CN114368976B - Quartz fiber reinforced carbon-silicon dioxide composite material crucible and preparation method thereof - Google Patents

Quartz fiber reinforced carbon-silicon dioxide composite material crucible and preparation method thereof Download PDF

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CN114368976B
CN114368976B CN202210118066.5A CN202210118066A CN114368976B CN 114368976 B CN114368976 B CN 114368976B CN 202210118066 A CN202210118066 A CN 202210118066A CN 114368976 B CN114368976 B CN 114368976B
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CN114368976A (en
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陈腾飞
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Central South University
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    • 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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    • 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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Abstract

The invention relates to a quartz fiber reinforced carbon-silicon dioxide composite material crucible and a preparation method thereof, belonging to the technical field of preparation of quartz fibers and carbon-based composite materials. The surface density is 180-600 g/m 2 The quartz fiber laid fabric or plain fabric has a density of 30-150 g/m 2 The short quartz fiber net blank is overlapped and needled to obtain the product with the density of 0.35-0.8 g/cm 3 The quartz fiber prefabricated member is solidified and shaped, densified by chemical vapor deposition or resin or asphalt impregnation-carbonization to be densified to 1.2 to 1.6g/cm 3 Then, performing high-temperature treatment for the first time, and mechanically adding the materials to the size; pressure dipping silica sol, drying, curing, sintering, secondary high-temperature treatment and surface polishing to obtain the product with the density of 1.5-1.8 g/cm 3 The product of (1). The crucible body and the surface of the crucible body basically do not react with the silicon vapor, and the service life of the crucible is prolonged.

Description

Quartz fiber reinforced carbon-silicon dioxide composite material crucible and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of quartz fibers and carbon-based composite materials, in particular to a quartz fiber reinforced carbon-silicon dioxide composite material crucible and a preparation method thereof.
Background
The carbon/carbon composite material is a carbon fiber reinforced carbon matrix composite material, has excellent performances of low density, high specific strength, high temperature resistance, small thermal expansion coefficient, good dimensional stability, strong structure designability, corrosion resistance and the like, is widely applied to the military industry and civil fields, particularly has the advantages of manufacturing large-size products and strong structure designability along with the technical progress and the reduction of manufacturing cost, and the like, and is widely applied to thermal field components of large-scale monocrystalline silicon furnaces in recent years, wherein a carbon/carbon composite material crucible is one of key components of a thermal field system of the monocrystalline furnace.
When the monocrystalline silicon is drawn, the thermal field component is in the mixed atmosphere of silicon vapor and inert gas, the silicon vapor can deposit on the surface of the thermal field component and partially react with the surface of the carbon/carbon composite material or graphite material to generate silicon carbide or permeate into pores with a certain depth on the surface to react with carbon to generate silicon carbide, and the silicon carbide is easy to fall off and pulverize due to the mismatch of thermal expansion coefficients of the silicon carbide and the carbon/carbon or graphite, so that the further use of the thermal field component is influenced, and the service life of the thermal field component is further influenced. And when the single crystal is pulled, the silicon material is placed in the quartz crucible, and the outside of the quartz crucible is sleeved with the carbon/carbon composite material or the graphite crucible, because the quartz crucible is better combined with the bottom profile of the carbon/carbon or the graphite crucible, partial reaction or adhesion is easy to occur at high temperature, the quartz crucible is difficult to clean, and sometimes the area at the bottom of the crucible needs to be knocked to clean, which seriously influences the service life of the crucible. Patent CN113149686A discloses a carbon/carbon composite crucible with a composite ceramic coating and a preparation method thereof, the crucible is composed of a carbon/carbon composite crucible base body and the composite ceramic coating attached to the inner surface of the crucible, and the components (by mass ratio) are as follows: 50-70% of silicon carbide, 10-40% of boron nitride and 10-20% of silicon, wherein the thickness is 1-5 mm, the method comprises the steps of firstly mixing resin, boron nitride and silicon powder, then carrying out hot press molding on the mixture to obtain a composite ceramic layer green body, carrying out carbonization treatment to obtain a composite ceramic layer green body, then adhering the composite ceramic coating green body into a carbon/carbon composite material crucible matrix by using a mixed binder of resin and silicon nitride, carrying out curing, carbonization and siliconizing treatment, and carrying out machining to obtain the carbon/carbon composite material crucible with the composite ceramic coating, wherein the method has the defects that the preparation and processing difficulty of the ceramic green body is large (the thickness of the coating is 1-5 mm), and after the ceramic green body is adhered and combined with the carbon/carbon crucible matrix, the coating is easy to be layered and locally cracked when a single crystal is pulled, and the mass production and the use are not facilitated; CN11848201A proposes to form a silicon carbide/silicon coating on the surface of a carbon/carbon crucible by using a plasma spraying process, so as to improve the anti-silicification corrosion capability of the carbon/carbon crucible, thereby prolonging the service life of the crucible, but the appearance characteristics of the crucible, the difficulty of achieving uniform coating on the inner and outer surfaces of the crucible by using the plasma spraying process is large, and the obtained coating is thin and has mismatched thermal expansion coefficients, which is very limited for the capability of inhibiting silicon vapor erosion.
