as boron, phosphorus, carbon, metal and the like in the electronic grade polycrystalline product, produce the obtained high-quality electronic grade polycrystalline product and reduce the production energy consumption.
Description
Technical Field
The invention relates to the technical field of polycrystalline silicon production, in particular to a system and a method for producing electronic grade polycrystalline silicon.
Background
Since the last 60 years of formation, the improved siemens process has become the mainstream polysilicon production technology through a great deal of technical improvement and is always used in the semiconductor industry. Around 2005, with the development of the photovoltaic industry, the cost control in the aspects of process parameters, equipment model selection, production environment control and the like is correspondingly adjusted by the improved siemens method, and the method is widely applied to the manufacture of photovoltaic grade polysilicon.
Electronic grade polysilicon is a basic raw material of the integrated circuit industry, and along with the continuous development of the processing capability of integrated circuits, the quality requirement of the electronic grade polysilicon is higher and higher. At present, only several polysilicon manufacturers in the world can produce high-purity electronic grade polysilicon which can be used for 12-inch semiconductor grade silicon chips, an improved Siemens process is adopted, the process route takes a chemical vapor deposition link as a core, and also comprises production links such as rectification, tail gas separation, hydrogenation, post-treatment and the like, so that a set of production system capable of being recycled is constructed. Due to the characteristics of the advanced process technology of integrated circuits, the requirements of electronic grade polysilicon on various impurity control and fluctuation stability are also continuously improved, which makes continuous technical progress in each link of improving siemens process to avoid quality bottleneck which can not be overcome in some production processes.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. To this end, it is an object of the present invention to provide an electronic grade polysilicon production system and method. The system can obviously reduce the content of impurities such as boron, phosphorus, carbon, metal and the like in the electronic grade polycrystalline silicon product, produce the obtained high-quality electronic grade polycrystalline silicon product and reduce the production energy consumption.
In one aspect of the invention, an electronic grade polysilicon production system is provided. According to an embodiment of the invention, the electronic grade polysilicon production system comprises:
the pretreatment device comprises a plurality of adsorption columns connected in series, wherein adsorption carriers and adsorption load components are arranged in the adsorption columns, and the adsorption load components comprise at least one of platinum tetrachloride and cuprous chloride; the pretreatment device is suitable for pretreating a trichlorosilane raw material to obtain pretreated trichlorosilane;
the rectifying device is connected with the pretreatment device and is suitable for rectifying the pretreated trichlorosilane to obtain rectified trichlorosilane;
the deposition device is connected with the rectification device and is suitable for performing chemical vapor deposition treatment by using hydrogen and the rectified trichlorosilane to obtain electronic grade polycrystalline silicon and discharging first tail gas containing trichlorosilane, dichlorosilane, silicon tetrachloride and hydrogen;
the first tail gas separation device is connected with the deposition device and is suitable for carrying out first separation treatment on the first tail gas to respectively obtain trichlorosilane, dichlorosilane, hydrogen and first treated tail gas containing silicon tetrachloride;
and the dichlorosilane storage tank is connected with the first tail gas separation device, is suitable for storing dichlorosilane separated by the first tail gas separation device, and supplies dichlorosilane separated by the first tail gas separation device to the deposition device for chemical vapor deposition treatment.
According to the electronic grade polycrystalline silicon production system provided by the embodiment of the invention, the trichlorosilane raw material is pretreated by the pretreatment device, so that impurities such as boron, phosphorus and the like in the trichlorosilane raw material can be removed.
