CN114232074A - 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

Info

Publication number
CN114232074A
CN114232074A CN202111563875.9A CN202111563875A CN114232074A CN 114232074 A CN114232074 A CN 114232074A CN 202111563875 A CN202111563875 A CN 202111563875A CN 114232074 A CN114232074 A CN 114232074A
Authority
CN
China
Prior art keywords
quartz fiber
carbon
cloth
fiber
quartz
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.)
Granted
Application number
CN202111563875.9A
Other languages
Chinese (zh)
Other versions
CN114232074B (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 CN202111563875.9A priority Critical patent/CN114232074B/en
Publication of CN114232074A publication Critical patent/CN114232074A/en
Application granted granted Critical
Publication of CN114232074B publication Critical patent/CN114232074B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Laminated Bodies (AREA)

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 (CN102731132A) on the surface of the carbon/carbon or graphite guide cylinder, and the silicon carbide coating is easy to layer 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; has an areal density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2The short quartz fiber net tires are alternately laminated and needled into the inner surface layer, and the apparent volume density of the short quartz fiber net tires is 0.3-0.6 g/cm3(ii) a The density of the alternate lamination surface on the outer surface of the inner surface layer is 280-600 g/m2The 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 is 80-120 g/m2The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.2-0.8 g/cm3The intermediate layer of (1); alternately laminating the layers on the surface of the intermediate layer at an areal density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2Short quartz fiber net tire is integrally needled to obtain an outer surface layer with apparent volume density of 0.3-0.6 g/cm3The preform of (4).
Preferably, the thickness of the inner surface layer is 3-10 mm; 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 middle layer 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.
Preferably, the thickness of the outer surface layer is 1-6 mm; 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 guide cylinder which is prepared by curing, shaping, densifying and graphitizing the prefabricated member of the quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder 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, preparation of a prefabricated member: the surface density is 180-300 g/m according to the weight ratio2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2The short quartz fiber net tires are alternately laminated and needled into the inner surface layer, and the apparent volume density of the short quartz fiber net tires is 0.3-0.6 g/cm3(ii) a The surface density of the alternating lamination on the outer surface of the inner surface layer is 280-600 g/m according to the weight ratio2The carbon fiber plain cloth or laid cloth or twill cloth and the surface density of the carbon fiber plain cloth or laid cloth are 80-120 g/m2The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.2-0.8 g/cm3The intermediate layer of (1); the surface of the intermediate layer is alternately laminated according to the weight ratio to have the surface density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2Short quartz fiber net tire is integrally needled to obtain an outer surface layer (3) with apparent volume density of 0.3-0.6 g/cm3The 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 process3And 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 10 mm; 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 6-15 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.
Preferably, in step S1, the thickness of the outer surface layer is 1-6 mm; 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 high carbon residue rate;
preferably, in the step S2, the setting temperature is controlled to be 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 22+2C ═ Si +2 CO; 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, 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 profile surfaces of the draft tube 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, and the service life of the draft tube can be prolonged by more than 50 percent (the service life of the common draft tube 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; has an areal density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2Short quartz fiber web batts are alternately laminated and needled into an inner surface layer 2, the surface of whichThe apparent volume density is 0.3-0.6 g/cm3(ii) a The surface density of the alternate lamination layer on the outer surface of the inner surface layer 2 is 280-600 g/m2The 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 is 80-120 g/m2The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.2-0.8 g/cm3The intermediate layer 1 of (a); the surface of the intermediate layer 1 is alternately laminated with an areal density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2Short quartz fiber net tire is integrally needled to obtain an outer surface layer 3 with an apparent volume density of 0.3-0.6 g/cm3The preform of (4).
Wherein the thickness of the inner surface layer 2 is 3 mm; 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 6 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.
Wherein the thickness of the outer surface layer 3 is 6 mm; 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 10 mm; 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 5 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 7: 3.
Wherein the thickness of the outer surface layer 3 is 6 mm; 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 3 mm; 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 1 mm; 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, preparation of a prefabricated member: the surface density is 180-300 g/m according to the weight ratio2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2The 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 0.3-0.6 g/cm3(ii) a The surface density of the alternate lamination on the outer surface of the inner surface layer 2 according to the weight ratio is 280-600 g/m2The carbon fiber plain cloth or laid cloth or twill cloth and the surface density of the carbon fiber plain cloth or laid cloth are 80-120 g/m2The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.2-0.8 g/cm3The intermediate layer 1 of (a); the surface of the intermediate layer 1 is alternately laminated according to the weight ratio to have the surface density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2Short quartz fiber net tire is integrally needled to obtain an outer surface layer 3 with an apparent volume density of 0.3-0.6 g/cm3The 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: adopting a chemical vapor deposition densification process or resin or asphalt impregnation-carbonization densification to the guide shell blank prepared in the step S2The densification process is to densify the guide shell blank to 1.2-1.5 g/cm3And 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.
In 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 non-woven cloth or the twill cloth to the short fiber net layer is 9: 1-7: 3.
In 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 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 step S2, the resin includes any one of phenolic resin and furan resin, and may be other resin with a high carbon residue rate;
in the step S2, the setting temperature is controlled to be 150-300 ℃, and when the oven does not smoke outwards, the temperature is kept for 1-10 hours.
In step S2, the inner mold 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 a guide cylinder prefabricated part, and the surface density of the carbon fiber plain cloth is 380-390 g/m2The surface density of the short carbon fiber net tire is 80-90 g/m2The 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/cm3Solidifying, shaping, and chemical vapor deposition to density of 1.45g/cm3Then graphitizing at high temperature, processing to size, coating pyrolytic carbon on the surface, and the density reaches 1.48g/cm3After 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/m2The surface density of the short carbon fiber net tire is 80-90 g/m2The 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/cm3Solidifying, shaping, and chemical vapor deposition to density of 1.45g/cm3Graphitizing at high temperature, processing to size, spraying or brushing silicon carbide coating on the surface to reach density of 1.48g/cm3After 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 on one hand, and the silicon carbide generated by reaction or the surface sprayed or painted silicon carbide coating is not matched with the thermal expansion coefficient of the carbon/carbon composite material substrate and is easy to fall off, so that the carbon/carbon composite material in the silicon vapor and the surface of the carbon/carbon guide cylinder cannot be protected from further reaction. 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 (10)