Disclosure of Invention
Aiming at the defect that the carbon/carbon composite material or the graphite crucible for the existing single crystal furnace is easily affected by siliconization of silicon vapor, the invention provides a quartz fiber reinforced carbon-silicon dioxide composite material crucible and a preparation method thereof, wherein a crucible prefabricated part is prepared by quartz fiber, and is subjected to curing and sizing, chemical vapor deposition densification or resin or asphalt impregnation-carbonization densification, and then is subjected to first high-temperature treatment, and is mechanically added to the designed size; pressurizing and dipping the silica sol, drying, curing, sintering, repeating the process if necessary, performing high-temperature treatment for the second time, and polishing the surface to obtain the silica sol. So that the crucible body and the surface are basically not reacted with the silicon vapor, the carbon content on the surface is reduced, and the service life of the crucible is obviously prolonged.
The present invention providesA quartz fiber crucible prefabricated member comprises a surface density of 180-600 g/m 2 The quartz fiber laid fabric or plain fabric has a density of 30-150 g/m 2 Short quartz fiber net is formed by alternate lamination and needling, the weight ratio of cloth to net is 5: 5-9: 1, and the density is 0.35-0.8 g/cm 3 。
The invention also provides a quartz fiber reinforced carbon-silicon dioxide composite material crucible which is formed by curing and shaping, chemical vapor deposition densification or resin or asphalt impregnation-carbonization densification to 1.2-1.6 g/cm 3 Then, carrying out first high-temperature treatment, and machining to the designed size; pressure dipping silica sol, drying, curing and sintering, the density is 1.5-1.8 g/cm 3 And carrying out high-temperature treatment for the second time, and polishing the surface to obtain the product.
Preferably, the temperature for curing and setting is 150-300 ℃.
Preferably, the temperature of the first high-temperature treatment is 1300-1900 ℃, and the holding time is 2-20 h.
Preferably, the mass fraction of the silica sol is 10 to 45%.
Preferably, the temperature of the second high-temperature treatment is 1300-1900 ℃, and the holding time is 2-10 h.
Further, the invention also provides a preparation method of the quartz fiber reinforced carbon-silica composite crucible, which comprises the following steps:
s1, with the areal density of 180-600 g/m 2 The quartz fiber laid fabric or plain fabric has a density of 30-150 g/m 2 Short quartz fiber net is formed by alternate lamination needling, the weight ratio of cloth to net is 5: 5-9: 1, and the obtained density is 0.35-0.8 g/cm 3 The silica fiber crucible preform of (1);
s2, sleeving the prepared quartz fiber crucible prefabricated part on a proper steel die or a graphite die to enable the inner surface of the crucible prefabricated part to be well attached to the outer surface of the die, then spraying or impregnating resin or organic binder, standing for 1-10 hours, sleeving an outer steel die on the outer surface of the crucible, enabling the inner profile surface of the outer steel die to be closely attached to the outer profile surface of the crucible prefabricated part, and enabling the outer diameter of the prefabricated part to be closely attached to the outer diameter of the crucibleThe outer diameter of the product is 1-2 mm larger, and then an outer die is fixed; then the sleeved prefabricated member (with a mold) is sent into an oven to be solidified and shaped, the temperature is controlled to be 150-300 ℃, when the oven does not smoke outwards, the temperature is kept for 1-10 hours, and the prefabricated member is cooled and demoulded to obtain a shaped quartz fiber prefabricated member; then adopting chemical vapor deposition densification process or resin or asphalt impregnation-carbonization densification process to densify the prefabricated member to 1.2-1.6 g/cm 3 Then, carrying out first high-temperature treatment at 1300-1900 ℃, preserving the heat for 2-20 hours, partially or completely converting the quartz fiber and the carbon interface of the matrix into silicon carbide, and mechanically adding the silicon carbide to the size of the product to obtain a quartz fiber reinforced carbon-based composite material crucible blank;
s3, impregnating the silica sol into the silica sol of the quartz fiber reinforced carbon-based composite material crucible blank by adopting a pressurized impregnation process, then drying, curing and sintering, and repeating the procedure if necessary to ensure that the density reaches 1.5-1.8 g/cm 3 And then carrying out secondary high-temperature treatment at 1300-1900 ℃, keeping the temperature for 2-10 hours, and carrying out polishing-polishing treatment on the surface of the crucible to obtain the quartz fiber reinforced carbon-silicon dioxide composite material crucible.
