CN113955758A - Control method for preventing silicon core from peeling in polycrystalline silicon production - Google Patents
Control method for preventing silicon core from peeling in polycrystalline silicon production Download PDFInfo
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- CN113955758A CN113955758A CN202111410846.9A CN202111410846A CN113955758A CN 113955758 A CN113955758 A CN 113955758A CN 202111410846 A CN202111410846 A CN 202111410846A CN 113955758 A CN113955758 A CN 113955758A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229920005591 polysilicon Polymers 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 4
- 230000008901 benefit Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 3
- 239000005052 trichlorosilane Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 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 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a control method for preventing silicon core from peeling in polycrystalline silicon production. A control method for preventing silicon core from peeling in polysilicon production comprises the following steps: the silicon core was immersed in flowing hydrogen. The control method for preventing the silicon core from being stripped in the production of the polycrystalline silicon can effectively remove the stripping phenomenon on the surface of the silicon core, improve the product quality, reduce the production cost and improve the economic benefit.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon production, and particularly relates to a control method for preventing silicon cores from being stripped in the polycrystalline silicon production.
Background
Polycrystalline silicon is a main raw material of photovoltaic industry, at present, the main process technology for producing polycrystalline silicon at home and abroad is an 'improved Siemens method', hydrogen, silicon tetrachloride and silicon powder are used for synthesizing trichlorosilane at a certain temperature, then the trichlorosilane is separated, rectified and purified, the purified high-purity trichlorosilane and the hydrogen are mixed in proportion and then are introduced into a polycrystalline silicon reduction furnace, deposition reaction is carried out on an electrified high-temperature silicon core at a certain temperature and under a certain pressure to generate polycrystalline silicon, the reaction temperature is controlled to be about 1080 ℃, and finally a rod-shaped polycrystalline silicon product is generated.
The problem of silicon core stripping in the production process of polycrystalline silicon is always a difficult problem and research content in the polycrystalline silicon industry, and the problem directly influences the quality of products, so that the development and survival of enterprises are directly influenced. It is well known that silicon core peeling occurs for many reasons, for example: the silicon core is not cleaned, trace dust in the charging process is removed, chlorosilane in hydrogen is recovered, and nitrogen, oxygen and the like in the replacement process are removed; various impurities form a layer of nitride, oxide film or amorphous silicon on the surface of the silicon core, so that the silicon core and deposited silicon cannot be well combined in the growth process of multiple silicon products, the silicon core stripping phenomenon occurs, and the product quality is influenced.
At present, after silicon cores of polysilicon manufacturers are drawn, the silicon cores are directly stored through acid washing and slight drying, but the silicon core stripping phenomenon of different degrees still occurs in actually produced products, and only the processing quality control of the silicon cores is enhanced. And the phenomenon of stripping oxygen, nitrogen oxide or chlorosilane formed on the surface of the silicon core is caused by incomplete cleaning work in the charging process, and the phenomenon of stripping the silicon core cannot be completely avoided only by strengthening management and control.
In view of this, the invention provides a control method for preventing silicon core from peeling off in polysilicon production, which can effectively avoid the phenomenon of silicon core surface peeling off, thereby improving the product quality.
Disclosure of Invention
The invention aims to provide a control method for preventing silicon core stripping in polycrystalline silicon production, which can effectively remove the silicon core surface stripping phenomenon, improve the product quality, reduce the production cost and improve the economic benefit.
In order to realize the purpose, the adopted technical scheme is as follows:
a control method for preventing silicon core from peeling in polysilicon production comprises the following steps: the silicon core was immersed in flowing hydrogen.
Further, the flow rate of the hydrogen is 200-500m3/h。
Further, the soaking time is 0.5-1 h.
Further, the control method further comprises: and burning the surface of the silicon core.
Further, the burning temperature is 1100-1200 ℃.
Furthermore, the burning is to improve the current of the silicon core according to the current which can be carried by the diameter and the shape of the silicon core.
Still further, the calculation equation of the current boost is as follows: Δ I ═ Φ η;
in the formula, delta I is lifting current; diameter of silicon core; eta is coefficient, and the value of the coefficient is 0.5-1.