1. A kind ofQuartz fiber/carbon fiber reinforcing carbon base combined material draft tube prefab, its characterized in that includes: an intermediate layer (1), an inner surface layer (2) and an outer surface layer (3); has an areal density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2The short quartz fiber net tires are alternately laminated and needled to form an inner surface layer (2) with the apparent volume density of 0.3-0.6 g/cm3(ii) a The outer surface of the inner surface layer (2) is alternately laminated with the surface density of 280-600 g/m2The 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 is 80-120 g/m2The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.2-0.8 g/cm3The intermediate layer (1); the surface of the intermediate layer (1) is alternately laminated with an areal density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2Short quartz fiber net tire is integrally needled to obtain an outer surface layer (3) with apparent volume density of 0.3-0.6 g/cm3The preform of (4).
2. The quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder prefabricated member as claimed in claim 1, wherein the thickness of the inner surface layer (2) is 3-10 mm; 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: 4-9: 1.
3. The quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder prefabricated part as claimed in claim 1, wherein the thickness of the intermediate 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 padding layer is 9: 1-7: 3.
4. The quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder prefabricated member as claimed in claim 1, wherein the thickness of the outer surface layer (3) is 1-6 mm; 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.
5. A guide shell made of a quartz fiber/carbon fiber reinforced carbon-based composite material is characterized in that the guide shell is prepared by the prefabricated part of the guide shell made of the quartz fiber/carbon fiber reinforced carbon-based composite material, which is disclosed by any one of claims 1 to 4, through curing, sizing, densification and high-temperature graphitization.
6. The preparation method of the guide shell made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 5, which is characterized by comprising the following steps:
s1, preparation of a prefabricated member: the surface density is 180-300 g/m according to the weight ratio2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2The short quartz fiber net tires are alternately laminated and needled to form an inner surface layer (2) with the apparent volume density of 0.3-0.6 g/cm3(ii) a The outer surface of the inner surface layer (2) is alternately laminated with the surface density of 280-600 g/m according to the weight ratio2The carbon fiber plain cloth or laid cloth or twill cloth and the surface density of the carbon fiber plain cloth or laid cloth are 80-120 g/m2The short fiber net layer is integrally needled to obtain the product with the apparent volume density of 0.2-0.8 g/cm3The intermediate layer (1); the surface of the intermediate layer (1) is alternately laminated according to the weight ratio to have the surface density of 180 to 300g/m2The quartz fiber laid fabric and/or the surface density of the quartz fiber laid fabric is 30-120 g/m2Short quartz fiber net tire is integrally needled to obtain an outer surface layer (3) with apparent volume density of 0.3-0.6 g/cm3The 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 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 process3Then, high temperature treatment is carried out at the treatment temperature ofAnd (3) preserving the heat at 1300-1800 ℃ for 3-15 hours, completely or partially converting the interface layer between the quartz fiber and the matrix carbon into a silicon carbide layer, and machining to the designed size to obtain the quartz fiber/carbon fiber reinforced carbon-based composite draft tube.
7. The preparation method of the guide cylinder made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 6, 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.
8. The preparation method of the guide cylinder made of the quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 6, wherein 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.
9. The method for preparing the guide cylinder made of the quartz fiber/carbon fiber reinforced carbon-based composite material according to claim 6, 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 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.
10. The method for preparing a guide cylinder made of a quartz fiber/carbon fiber reinforced carbon-based composite material as claimed in claim 6, wherein in step S2, the resin comprises any one of phenolic resin or furan resin; the shaping temperature is controlled to be 150-300 ℃, and the heat is preserved for 1-10 hours when the oven does not smoke outwards.
CN202111563875.9A 2021-12-20 2021-12-20 Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof Active CN114232074B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111563875.9A CN114232074B (en) 2021-12-20 2021-12-20 Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111563875.9A CN114232074B (en) 2021-12-20 2021-12-20 Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof

Publications (2)

Publication Number Publication Date
CN114232074A true CN114232074A (en) 2022-03-25
CN114232074B CN114232074B (en) 2023-03-21

Family

ID=80759578

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111563875.9A Active CN114232074B (en) 2021-12-20 2021-12-20 Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114232074B (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102021648A (en) * 2011-01-10 2011-04-20 湖南金博复合材料科技有限公司 Guide cylinder antioxidation coating and preparation method thereof
CN102995297A (en) * 2012-08-17 2013-03-27 江苏天鸟高新技术股份有限公司 Manufacturing method of quartz fiber quasi-three dimensional profile modeling prefabricated piece
CN203007475U (en) * 2012-12-20 2013-06-19 湖南金博复合材料科技有限公司 Composite material guide cylinder
CN103232255A (en) * 2013-05-07 2013-08-07 湖南友缘新材料有限公司 Preparation method of carbon/carbon composite material flat plate with carbide coating on surface
CN111848201A (en) * 2020-07-24 2020-10-30 西安超码科技有限公司 Carbon/carbon crucible with silicon carbide/silicon coating and preparation method thereof
CN112694347A (en) * 2020-12-28 2021-04-23 湖南世鑫新材料有限公司 Carbon-carbon composite material crucible with silicon carbide coating and preparation method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102021648A (en) * 2011-01-10 2011-04-20 湖南金博复合材料科技有限公司 Guide cylinder antioxidation coating and preparation method thereof
CN102995297A (en) * 2012-08-17 2013-03-27 江苏天鸟高新技术股份有限公司 Manufacturing method of quartz fiber quasi-three dimensional profile modeling prefabricated piece
CN203007475U (en) * 2012-12-20 2013-06-19 湖南金博复合材料科技有限公司 Composite material guide cylinder
CN103232255A (en) * 2013-05-07 2013-08-07 湖南友缘新材料有限公司 Preparation method of carbon/carbon composite material flat plate with carbide coating on surface
CN111848201A (en) * 2020-07-24 2020-10-30 西安超码科技有限公司 Carbon/carbon crucible with silicon carbide/silicon coating and preparation method thereof
CN112694347A (en) * 2020-12-28 2021-04-23 湖南世鑫新材料有限公司 Carbon-carbon composite material crucible with silicon carbide coating and preparation method

Also Published As

Publication number Publication date
CN114232074B (en) 2023-03-21

Similar Documents

Publication Publication Date Title
CN108046819B (en) C/C-SiC friction material with integrated structure and function and preparation method thereof
CN106946582B (en) Large-size special-shaped carbon-based composite material component and preparation method thereof
CN107266075B (en) C/C-SiC composite material and preparation method and application thereof
CN110256082B (en) Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material by reaction sintering
JP2008531448A (en) Manufacturing method of ceramic matrix composite member and component obtained by the method
CN110483086B (en) Preparation method of carbon-ceramic brake disc
CN113072387A (en) Carbon fiber winding crucible and preparation method thereof
CN113024269A (en) Preparation method of high-performance super-large and super-thick carbon/carbon composite material
CN114014678B (en) Quartz fiber/carbon fiber reinforced carbon-based composite flat plate and preparation method thereof
CN114276157A (en) High-purity carbon-based composite material
CN114014676B (en) Quartz fiber/carbon fiber reinforced carbon-based composite material heat-insulating barrel and preparation method thereof
CN111170754A (en) Composite material with Si-Y-C ternary ceramic matrix and preparation method thereof
CN108129155B (en) Composite structure carbon-carbon heat-preservation cylinder and preparation method thereof
CN112266259B (en) Ceramic matrix composite material and preparation method and application thereof
CN114368976B (en) Quartz fiber reinforced carbon-silicon dioxide composite material crucible and preparation method thereof
CN114411242B (en) Quartz fiber reinforced carbon-silicon dioxide composite material guide cylinder and preparation method thereof
JP2005536420A (en) Carbon honeycomb body
CN114232074B (en) Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof
CN114368975B (en) Containing alpha-Al 2 O 3 Coated low density C/C-SiC composite crucible
CN114014677B (en) Quartz fiber/carbon fiber reinforced carbon-based composite material crucible and preparation method thereof
CN114455963B (en) A composition containing alpha-Al 2 O 3 Coated carbon/carbon-silicon carbide composite crucible
JP3116005B2 (en) Manufacturing method of C / C crucible for pulling semiconductor single crystal
CN114230347A (en) Preparation method and product of continuous fiber reinforced ZrC/SiC composite part
CN112919921A (en) Preparation method of low-cost super-large and super-thick carbon/carbon composite material
CN111112582A (en) Preparation method of high-density aluminum silicon carbide composite material

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