The inventor finds that the commercial trichlorosilane raw material is mostly produced by a trichlorosilane synthesis device or a cold hydrogenation device in research. The trichlorosilane synthesis device uses HCl and silicon powder to react in a fixed bed or fluidized bed reactor, the cold hydrogenation device uses silicon tetrachloride, hydrogen and silicon powder to react in a fluidized bed, and both silicon powder and hydrogen are used as reactants. The silicon powder contains a large amount of phosphorus-containing impurities, boron-containing impurities and metal impurities, and cannot be removed in the process of preparing trichlorosilane. Meanwhile, the two production processes are easy to introduce organic impurities such as methyl chlorosilane, methyl chloride and the like into the trichlorosilane product. However, the above impurities cannot be effectively removed by the rectification system, and the production system is contaminated. The inventors have found that platinum tetrachloride is present on BClxHas good adsorption effect, and cuprous chloride is used for adsorbing PClyHas good adsorption effect (PCl)yP in the adsorption column has lone pair electrons, and is easy to form alpha-pi bond interaction with Cu so as to be adsorbed on Cu), and the metal impurities and organic impurities can be adsorbed on the adsorption column carrier. Therefore, the trichlorosilane raw material is pretreated by adopting a plurality of adsorption columns which take platinum tetrachloride and cuprous chloride as adsorption load components, so that the content of impurities such as boron, phosphorus, carbon, metal and the like in the electronic grade polycrystalline silicon product can be obviously reduced, and the high-quality electronic grade polycrystalline silicon product is produced.
On the other hand, for the first tail gas containing trichlorosilane, dichlorosilane, silicon tetrachloride and hydrogen generated in the chemical vapor deposition treatment, in the prior art, the tail gas is generally subjected to disproportionation treatment to obtain trichlorosilane for continuous use. However, the inventors have found that during the chemical vapor deposition process, the heterogeneous chemical deposition rates of different substances and the reaction selectivity between the gas phase and the solid phase are significantly different. By adjusting the content of dichlorosilane in reaction systems at different stages in the chemical vapor deposition process, the boron and phosphorus in the polycrystalline silicon rod body, the deposition rate and the overall reaction rate can be obviously influenced. Therefore, the dichlorosilane separated from the first tail gas is stored in an independent storage tank, and the storage tank is independently controlled to supply the dichlorosilane to the deposition device according to the progress of chemical vapor deposition, so that impurities can be further prevented from being deposited on the silicon rod, and the production energy consumption is reduced.
In addition, the electronic grade polysilicon production system according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the present invention, the adsorption column comprises a first adsorption column, a second adsorption column and a third adsorption column, wherein the pore diameter of the adsorption carrier in the first adsorption column is 12-9 nm, the pore diameter of the adsorption carrier in the second adsorption column is 7-5 nm, and the pore diameter of the adsorption carrier in the third adsorption column is 3-2 nm.
In some embodiments of the invention, the adsorbent support is selected from at least one of silica gel, ion exchange resin.
In some embodiments of the present invention, the first tail gas separation device is further connected to the rectification device, and is adapted to supply the separated trichlorosilane to the rectification device for the rectification treatment.
In some embodiments of the present invention, the electronic grade polysilicon production system further comprises: and the thermal hydrogenation device is connected with the first tail gas separation device and is suitable for carrying out thermal hydrogenation treatment on the first treated tail gas to obtain a second tail gas containing trichlorosilane, silicon tetrachloride and hydrogen.
In some embodiments of the present invention, the electronic grade polysilicon production system further comprises: and the second tail gas separation device is connected with the thermal hydrogenation device and is suitable for carrying out second separation treatment on the second tail gas to respectively obtain trichlorosilane and second treated tail gas containing silicon tetrachloride and hydrogen, and the trichlorosilane obtained by separation is supplied to the rectification device for rectification treatment, and the second treated tail gas obtained by separation is supplied to the thermal hydrogenation device for thermal hydrogenation treatment.
In another aspect of the invention, the invention provides a method for producing electronic grade polycrystalline silicon. According to the embodiment of the invention, the electronic grade polycrystalline silicon production method comprises the following steps:
(1) feeding a trichlorosilane raw material into a pretreatment device for pretreatment to obtain pretreated trichlorosilane;
(2) feeding the pretreated trichlorosilane into a rectifying device for rectification to obtain rectified trichlorosilane;
(3) supplying hydrogen and the rectified trichlorosilane into a deposition device for chemical vapor deposition treatment to obtain electronic grade polycrystalline silicon and first tail gas containing trichlorosilane, dichlorosilane, silicon tetrachloride and hydrogen;
(4) supplying the first tail gas into a first tail gas separation device for first separation treatment to respectively obtain trichlorosilane, dichlorosilane, hydrogen and first-treated tail gas containing silicon tetrachloride;
(5) and supplying the dichlorosilane separated by the first tail gas separation device to a dichlorosilane storage tank for storage, and supplying the dichlorosilane separated by the first tail gas separation device to the deposition device for the chemical vapor deposition treatment.
