CN114014677B - Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof - Google Patents

Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof Download PDF

Info

Publication number
CN114014677B
CN114014677B CN202111562959.0A CN202111562959A CN114014677B CN 114014677 B CN114014677 B CN 114014677B CN 202111562959 A CN202111562959 A CN 202111562959A CN 114014677 B CN114014677 B CN 114014677B
Authority
CN
China
Prior art keywords
quartz fiber
carbon
crucible
fiber
cloth
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111562959.0A
Other languages
Chinese (zh)
Other versions
CN114014677A (en
Inventor
陈腾飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Central South University
Original Assignee
Central South University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Central South University filed Critical Central South University
Priority to CN202111562959.0A priority Critical patent/CN114014677B/en
Publication of CN114014677A publication Critical patent/CN114014677A/en
Application granted granted Critical
Publication of CN114014677B publication Critical patent/CN114014677B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/82—Asbestos; Glass; Fused silica
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/608—Green bodies or pre-forms with well-defined density

Abstract

The invention provides a quartz fiber/carbon fiber reinforced carbon-based composite crucible and a preparation method thereof, belonging to the technical field of single crystal silicon furnaces and carbon-based composite preparation. The crucible is prepared by a crucible prefabricated part through solidification and shaping, chemical densification and high-temperature graphitization. The crucible prefabricated member has a middle layer of carbon fiber and inner and outer surface layers of quartz fiber, and is formed by alternately laminating and needling carbon fiber plain cloth or twill cloth and short carbon fiber net blank or alternately laminating and needling quartz fiber non-woven cloth and short quartz fiber net blank. The obtained quartz fiber/carbon fiber reinforced carbon-based composite material crucible is high in strength, the inner surface and the outer surface of the crucible consist of quartz fiber, a silicon carbide interface layer and matrix carbon, the reaction between the inner surface layer and the outer surface layer of the crucible and silicon vapor can be effectively reduced or avoided, the service life of the crucible can be prolonged by more than 50%, and the crucible is suitable for batch production of crucibles and crucible sides of efficient single crystal furnaces.