Preferably, in step S2, the resin is a phenolic resin, a furan resin or other resin with a high carbon residue rate.
Preferably, in step S2, the outer steel mold is divided into 3 to 6 petals.
The technical scheme of the invention has the following advantages:
the invention provides a quartz fiber reinforced carbon-silicon dioxide composite material crucible, wherein a prefabricated part is formed by alternately laminating and needling quartz fiber laid cloth or plain cloth and short quartz fiber net tire; the prefabricated member obtained by alternately laminating and needling the quartz fiber cloth and the short quartz fiber net blank has more pores, and the pore size can be controlled by controlling the surface density, the cloth net weight ratio and the final density of the quartz fiber cloth and the short quartz fiber net blank, so that the density of the quartz fiber reinforced carbon-based composite material crucible blank and the final product can be controlled during chemical deposition densification. The prefabricated member is solidified and shaped by a cover die, then is densified by chemical vapor deposition or liquid phase dipping-carbonization to the required density, and is processed at high temperature, and the interface layer between the quartz fiber and the matrix carbon is partially or completely converted into silicon carbide. Then machining, pressurizing, dipping, drying, curing and sintering the silica sol, and finally carrying out high-temperature treatment to partially or completely convert the interface between the carbon matrix and the silicon dioxide into silicon carbide and improve the bonding strength of the interface; and because the inner and outer molds are adopted for solidification and shaping, the processing amount of the inner and outer surface of the crucible is reduced, the fiber volume content of the crucible is increased, and the obtained quartz fiber reinforced carbon-silicon dioxide composite material crucible has high strength and low porosity, and the service life is prolonged by more than 50 percent compared with the service life of a common carbon/carbon composite material crucible; the quartz fiber reinforced carbon-silicon dioxide composite material crucible prepared by the process mainly comprises quartz fibers, silicon dioxide, silicon carbide and matrix carbon, the content of the matrix carbon is obviously reduced, and the quartz or the silicon dioxide is arranged around the crucible, so that the carbon content of a crystal pulling atmosphere can be obviously reduced, and the crucible is suitable for preparing a thermal field part of a high-efficiency single crystal furnace.
Detailed Description
Supporting each of the solutions defined in the claims.
