CN110182813B - Method for maintaining electrode of reduction furnace - Google Patents
Method for maintaining electrode of reduction furnace Download PDFInfo
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- CN110182813B CN110182813B CN201910505175.0A CN201910505175A CN110182813B CN 110182813 B CN110182813 B CN 110182813B CN 201910505175 A CN201910505175 A CN 201910505175A CN 110182813 B CN110182813 B CN 110182813B
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- electrode
- reduction furnace
- insulating
- coating layer
- insulating fiber
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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
Abstract
The invention relates to the technical field of polycrystalline silicon production equipment, in particular to an improvement of a reduction furnace electrode. The invention discloses a method for maintaining electrodes of a reduction furnace, which comprises the following specific steps: and coating the part of the electrode of the reduction furnace, which needs to be insulated and isolated, in the bell jar of the reduction furnace, and arranging an insulating fiber coating layer, removing the silicon crystal insulating fiber coating layer deposited on the electrode of the reduction furnace after the electrode of the reduction furnace coated with the insulating fiber coating layer is installed in the reduction furnace for a period of time and deposits silicon crystals, and then coating the electrode of the reduction furnace again and arranging an insulating fiber coating layer. By adopting the technical scheme, the electrode maintenance period of the reduction furnace can be prolonged, and the maintenance cost can be reduced.
Description
Technical Field
The invention relates to the technical field of polycrystalline silicon production equipment, in particular to an improvement of a reduction furnace electrode.
Background
At present, an improved Siemens process is mainly adopted for polycrystalline silicon production, and the principle is that a silicon core is made into a conductor in a reduction furnace in a high-voltage breakdown mode, the temperature of the silicon core is rapidly increased by increasing current, high-purity trichlorosilane is reduced by high-purity hydrogen on a high-purity silicon core at about 1100 ℃, and polycrystalline silicon is generated and deposited on the silicon core to generate a polycrystalline silicon rod. The reduction furnace required by the method mainly comprises a reduction furnace bell jar and a reduction furnace chassis, wherein the reduction furnace chassis is provided with a reduction furnace electrode. The electrode of the reduction furnace is one of important components, can bear high-temperature and high-pressure conditions, cannot influence silicon crystals in the reduction furnace, and ensures the stable operation of the polycrystalline silicon reduction furnace.
In order to meet the above requirements, the electrode structure of the existing reduction furnace is often designed to be relatively complex, for example, CN208561705U proposes an electrode structure of a polycrystalline silicon reduction furnace, which has a structure as shown in fig. 1, and includes an electrode body 1, the electrode body 1 is installed in a reduction furnace chassis 2, an electrode insulating sleeve 3 is provided between the electrode body 1 and the reduction furnace chassis 2, the electrode insulating sleeve 3 is sleeved and tightly attached to the electrode body 1, an insulating ring 4 is further sleeved on the electrode body 1, the insulating ring 4 is tightly attached to the electrode body 1, the insulating ring 4 is located above the electrode insulating sleeve 3, the electrode body 1 is provided with an upper flange 5 and a lower flange, the insulating ring 4 is installed below the upper flange 5, an upper gasket 6 is provided between the upper end face of the upper flange 5 and the insulating ring 4, a lower gasket 7 is provided between the lower end face of the insulating ring 4 and the upper end face of the reduction furnace chassis 2, and an annular protrusion, the annular bulge 8 extends into the space between the electrode insulating sleeve 3 and the top of the reduction furnace chassis 2, the electrode insulating sleeve 3 is provided with a step corresponding to the lower flange, and an inner fluororubber gasket 9 and an outer fluororubber gasket 10 are respectively assembled inside and outside the step. For another example, CN207091011U also provides another polysilicon reduction furnace electrode, which includes a red copper ring 5, a ceramic ring 2 and an electrode insulating sleeve 8, where the red copper ring 5 is sleeved on the electrode 1 and is in interference fit with the electrode 1, so as to fix the red copper ring 5 on the electrode 1, the electrode insulating sleeve 8 is embedded in the reduction furnace