According to the production method of the electronic grade polycrystalline silicon, provided by the embodiment of the invention, the trichlorosilane raw material is pretreated by the pretreatment device, so that impurities such as boron, phosphorus and the like in the trichlorosilane raw material can be removed.
The inventor finds that the commercial trichlorosilane raw material is mostly produced by a trichlorosilane synthesis device or a cold hydrogenation device in research. The trichlorosilane synthesis device uses HCl and silicon powder to react in a fixed bed or fluidized bed reactor, the cold hydrogenation device uses silicon tetrachloride, hydrogen and silicon powder to react in a fluidized bed, and both silicon powder and hydrogen are used as reactants. The silicon powder contains a large amount of phosphorus-containing impurities, boron-containing impurities and metal impurities, and has no phosphorus impurities, boron-containing impurities and metal impuritiesThe method is removed in the process of preparing the trichlorosilane. Meanwhile, the two production processes are easy to introduce organic impurities such as methyl chlorosilane, methyl chloride and the like into the trichlorosilane product. However, the above impurities cannot be effectively removed by the rectification system, and the production system is contaminated. The inventors have found that platinum tetrachloride is present on BClxHas good adsorption effect, and cuprous chloride is used for adsorbing PClyHas good adsorption effect (PCl)yP in the adsorption column has lone pair electrons, and is easy to form alpha-pi bond interaction with Cu so as to be adsorbed on Cu), and the metal impurities and organic impurities can be adsorbed on the adsorption column carrier. Therefore, the trichlorosilane raw material is pretreated by adopting a plurality of adsorption columns which take platinum tetrachloride and cuprous chloride as adsorption load components, so that the content of impurities such as boron, phosphorus, carbon, metal and the like in the electronic grade polycrystalline product can be obviously reduced, and the high-quality electronic grade polycrystalline product is produced.
On the other hand, for the first tail gas containing trichlorosilane, dichlorosilane, silicon tetrachloride and hydrogen generated in the chemical vapor deposition treatment, in the prior art, the tail gas is generally subjected to disproportionation treatment to obtain trichlorosilane for continuous use. However, the inventors have found that during the chemical vapor deposition process, the heterogeneous chemical deposition rates of different substances and the reaction selectivity between the gas phase and the solid phase are significantly different. By adjusting the content of dichlorosilane in reaction systems at different stages in the chemical vapor deposition process, the boron and phosphorus in the polycrystalline silicon rod body, the deposition rate and the overall reaction rate can be obviously influenced. Therefore, the dichlorosilane separated from the first tail gas is stored in an independent storage tank, and the storage tank is independently controlled to supply the dichlorosilane to the deposition device according to the progress of chemical vapor deposition, so that impurities can be further prevented from being deposited on the silicon rod, and the production energy consumption is reduced.
In addition, the method for producing electronic grade polysilicon according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the invention, during the process of supplying dichlorosilane separated by the first tail gas separation device to the deposition device, the feeding amount of dichlorosilane is controlled to meet the following conditions: in the stage of the reaction time of 15-30 h, the molar ratio of dichlorosilane to trichlorosilane is (0.03-0.07): 1; in the stage of reaction time of 30-90 h, the molar ratio of dichlorosilane to trichlorosilane is (0.05-0.08): 1; in the reaction time of 90-150 h, the molar ratio of dichlorosilane to trichlorosilane is (0.03-0.05): 1.
In some embodiments of the present invention, the electronic grade polysilicon production method further comprises: and supplying the trichlorosilane separated by the first tail gas separation device to the rectification device for rectification treatment.
In some embodiments of the present invention, the electronic grade polysilicon production method further comprises: and supplying the tail gas after the first treatment to a thermal hydrogenation device for thermal hydrogenation treatment to obtain a second tail gas containing trichlorosilane, silicon tetrachloride and hydrogen.