Example 1
A quartz fiber crucible prefabricated member is composed of a prefabricated member with an area density of 180-600 g/m 2 The quartz fiber laid fabric or plain fabric has a density of 30-150 g/m 2 Short quartz fiber net blank is formed by alternate lamination and needling, the weight ratio of cloth to net is 5: 5, and the density is 0.35g/cm 3 。
Example 2
A quartz fiber crucible prefabricated member comprises a surface density of 180-600 g/m 2 The quartz fiber laid fabric or plain fabric has a density of 30-150 g/m 2 Short quartz fiber net is formed by alternate lamination and needling, the weight ratio of cloth to net is 9: 1, and the density is 0.8g/cm 3 。
Example 3
A preparation method of a quartz fiber reinforced carbon-silicon dioxide composite material crucible comprises the following steps:
s1, sleeving the quartz fiber crucible preform prepared in the embodiment 1 on a proper steel mould or graphite mould to enable the crucible to be in a shape of a cylinderThe inner surface of the crucible prefabricated member is well attached to the outer surface of the mold, then resin or organic binder is sprayed or impregnated, the crucible is placed for 1 to 10 hours, an outer steel mold is sleeved on the outer surface of the crucible, the inner profile of the outer steel mold is closely attached to the outer surface of the crucible prefabricated member, the outer diameter of the prefabricated member is 1 to 2mm larger than the outer diameter of a crucible product, and then an outer mold is fixed; then the sleeved prefabricated member (with a mold) is sent into an oven to be solidified and shaped, the temperature is controlled to be 150-300 ℃, when the oven does not smoke outwards, the temperature is kept for 1-10 hours, and the prefabricated member is cooled and demoulded to obtain a shaped quartz fiber prefabricated member; then, the prefabricated part is densified to 1.2g/cm by adopting a chemical vapor deposition densification process or a resin or asphalt impregnation-carbonization densification process 3 Then, carrying out first high-temperature treatment at 1300-1900 ℃, preserving the heat for 2-20 hours, partially or completely converting the quartz fiber and the carbon interface of the matrix into silicon carbide, and mechanically adding the silicon carbide to the size of the product to obtain a quartz fiber reinforced carbon-based composite material crucible blank;
s2, dipping the silica sol into silica sol of a quartz fiber reinforced carbon-based composite material crucible blank by adopting a pressurized dipping process, and then drying, curing and sintering to ensure that the density reaches 1.5g/cm 3 And then carrying out secondary high-temperature treatment at 1300-1900 ℃, keeping the temperature for 2-10 hours, and grinding and polishing the surface of the crucible to obtain the quartz fiber reinforced carbon-silicon dioxide composite material crucible.
In the step S1, the resin is phenolic resin, furan resin or other resin with a high carbon residue rate.
In the step S2, the outer steel mould is divided into 3-6 petals.
Example 4
A preparation method of a quartz fiber reinforced carbon-silicon dioxide composite material crucible comprises the following steps:
s1, sleeving the quartz fiber crucible prefabricated part prepared in the embodiment 2 on a proper steel mould or graphite mould to ensure that the inner surface of the crucible prefabricated part is well attached to the outer surface of the mould, then spraying or impregnating resin or an organic binder, standing for 1-10 hours, sleeving an outer steel mould on the outer surface of the crucible, and sleeving the inner profile surface of the outer steel mould and the inner profile surface of the crucible prefabricated partThe outer surface is tightly attached, the outer diameter of the prefabricated part is 1-2 mm larger than that of the crucible product, and then the outer mold is fixed; then the sleeved prefabricated member (with a mold) is sent into an oven to be solidified and shaped, the temperature is controlled to be 150-300 ℃, when the oven does not smoke outwards, the temperature is kept for 1-10 hours, and the prefabricated member is cooled and demoulded to obtain a shaped quartz fiber prefabricated member; then adopting a chemical vapor deposition densification process or a resin or asphalt impregnation-carbonization densification process to densify the prefabricated member to 1.6g/cm 3 Then, carrying out first high-temperature treatment at 1300-1900 ℃, keeping the temperature for 2-20 hours, partially or completely converting the interface between the quartz fiber and the matrix carbon into silicon carbide, and mechanically adding the silicon carbide to the size of the product to obtain a quartz fiber reinforced carbon-based composite crucible blank;
s2, impregnating the silica sol into silica sol of a quartz fiber reinforced carbon-based composite material crucible blank by adopting a pressurized impregnation process, drying, curing and sintering, and repeating the pressurized impregnation, drying, curing and sintering to ensure that the density reaches 1.8g/cm 3 And then carrying out secondary high-temperature treatment at 1300-1900 ℃, keeping the temperature for 2-10 hours, and grinding and polishing the surface of the crucible to obtain the quartz fiber reinforced carbon-silicon dioxide composite material crucible.
In the step S1, the resin is phenolic resin, furan resin or other resin with a high carbon residue rate.
In the step S2, the outer steel mould is divided into 3-6 petals.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications derived therefrom are intended to be within the scope of the invention.