Description

Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof
Technical Field
The invention relates to the technical field of single crystal silicon furnaces and preparation of carbon-based composite materials, in particular to a quartz fiber/carbon fiber reinforced carbon-based 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 substrate and the composite ceramic coating attached to the inner surface of the crucible, and the components are (by mass ratio): 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 crucible by using a plasma spraying process, so as to improve the anti-silicification corrosion capability of the 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 high, and the obtained coating is thin and has mismatched thermal expansion coefficient, and the capability of inhibiting silicon vapor corrosion is very limited.
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 silicification of silicon vapor, the invention provides the quartz fiber/carbon fiber reinforced carbon-based composite material crucible and the preparation method thereof.
The invention provides a quartz fiber/carbon fiber reinforced carbon-based composite crucible prefabricated part, which comprises the following components in percentage by weight: an intermediate layer, an inner surface layer and an outer surface layer; the surface density is 180-300 g/m 2 The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m 2 The short quartz fiber net tire is alternately laminated and needled into the inner surface layer, and the apparent volume density of the inner surface layer is 0.3 to 0.6g/cm 3 (ii) a The surface density of the alternate lamination on the outer surface of the inner surface layer is 280-600 g/m 2 The carbon fiber plain cloth or twill cloth and the surface density of the carbon fiber plain cloth or twill cloth are 80 to 120g/m 2 The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.5-0.8 g/cm 3 The intermediate layer of (a); the surface density of the intermediate layer is alternately laminated on the surface of the intermediate layer, and the lamination surface density is 180 to 300g/m 2 The quartz fiber laid fabric and/or the surface density is 30-120 g/m 2 Short quartz fiber net tire is needled into a whole to obtain the outer surface layer with the apparent volume density of 0.3 to 0.6g/cm 3 The preform of (4).
Preferably, the thickness of the inner surface layer is 3 to 10mm; when the inner surface layer is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4-9: 1.
Preferably, the thickness of the intermediate layer is 6 to 15mm; wherein the weight ratio of the carbon fiber plain cloth or the twill cloth to the short fiber net layer is 9: 1-7: 3.
Preferably, the thickness of the outer surface layer is 1 to 6mm; when the outer surface layer is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4-9: 1.
The invention also provides a quartz fiber/carbon fiber reinforced carbon-based composite material crucible, which is prepared by curing, shaping, chemical densification and high-temperature graphitization of the quartz fiber/carbon fiber reinforced carbon-based composite material crucible prefabricated part.
The invention also provides a preparation method of the quartz fiber/carbon fiber reinforced carbon-based composite material crucible, which comprises the following steps:
s1, preparing a prefabricated member: push buttonThe weight ratio of the surface density to the surface density is 180 to 300g/m 2 The quartz fiber laid fabric and/or the surface density is 30-120 g/m 2 Short quartz fiber net tires are alternately laminated and needled to form an inner surface layer, and the apparent volume density of the inner surface layer is 0.3-0.6 g/cm 3 (ii) a The surface density of the inner surface layer is 280-600 g/m 2 The carbon fiber plain cloth or the twill cloth has the surface density of 80 to 120g/m 2 The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.5-0.8 g/cm 3 The intermediate layer of (a); the surface of the intermediate layer is alternately laminated according to the weight ratio to have the surface density of 180-300 g/m 2 The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m 2 Short quartz fiber net tire is integrally needled to obtain an outer surface layer (3) with apparent volume density of 0.3-0.6 g/cm 3 The preform of (4);
s2, curing the prefabricated part: placing the inner part of the prefabricated part prepared in the step S1 into an inner mold matched with the inner surface, spraying resin or organic adhesive (starch glue and the like), drying in the shade, additionally arranging an outer mold on the outer surface, sending the outer mold into an oven for curing and shaping, cooling after shaping is finished, and demolding to obtain a crucible blank;
s3, densification and graphitization treatment: the crucible blank prepared in the step S2 is densified to 1.4 to 1.6g/cm by adopting a chemical vapor deposition densification process or a resin or asphalt impregnation-carbonization densification process 3 And then, carrying out high-temperature treatment at 1300-1800 ℃ for 3-15 hours, and processing to a designed size to obtain the quartz fiber/carbon fiber reinforced carbon-based composite material crucible.
Preferably, in step S1, the thickness of the inner surface layer is 3 to 10mm; if the inner surface layer is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4-9: 1.
Preferably, in step S1, the thickness of the intermediate layer is 6 to 15mm; wherein the weight ratio of the carbon fiber plain cloth or the twill cloth to the short fiber net layer is 9: 1-7: 3.
Preferably, in step S1, the thickness of the outer surface layer is 1 to 6mm; if the outer surface layer is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4-9: 1.
Preferably, in step S2, the resin includes any one of phenolic resin or furan resin, and may be other resin with a high carbon residue rate;
