CN114232074B - Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof - Google Patents

Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof Download PDF

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CN114232074B
CN114232074B CN202111563875.9A CN202111563875A CN114232074B CN 114232074 B CN114232074 B CN 114232074B CN 202111563875 A CN202111563875 A CN 202111563875A CN 114232074 B CN114232074 B CN 114232074B
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quartz fiber
carbon
cloth
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layer
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CN114232074A (en
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陈腾飞
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Central South University
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Central South University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0036—Heat treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/08—Impregnating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/028—Net structure, e.g. spaced apart filaments bonded at the crossing points
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/06—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B2038/0052—Other operations not otherwise provided for
    • B32B2038/0076—Curing, vulcanising, cross-linking
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/20—All layers being fibrous or filamentary
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/106—Carbon fibres, e.g. graphite fibres

Abstract

The invention provides a quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and a preparation method thereof, belonging to the technical field of single crystal silicon furnaces and carbon-based composite material preparation. The guide shell is prepared from a guide shell prefabricated part through solidification and shaping, chemical densification and high-temperature graphitization. The middle layer of the prefabricated member of the guide cylinder is made of carbon fiber, the inner surface layer and the outer surface layer are made of quartz fiber, and the prefabricated member is respectively formed by alternately laminating and needling carbon fiber plain cloth, twill cloth, non-woven cloth and short carbon fiber net tire or alternately laminating and needling quartz fiber non-woven cloth and short quartz fiber net tire. The obtained quartz fiber/carbon fiber reinforced carbon-based composite draft tube has high strength, the inner surface and the outer surface of the draft tube 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 draft tube and silicon vapor can be effectively reduced or avoided, the service life of the draft tube can be prolonged by more than 50%, and the draft tube is suitable for batch production of high-efficiency single crystal furnace draft tubes.