Still further, the coefficient is 0.5 when the silicon core is a round silicon core, and the coefficient is 1 when the silicon core is a square silicon core.
Still further, the burning is performed under hydrogen conditions.
Compared with the prior art, the invention has the beneficial effects that:
1. the control method for preventing the silicon core from being stripped in the production of the polycrystalline silicon can avoid the stripping of the primary silicon core and the generated silicon and improve the product quality.
2. The control method for preventing the silicon core from being stripped in the production of the polycrystalline silicon can reduce the crushing difficulty of the silicon material and reduce the manual workload: after the silicon core is stripped, the silicon core can not be mechanically crushed and can only be manually treated.
Detailed Description
In order to further illustrate the control method for preventing silicon core from peeling off in polysilicon production according to the present invention, and achieve the intended purpose of the invention, the following detailed description is provided with reference to the preferred embodiments, and the detailed description is provided for the specific implementation, structure, features and effects thereof in polysilicon production according to the present invention. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The following will describe in further detail a control method for preventing silicon core peeling in polysilicon production according to the present invention with reference to specific embodiments:
the technical scheme of the invention is as follows:
a control method for preventing silicon core from peeling in polysilicon production comprises the following steps: the silicon core was immersed in flowing hydrogen.
Preferably, the flow rate of the hydrogen is 200-500m3/h。
Preferably, the soaking time is 0.5-1 h.
Preferably, the control method further comprises: and burning the surface of the silicon core.
Further preferably, the burning temperature is 1100-1200 ℃.
Further preferably, the burning is to increase the current of the silicon core according to the current which can be carried by the diameter and the shape of the silicon core.
Further preferably, the calculation equation of the current boost is: Δ I ═ Φ η;
in the formula, delta I is lifting current; diameter of silicon core; eta is coefficient, and the value of the coefficient is 0.5-1.
More preferably, the coefficient of the round silicon core is 0.5, and the coefficient of the square silicon core is 1.
Further preferably, the burning is performed under hydrogen gas.
Through analysis and multiple tests, the control technology can effectively remove the silicon core surface stripping phenomenon and improve the product quality. The control method has low cost, convenient use and no pollution to environment protection, and can be adjusted according to the diameter and the length of the silicon core.
Example 1.
In the prior art, the blow-in of a reduction furnace is carried out according to certain steps, and part of the blow-in steps are shown in the following table:
the present embodiment adds the following controls to the furnace 504:
(1) the temperature of the silicon core is raised by increasing the current of the silicon core, and the surface of the silicon core is burnt, so that an impurity layer on the surface of the silicon core is damaged. Certain current delta I is increased according to the current which can be carried by the diameter and the shape of the silicon core, so that the surface energy of the silicon core reaches 1100-1200 ℃.
The calculation method is as follows: Δ I ═ Φ η;
in the formula, the diameter of a silicon core is phi (millimeters);
eta is a coefficient (millimeter/ampere), the value of the coefficient is 0.5-1, and reference factors are the diameter and the shape of the silicon core; the round silicon core is generally 0.5, the square silicon core is generally 1, and the value can be adjusted according to the requirement.
(2) Hydrogen with a certain flow is introduced to soak the silicon core for a certain time, so that impurities on the surface of the silicon core are separated out and taken away by the hydrogen.
The flow rate of the introduced hydrogen is 200-500m according to the size of the furnace type3Soaking for 0.5-1h, wherein the soaking time is determined according to the diameter and the shape of the silicon core.
Through the two steps, the purity of the silicon core can be improved, and the silicon core is prevented from being stripped.
The polysilicon production device of the company adopts the control process to achieve the purpose of preventing silicon core from peeling. Before the method is adopted, more than 100 batches of silicon cores are stripped by one device per month, the silicon cores account for one fifth of the total production batch, the product quality is seriously influenced, the crushing workload is multiplied, the silicon core stripping is obviously reduced after the method is adopted, the silicon core stripping is less than 5 batches per month, and the best silicon core stripping can be 0 batch.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (9)
1. A control method for preventing silicon core from peeling in polysilicon production is characterized in that the control method comprises the following steps: the silicon core was immersed in flowing hydrogen.
