CN111058087A - Carbon/silicon carbide composite material feeding cylinder for repeatedly feeding single crystal silicon furnace - Google Patents
Carbon/silicon carbide composite material feeding cylinder for repeatedly feeding single crystal silicon furnace Download PDFInfo
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- CN111058087A CN111058087A CN202010029055.0A CN202010029055A CN111058087A CN 111058087 A CN111058087 A CN 111058087A CN 202010029055 A CN202010029055 A CN 202010029055A CN 111058087 A CN111058087 A CN 111058087A
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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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
- C23C10/08—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases only one element being diffused
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a carbon/silicon carbide composite material feeding cylinder for repeatedly feeding a single crystal silicon furnace, which comprises the following steps: step one, alternately laminating and needling T700 carbon fiber cloth and carbon fiber net tire into a cylindrical preform, wherein the density of the preform is 0.4-0.5 g/cm3(ii) a Step two, putting the cylindrical prefabricated body into a chemical vapor deposition furnace to densify to 1.2-1.3 g/cm3(ii) a Step three, putting the blank into a high-temperature graphitization furnace for graphitization treatment; machining the blank into a specification of a feeding cylinder; step five, the machined blank bodyAnd putting the blank into a vertical high-temperature ceramic furnace, and preparing silicon carbide inside and on the surface of the blank. The technical scheme has the advantages that the carbon/silicon carbide composite material has high hardness and wear resistance, and does not cause secondary pollution to the silicon material; the mechanical property is excellent, the reliability of the feeding cylinder is greatly improved, and the accident risk is reduced; the silicon single crystal silicon rod pulling device has good thermal shock resistance, can bear rapid cooling and rapid heating, greatly shortens the time for transferring the feeding barrel from the pulling barrel, and effectively improves the production efficiency of the silicon single crystal rod.
Description
Technical Field
The invention relates to the field of production of single crystal silicon rods, in particular to a carbon/silicon carbide composite material feeding cylinder for repeated feeding of a single crystal silicon furnace.
Background
With the continuous maturity of monocrystalline silicon production technology, it is common in the field of monocrystalline silicon production to use a repeated feeder for continuous feeding. Patent CN 107653488A proposes "a quartz charging barrel for repeated charging of a single crystal furnace", which has been successfully applied in a single crystal silicon growth furnace. The quartz material is used as the feeding cylinder to prevent the polycrystalline silicon raw material from being secondarily polluted in the feeding process to a certain extent. However, quartz is easy to crack and is not collision-resistant, a charging barrel needs to avoid collision in the charging and charging processes, and particularly collision and fragmentation in the charging process can cause stewing accidents. In order to prevent the quartz feeding pipe from being collided, the quartz pipe is used as the inner cylinder combination by taking heat-resistant stainless steel as a protective cylinder. However, the difference between the thermal expansion coefficients of quartz and heat-resistant steel is large, and the quartz and the heat-resistant steel are mutually extruded and easily broken in use. Patent CN 207210578U proposes that a teflon sheath is added between the quartz inner cylinder and the stainless steel outer protective cylinder to solve the problem of large difference between the thermal expansion coefficients of the two materials. But the polytetrafluoroethylene has low temperature resistance and is easy to damage in use. In addition, the quartz material has poor thermal shock resistance and is not resistant to rapid cooling and rapid heating, and the feeding barrel can be transferred out only after being cooled in the pulling barrel after feeding is finished, so that hidden cracks of the quartz feeding barrel caused by high-temperature and low-temperature alternation are prevented, and accidents are prevented when the quartz feeding barrel is used again.
Therefore, a new concept, a new process and a new material need to be developed to prepare the carbon/silicon carbide composite material charging barrel with high temperature resistance, good thermal shock resistance and no silicon material pollution.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a carbon/silicon carbide composite material feeding cylinder for repeatedly feeding a single crystal furnace on the basis of the patent CN 107653488A. The structure of the charging barrel is the same as that provided in CN 107653488A, except that the charging barrel is prepared by using carbon/silicon carbide composite material instead of quartz. The preparation method of the feeding cylinder comprises the steps of adopting a needle-punched prefabricated body as a blank body, firstly preparing a low-density carbon/carbon composite material blank body through chemical vapor deposition, then machining the blank body into the required specification of the feeding cylinder, and then carrying out ceramic treatment through a vapor phase siliconizing technology to obtain the feeding cylinder of the carbon/silicon carbide composite material.