preferably, in the step S2, the setting temperature is controlled at 150-300 ℃, and the temperature is kept for 1-10 hours when the oven does not smoke outwards.
Preferably, in step S2, the material of the inner mold is graphite or stainless steel; the outer die is a stainless steel die, and particularly is formed by combining 3-6 petals and other large die blocks, a limiting groove is formed in the surface of each die block, and the die blocks are fixedly sealed through hoops.
In the invention, the interface between the quartz fiber and the matrix carbon reacts at high temperature, and the reaction equation is as follows: siO 2 2 +2C = Si+2CO; si + C = SiC; after the reaction generates a silicon carbide interface layer, the further reaction is difficult, so that only the surface part of the quartz fiber is converted into silicon carbide; because the upper surface layer and the lower surface layer are composed of quartz fiber, silicon carbide and matrix carbon, the carbon content is reduced, and the reaction speed and the reaction degree of silicon vapor and the surface of the crucible are reduced, thereby being beneficial to prolonging the service life of the crucible. And due to the design of the prefabricated member, the utilization rate of the carbon source gas reaches more than 85 percent in the vapor deposition densification process.
The technical scheme of the invention has the following advantages:
the invention relates to a quartz fiber/carbon fiber reinforced carbon-based composite material flat crucible, which is designed and prepared, wherein the middle layer of a prefabricated part is made of carbon fibers, the inner surface layer and the outer surface layer of the prefabricated part are made of quartz fibers, and the quartz fiber/carbon fiber composite prefabricated part is respectively formed by alternately laminating and needling carbon fiber plain cloth or twill cloth and short carbon fiber net blank or alternately laminating and needling quartz fiber laid cloth and short quartz fiber net blank; then, chemical vapor deposition densification or liquid phase impregnation-carbonization densification is carried out to obtain the required density, and then high temperature treatment is carried out to partially or completely convert the interface layer between the quartz fiber and the matrix carbon into silicon carbide; the utilization rate of the carbon source gas is more than 85 percent. 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, the obtained quartz fiber/carbon fiber reinforced carbon-based composite crucible has high strength, the inner and outer surfaces consist of quartz fiber, a silicon carbide interface layer and matrix carbon, the reaction between the inner and outer surface layers of the crucible and silicon vapor can be effectively reduced or avoided, compared with the carbon/carbon composite crucible which is commonly used at present, the service life of the crucible can be prolonged by more than 50%, single crystals can be normally drawn in a single crystal furnace, and the crucible can be continuously used after being used for 12 months, so that the crucible is suitable for batch production of the crucible and the crucible side of a high-efficiency single crystal furnace.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a cross-sectional view of a preform in example 1 of the present invention;
fig. 2 is a top view of the outer mold of the present invention.
Reference numerals:
1. an intermediate layer; 2. an inner surface layer; 3. an outer surface layer.
Detailed Description
Example 1
A silica fiber/carbon fiber reinforced carbon-based composite crucible preform, as shown in fig. 1, comprising: an intermediate layer 1, an inner surface layer 2 and an outer surface layer 3; the surface density is 180-300 g/m 2 The quartz fiber laid fabric and/or the surface density is 30-120 g/m 2 The short quartz fiber net tires are alternately laminated and needled into the inner surface layer 2, and the apparent volume density of the inner surface layer is 0.3 to 0.6g/cm 3 (ii) a The surface density of the alternate lamination layer on the outer surface of the inner surface layer 2 is 280-600 g/m 2 The carbon fiber plain cloth or the twill cloth has the surface density of 80 to 120g/m 2 The short fiber net layer of (2) is integrally needled to obtain an apparent volume density of 0.5 to up0.8g/cm 3 The intermediate layer 1 of (a); the surface density of the intermediate layer 1 is 180 to 300g/m 2 The quartz fiber laid fabric and/or the surface density is 30-120 g/m 2 Short quartz fiber net tire is needled into a whole to obtain an outer surface layer 3 with an apparent volume density of 0.3-0.6 g/cm 3 The preform of (4).
Wherein the thickness of the inner surface layer 2 is 5mm; the inner surface layer 2 is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, and the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4.
Wherein the thickness of the intermediate layer 1 is 15mm; wherein the weight ratio of the carbon fiber plain cloth or twill cloth to the short fiber net layer is 9: 1.
Wherein the thickness of the outer surface layer 3 is 4mm; the outer surface layer 3 is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, and the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4.
Example 2
Wherein the thickness of the inner surface layer 2 is 10mm; the inner surface layer 2 is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, and the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 9: 1.
Wherein the thickness of the intermediate layer 1 is 6mm; wherein the weight ratio of the carbon fiber plain cloth or twill cloth to the short fiber net layer is 7: 3.
Wherein the thickness of the outer surface layer 3 is 6mm; the outer surface layer 3 is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, and the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4.