In some embodiments of the present invention, the electronic grade polysilicon production method further comprises: and supplying the second tail gas into a second tail gas separation device for second separation treatment to respectively obtain trichlorosilane and second treated tail gas containing silicon tetrachloride and hydrogen, supplying the separated trichlorosilane into the rectification device for rectification treatment, and supplying the second treated tail gas obtained by separation into the thermal hydrogenation device for thermal hydrogenation treatment.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic block diagram of an electronic grade polysilicon production system according to one embodiment of the present invention;
fig. 2 is a schematic diagram of an electronic grade polysilicon production system according to yet another embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Abbreviations of names referred to in the present invention include: TCS: trichlorosilane, DCS: dichlorosilane, STC: silicon tetrachloride.
In one aspect of the invention, an electronic grade polysilicon production system is provided. Referring to fig. 1, the electronic grade polysilicon production system, according to an embodiment of the present invention, comprises: the device comprises a pretreatment device 100, a rectification device 200, a deposition device 300, a first tail gas separation device 400 and a dichlorosilane storage tank 500.
The electronic grade polysilicon production system according to the embodiment of the invention is further described in detail below.
According to an embodiment of the present invention, the pretreatment device 100 includes a plurality of adsorption columns (not shown in the drawings) connected in series, and the adsorption columns are provided with adsorption carriers and adsorption load components, and the adsorption load components include at least one of platinum tetrachloride and cuprous chloride; the pretreatment device is suitable for pretreating the trichlorosilane raw material to obtain pretreated trichlorosilane. In some embodiments, the adsorption column may include 3 to 4 columns. Therefore, the effect of removing impurities in the trichlorosilane raw material is better.
According to the embodiment of the invention, the adsorption columns comprise a first adsorption column, a second adsorption column and a third adsorption column, the pore diameter of an adsorption carrier in the first adsorption column is 12-9 nm, the pore diameter of an adsorption carrier in the second adsorption column is 7-5 nm, and the pore diameter of an adsorption carrier in the third adsorption column is 3-2 nm. Therefore, organic impurities (such as methyl chlorosilane, methyl chloride and the like) in the trichlorosilane raw material can be respectively and directionally adsorbed, the content of the organic impurities in the trichlorosilane raw material is further reduced, and the quality of electronic grade polycrystalline silicon products is improved.
According to an embodiment of the present invention, the adsorption carrier may be at least one selected from silica gel and ion exchange resin. Preferably, in the first to third adsorption columns, a combination of a silica gel carrier and platinum tetrachloride and a combination of a resin carrier and cuprous chloride are used for the packing of the two adsorption columns, respectively. Therefore, the effect of removing impurities in the trichlorosilane raw material is better.
According to the embodiment of the invention, the rectifying device 200 is connected with the pretreatment device 100 and is suitable for rectifying the pretreated trichlorosilane to obtain the rectified trichlorosilane. The specific type of the rectification device 200 is not particularly limited, and a rectification device commonly used in the art can be adopted, and a mature rectification process is adopted to carry out distillation treatment on the pretreated trichlorosilane.
According to the embodiment of the invention, the deposition device 300 is connected with the rectification device 200 and is suitable for performing chemical vapor deposition treatment by using hydrogen and rectified trichlorosilane to obtain electronic grade polycrystalline silicon, and discharging first tail gas containing trichlorosilane, dichlorosilane, silicon tetrachloride and hydrogen. The specific kind of the deposition apparatus 300 is not particularly limited, and a deposition apparatus commonly used in the art, such as a polysilicon reduction furnace, may be used.
According to the embodiment of the invention, the first tail gas separation device 400 is connected with the deposition device 300 and is suitable for performing a first separation treatment on the first tail gas to obtain trichlorosilane, dichlorosilane, hydrogen and a first treated tail gas containing silicon tetrachloride. Wherein the separated hydrogen can be returned to the deposition device for chemical vapor deposition treatment. The specific kind of the first off-gas separation device 400 is not particularly limited, and a separation device for off-gas in the production of polycrystalline silicon, which is commonly used in the art, may be employed.