The technical purpose of the invention is realized by the following technical scheme:
a carbon/silicon carbide composite material feeding cylinder for repeatedly feeding a single crystal silicon furnace comprises the following steps:
the method comprises the following steps:
step one, alternately laminating and needling T700 carbon fiber cloth and carbon fiber net tire into a cylindrical preform, wherein the density of the preform is 0.4-0.5 g/cm3;
Step two, putting the cylindrical prefabricated body into a chemical vapor deposition furnace for densification;
step three, putting the blank into high-temperature graphitization for graphitization treatment;
machining the blank into a specification of a feeding cylinder;
and step five, putting the machined blank into a vertical high-temperature ceramic furnace, and preparing silicon carbide on the blank.
Further, in the second step, the parameter temperature in the deposition furnace is 950-1000 ℃, the furnace pressure is 1000-2500 Pa, the heat preservation deposition is carried out for 200-300 h, and the density is 1.2-1.3 g/cm3The carbon/carbon composite material charging barrel blank.
Further, propylene and nitrogen are introduced into the deposition furnace, the propylene is a carbon source gas, the nitrogen is a carrier gas and a diluent gas, the propylene flow rate is 1m for thin film plantation/h, and the nitrogen flow rate is 1m for thin film plantation/h.
Further, in the third step, the graphitization treatment temperature is 2000-2300 ℃, and the heat preservation time is 2-4 h.
Further, in the fifth step, a charging tray is placed at the bottom of the charging barrel, a silicon material block is placed in the charging tray, the temperature is 1500-1800 ℃, the furnace pressure is 100-1000 Pa, the temperature is kept for 2-4 h, silicon vapor is utilized to react with carbon in the inner part and on the surface of the low-density carbon/carbon blank body to generate silicon carbide, and the carbon/silicon carbide composite material charging barrel is obtained, wherein the density is 2.2-2.5 g/cm3。
Furthermore, in the fifth step, the amount of the silicon material block is calculated by the weight of the low-density carbon/carbon blank, and is placed according to 0.9-1.1 times of the weight of the silicon material block.
In conclusion, the invention has the following beneficial effects:
1. the carbon/silicon carbide composite material has high hardness and wear resistance, and does not cause secondary pollution to the silicon material.
2. The carbon/silicon carbide composite material has excellent mechanical property, the reliability of the charging barrel is greatly improved, and the accident risk is reduced.
3. The carbon/silicon carbide composite material has good thermal shock resistance, can bear rapid cooling and rapid heating, greatly shortens the time for transferring the charging barrel from the pulling barrel, and effectively improves the production efficiency of the single crystal silicon rod.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example one
The carbon/silicon carbide composite material feeding cylinder for repeatedly feeding the single crystal silicon furnace in the preferred embodiment of the invention comprises the following steps:
step one, alternately laminating and needling T700 carbon fiber cloth and carbon fiber net tire into a cylindrical preform, wherein the density of the preform is 0.45g/cm3;
Step two, placing the cylindrical preform into a chemical vapor deposition furnace, wherein the temperature is 950 ℃, propylene is a carbon source gas, nitrogen is a carrier gas and a diluent gas, the propylene flow is 1m for each hour, the nitrogen flow is 1m for each hour, the furnace pressure is 2000Pa, and the heat preservation deposition is carried out for 300 hours to obtain the powder with the density of 1.25g/cm3The carbon/carbon composite material charging cylinder blank;
step three, putting the blank into high-temperature graphitization for graphitization treatment, wherein the temperature is 2300 ℃, and keeping the temperature for 4 hours;
machining the blank into a specification of a feeding cylinder;
step five, putting the machined green body into a vertical high-temperature ceramic furnace, placing a material tray at the bottom of a feeding cylinder, placing a silicon material block in the material tray, and heatingThe temperature is 1600 ℃, the furnace pressure is 500Pa, the temperature is kept for 4h, and the carbon/silicon carbide composite material charging barrel with the density of 2.4g/cm is obtained3。
In conclusion, the carbon/silicon carbide composite material has high hardness and wear resistance, and does not cause secondary pollution to the silicon material; the carbon/silicon carbide composite material has excellent mechanical property, the reliability of the charging barrel is greatly improved, and the accident risk is reduced; the carbon/silicon carbide composite material has good thermal shock resistance, can bear rapid cooling and rapid heating, greatly shortens the time for transferring the charging barrel from the pulling barrel, and effectively improves the production efficiency of the single crystal silicon rod.
