CN111635702A - Graphite repairing agent and preparation method and application thereof - Google Patents
Graphite repairing agent and preparation method and application thereof Download PDFInfo
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- CN111635702A CN111635702A CN202010520644.9A CN202010520644A CN111635702A CN 111635702 A CN111635702 A CN 111635702A CN 202010520644 A CN202010520644 A CN 202010520644A CN 111635702 A CN111635702 A CN 111635702A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a graphite repairing agent and a preparation method and application thereof, and also discloses a method for recycling a graphite piece, wherein a ZS-1071 type high-temperature resistant inorganic adhesive and industrial alcohol are mixed and uniformly stirred, and a vessel is sealed and placed in an environment at 15-30 ℃ for 20-30min to be cured to obtain the graphite repairing agent; taking out the cracked or fractured graphite piece, polishing, transplanting the polished graphite piece into a special graphite piece repairing room, and completely wiping floating ash at the fracture part; coating the prepared graphite repairing agent, placing the repaired graphite piece at normal temperature after repairing, and then baking the repaired part at high temperature. According to the invention, the graphite crucible piece fracture part is directly bonded by adopting graphite glue, so that the service life of each graphite piece can be prolonged by 10-20 furnaces. The method of the invention has simple operation, convenient implementation and low cost; the method is not limited by the structure of the graphite piece, and is suitable for the graphite pieces with any various structures; the graphite piece is not limited by the size of the thermal field and is suitable for the thermal field graphite piece with any size.
Description
Technical Field
The invention belongs to the technical field of graphite piece recovery, and particularly relates to a graphite repairing agent and a preparation method and application thereof.
Background
The growth method of single crystal silicon is mainly represented by a Czochralski method (Czochralski method). The main components of the thermal field of the Czochralski method single crystal furnace comprise a graphite crucible spliced by single-petal blocks, a heat insulator, a heater, a heat shield, a heat preservation cylinder, a crucible support, a heat preservation cover and the like.
The graphite piece in the following text refers to a graphite crucible, a heat insulator, a heater, a heat shield and a crucible support.
In the Czochralski process, the temperature in the single crystal furnace is higher than 1400 ℃, the quartz crucible is softened at a high temperature, and reacts with the polycrystalline silicon raw material to thereby generate SiO gas. The SiO gas continues to react with the graphite piece to generate carbon monoxide, silicon carbide and the like, so that the graphite piece is corroded, and the reaction equation is as follows:
SiO2+Si＝2SiO，SiO+2C＝SiC+CO，SiO2+C＝SiO+CO。
the mixture of high temperature, low pressure and silicon vapor during the crystal pulling process results in a reaction between the silicon and the graphite part to form silicon carbide, with the longer the reaction time, the deeper the silicon carbide penetrates the graphite part.
The silicon carbide and the graphite have different thermal expansion coefficients, and when the silicon carbide reaches a certain depth, the graphite piece can be broken, so that the service life of the graphite piece is reduced; the silicon carbide is also easy to react with the quartz crucible, so that the quartz crucible becomes thin, the silicon leakage of the quartz crucible is easy to cause, and the production cost is increased. In order to prevent the risk of silicon leakage, the thinned or broken graphite piece needs to be replaced and directly scrapped or repaired.
At present, related technical reports about solving the problems of graphite piece breakage and corrosion are provided. Patent No. 201020653402.9 discloses a method of covering graphite paper over the seams of graphite crucible blocks to extend the life of the graphite crucible. Patent No. 201110148718.1 discloses a graphite coating formed by mixing graphite powder and ethanol, which is uniformly coated on the R part at the block interface of a graphite crucible, so as to reduce the corrosion of the R part and prolong the service life of the graphite crucible. Patent No. 201010583556.X discloses a mode of opening an exhaust hole at a joint of a graphite crucible, which is used for removing generated gases such as silicon monoxide, carbon dioxide and silicon carbide from an air hole, reducing corrosion to an R part and prolonging the service life of the graphite crucible. The method reduces the corrosion of the graphite crucible in a manner of preventing in advance and prolongs the service life of the crucible. There are also currently used methods of repairing existing graphite pieces with graphite pieces to extend the useful life of all graphite pieces.
The graphite piece belongs to consumables in the Czochralski silicon process, occupies a certain proportion in the production cost, realizes the recycling of the graphite piece, is an important means for prolonging the service life of the graphite piece, and has very important significance for reducing the production cost.
However, the existing method for repairing the graphite piece is complex to operate, and the graphite piece to be repaired is easily damaged in the repairing process, so that the graphite piece cannot be used;
2. the existing repair is carried out by patching on the surface of an original graphite piece, the existing thermal field is compact for good heat insulation performance, and the repaired graphite piece is easy to contact other thermal field components to cause abnormity such as ignition, so that the whole furnace is scrapped, accidents are caused, and the loss is large.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing a graphite healant.