Referring to fig. 2, according to the embodiment of the present invention, the first tail gas separation device 400 is further connected to the rectification device 200, and is adapted to supply the separated trichlorosilane to the rectification device for rectification treatment.
According to the embodiment of the invention, the dichlorosilane storage tank 500 is connected with the first tail gas separation device 400, and is suitable for storing dichlorosilane separated by the first tail gas separation device 400, and supplying dichlorosilane separated by the first tail gas separation device 400 to a deposition device for chemical vapor deposition treatment.
According to the embodiment of the invention, in the process of supplying dichlorosilane separated by the first tail gas separation device to the deposition device 200, the feeding amount of dichlorosilane is controlled to meet the following conditions: in the stage of the reaction time of 15-30 h, the molar ratio of dichlorosilane to trichlorosilane is (0.03-0.07): 1; in the stage of reaction time of 30-90 h, the molar ratio of dichlorosilane to trichlorosilane is (0.05-0.08): 1; in the reaction time of 90-150 h, the molar ratio of dichlorosilane to trichlorosilane is (0.03-0.05): 1. In the deposition apparatus 300, the time for starting the chemical vapor deposition was recorded as 0h, and the supply of dichlorosilane to the deposition apparatus 200 by the dichlorosilane storage tank 500 was individually controlled from 15h after the start of the chemical vapor deposition. By controlling the feeding amount of the dichlorosilane to meet the conditions, the deposition of impurities on the silicon rod can be further avoided, and the production energy consumption is reduced. In actual production, compared with the process without independently controlling the feeding of dichlorosilane, the boron impurity content of the product can be reduced by about 3ppta, the phosphorus impurity content can be reduced by about 9ppta, and the production energy consumption can be reduced by about 3 kW.h/kg of polycrystalline silicon.
In conclusion, the electronic grade polysilicon production system can obviously reduce the content of impurities such as boron, phosphorus, carbon and the like in the product and the production energy consumption by pretreating the trichlorosilane raw material and independently controlling the feeding of dichlorosilane. In actual production, the boron impurity content of the product can be reduced from about 20ppt to about 10ppt, the phosphorus impurity content can be reduced from about 60ppt to about 25ppt, the carbon impurity content can be reduced from about 10ppb to less than 5ppb, and the production energy consumption can be reduced by about 3 kW-h/kg of polycrystalline silicon.
Referring to fig. 2, the electronic grade polysilicon production system of the present invention further includes, according to an embodiment of the present invention: a thermal hydrogenation apparatus 600. The thermal hydrogenation device 600 is connected to the first tail gas separation device 400, and is adapted to perform thermal hydrogenation treatment on the first treated tail gas to obtain a second tail gas containing trichlorosilane, silicon tetrachloride and hydrogen. The specific type of the thermal hydrogenation apparatus 600 is not particularly limited, and thermal hydrogenation equipment commonly used in the art can be used, and the thermal hydrogenation treatment can be performed on the tail gas after the first treatment by using a mature thermal hydrogenation process.
Referring to fig. 2, the electronic grade polysilicon production system of the present invention further includes, according to an embodiment of the present invention: a second tail gas separation device 700. The second tail gas separation device 700 is connected to the thermal hydrogenation device 600, and is adapted to perform a second separation treatment on the second tail gas to obtain trichlorosilane and a second treated tail gas containing silicon tetrachloride and hydrogen, respectively, supply the separated trichlorosilane to the rectification device for rectification treatment, and supply the separated second treated tail gas to the thermal hydrogenation device for thermal hydrogenation treatment. The specific kind of the second off-gas separation device 700 is not particularly limited, and a separation device for off-gas in polysilicon production, which is commonly used in the art, may be employed.
In another aspect of the invention, the invention provides a method for producing electronic grade polycrystalline silicon. According to the embodiment of the invention, the electronic grade polycrystalline silicon production method comprises the following steps:
(1) and (3) supplying the trichlorosilane raw material to a pretreatment device for pretreatment to obtain pretreated trichlorosilane.