chassis 9, and the ceramic ring 2 is inserted between the red copper ring 5 and the electrode insulating sleeve 8, so as to improve the insulating performance of the electrode 1 on the reduction furnace chassis 9, and reduce the enrichment of silicon powder particles, and the electrode 1 is installed on the reduction furnace chassis 9. The position that 2 tops of porcelain ring are close to electrode 1 is equipped with annular breach, is equipped with cyclic annular porcelain ring pressing member 3 in this breach, and the inboard of porcelain ring pressing member 3 is provided with the screw thread, and the outside of copper ring 5 is provided with the screw thread, carries out threaded connection with the external screw thread of copper ring 5 through the internal thread of porcelain ring pressing member 3 with compress tightly porcelain ring 2 downwards to realize the sealed between porcelain ring 2 and the copper ring 5. A first gasket 6 is arranged between the upper part of the ceramic ring and the ceramic ring pressing piece 3, and a second gasket 7 is arranged between the upper part of the ceramic ring and a reduction furnace chassis 9. The insulating member further comprises a shielding case 4 which is positioned on the reduction furnace chassis 9 and is sleeved outside the ceramic ring 2 (specifically, on the upper part of the ceramic ring) to prevent silicon powder from depositing on the ceramic ring 2.
The reduction furnace electrode structure in the prior art is relatively complex, and the applicant organizes that through diligent research, an inventor proposes an improved reduction furnace electrode and a patent application, and authorizes CN206955649U in 2018-02-02, and the structure of the polycrystalline silicon reduction furnace electrode breakthroughs adopts the steps of arranging a conductor layer, such as a sprayed silver coating, on the periphery of a cone head of the electrode and spraying an insulating layer made of pure ceramic powder on the periphery of a connecting section except the cone head, so that the improved reduction furnace electrode is formed. In view of the preparation method of the improved electrode for the reduction furnace, another person also proposed and issued patent CN108002390B in 2017-11-30.
However, both the reduction furnace electrode with a complex structure in the prior art and the reduction furnace electrode proposed by the applicant are consumable parts for polysilicon production, and after the reduction furnace electrode is used at intervals, the production needs to be stopped, and the reduction furnace electrode is dismounted from the reduction furnace for maintenance. As shown in fig. 3, after the electrode of the prior reduction furnace is used for a period of time, silicon is deposited on the whole electrode of the reduction furnace including the electrode rod and the insulating sleeve, and maintenance procedures such as disassembly, acid cleaning, re-spraying and the like are required. As shown in fig. 4, the reduction furnace electrode modified by the applicant also deposited silicon (black portion) after a period of use. As shown in fig. 5, a plurality of reducing furnace electrodes are installed on the reducing furnace chassis, wherein 2 reducing furnace electrodes are installed back after finishing maintenance (i.e. re-polishing and re-coating), and the other reducing furnace electrodes are waiting for disassembly and maintenance.
It is seen that how to increase the maintenance period of the electrode of the reduction furnace, especially for the improved electrode of the reduction furnace proposed by the applicant, and to reduce the maintenance cost is a technical problem that needs further research and improvement.
Disclosure of Invention
In order to solve the technical problems, the applicant organizes a great deal of research and provides a method capable of improving the electrode maintenance period of the reduction furnace and reducing the maintenance cost, and specifically adopts the following technical scheme:
the maintenance method of the electrode of the reduction furnace specifically comprises the following steps: and coating the part of the electrode of the reduction furnace, which needs to be insulated and isolated, in the bell jar of the reduction furnace, and arranging an insulating fiber coating layer, removing the silicon crystal insulating fiber coating layer deposited on the electrode of the reduction furnace after the electrode of the reduction furnace coated with the insulating fiber coating layer is installed in the reduction furnace for a period of time and deposits silicon crystals, and then coating the electrode of the reduction furnace again and arranging an insulating fiber coating layer.
By adopting the technical scheme, the electrode maintenance period of the reduction furnace can be prolonged, and the maintenance cost can be reduced.