Claims (4)

1. A quartz fiber reinforced carbon-silicon dioxide composite material crucible is characterized in that a quartz fiber crucible prefabricated member is adopted to be solidified and shaped, impregnated by resin or asphalt and carbonized to increase the volumeThe density is 1.2 to 1.6g/cm 3 Then, carrying out first high-temperature treatment, and machining to a designed size, wherein the temperature of the first high-temperature treatment is 1300-1900 ℃, and the heat preservation time is 2-20 h; pressure dipping silica sol, drying, curing and sintering, wherein the density is 1.5 to 1.8g/cm 3 Carrying out high-temperature treatment for the second time, and polishing the surface to obtain the material, wherein the temperature of the high-temperature treatment for the second time is 1300 to 1900 ℃, and the heat preservation time is 2 to 10 hours;
the surface density of the quartz fiber crucible prefabricated part is 180 to 600g/m 2 The additive surface density of the quartz fiber laid fabric or plain cloth is 30 to 150g/m 2 The short quartz fiber net blank is formed by overlapping and needling, the weight ratio of cloth to net is 5: 5 to 9: 1, and the density of the quartz fiber crucible prefabricated member is 0.35 to 0.8g/cm 3 (ii) a The prefabricated member is sleeved on a steel die or a graphite inner die with the inner profile smaller than that of a crucible finished product by 1-2mm, the prefabricated member is tightly attached, an outer die with 3-6 petals is added outside the prefabricated member, the prefabricated member is fastened and then solidified, and the temperature for solidification and shaping is 150-300 ℃.
2. The quartz fiber reinforced carbon-silica composite crucible according to claim 1, wherein the silica sol accounts for 10 to 45 mass%.
3. The method for preparing a quartz fiber-reinforced carbon-silica composite crucible according to any one of claims 1 to 2, comprising the steps of:
s1, the surface density is 180 to 600g/m 2 The additive surface density of the quartz fiber laid fabric or plain cloth is 30 to 150g/m 2 The short quartz fiber net blank is formed by overlapping and needling, the weight ratio of cloth to net is 5: 5 to 9: 1, and the obtained density is 0.35 to 0.8g/cm 3 The quartz fiber crucible preform of (1);
s2, sleeving the prepared quartz fiber crucible prefabricated part on a proper steel mould or graphite mould to enable the inner surface of the crucible prefabricated part to be well fitted with the outer profile of the mould, then spraying or soaking an organic binder, standing for 1 to 10 hours, sleeving an outer steel mould on the outer surface of the crucible, enabling the inner profile of the outer steel mould to be tightly fitted with the outer profile of the crucible prefabricated part, and enabling the outer diameter of the prefabricated part to be 1 to 2mm larger than the outer diameter of a crucible product,then fixing the outer die; then, the sleeved prefabricated member is sent into an oven to be solidified and shaped, the temperature is controlled within 150 to 300 ℃, when the oven does not smoke outwards, the temperature is kept for 1 to 10 hours, the temperature is reduced, and demoulding is carried out to obtain a shaped quartz fiber prefabricated member; then, a resin or asphalt impregnation-carbonization densification process is adopted to densify the prefabricated member to 1.2 to 1.6g/cm 3 Then, carrying out first high-temperature treatment at 1300-1900 ℃, keeping the temperature for 2-20 hours, converting part or all of the quartz fiber and matrix carbon interface into silicon carbide, and then mechanically adding the silicon carbide to the size of a product to obtain a quartz fiber reinforced carbon-based composite crucible blank;
s3, dipping the silica sol into the quartz fiber reinforced carbon-based composite material crucible blank by adopting a pressurized dipping process, and then drying, curing and sintering to ensure that the density reaches 1.5 to 1.8g/cm 3 And then carrying out high-temperature treatment for the second time, wherein the treatment temperature is 1300-1900 ℃, the heat preservation time is 2-10 hours, and grinding and polishing the surface of the crucible to obtain the quartz fiber reinforced carbon-silicon dioxide composite material crucible.
4. The method for preparing a quartz fiber-reinforced carbon-silica composite crucible according to claim 3, wherein in the step S2, the resin is a phenol resin or a furan resin.
CN202210118066.5A 2022-02-08 2022-02-08 Quartz fiber reinforced carbon-silicon dioxide composite material crucible and preparation method thereof Active CN114368976B (en)

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