According to the embodiment of the invention, the pretreatment device comprises a plurality of adsorption columns which are connected in series, wherein adsorption carriers and adsorption load components are arranged in the adsorption columns, and the adsorption load components comprise at least one of platinum tetrachloride and cuprous chloride; the pretreatment device is suitable for pretreating the trichlorosilane raw material to obtain pretreated trichlorosilane. In some embodiments, the adsorption column may include 3 to 4 columns. Therefore, the effect of removing impurities in the trichlorosilane raw material is better.
According to the embodiment of the invention, the adsorption columns comprise a first adsorption column, a second adsorption column and a third adsorption column, the pore diameter of an adsorption carrier in the first adsorption column is 12-9 nm, the pore diameter of an adsorption carrier in the second adsorption column is 7-5 nm, and the pore diameter of an adsorption carrier in the third adsorption column is 3-2 nm. Therefore, organic impurities (such as methyl chlorosilane, methyl chloride and the like) in the trichlorosilane raw material can be respectively and directionally adsorbed, the content of the organic impurities in the trichlorosilane raw material is further reduced, and the quality of electronic grade polycrystalline silicon products is improved.
According to an embodiment of the present invention, the adsorption carrier may be at least one selected from silica gel and ion exchange resin. Preferably, in the first to third adsorption columns, a combination of a silica gel carrier and platinum tetrachloride and a combination of a resin carrier and cuprous chloride are used for the packing of the two adsorption columns, respectively. Therefore, the effect of removing impurities in the trichlorosilane raw material is better.
(2) And (4) supplying the pretreated trichlorosilane into a rectifying device for rectifying treatment to obtain the rectified trichlorosilane.
It should be noted that the specific type of the rectification device is not particularly limited, and a rectification device commonly used in the art may be adopted, and a mature rectification process is adopted to perform distillation treatment on the pretreated trichlorosilane.
(3) And supplying the hydrogen and the rectified trichlorosilane into a deposition device for chemical vapor deposition treatment to obtain electronic grade polycrystalline silicon and first tail gas containing the trichlorosilane, dichlorosilane, silicon tetrachloride and the hydrogen.
It should be noted that the specific type of the deposition apparatus is not particularly limited, and deposition apparatuses commonly used in the art, such as a polysilicon reduction furnace, may be used.
(4) And supplying the first tail gas to a first tail gas separation device for first separation treatment to respectively obtain trichlorosilane, dichlorosilane, hydrogen and first-treated tail gas containing silicon tetrachloride.
It should be noted that the specific type of the first off-gas separation device is not particularly limited, and a separation device for off-gas in polysilicon production, which is commonly used in the art, may be used.
According to an embodiment of the present invention, the method for producing electronic grade polysilicon further comprises: and supplying the trichlorosilane separated by the first tail gas separation device to a rectification device for rectification treatment.
(5) And supplying the dichlorosilane separated by the first tail gas separation device to a dichlorosilane storage tank for storage, and supplying the dichlorosilane separated by the first tail gas separation device to a deposition device for chemical vapor deposition treatment.
According to the embodiment of the invention, in the process of supplying dichlorosilane separated by the first tail gas separation device to the deposition device, the feeding amount of dichlorosilane is controlled to meet the following conditions: in the stage of the reaction time of 15-30 h, the molar ratio of dichlorosilane to trichlorosilane is (0.03-0.07): 1; in the stage of reaction time of 30-90 h, the molar ratio of dichlorosilane to trichlorosilane is (0.05-0.08): 1; in the reaction time of 90-150 h, the molar ratio of dichlorosilane to trichlorosilane is (0.03-0.05): 1. In the deposition apparatus 300, the time for starting the chemical vapor deposition was recorded as 0h, and the supply of dichlorosilane to the deposition apparatus 200 by the dichlorosilane storage tank 500 was individually controlled from 15h after the start of the chemical vapor deposition. By controlling the feeding amount of the dichlorosilane to meet the conditions, the deposition of impurities on the silicon rod can be further avoided, and the production energy consumption is reduced. In actual production, compared with the process without independently controlling the feeding of dichlorosilane, the boron impurity content of the product can be reduced by about 3ppta, the phosphorus impurity content can be reduced by about 9ppta, and the production energy consumption can be reduced by about 3 kW.h/kg of polycrystalline silicon.