Drawings
FIG. 1 is a schematic view showing the structure of an electrode for a reduction furnace according to a first prior art;
FIG. 2 is a schematic view showing the structure of an electrode for a reduction furnace of a second prior art;
FIG. 3 is a schematic illustration of a prior reduction furnace electrode after a period of use;
FIG. 4 is a schematic representation of the electrode of applicants' improved reduction furnace after a period of use;
FIG. 5 is a schematic view of a portion of a reduction furnace electrode on a reduction furnace chassis for maintenance;
FIG. 6 is a schematic structural view of an electrode of the improved polysilicon reduction furnace proposed in the prior patent CN 206955649U; FIG. 7a is a schematic view of an outer sheath of insulating fibers for sheathing;
FIG. 7b is a schematic representation of an insulating fiber layer for wrapping;
fig. 8 is a schematic structural view of a reduction furnace electrode according to an embodiment of the present invention.
Detailed Description
To further illustrate the various embodiments, the invention provides the accompanying drawings. The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the embodiments. Those skilled in the art will appreciate still other possible embodiments and advantages of the present invention with reference to these figures. Elements in the figures are not drawn to scale and like reference numerals are generally used to indicate like elements.
The invention will now be further described with reference to the accompanying drawings and detailed description.
Referring to fig. 6, in the structure of the improved electrode for a polysilicon reduction furnace proposed in the prior patent CN206955649U, the inventor only sets a conductive layer 4, such as a silver coating, on the periphery of the conical head 11 of the electrode 1, and sprays an insulating layer 5 made of pure ceramic powder on the periphery of the connection segment except the conical head 11, and specifically, the surface layer of the electrode 1 is roughened to form a roughened layer 2, and then the bonding layer 3 is sprayed, and then the conductive layer 4 and the insulating layer 5 are respectively sprayed to improve the firmness of the sprayed layer, thereby forming an improved electrode for a reduction furnace.
The inventor finds that, in the process of implementing the technical scheme of the patent later, although the polycrystalline silicon reduction furnace electrode tries to realize insulation isolation by arranging the conductor layer 4 at the periphery of the cone head 11 which is a necessary functional part of the electrode 1 and spraying ceramic powder as the insulation layer 5 at other parts, compared with the polycrystalline silicon reduction furnace electrode of the prior art, the defect of complicated structure caused by the fact that the inner layer and the outer layer of the electrode are sleeved with the silicon nitride insulation inner sleeve and the silicon dioxide insulation outer sleeve respectively can be overcome, and the structure is simpler. However, in the actual use process, since the insulating layer 5 is disposed in the region of the electrode 1 except the conical head 11 and a ceramic powder layer is bonded by spraying, considering the process difficulty and the stability and cost of the sprayed layer, the thickness of the ceramic powder layer as the insulating layer 5 may not be very thick, so as to ensure the voltage-withstanding reliability of the electrode, in the actual application, an insulating sleeve (as shown in fig. 4) is still sleeved on the rod portion (i.e., the connecting section portion) of the ceramic-sprayed insulating layer 5 of the electrode 1 to prevent creepage, thereby improving the voltage-withstanding reliability. Therefore, after the electrode of the polycrystalline silicon reduction furnace is used for a period of time, when the electrode deposited silicon of the polycrystalline silicon reduction furnace reaches a certain thickness, the electrode needs to be maintained, the insulating sleeve needs to be removed, the whole electrode is detached from the chassis of the reduction furnace, polishing and grinding are carried out again, and then the coating is sprayed again. Therefore, the improved polysilicon reduction furnace electrode still costs more manpower, material resources and time in maintenance and maintenance, and the production efficiency of polysilicon is also influenced.
Therefore, the inventors have made long-term experiments and studies to provide a method for maintaining an electrode of a reduction furnace, which can improve the maintenance period of the electrode of the reduction furnace and reduce the maintenance cost. As an embodiment, specifically:
and A, sleeving a circle of insulating fiber outer sleeve as shown in figure 7a at the part of the reduction furnace electrode needing insulation isolation in the reduction furnace bell jar, or wrapping one or more circles (according to actual needs) of insulating fiber layers as shown in figure 7b at the part needing insulation isolation.