Example two
The carbon/silicon carbide composite material feeding cylinder for repeatedly feeding the single crystal silicon furnace in the preferred embodiment of the invention comprises the following steps:
step one, alternately laminating and needling T700 carbon fiber cloth and carbon fiber net tire into a cylindrical preform, wherein the density of the preform is 0.5g/cm3;
Step two, placing the cylindrical preform into a chemical vapor deposition furnace, wherein the temperature is 920 ℃, propylene is a carbon source gas, nitrogen is a carrier gas and a diluent gas, the propylene flow is 1m for each hour, the nitrogen flow is 1m for each hour, the furnace pressure is 1500Pa, and heat preservation deposition is carried out for 400 hours to obtain the powder with the density of 1.3g/cm3The carbon/carbon composite material charging cylinder blank;
step three, putting the blank into high-temperature graphitization for graphitization treatment, wherein the temperature is 2200 ℃, and preserving heat for 3 hours;
machining the blank into a specification of a feeding cylinder;
putting the machined blank into a vertical high-temperature ceramic furnace, placing a material tray at the bottom of a feeding cylinder, placing a silicon material block in the material tray, keeping the temperature at 1650 ℃ and the furnace pressure at 600Pa, and preserving the heat for 4 hours to obtain a carbon/silicon carbide composite material feeding cylinder with the density of 2.35g/cm3。
In conclusion, the carbon/silicon carbide composite material has high hardness and wear resistance, and does not cause secondary pollution to the silicon material; the carbon/silicon carbide composite material has excellent mechanical property, the reliability of the charging barrel is greatly improved, and the accident risk is reduced; the carbon/silicon carbide composite material has good thermal shock resistance, can bear rapid cooling and rapid heating, greatly shortens the time for transferring the charging barrel from the pulling barrel, and effectively improves the production efficiency of the single crystal silicon rod.
EXAMPLE III
The carbon/silicon carbide composite material feeding cylinder for repeatedly feeding the single crystal silicon furnace in the preferred embodiment of the invention comprises the following steps:
step one, alternately laminating and needling T700 carbon fiber cloth and carbon fiber net tire into a cylindrical preform, wherein the density of the preform is 0.4g/cm3;
Step two, placing the cylindrical preform into a chemical vapor deposition furnace, wherein the temperature is 960 ℃, propylene is a carbon source gas, nitrogen is a carrier gas and a diluent gas, the propylene flow is 1m for each hour, the nitrogen flow is 1m for each hour, the furnace pressure is 2500Pa, and the heat preservation deposition is carried out for 300 hours to obtain the powder with the density of 1.3g/cm3The carbon/carbon composite material charging cylinder blank;
step three, putting the blank into high-temperature graphitization for graphitization treatment at 2250 ℃, and preserving heat for 3 h;
machining the blank into a specification of a feeding cylinder;
putting the machined blank into a vertical high-temperature ceramic furnace, placing a material tray at the bottom of a feeding cylinder, placing a silicon material block in the material tray, keeping the temperature at 1630 ℃, keeping the furnace pressure at 1000Pa, and keeping the temperature for 4 hours to obtain a carbon/silicon carbide composite material feeding cylinder with the density of 2.45g/cm3。
In conclusion, the carbon/silicon carbide composite material has high hardness and wear resistance, and does not cause secondary pollution to the silicon material; the carbon/silicon carbide composite material has excellent mechanical property, the reliability of the charging barrel is greatly improved, and the accident risk is reduced; the carbon/silicon carbide composite material has good thermal shock resistance, can bear rapid cooling and rapid heating, greatly shortens the time for transferring the charging barrel from the pulling barrel, and effectively improves the production efficiency of the single crystal silicon rod.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The utility model provides a carbon/carborundum combined material charging barrel for single crystal silicon stove is reinforced repeatedly which characterized in that: the method comprises the following steps:
step one, alternately laminating and needling T700 carbon fiber cloth and carbon fiber net tire into a cylindrical preform, wherein the density of the preform is 0.4-0.5 g/cm3;
Step two, putting the cylindrical prefabricated body into a chemical vapor deposition furnace for densification;
step three, putting the blank into high-temperature graphitization for graphitization treatment;
machining the blank into a specification of a feeding cylinder;
and step five, putting the machined blank into a vertical high-temperature ceramic furnace, and preparing silicon carbide on the blank.