In conclusion, the method for producing the electronic grade polysilicon can obviously reduce the content of impurities such as boron, phosphorus, carbon and the like in the product and the production energy consumption by pretreating the trichlorosilane raw material and independently controlling the feeding of dichlorosilane. In actual production, the boron impurity content of the product can be reduced from about 20ppt to about 10ppt, the phosphorus impurity content can be reduced from about 60ppt to about 25ppt, the carbon impurity content can be reduced from about 10ppb to less than 5ppb, and the production energy consumption can be reduced by about 3 kW-h/kg of polycrystalline silicon.
According to an embodiment of the present invention, the method for producing electronic grade polysilicon further comprises: and supplying the tail gas after the first treatment to a thermal hydrogenation device for thermal hydrogenation treatment to obtain a second tail gas containing trichlorosilane, silicon tetrachloride and hydrogen. It should be noted that the specific type of the thermal hydrogenation apparatus is not particularly limited, and thermal hydrogenation equipment commonly used in the art can be adopted, and the thermal hydrogenation treatment can be performed on the tail gas after the first treatment by using a mature thermal hydrogenation process.
According to an embodiment of the present invention, the method for producing electronic grade polysilicon further comprises: and supplying the second tail gas into a second tail gas separation device for second separation treatment to respectively obtain trichlorosilane and second treated tail gas containing silicon tetrachloride and hydrogen, supplying the separated trichlorosilane into a rectification device for rectification treatment, and supplying the second treated tail gas obtained by separation into a thermal hydrogenation device for thermal hydrogenation treatment. It should be noted that the specific type of the second off-gas separation device is not particularly limited, and a separation device for off-gas in polysilicon production, which is commonly used in the art, may be used.
In addition, it should be noted that all the features and advantages described above for the electronic grade polysilicon production system are also applicable to the electronic grade polysilicon production method, and are not described in detail herein.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. An electronic grade polysilicon production system, comprising:
the pretreatment device comprises a plurality of adsorption columns connected in series, wherein adsorption carriers and adsorption load components are arranged in the adsorption columns, and the adsorption load components comprise at least one of platinum tetrachloride and cuprous chloride; the pretreatment device is suitable for pretreating a trichlorosilane raw material to obtain pretreated trichlorosilane;
the rectifying device is connected with the pretreatment device and is suitable for rectifying the pretreated trichlorosilane to obtain rectified trichlorosilane;
the deposition device is connected with the rectification device and is suitable for performing chemical vapor deposition treatment by using hydrogen and the rectified trichlorosilane to obtain electronic grade polycrystalline silicon and discharging first tail gas containing trichlorosilane, dichlorosilane, silicon tetrachloride and hydrogen;
the first tail gas separation device is connected with the deposition device and is suitable for carrying out first separation treatment on the first tail gas to respectively obtain trichlorosilane, dichlorosilane, hydrogen and first treated tail gas containing silicon tetrachloride;
and the dichlorosilane storage tank is connected with the first tail gas separation device, is suitable for storing dichlorosilane separated by the first tail gas separation device, and supplies dichlorosilane separated by the first tail gas separation device to the deposition device for chemical vapor deposition treatment.
2. The electronic grade polysilicon production system according to claim 1, wherein the adsorption columns comprise a first adsorption column, a second adsorption column and a third adsorption column, the pore diameter of the adsorption carrier in the first adsorption column is 12-9 nm, the pore diameter of the adsorption carrier in the second adsorption column is 7-5 nm, and the pore diameter of the adsorption carrier in the third adsorption column is 3-2 nm;
optionally, the adsorption carrier is selected from at least one of silica gel and ion exchange resin.
3. The electronic grade polysilicon production system according to claim 1, wherein the first tail gas separation device is further connected with the rectification device and is adapted to supply the separated trichlorosilane to the rectification device for the rectification treatment.