The invention also aims to solve the technical problem of providing a preparation method and application of the graphite healant.
The invention finally solves the technical problem of providing a method for recycling the graphite piece.
The regenerated graphite piece has an antioxidation effect at the repaired position, prevents the graphite piece from being oxidized and prolongs the service life.
The technical scheme is as follows: in order to solve the technical problems, the invention provides a graphite healant which comprises a ZS-1071 type high-temperature resistant inorganic adhesive and industrial alcohol.
The ZS-1071 type high-temperature-resistant inorganic adhesive comprises 5-20% by mass of graphite adhesive A and 10-25% by mass of graphite adhesive B in the graphite healant, and the balance of industrial alcohol.
Preferably, the ZS-1071 type high-temperature resistant inorganic adhesive comprises 8-15% by mass of graphite adhesive a and 16-25% by mass of graphite adhesive B in the graphite healant, and the balance is industrial alcohol.
Preferably, the ZS-1071 type high-temperature resistant inorganic adhesive comprises 8-10% by mass of graphite adhesive a and 16-20% by mass of graphite adhesive B in the graphite healant, and the balance is industrial alcohol.
The invention also discloses a preparation method of the graphite healant, which comprises the following steps: mixing the ZS-1071 type high-temperature resistant inorganic adhesive and industrial alcohol, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod, and then sealing the vessel and curing the vessel at the temperature of 15-30 ℃ for 20-30min to obtain the graphite healant.
The invention also discloses the application of the graphite repairing agent in repairing graphite parts.
The invention also discloses a recycling method of the graphite piece, which comprises the following steps:
1) preparing a graphite repairing agent: mixing the ZS-1071 type high-temperature resistant inorganic adhesive and industrial alcohol, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod, and sealing the vessel and curing the vessel at the temperature of 15-30 ℃ for 20-30min to obtain a graphite healant;
2) taking out the cracked or fractured graphite piece, polishing the periphery of the graphite piece by using scouring pad to ensure that the roughness of the surface reaches 25-40 mu m, moving the polished graphite piece to a special graphite piece repairing room, and wiping all floating ash at the fracture part by using dust-free paper dipped with alcohol;
3) and (3) smearing the prepared graphite repairing agent on the fracture part of the graphite piece, wherein the smearing of the graphite repairing agent is not more than 0.1mm each time in the smearing process, and the smearing is performed for 3-4 times, after the repairing is completed, the repaired graphite piece is placed at normal temperature for 1-2 hours, and then the repaired part is baked at the high temperature of 900 ℃ for 10-20 min.
The ZS-1071 type high-temperature-resistant inorganic adhesive in the step 1) comprises 8-10% by mass of graphite adhesive A and 16-20% by mass of graphite adhesive B in the graphite healant, and the balance is industrial alcohol.
Wherein, the graphite adhesive A is slowly poured into the mixture of the graphite adhesive B and the industrial alcohol in the step 1), and the mixture is fully mixed and stirred uniformly, the stirring speed is 100-.
Wherein, the volume concentration of the industrial alcohol in the step 1) is 99.9%.
Wherein, the graphite piece is one of a graphite crucible piece, a heater, a graphite middle shaft, a graphite heat preservation cylinder or a graphite inner guide.
Has the advantages that: compared with the prior art, the invention has the advantages that: according to the invention, the graphite piece fracture part is directly bonded by the graphite repairing agent, the original thickness can be kept, the service life of each graphite piece can be prolonged, and the service life of the graphite piece can be prolonged by 10-20 furnaces. The method of the invention has simple operation, convenient implementation and low cost; the method is not limited by the structure of the graphite piece, and is suitable for the graphite pieces with any various structures; and is not limited by the size of the thermal field, and is suitable for the thermal field graphite piece with any size.
Drawings
FIG. 1 is a schematic diagram of the repair of a circular arc of a heater, which cannot be repaired normally by a normal repair method, and can be completely repaired by the repair agent and the repair method of example 1;
fig. 2 is a schematic diagram of repairing a crack of a heat-insulating cylinder, which cannot be repaired normally by a normal repairing method, and can be completely repaired by the repairing method of embodiment 2.
Detailed Description
The present invention is further illustrated by the following specific examples, it should be noted that, for those skilled in the art, variations and modifications can be made without departing from the principle of the present invention, and these should also be construed as falling within the scope of the present invention.
The ZS-1071 type high-temperature resistant inorganic adhesive is purchased from Beijing Zhi Shengwei Huake technology development Limited company, and comprises two components of graphite adhesive A and graphite adhesive B.