2. The control method according to claim 1,
the flow rate of the hydrogen is 200-500m3/h。
3. The control method according to claim 1,
the soaking time is 0.5-1 h.
4. The control method according to claim 1,
the control method further comprises the following steps: and burning the surface of the silicon core.
5. The control method according to claim 4,
the ignition temperature is 1100-1200 ℃.
6. The control method according to claim 4,
the burning is to improve the current of the silicon core according to the current which can be carried by the diameter and the shape of the silicon core.
7. The control method according to claim 6,
the calculation equation of the current boost is as follows: Δ I ═ Φ η;
in the formula, delta I is lifting current; diameter of silicon core; eta is coefficient, and the value of the coefficient is 0.5-1.
8. The control method according to claim 7,
the coefficient is 0.5 when the silicon core is a round silicon core, and the coefficient is 1 when the silicon core is a square silicon core.
9. The control method according to claim 4,
the burning is carried out under hydrogen condition.
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| CN202111410846.9A CN113955758A (en) | 2021-11-25 | 2021-11-25 | Control method for preventing silicon core from peeling in polycrystalline silicon production |
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| CN202111410846.9A CN113955758A (en) | 2021-11-25 | 2021-11-25 | Control method for preventing silicon core from peeling in polycrystalline silicon production |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030021894A1 (en) * | 2001-07-30 | 2003-01-30 | Komatsu Ltd. | Method of producing high-purity polycrystallin silicon |
| CN101092752A (en) * | 2007-05-31 | 2007-12-26 | 无锡中彩科技有限公司 | Technique for cleaning silicon chip |
| CN101759185A (en) * | 2009-12-31 | 2010-06-30 | 江苏中能硅业科技发展有限公司 | Method for manufacturing polysilicon silicon rod |
| CN102515166A (en) * | 2011-12-20 | 2012-06-27 | 国电宁夏太阳能有限公司 | Preparation method of polysilicon rod |
| CN109292777A (en) * | 2017-07-24 | 2019-02-01 | 新特能源股份有限公司 | Polycrystalline silicon reducing furnace opens the silicon core breakdown method of furnace, opens the method and device of furnace method, production polysilicon |
| CN112110449A (en) * | 2019-06-21 | 2020-12-22 | 新特能源股份有限公司 | Polycrystalline silicon production method and system |
| CN113387360A (en) * | 2021-05-25 | 2021-09-14 | 河南硅烷科技发展股份有限公司 | Interface wettability regulation and control method for inhibiting silicon dendritic crystal growth in zone melting level polycrystalline silicon CVD process |
-
2021
- 2021-11-25 CN CN202111410846.9A patent/CN113955758A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030021894A1 (en) * | 2001-07-30 | 2003-01-30 | Komatsu Ltd. | Method of producing high-purity polycrystallin silicon |
| CN101092752A (en) * | 2007-05-31 | 2007-12-26 | 无锡中彩科技有限公司 | Technique for cleaning silicon chip |
| CN101759185A (en) * | 2009-12-31 | 2010-06-30 | 江苏中能硅业科技发展有限公司 | Method for manufacturing polysilicon silicon rod |
| CN102515166A (en) * | 2011-12-20 | 2012-06-27 | 国电宁夏太阳能有限公司 | Preparation method of polysilicon rod |
| CN109292777A (en) * | 2017-07-24 | 2019-02-01 | 新特能源股份有限公司 | Polycrystalline silicon reducing furnace opens the silicon core breakdown method of furnace, opens the method and device of furnace method, production polysilicon |
| CN112110449A (en) * | 2019-06-21 | 2020-12-22 | 新特能源股份有限公司 | Polycrystalline silicon production method and system |
| CN113387360A (en) * | 2021-05-25 | 2021-09-14 | 河南硅烷科技发展股份有限公司 | Interface wettability regulation and control method for inhibiting silicon dendritic crystal growth in zone melting level polycrystalline silicon CVD process |
Non-Patent Citations (1)
| Title |
|---|
| 柯曾鹏;杨志国;刘欣;宗文婷;: "多晶硅还原炉倒棒原因探讨", 半导体技术, vol. 35, no. 10, pages 994 - 998 * |
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