This embodiment is described by taking the electrode of the polysilicon reduction furnace proposed in the prior patent CN206955649U as an example, and referring to fig. 8, the embodiment is to form an insulating fiber coating layer 6 by covering an insulating fiber sheath as shown in fig. 7a or wrapping an insulating fiber layer as shown in fig. 7b in the area between the lower part of the conical head 11 and the upper part of the boss of the ceramic sprayed insulating layer 5 of the rod body part (connecting section part) of the electrode 1, the area is just cylindrical in shape and easy to operate, and is just exposed out of the bottom plate of the reduction furnace and in the bell jar of the reduction furnace, and a region for accumulating silicon crystal is easy to generate.
The insulating fiber coating layer 6 in this embodiment is made of a fiber material having high temperature resistance and excellent insulating property, and preferably, a material having a certain flexibility. In this embodiment, a ceramic fiber material is preferably used. Specifically, for example, the product code provided by the jinan dragon thermal ceramic limited liability company is HLGX-236 standard ceramic fiber paper or HLGX-436 high-alumina ceramic fiber paper, or the product code provided by the shandongtirerre refractory fiber limited company is MYTX-BZ-06 standard ceramic fiber paper or MYTX-GL-06 high-alumina ceramic fiber paper, or the ceramic fiber sleeve type component customized by the applicant of the present application is adopted for sleeving.
And B, after the electrode of the reduction furnace coated with the insulating fiber coating layer 6 is installed in the reduction furnace for use for a period of time, when silicon crystals are deposited on the electrode until production is influenced, removing the silicon crystal insulating fiber coating layer 6, sleeving the insulating fiber sleeve shown in the figure 7a or wrapping the insulating fiber layer shown in the figure 7B on the area of the rod body part of the electrode 1 from the position below the conical head 11 to the position above the lug boss in the mode of the A, and forming a new insulating fiber coating layer 6 for reuse.
In the embodiment, the silicon crystal insulating fiber coating layer 6 is removed and then a new insulating fiber coating layer 6 is coated, so that the electrode of the reduction furnace can be quickly maintained. After tests, after the embodiment mode is adopted for quick maintenance for a plurality of times, conventional maintenance procedures such as disassembly, acid cleaning, re-spraying and the like need to be carried out according to the traditional mode, so that the aims of prolonging the period of conventional maintenance and reducing the maintenance cost are fulfilled.
Meanwhile, in the embodiment, the insulating fiber coating layer 6 is adopted to cover the ceramic spraying insulating layer 5 of the rod body part of the electrode, so that the quick maintenance is realized by dismantling and recoating, and the insulating reliability of the electrode is further improved due to the existence of the insulating fiber coating layer 6, so that in practical application, an insulating sleeve shown in figure 4 can be completely omitted, the electrode structure is simplified to a certain extent, the installation difficulty is reduced, the installation efficiency is improved, and the hardware cost is reduced.
According to the maintenance method of the electrode of the reduction furnace, the invention also provides the electrode of the reduction furnace, which has a simple structure and a function of quick maintenance.
Referring to fig. 8, in the reduction furnace electrode according to the embodiment of the present invention, a conductive layer 4 is disposed on the periphery of the conical head 11 of the electrode 1, such as a silver coating, and an insulating layer 5 made of pure ceramic powder is sprayed on the periphery of the connecting segment except the conical head 11. Wherein: the insulating layer 5 on the rod body of the electrode 1 is covered with an insulating fiber coating layer 6 at least at the exposed part (i.e. the region where insulation is needed and silicon crystals are easy to deposit) in the reduction furnace bell jar, and the insulating fiber coating layer 6 of the embodiment is formed by sleeving an insulating fiber sleeve as shown in fig. 7a or wrapping an insulating fiber layer as shown in fig. 7b on the electrode 1.
In this embodiment, the surface layer of the electrode 1 is roughened to form the roughened layer 2, and then the conductive layer 4 and the insulating layer 5 are respectively sprayed on the surface layer of the electrode on the basis of the bonding layer 3 to improve the firmness of the sprayed layer.