2. The carbon/silicon carbide composite material feeding cylinder for the repeated feeding of the single crystal silicon furnace as claimed in claim 1, wherein: in the second step, the parameter temperature in the deposition furnace is 950-1000 ℃, the furnace pressure is 1000-2500 Pa, the heat preservation deposition is carried out for 200-300 h, and the density is 1.2-1.3 g/cm3The carbon/carbon composite material charging barrel blank.
3. The carbon/silicon carbide composite material feeding cylinder for the repeated feeding of the single crystal silicon furnace as claimed in claim 2, wherein: and introducing propylene and nitrogen into the deposition furnace, wherein the propylene is a carbon source gas, the nitrogen is a carrier gas and a diluent gas, the propylene flow is 1m for cultivation/h, and the nitrogen flow is 1m for cultivation/h.
4. The carbon/silicon carbide composite material feeding cylinder for the repeated feeding of the single crystal silicon furnace as claimed in claim 1, wherein: in the third step, the graphitization treatment temperature is 2000-2300 ℃, and the heat preservation time is 2-4 h.
5. The carbon/silicon carbide composite material feeding cylinder for the repeated feeding of the single crystal silicon furnace as claimed in claim 1, wherein: placing a material tray at the bottom of the feeding cylinder, placing a silicon material block in the material tray, keeping the temperature at 1500-1800 ℃, the furnace pressure at 100-1000 Pa, preserving the heat for 2-4 h, and generating silicon carbide by utilizing the carbon reaction of silicon steam in the inner part and the surface of the low-density carbon/carbon blank body to obtain the carbon/silicon carbide composite material feeding cylinder with the density of 2.2-2.5 g/cm3。
6. The carbon/silicon carbide composite material feeding cylinder for the repeated feeding of the single crystal silicon furnace as claimed in claim 2, wherein: in the fifth step, the silicon material block is placed according to the weight of 0.9-1.1 times of the weight of the low-density carbon/carbon blank by using the amount of the silicon material block calculated by the weight of the low-density carbon/carbon blank.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN117623795A (en) * | 2024-01-26 | 2024-03-01 | 浙江星辉新材料科技有限公司 | Carbon-carbon plate and preparation method thereof |
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CN103193497A (en) * | 2013-04-07 | 2013-07-10 | 山东国晶新材料有限公司 | Sticky product with silicon erosion resistance of carbon/carbon composite material and preparation method thereof |
CN106946582A (en) * | 2017-03-31 | 2017-07-14 | 中南大学 | A kind of Large Size Special Shaped C-base composte material component and preparation method thereof |
CN107653488A (en) * | 2017-08-22 | 2018-02-02 | 东海县奥博石英制品有限公司 | A kind of quartzy casing drum that charging is repeated for single crystal growing furnace |
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2020
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US20020109250A1 (en) * | 2001-02-12 | 2002-08-15 | Agency For Defense Development | Method for manufacturing carbon/silicon-carbide composite |
CN101260005A (en) * | 2008-01-09 | 2008-09-10 | 西安航天复合材料研究所 | Method for preparing carbon/carbon/silicon carbide composite material |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN117623795A (en) * | 2024-01-26 | 2024-03-01 | 浙江星辉新材料科技有限公司 | Carbon-carbon plate and preparation method thereof |
CN117623795B (en) * | 2024-01-26 | 2024-04-12 | 浙江星辉新材料科技有限公司 | Carbon-carbon plate and preparation method thereof |
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