Description

Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof
Technical Field
The invention relates to the technical field of monocrystalline silicon furnaces and preparation of carbon-based composite materials, in particular to a quartz fiber/carbon fiber reinforced carbon-based composite material guide cylinder 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 has very wide application in thermal field components of large-scale monocrystalline silicon furnaces in recent years, wherein the carbon/carbon composite guide cylinder 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 during the pulling of the single crystal, the single crystal silicon rod can pass through the guide cylinder, and the distance between the lower opening of the guide cylinder and the outer diameter of the silicon rod is very small, so that the silicon rod which passes through the guide cylinder generally has higher carbon and oxygen contents, thereby influencing the quality of the silicon wafer made of the silicon rod. Therefore, some manufacturers make a silicon carbide coating (CN 102731132A) on the surface of the carbon/carbon or graphite guide cylinder, and the silicon carbide coating is easy to delaminate or fall off after being used for a period of time due to the mismatch of the thermal expansion coefficients of the silicon carbide and the carbon/carbon or graphite, so that the continuous use is influenced; some manufacturers use quartz guide cylinders, but quartz is easy to soften at high temperature and is fragile, so that risks are brought to use.
Therefore, in order to fundamentally solve the problem of the draft tube, a new material structure is urgently needed to be designed so as to prolong the service life of the carbon/carbon composite material draft tube for the single crystal silicon furnace and improve the quality of the silicon rod.
Disclosure of Invention
Aiming at the defect that the carbon/carbon composite material or quartz guide cylinder 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 guide cylinder and the preparation method thereof.
The invention provides a quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder prefabricated part, which comprises the following components in part 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 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 alternate lamination on the outer surface of the inner surface layer is 280-600 g/m 2 The carbon fiber plain cloth, the non-woven cloth or the twill cloth and/or the surface density of the carbon fiber plain cloth, the non-woven cloth or the 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 0.2-0.8 g/cm 3 The intermediate layer of (1); the surface density of the intermediate layer 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 non-woven 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 guide cylinder which is prepared by curing, sizing, densifying and graphitizing the prefabricated member at high temperature.
The invention also provides a preparation method of the quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder, which 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 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 according to the weight ratio and the alternate lamination surface density 2 The surface density of the carbon fiber plain cloth or the non-woven cloth or the twill cloth is 80 to 120g/m 2 The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.2-0.8 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 is 30-120 g/m 2 Short quartz fibre net tyre and needleIntegrally needling to obtain the 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: 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 guide cylinder blank;
s3, densification and graphitization treatment: densifying the guide shell blank prepared in the step S2 to 1.2-1.5 g/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 guide cylinder.
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 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.
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 non-woven 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 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.
Preferably, in step S2, the resin includes any one of phenolic resin or furan resin, and may also 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 is formed by combining 3-6 pieces of die blocks with the same size, limiting grooves are formed in the surfaces of the die blocks, 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 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, the reaction speed and the reaction degree of silicon vapor and the surface of the guide cylinder are reduced, and the service life of the guide cylinder and the quality of the single crystal silicon rod are improved.
The technical scheme of the invention has the following advantages:
the invention relates to a quartz fiber/carbon fiber reinforced carbon-based composite material guide cylinder which is designed and prepared, the structure and the function of the guide cylinder are integrated, the middle layer of a prefabricated part is carbon fiber, the inner surface layer and the outer surface layer are composed of quartz fiber, and the quartz fiber/carbon fiber composite prefabricated part is formed by respectively adopting carbon fiber plain cloth or twill cloth and a section of carbon fiber net tire to be alternately laminated and needled or alternately laminating and needling quartz fiber weftless cloth and a short quartz fiber net tire to be alternately laminated and needled; then using chemical vapor deposition to densify or liquid phase dipping-carbonization to densify to required density, then using high temperature treatment to convert part or all of interface layer between quartz fiber and matrix carbon into silicon carbide. And because the inner and outer dies are adopted for solidification and shaping, the processing amount of the inner and outer surfaces of the guide cylinder is reduced, the fiber volume content of the crucible is increased, the obtained quartz fiber/carbon fiber reinforced carbon-based composite material 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, and the service life of the guide cylinder can be prolonged by over 50 percent (the service life of a common guide cylinder is 18 months).
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.
Reference numerals:
1. an intermediate layer; 2. an inner surface layer; 3. an outer surface layer.
Detailed Description
Example 1
A prefabricated component of a guide shell made of a quartz fiber/carbon fiber reinforced carbon-based composite material, 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 of the quartz fiber laid fabric 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, the non-woven cloth or the twill cloth and/or the surface density of the carbon fiber plain cloth, the non-woven cloth or the 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 0.2-0.8 g/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 the apparent volume density of 0.3-0.6 g/cm 3 The preform of (4).
Wherein the inner surface layer 2 has a thickness of 3mm; the inner surface layer 2 is formed by needling quartz fiber non-woven cloth or twill cloth and a short quartz fiber net tire, and the weight ratio of the quartz fiber non-woven cloth to the short quartz fiber net tire is 6: 4.
Wherein the thickness of the intermediate layer 1 is 6mm; wherein the weight ratio of the carbon fiber plain cloth or the non-woven cloth or the twill cloth to the short fiber net layer is 9: 1.
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.
Example 2
Wherein the thickness of the inner surface layer 2 is 10mm; the inner surface layer 2 is formed by needling quartz fiber non-woven cloth or twill cloth and a short quartz fiber net tire, and the weight ratio of the quartz fiber non-woven cloth to the short quartz fiber net tire is 9: 1.
Wherein the thickness of the intermediate layer 1 is 5mm; wherein the weight ratio of the carbon fiber plain cloth or the non-woven cloth or the 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 9: 1.
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 tire.
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.
The rest is the same as example 1.
Example 4
A quartz fiber/carbon fiber reinforced carbon-based composite draft tube is prepared by curing, sizing, densifying and graphitizing a quartz fiber/carbon fiber reinforced carbon-based composite draft tube prefabricated part prepared in the embodiment 1-3; 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 Alternating by weight on the outer surface of the inner surface layer 2The density of the laminated surface is 280-600 g/m 2 The surface density of the carbon fiber plain cloth or the non-woven cloth or the twill cloth is 80 to 120g/m 2 The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.2-0.8 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 an 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 guide cylinder blank;
s3, densification and graphitization treatment: densifying the guide shell blank prepared in the step S2 to 1.2-1.5 g/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 guide cylinder.
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 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 S1, the thickness of the middle layer 1 is 6-15 mm; wherein the weight ratio of the carbon fiber plain cloth or the non-woven 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, a limiting groove is formed in the surface of each die block, and the die blocks are fixedly sealed through hoops.
Comparative example 1
The carbon fiber plain cloth and the short carbon fiber net tire are alternately laminated and needled to form the guide cylinder prefabricated part, and 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 volume density of the prefabricated part of the guide shell is 0.45-0.46 g/cm 3 Solidifying, shaping, and chemical vapor deposition to density of 1.45g/cm 3 Then graphitizing at high temperature, processing to size, coating pyrolytic carbon on the surface, and the density reaches 1.48g/cm 3 After the guide cylinder is used for 15 months, the outer surface of the guide cylinder is obviously rough, and is locally pulverized, so that the guide cylinder cannot be used continuously; compared with the invention, the service life is reduced by more than 50%.
Comparative example 2
The carbon fiber plain cloth and the short carbon fiber net tire are alternately laminated and needled to form a guide cylinder prefabricated part, and 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 volume density of the prefabricated part of the guide shell is 0.45 to 0.46g/cm 3 Solidifying, shaping, and chemical vapor deposition to densify to 1.45g/cm 3 Graphitizing at high temperature, processing to size, spraying or brushing silicon carbide coating on the surface to reach density of 1.48g/cm 3 After the flow guide cylinder is used for 13 months, the outer surface of the flow guide cylinder is obviously rough, local bubbles are generated, and the flow guide cylinder cannot be used continuously; compared with the invention, the service life is reduced by more than 50%.
The silicon vapor and the surface of the carbon/carbon guide cylinder are easy to react to generate silicon carbide, so that the carbon/carbon composite material with a certain depth on the surface is damaged, and the silicon carbide generated by reaction or the silicon carbide coating sprayed or painted on the surface is not matched with the thermal expansion coefficient of the matrix of the carbon/carbon composite material, is easy to fall off and cannot protect the carbon/carbon composite material in the matrix from further reaction. The inner surface and the outer surface of the invention are the quartz fiber, the silicon carbide interface layer and the 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 derived therefrom are intended to be within the scope of the invention.