4. The electronic grade polysilicon production system of claim 1, further comprising:
and the thermal hydrogenation device is connected with the first tail gas separation device and is suitable for carrying out thermal hydrogenation treatment on the first treated tail gas to obtain a second tail gas containing trichlorosilane, silicon tetrachloride and hydrogen.
5. The electronic grade polysilicon production system of claim 4, further comprising:
and the second tail gas separation device is connected with the thermal hydrogenation device and is suitable for carrying out second separation treatment on the second tail gas to respectively obtain trichlorosilane and second treated tail gas containing silicon tetrachloride and hydrogen, and the trichlorosilane obtained by separation is supplied to the rectification device for rectification treatment, and the second treated tail gas obtained by separation is supplied to the thermal hydrogenation device for thermal hydrogenation treatment.
6. An electronic grade polysilicon production method implemented by the electronic grade polysilicon production system according to any one of claims 1 to 5, comprising:
(1) feeding a trichlorosilane raw material into a pretreatment device for pretreatment to obtain pretreated trichlorosilane;
(2) feeding the pretreated trichlorosilane into a rectifying device for rectification to obtain rectified trichlorosilane;
(3) supplying hydrogen and the rectified trichlorosilane into a deposition device for chemical vapor deposition treatment to obtain electronic grade polycrystalline silicon and first tail gas containing trichlorosilane, dichlorosilane, silicon tetrachloride and hydrogen;
(4) supplying the first tail gas into a first tail gas separation device for first separation treatment to respectively obtain trichlorosilane, dichlorosilane, hydrogen and first-treated tail gas containing silicon tetrachloride;
(5) and supplying the dichlorosilane separated by the first tail gas separation device to a dichlorosilane storage tank for storage, and supplying the dichlorosilane separated by the first tail gas separation device to the deposition device for the chemical vapor deposition treatment.
7. The electronic grade polycrystalline silicon production method according to claim 6, wherein in the process of supplying dichlorosilane separated by the first tail gas separation device to the deposition device, the feeding amount of dichlorosilane is controlled to meet the following conditions:
in the stage of the reaction time of 15-30 h, the molar ratio of dichlorosilane to trichlorosilane is (0.03-0.07): 1;
in the stage of reaction time of 30-90 h, the molar ratio of dichlorosilane to trichlorosilane is (0.05-0.08): 1;
in the reaction time of 90-150 h, the molar ratio of dichlorosilane to trichlorosilane is (0.03-0.05): 1.
8. The electronic grade polysilicon production method according to claim 6, further comprising:
and supplying the trichlorosilane separated by the first tail gas separation device to the rectification device for rectification treatment.
9. The electronic grade polysilicon production method according to claim 6, further comprising:
and supplying the tail gas after the first treatment to a thermal hydrogenation device for thermal hydrogenation treatment to obtain a second tail gas containing trichlorosilane, silicon tetrachloride and hydrogen.
10. The electronic grade polysilicon production method of claim 9, further comprising:
and supplying the second tail gas into a second tail gas separation device for second separation treatment to respectively obtain trichlorosilane and second treated tail gas containing silicon tetrachloride and hydrogen, supplying the separated trichlorosilane into the rectification device for rectification treatment, and supplying the second treated tail gas obtained by separation into the thermal hydrogenation device for thermal hydrogenation treatment.
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Address after: 221004 No.66, Yangshan Road, Xuzhou Economic and Technological Development Zone, Jiangsu Province Patentee after: Jiangsu Xinhua Semiconductor Technology Co.,Ltd. Address before: 221004 No.66, Yangshan Road, Xuzhou Economic and Technological Development Zone, Jiangsu Province Patentee before: JIANGSU XINHUA SEMICONDUCTOR MATERIALS TECHNOLOGY CO.,LTD. |
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Application publication date: 20210223 Assignee: Yangzhou Xinhua Semiconductor Technology Co.,Ltd. Assignor: Jiangsu Xinhua Semiconductor Technology Co.,Ltd. Contract record no.: X2024980007191 Denomination of invention: Electronic grade polycrystalline silicon production system and method Granted publication date: 20210921 License type: Common License Record date: 20240614 |