The invention discloses a reduction furnace electrode of other embodiments, which can adopt other reduction furnace electrode structures in the prior art, and is characterized in that an insulating fiber sleeve shown in fig. 7a is sleeved outside an insulating fiber sleeve or an insulating fiber layer shown in fig. 7b is wound on an electrode 1 to form an insulating fiber coating layer 6 at the exposed part of the electrode, which is positioned in a reduction furnace bell jar and needs to be insulated and isolated, so as to realize the function of quick maintenance.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. The maintenance method of the electrode of the reduction furnace is characterized in that: and coating the part of the electrode of the reduction furnace, which needs to be insulated and isolated, in the bell jar of the reduction furnace, and arranging an insulating fiber coating layer, removing the silicon crystal insulating fiber coating layer deposited on the electrode of the reduction furnace after the electrode of the reduction furnace coated with the insulating fiber coating layer is installed in the reduction furnace for a period of time and deposits silicon crystals, and then coating the electrode of the reduction furnace again and arranging an insulating fiber coating layer.
2. A method of maintaining an electrode for a reduction furnace according to claim 1, characterized in that: the coating setting mode of the insulating fiber coating layer is as follows: and sheathing by using an insulating fiber outer sleeve.
3. A method of maintaining an electrode for a reduction furnace according to claim 1, characterized in that: the coating setting mode of the insulating fiber coating layer is as follows: the wrapping is performed one or more times with a layer of insulating fibers.
4. A method of maintaining an electrode for a reduction furnace according to claim 1, characterized in that: the insulating fiber coating layer is made of ceramic fiber.
5. A method of maintaining an electrode for a reduction furnace according to claim 1, characterized in that: the coating part of the electrode of the reduction furnace is positioned in the region from the lower part of the conical head of the electrode to the upper part of the lug boss.
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| CN201910505175.0A CN110182813B (en) | 2019-06-12 | 2019-06-12 | Method for maintaining electrode of reduction furnace |
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| CN201910505175.0A CN110182813B (en) | 2019-06-12 | 2019-06-12 | Method for maintaining electrode of reduction furnace |
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| CN110182813B true CN110182813B (en) | 2021-01-12 |
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Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2108619B1 (en) * | 2008-03-21 | 2011-06-22 | Mitsubishi Materials Corporation | Polycrystalline silicon reactor |
| KR101620635B1 (en) * | 2008-06-24 | 2016-05-12 | 미쓰비시 마테리알 가부시키가이샤 | Apparatus for producing polycrystalline silicon |
| JP5792657B2 (en) * | 2012-02-23 | 2015-10-14 | 信越化学工業株式会社 | Method for producing polycrystalline silicon rod |
| CN203021302U (en) * | 2012-11-30 | 2013-06-26 | 四川永祥多晶硅有限公司 | Quartz insulating element of electrode for reduction furnace |
| CN106629737B (en) * | 2016-08-23 | 2019-07-30 | 内蒙古盾安光伏科技有限公司 | The electrode assembly of polycrystalline silicon reducing furnace |
| CN206955649U (en) * | 2017-03-10 | 2018-02-02 | 厦门佰事兴新材料科技有限公司 | Polycrystalline silicon reducing furnace electrode |
| CN206799174U (en) * | 2017-06-15 | 2017-12-26 | 新特能源股份有限公司 | A kind of polycrystalline silicon reducing furnace electrode insulation component |
| CN208948861U (en) * | 2018-09-30 | 2019-06-07 | 新特能源股份有限公司 | A kind of polycrystalline silicon reducing furnace electrode structure |
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Denomination of invention: Maintenance method of reduction furnace electrode Effective date of registration: 20211101 Granted publication date: 20210112 Pledgee: Bank of China Limited by Share Ltd. Xiamen branch Pledgor: XIAMEN BAISHIXING NEW MATERIAL TECHNOLOGY CO.,LTD. Registration number: Y2021980011685 |