Claims (7)

1. A quartz fiber/carbon fiber reinforced carbon-based composite draft tube prefabricated part is characterized by comprising: 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 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), 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 (2) is 280 to 600g/m 2 The surface density of the carbon fiber plain cloth, the non-woven cloth or the twill cloth is 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 0.2 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 density of the surface 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); 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 short quartz fiber net tires, the quartz fiber laid cloth and the short quartz fiber net tiresThe weight ratio of the short quartz fiber net tire is 6: 4~9: 1; the thickness of the intermediate layer (1) is 6-15mm; wherein the weight ratio of the carbon fiber plain cloth or the non-woven cloth or the twill cloth to the short fiber net layer is 9: 1~7: 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: 4~9: 1.
2. A guide shell made of a quartz fiber/carbon fiber reinforced carbon-based composite material is characterized in that the guide shell is prepared from the prefabricated member of the guide shell made of the quartz fiber/carbon fiber reinforced carbon-based composite material of claim 1 through curing, sizing, densification and high-temperature graphitization.
3. The preparation method of the guide shell made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 2, which is characterized by comprising the following steps:
s1, preparing a prefabricated member: the areal density is 180 to 300g/m according to the weight ratio 2 The density of the surface 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), and the apparent volume density of the inner surface layer is 0.3 to 0.6g/cm 3 (ii) a The external surface of the internal surface layer (2) is alternately laminated with the surface density of 280 to 600g/m according to the weight ratio 2 The surface density of the carbon fiber plain cloth, the non-woven cloth or the twill cloth is 80 to 120g/m 2 The short fiber net layer is integrally needled to obtain the short fiber net layer with the apparent volume density of 0.2 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 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: placing 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 guide cylinder blank;
s3, densification and graphitization treatment: densifying the guide cylinder blank prepared in the step S2 to 1.2 to 1.5g/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, converting all or part of an interface layer between the quartz fiber and the matrix carbon into a silicon carbide layer, and machining to a designed size to obtain the quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder.
4. The preparation method of the guide cylinder made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 3, 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 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.
5. The preparation method of the guide cylinder made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 3, 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 non-woven cloth or the twill cloth to the short fiber net layer is 9: 1~7: 3.
6. The preparation method of the guide cylinder made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 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 non-woven cloth and a short quartz fiber net tire, the weight ratio of the quartz fiber non-woven cloth to the short quartz fiber net tire is 6: 4~9: 1.
7. The method for preparing the guide cylinder made of the quartz fiber/carbon fiber reinforced carbon-based composite material according to claim 3, wherein in the 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.
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CN101445377A (en) * 2008-12-31 2009-06-03 西安超码科技有限公司 Method for preparing high temperature furnace used carbon/carbon insulating cylinders
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