Example 1 preparation of graphite healing agent
Mixing 10% by mass of graphite adhesive A, 16% by mass of graphite adhesive B and 74% by mass of industrial alcohol in the ZS-1071 type high-temperature-resistant inorganic adhesive, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at a stirring speed of 120 revolutions per minute for 8 minutes, sealing the vessel, and curing the vessel at 15 ℃ for 30 minutes to obtain the graphite healant.
Example 2 preparation of graphite healing agent
Mixing 8% by mass of graphite adhesive A, 20% by mass of graphite adhesive B and 72% by mass of industrial alcohol in the ZS-1071 type high-temperature-resistant inorganic adhesive, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at a stirring speed of 100 revolutions per minute for 10 minutes, sealing the vessel, and curing the vessel at the temperature of 30 ℃ for 20 minutes to obtain the graphite healant.
Example 3 preparation of graphite healing agent
Mixing 9 mass percent of graphite adhesive A, 18 mass percent of graphite adhesive B and 73 mass percent of industrial alcohol in the ZS-1071 type high-temperature resistant inorganic adhesive, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at a stirring rotating speed of 120 revolutions per minute for 8 minutes, sealing the vessel, and curing the vessel at 25 ℃ for 25 minutes to obtain the graphite healant.
Example 4 preparation of graphite healing agent
Mixing 10% by mass of graphite adhesive A, 25% by mass of graphite adhesive B and 65% by mass of industrial alcohol in the ZS-1071 type high-temperature-resistant inorganic adhesive, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at a stirring speed of 110 revolutions per minute for 9 minutes, sealing the vessel, and curing the vessel at 25 ℃ for 25 minutes to obtain the graphite healant.
Example 5 preparation of graphite healing agent
Mixing 5 mass percent of graphite adhesive A, 25 mass percent of graphite adhesive B and 70 mass percent of industrial alcohol in the ZS-1071 type high-temperature resistant inorganic adhesive, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at the stirring speed of 100 revolutions per minute for 10 minutes, sealing the vessel, and curing the vessel at the temperature of 25 ℃ for 25 minutes to obtain the graphite healant.
Example 6 preparation of graphite healing agent
Mixing 20 mass percent of graphite adhesive A, 25 mass percent of graphite adhesive B and 55 mass percent of industrial alcohol in the ZS-1071 type high-temperature resistant inorganic adhesive, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at a stirring rotating speed of 120 revolutions per minute for 8 minutes, sealing the vessel, and curing the vessel at the temperature of 25 ℃ for 25 minutes to obtain the graphite healant.
Example 7 preparation of graphite healing agent
Mixing 12% of graphite adhesive A, 17% of graphite adhesive B and 71% of industrial alcohol in the ZS-1071 type high-temperature-resistant inorganic adhesive by mass percent, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at a stirring rotating speed of 110 revolutions per minute for 9 minutes, sealing the vessel, and curing the vessel at the temperature of 25 ℃ for 25 minutes to obtain the graphite healant.
Example 8 preparation of graphite healing agent
Mixing 13% of graphite adhesive A, 24% of graphite adhesive B and 63% of industrial alcohol in the ZS-1071 type high-temperature-resistant inorganic adhesive by mass percent, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at the stirring speed of 100 revolutions per minute for 10 minutes, sealing the vessel, and curing the vessel at the temperature of 25 ℃ for 25 minutes to obtain the graphite repairing agent.
Comparative example 1
Mixing 25 mass percent of graphite adhesive A, 26 mass percent of graphite adhesive B and 49 mass percent of industrial alcohol in the ZS-1071 type high-temperature-resistant inorganic adhesive, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at the stirring speed of 100 revolutions per minute for 10 minutes, sealing the vessel, and curing the vessel at the temperature of 25 ℃ for 25 minutes to obtain the comparative graphite healant 1.
Comparative example 2
Mixing 4% by mass of graphite adhesive A, 8% by mass of graphite adhesive B and 88% by mass of industrial alcohol in the ZS-1071 type high-temperature-resistant inorganic adhesive, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod at a stirring speed of 120 revolutions per minute for 8 minutes, sealing the vessel, and curing the vessel at 25 ℃ for 25 minutes to obtain the comparative graphite healant 1.
Experimental example 1
Examples 1-8 and comparative examples 1-2 were tested for quick drying times as given in Table 1 below:
TABLE 1
Experimental example 2
The graphite pieces were repaired in examples 1 to 8 and comparative examples 1 to 2. The specific method comprises the following steps:
taking out a cracked or fractured graphite piece (the graphite piece in the experimental example is a heater and a heat-insulating cylinder), polishing the periphery by using scouring pad to ensure that the roughness of the surface reaches 25-40 mu m, moving the polished graphite piece to a special graphite piece repairing room, and wiping all floating ash at the fracture part by using dust-free paper dipped with alcohol;
coating the prepared graphite repairing agent on the graphite piece with cracks or fractures, wherein the graphite repairing agent is coated for 3-4 times without exceeding 0.1mm each time in the coating process, and after the repairing is finished, the repaired graphite piece is placed at normal temperature for 1-2 hours and then the repaired part is baked at the high temperature of 800 ℃ for 10-20 min. The heat-resistant temperatures of the graphite repair agents of examples 1 to 8 were 2600 ℃, and the heat-resistant temperatures of comparative examples 1 to 2 were 2600 ℃.