The rest is the same as example 1.
Example 3
Wherein the thickness of the inner surface layer 2 is 3mm; the inner surface layer 2 is formed by needling a short quartz fiber mesh blank.
Wherein the thickness of the intermediate layer 1 is 15mm; wherein the weight ratio of the carbon fiber plain cloth or the twill cloth to the short fiber net layer is 9: 1.
Wherein the thickness of the outer surface layer 3 is 1mm; the outer surface layer 3 is formed by needling a short quartz fiber mesh tire.
Example 4
A quartz fiber/carbon fiber reinforced carbon-based composite material crucible is prepared by curing, sizing, chemical densification and high-temperature graphitization of a quartz fiber/carbon fiber reinforced carbon-based composite material crucible prefabricated member in embodiment 1 or embodiment 2 or embodiment 3, and the preparation method comprises the following steps:
s1, preparing a prefabricated member: the surface density is 180 to 300g/m according to the weight ratio 2 The quartz fiber laid fabric and/or the surface density is 30-120 g/m 2 The short quartz fiber net tires are alternately laminated and needled into the inner surface layer 2, and the apparent volume density of the inner surface layer is 0.3 to 0.6g/cm 3 (ii) a The surface density of the inner surface layer 2 is 280-600 g/m 2 The carbon fiber plain cloth or twill cloth and the surface density of the carbon fiber plain cloth or twill cloth are 80 to 120g/m 2 The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.5-0.8 g/cm 3 The intermediate layer 1 of (a); the surface of the intermediate layer 1 is alternately laminated according to the weight ratio, and the surface density is 180 to 300g/m 2 The quartz fiber laid fabric and/or the surface density is 30-120 g/m 2 Short quartz fiber net tire is needled into a whole to obtain an outer surface layer 3 with the apparent volume density of 0.3-0.6 g/cm 3 The preform of (4);
s2, curing the prefabricated part: putting the inner part of the prefabricated part prepared in the step S1 into an inner mold matched with the inner surface, spraying resin or organic adhesive (starch glue and the like), drying in the shade, additionally arranging an outer mold on the outer surface, sending the outer mold into an oven for curing and shaping, cooling after shaping is finished, and demolding to obtain a crucible blank;
s3, densification and graphitization treatment: the crucible blank prepared in the step S2 is densified to 1.4 to 1.6g/cm by adopting a chemical vapor deposition densification process or a resin or asphalt impregnation-carbonization densification process 3 And then, carrying out high-temperature treatment at 1300-1800 ℃ for 3-15 hours, and processing to a designed size to obtain the quartz fiber/carbon fiber reinforced carbon-based composite material crucible.
Wherein, in the step S1, the thickness of the inner surface layer 2 is 3-10 mm; if the inner surface layer 2 is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4-9: 1.
In the step S1, the thickness of the middle layer 1 is 6-15 mm; wherein the weight ratio of the carbon fiber plain cloth or the twill cloth to the short fiber net layer is 9: 1-7: 3.
Wherein, in the step S1, the thickness of the outer surface layer 3 is 1-6 mm; if the outer surface layer 3 is formed by needling quartz fiber laid cloth and short quartz fiber net tires, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tires is 6: 4-9: 1.
In the step S2, the resin includes any one of phenolic resin or furan resin, and may be other resin with a high carbon residue rate;
in the step S2, the temperature of the shaping is controlled to be 150-300 ℃, and the temperature is kept for 1-10 hours when the oven does not smoke outwards.
In the step S2, the inner die is made of graphite or stainless steel; the outer die is a stainless steel die and is formed by combining 3-6 petals and other large die blocks as shown in figure 2, and the surfaces of the die blocks are provided with limiting grooves which are fixedly sealed through hoops.
Comparative example 1
Alternately laminating and needling carbon fiber plain cloth and short carbon fiber net blank to form a crucible prefabricated part, wherein the surface density of the carbon fiber plain cloth is 380-390 g/m 2 The surface density of the short carbon fiber net tire is 80 to 90g/m 2 The weight ratio of the carbon fiber plain cloth to the short carbon fiber net tire is 7:3, the apparent bulk density of the crucible prefabricated member is 0.45-0.46 g/cm 3 Curing, shaping, and chemically densifying to obtain a density of 1.45g/cm 3 Graphitizing at high temperature, processing to size, coating pyrolytic carbon on the surface, and making the density reach 1.48g/cm 3 And the service life is 7 months, and compared with the invention, the service life is reduced by more than 70%.
The main reason is that silicon vapor and the surface of the carbon/carbon crucible are easy to react to generate silicon carbide, on one hand, the carbon/carbon composite material with a certain depth on the surface is damaged, especially the R angular contact part, on the other hand, the thermal expansion coefficient of the generated silicon carbide and the matrix of the carbon/carbon composite material is not matched, the silicon carbide is easy to fall off, and the further reaction of the carbon/carbon composite material in the silicon carbide and the matrix of the carbon/carbon composite material cannot be protected. The inner surface and the outer surface of the invention are quartz fiber, a silicon carbide interface layer and a pyrolytic carbon layer, which can effectively reduce or avoid the reaction with silicon vapor.
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. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (6)