The graphite piece repaired by the method has an antioxidation effect at the repaired position, prevents the graphite piece from being oxidized and prolongs the service life.
The graphite piece repaired by the method can be continuously used, the service life is calculated according to the number of the used furnaces, and the specific experimental results are shown in the following tables 2 and 3:
table 2: comparison of service life before and after repairing heater with graphite repairing agent
Table 3: comparison of service life of graphite repairing agent before and after repairing heat-insulating cylinder
Claims (9)
1. The graphite repairing agent is characterized by comprising a ZS-1071 type high-temperature-resistant inorganic adhesive and industrial alcohol.
2. The graphite healant as claimed in claim 1, wherein the ZS-1071 type refractory inorganic binder comprises 5-20% by mass of graphite adhesive a and 10-25% by mass of graphite adhesive B, with the balance being industrial alcohol.
3. The method for preparing the graphite healing agent according to claim 1 or 2, comprising the steps of: mixing the ZS-1071 type high-temperature resistant inorganic adhesive and industrial alcohol, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod, and then sealing the vessel and curing the vessel at the temperature of 15-30 ℃ for 20-30min to obtain the graphite healant.
4. Use of the graphite healing agent according to claim 1 or 2 for repairing graphite parts.
5. A method for recycling a graphite piece is characterized by comprising the following steps:
1) preparing a graphite repairing agent: mixing the ZS-1071 type high-temperature resistant inorganic adhesive and industrial alcohol, pouring the mixture into a vessel, uniformly stirring the mixture along a uniform clockwise direction by using a glass rod, and sealing the vessel and curing the vessel at the temperature of 15-30 ℃ for 20-30min to obtain a graphite healant;
2) taking out the cracked or fractured graphite piece, polishing the periphery of the graphite piece by using scouring pad to ensure that the roughness of the surface reaches 25-40 mu m, moving the polished graphite piece to a special graphite piece repairing room, and wiping all floating ash at the fracture part by using dust-free paper dipped with alcohol;
3) and (3) smearing the prepared graphite repairing agent on the fracture part of the graphite piece, wherein the smearing of the graphite repairing agent is not more than 0.1mm each time in the smearing process, and the smearing is performed for 3-4 times, after the repairing is completed, the repaired graphite piece is placed at normal temperature for 1-2 hours, and then the repaired part is baked at the high temperature of 900 ℃ for 10-20 min.
6. The method for recycling the graphite piece according to claim 5, wherein the step 1) ZS-1071 type high-temperature resistant inorganic adhesive comprises 8-10% by mass of graphite adhesive A and 16-20% by mass of graphite adhesive B in the graphite healant, and the balance is industrial alcohol.
7. The method for recycling the graphite piece as claimed in claim 5, wherein the step 1) is to slowly pour the graphite adhesive A into the mixture of the graphite adhesive B and the industrial alcohol, and fully mix and stir the mixture uniformly, wherein the stirring speed is 100 revolutions per minute, and the stirring time is 8-10 minutes.
8. The method for recycling the graphite piece according to claim 5, wherein the industrial alcohol concentration in step 1) is 99.9% by volume.
9. The method of claim 5, wherein the graphite member is one of a graphite crucible member, a heater, a graphite central shaft, a graphite heat-insulating cylinder, or a graphite inner guide.
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| CN202010520644.9A CN111635702A (en) | 2020-06-09 | 2020-06-09 | Graphite repairing agent and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112143384A (en) * | 2020-10-20 | 2020-12-29 | 内蒙古斯诺新材料科技有限公司 | Graphite crucible repairing paste and graphite crucible repairing method |
| CN115028475A (en) * | 2022-06-23 | 2022-09-09 | 湖南世鑫新材料有限公司 | Method for repairing carbon-carbon thermal field product |
| CN115534435A (en) * | 2022-11-02 | 2022-12-30 | 双良硅材料(包头)有限公司 | Method for recycling cured felt |
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| CN115028475A (en) * | 2022-06-23 | 2022-09-09 | 湖南世鑫新材料有限公司 | Method for repairing carbon-carbon thermal field product |
| CN115534435A (en) * | 2022-11-02 | 2022-12-30 | 双良硅材料(包头)有限公司 | Method for recycling cured felt |
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Application publication date: 20200908 |