1. A quartz fiber/carbon fiber reinforced carbon-based composite crucible is characterized in that the crucible is prepared by solidifying and shaping a quartz fiber/carbon fiber reinforced carbon-based composite crucible prefabricated part, chemically densifying and graphitizing at high temperature; the chemical densification is a chemical vapor deposition densification process or a resin or asphalt impregnation-carbonization densification process, and the high-temperature graphitization treatment temperature is 1300-1800 ℃; the preform comprises: an intermediate layer (1), an inner surface layer (2) and an outer surface layer (3); the surface density is from 180 to 300g/m 2 The quartz fiber laid fabric and/or the areal density of the quartz fiber laid fabric are/is 30 to 120g/m 2 Short quartz fiber net tires are alternately laminated and needled to form an inner surface layer (2) with apparent volume density of 0.3 to 0.6g/cm 3 (ii) a The surface density of the alternate lamination on the outer surface of the inner surface layer (2) is 280 to 600g/m 2 The carbon fiber plain cloth or the carbon fiber twill cloth and the surface density of the carbon fiber twill cloth or the twill cloth are 80 to 120g/m 2 The short fiber net layer is needled into a whole to obtain the material with the apparent volume density of 0.5 to 0.8g/cm 3 The intermediate layer (1); the surface of the intermediate layer (1) is alternately laminated with the surface density of 180 to 300g/m 2 The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30 to 120g/m 2 The short quartz fiber net is needled into a whole to obtain the apparent volume density of the outer surface layer (3)The degree of the reaction is 0.3 to 0.6g/cm 3 The preform of (4);
the thickness of the inner surface layer (2) is 3-10mm; when the inner surface layer (2) is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4 to 9: 1;
the thickness of the intermediate layer (1) is 6-15mm; wherein the weight ratio of the carbon fiber plain cloth or the twill cloth to the short fiber net tire layer is 9: 1 to 7: 3;
the thickness of the outer surface layer (3) is 1 to 6mm; when the outer surface layer (3) is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4 to 9: 1.
2. The method for preparing the crucible made of the quartz fiber/carbon fiber reinforced carbon-based composite material of claim 1, which is characterized by comprising the following steps:
s1, preparing a prefabricated part: the areal density is 180 to 300g/m according to the weight ratio 2 The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30 to 120g/m 2 Short quartz fiber net tires are alternately laminated and needled to form an inner surface layer (2) with apparent volume density of 0.3 to 0.6g/cm 3 (ii) a The external surface of the inner surface layer (2) is alternately laminated with the external surface of the inner surface layer according to the weight ratio, and the density of the laminated surface is 280 to 600g/m 2 The carbon fiber plain cloth or the carbon fiber twill cloth and the surface density of the carbon fiber twill cloth or the twill cloth are 80 to 120g/m 2 The short fiber net layer is integrally needled to obtain the material with the apparent volume density of 0.5 to 0.8g/cm 3 The intermediate layer (1); the surface of the intermediate layer (1) is alternately laminated according to the weight ratio, and the surface density is 180 to 300g/m 2 The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30 to 120g/m 2 Short quartz fiber net tire is needled into a whole to obtain the outer surface layer (3) with the apparent volume density of 0.3 to 0.6g/cm 3 The preform of (4);
s2, curing the prefabricated part: putting the inner part of the prefabricated part prepared in the step S1 into an inner mold adaptive to the inner surface, spraying resin or organic adhesive, drying in the shade, additionally arranging an outer mold adaptive to the outer surface of the prefabricated part on the outer surface, sending the prefabricated part into an oven for curing and shaping, cooling after shaping is finished, and demolding to obtain a crucible blank;
s3, densification and graphitization treatment: densifying the crucible blank prepared in the step S2 to 1.4 to 1.6g/cm by adopting a chemical vapor deposition densification process or a resin or asphalt impregnation-carbonization densification process 3 And then, performing high-temperature treatment at 1300-1800 ℃ for 3-15 hours, and processing to a designed size to obtain the quartz fiber/carbon fiber reinforced carbon-based composite material crucible.
3. The method for preparing the crucible made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 2, wherein in the step S1, the thickness of the inner surface layer (2) is 3-10 mm; if the inner surface layer (2) is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4 to 9: 1.
4. The method for preparing the crucible made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 2, wherein in the step S1, the thickness of the intermediate layer (1) is 6-15mm; wherein the weight ratio of the carbon fiber plain cloth or the twill cloth to the short fiber net padding layer is 9: 1 to 7: 3.
5. The method for preparing the crucible made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 2, wherein in the step S1, the thickness of the outer surface layer (3) is 1 to 6mm; if the outer surface layer (3) is formed by needling quartz fiber laid cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber laid cloth to the short quartz fiber net tire is 6: 4 to 9: 1.
6. The method for preparing a crucible of quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 2, wherein in step S2, the resin comprises any one of phenolic resin or furan resin; the temperature of the shaping is controlled to be 150 to 300 ℃, and the heat is preserved for 1 to 10 hours when the oven does not smoke outwards.
CN202111562959.0A 2021-12-20 2021-12-20 Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof Active CN114014677B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111562959.0A CN114014677B (en) 2021-12-20 2021-12-20 Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111562959.0A CN114014677B (en) 2021-12-20 2021-12-20 Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof

Publications (2)

Publication Number Publication Date
CN114014677A CN114014677A (en) 2022-02-08
CN114014677B true CN114014677B (en) 2022-11-29

Family

ID=80069381

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111562959.0A Active CN114014677B (en) 2021-12-20 2021-12-20 Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114014677B (en)

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0933450B1 (en) * 1998-01-19 2002-04-17 Sumitomo Electric Industries, Ltd. Method of making SiC single crystal and apparatus for making SiC single crystal
CN101319353B (en) * 2008-05-20 2010-06-16 湖南金博复合材料科技有限公司 Carbon/carbon composite material crucible pot and preparing technique thereof
CN103724030B (en) * 2013-05-28 2016-08-10 苏州宏久航空防热材料科技有限公司 A kind of carbon fiber enhanced porous composite and preparation method thereof
CN111848201B (en) * 2020-07-24 2022-09-02 西安超码科技有限公司 Carbon/carbon crucible with silicon carbide/silicon coating and preparation method thereof

Also Published As

Publication number Publication date
CN114014677A (en) 2022-02-08

Similar Documents

Publication Publication Date Title
RU2176628C2 (en) Composite material (variants) and method or preparing thereof, method of treating fibrous semi-finished product (variants)
CN107266075B (en) C/C-SiC composite material and preparation method and application thereof
WO1991002705A1 (en) Fiber reinforced composite having an aluminum phosphate bonded matrix
US7179532B2 (en) Composite ceramic body and method for producing the same
CN105541364B (en) A kind of method of step densification production carbon pottery automobile brake disc
CN111038022B (en) Anti-corrosion composite heat-preservation cover felt for industrial vacuum furnace and preparation method thereof
CN114014678B (en) Quartz fiber/carbon fiber reinforced carbon-based composite flat plate and preparation method thereof
CN113045325B (en) Preparation method of high-strength carbon/carbon-silicon carbide composite material
EP0417493A2 (en) Fiber reinforced composite having an aluminum phosphate bonded matrix
CN110483086A (en) A kind of preparation method of carbon pottery brake disc
CN112552063A (en) Preparation method of carbon fiber reinforced silicon carbide composite material
CN114014676B (en) Quartz fiber/carbon fiber reinforced carbon-based composite material heat-insulating barrel and preparation method thereof
CN108754357B (en) SiC nanowire reinforced aluminum silicon carbide composite material and preparation method thereof
US11332411B2 (en) Method for producing a consolidated fiber preform
CN114368976B (en) Quartz fiber reinforced carbon-silicon dioxide composite material crucible and preparation method thereof
CN114014677B (en) Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof
JPH0244271B2 (en)
CN104844246A (en) Cf/SiC composite material for use in automobile brake disc and manufacturing method therefor
CN114411242B (en) Quartz fiber reinforced carbon-silicon dioxide composite material guide cylinder and preparation method thereof
CN114232074B (en) Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof
JP3116005B2 (en) Manufacturing method of C / C crucible for pulling semiconductor single crystal
KR100419778B1 (en) Manufacturing method of silicon cabide-boron carbide composites by liquid phase reaction sintering
CN115286393B (en) Low-cost long-life carbon Tao Re field product and preparation method thereof
CN114455981B (en) A composition containing alpha-Al 2 O 3 Medium-density C/C-SiC composite material crucible of coating
JPH1160357A (en) Oxidation resistant c/c composite material and its production

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant